#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/00/00/1000006.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1000006
loop_
_publ_author_name
'Armel Le Bail'
_publ_contact_author_address
;
Laboratoire des Fluorures - UPRES-A 6010
Facult\'e des Sciences, Universit\'e du Maine, Avenue Olivier-Messiaen,
 72085 LE MANS Cedex 9, FRANCE
;
_publ_contact_author_name        'Le Bail, Armel'
_journal_name_full               'Personal Communication to COD'
_chemical_formula_sum            'C22 H25 Cl N2 O8'
_chemical_formula_weight         480.89
_chemical_name_common            'tetracycline hydrochloride'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9300(9)
_cell_length_b                   12.7162(11)
_cell_length_c                   15.7085(13)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      2.51
_cell_volume                     2183.3(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6883
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8955
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(8)
_refine_ls_extinction_coef       0.0038(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                3937
_reflns_number_total             4915
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               1000006
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.92963(7) 0.41939(6) -0.00197(4) 0.01949(17) Uani 1 1 d . . .
O1 O 0.0086(3) 0.3656(3) 0.43967(14) 0.0392(7) Uani 1 1 d . . .
H1 H 0.039(4) 0.433(4) 0.435(2) 0.047(13) Uiso 1 1 d . . .
O6 O 0.1453(2) 0.46012(16) 0.12979(12) 0.0194(5) Uani 1 1 d . . .
H6 H 0.086(4) 0.449(3) 0.088(2) 0.045(12) Uiso 1 1 d . . .
O11 O 0.7514(2) 0.64335(19) 0.07408(14) 0.0268(5) Uani 1 1 d . . .
O13 O 0.3634(2) 0.71743(18) 0.18883(13) 0.0250(5) Uani 1 1 d . . .
O14 O 0.5800(2) 0.60174(18) 0.29547(12) 0.0212(5) Uani 1 1 d . . .
H14 H 0.565(4) 0.614(3) 0.338(2) 0.033(11) Uiso 1 1 d . . .
O15 O 0.3506(2) 0.60822(17) 0.35612(12) 0.0198(5) Uani 1 1 d . . .
H15 H 0.283(4) 0.580(4) 0.385(2) 0.045(12) Uiso 1 1 d . . .
O17 O 0.1647(2) 0.50211(18) 0.38835(12) 0.0234(5) Uani 1 1 d . . .
O19 O 0.6623(3) 0.81863(18) 0.04211(13) 0.0269(6) Uani 1 1 d . . .
H19 H 0.734(5) 0.757(4) 0.055(3) 0.061(14) Uiso 1 1 d . . .
N10 N 0.7465(3) 0.4488(2) 0.14281(16) 0.0193(6) Uani 1 1 d . . .
H10 H 0.793(4) 0.464(3) 0.100(2) 0.035(11) Uiso 1 1 d . . .
N19 N 0.4694(3) 0.8551(2) 0.08138(17) 0.0288(7) Uani 1 1 d . . .
H19A H 0.475(4) 0.921(3) 0.058(2) 0.034(10) Uiso 1 1 d . . .
H19B H 0.408(4) 0.833(4) 0.112(2) 0.049(14) Uiso 1 1 d . . .
C1 C 0.0207(3) 0.3204(3) 0.36224(18) 0.0272(8) Uani 1 1 d . . .
C2 C -0.0525(4) 0.2345(3) 0.3435(2) 0.0314(9) Uani 1 1 d . . .
H2 H -0.111(3) 0.211(3) 0.388(2) 0.026(9) Uiso 1 1 d . . .
C3 C -0.0436(4) 0.1888(3) 0.2657(2) 0.0302(8) Uani 1 1 d . . .
H3 H -0.084(4) 0.134(3) 0.253(2) 0.040(12) Uiso 1 1 d . . .
C4 C 0.0378(3) 0.2253(3) 0.2036(2) 0.0240(7) Uani 1 1 d . . .
H4 H 0.038(3) 0.189(3) 0.148(2) 0.028(9) Uiso 1 1 d . . .
C5 C 0.1113(3) 0.3105(2) 0.22057(18) 0.0183(7) Uani 1 1 d . . .
C6 C 0.1962(3) 0.3609(2) 0.15436(17) 0.0178(7) Uani 1 1 d . . .
C7 C 0.3178(3) 0.3872(2) 0.19906(16) 0.0145(6) Uani 1 1 d . . .
H7 H 0.337(4) 0.318(3) 0.222(2) 0.028(9) Uiso 1 1 d . . .
C8 C 0.4148(3) 0.4314(2) 0.13903(16) 0.0170(6) Uani 1 1 d . . .
H8A H 0.378(4) 0.486(3) 0.107(2) 0.035(10) Uiso 1 1 d . . .
H8B H 0.444(3) 0.378(3) 0.1001(19) 0.025(9) Uiso 1 1 d . . .
C9 C 0.5241(3) 0.4766(2) 0.18811(16) 0.0141(6) Uani 1 1 d . . .
H9 H 0.554(3) 0.423(3) 0.2292(18) 0.020(8) Uiso 1 1 d . . .
C10 C 0.6283(3) 0.5041(2) 0.12622(17) 0.0156(6) Uani 1 1 d . . .
H10A H 0.615(3) 0.482(2) 0.0715(17) 0.007(7) Uiso 1 1 d . . .
C11 C 0.6526(3) 0.6204(2) 0.11090(16) 0.0180(6) Uani 1 1 d . . .
C12 C 0.5579(3) 0.6923(2) 0.12673(16) 0.0170(6) Uani 1 1 d . . .
C13 C 0.4588(3) 0.6663(2) 0.18199(15) 0.0171(7) Uani 1 1 d . . .
C14 C 0.4828(3) 0.5705(2) 0.24083(15) 0.0150(6) Uani 1 1 d . . .
C15 C 0.3690(3) 0.5439(2) 0.29061(15) 0.0158(6) Uani 1 1 d . . .
C16 C 0.2940(3) 0.4624(2) 0.27178(16) 0.0149(6) Uani 1 1 d . . .
C17 C 0.1867(3) 0.4446(2) 0.32353(16) 0.0184(7) Uani 1 1 d . . .
C18 C 0.1060(3) 0.3578(3) 0.30253(17) 0.0187(7) Uani 1 1 d . . .
C19 C 0.5622(3) 0.7911(2) 0.08265(16) 0.0204(7) Uani 1 1 d . . .
C20 C 0.2161(4) 0.2919(3) 0.0769(2) 0.0246(8) Uani 1 1 d . . .
H20A H 0.135(3) 0.284(3) 0.0479(18) 0.015(8) Uiso 1 1 d . . .
H20B H 0.245(4) 0.225(4) 0.090(2) 0.038(11) Uiso 1 1 d . . .
H20C H 0.259(3) 0.329(3) 0.034(2) 0.025(9) Uiso 1 1 d . . .
C21 C 0.7318(4) 0.3324(3) 0.1384(2) 0.0259(8) Uani 1 1 d . . .
H21A H 0.688(4) 0.311(3) 0.184(2) 0.041(11) Uiso 1 1 d . . .
H21B H 0.810(4) 0.303(3) 0.1312(19) 0.019(9) Uiso 1 1 d . . .
H21C H 0.698(3) 0.321(3) 0.085(2) 0.028(10) Uiso 1 1 d . . .
C22 C 0.8096(4) 0.4811(3) 0.2228(2) 0.0308(9) Uani 1 1 d . . .
H22A H 0.820(3) 0.559(3) 0.223(2) 0.028(9) Uiso 1 1 d . . .
H22B H 0.885(4) 0.458(4) 0.222(2) 0.039(12) Uiso 1 1 d . . .
H22C H 0.761(4) 0.457(3) 0.269(2) 0.030(10) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0148(4) 0.0225(3) 0.0212(3) 0.0011(3) 0.0017(3) -0.0031(3)
O1 0.0359(18) 0.0553(19) 0.0265(11) 0.0003(11) 0.0098(10) -0.0166(16)
O6 0.0161(13) 0.0172(11) 0.0248(10) 0.0008(8) -0.0052(9) 0.0042(11)
O11 0.0167(14) 0.0226(12) 0.0412(11) 0.0072(10) 0.0086(10) -0.0041(11)
O13 0.0229(15) 0.0233(12) 0.0288(10) 0.0014(9) 0.0041(9) 0.0096(12)
O14 0.0140(13) 0.0322(13) 0.0174(9) -0.0005(8) -0.0032(8) -0.0055(11)
O15 0.0154(13) 0.0240(12) 0.0200(9) -0.0047(8) 0.0013(8) 0.0000(11)
O17 0.0180(13) 0.0292(12) 0.0229(9) -0.0026(9) 0.0037(8) 0.0002(12)
O19 0.0310(16) 0.0199(12) 0.0297(11) 0.0052(9) -0.0002(10) -0.0075(13)
N10 0.0132(15) 0.0194(13) 0.0254(11) 0.0042(10) 0.0046(10) -0.0001(12)
N19 0.038(2) 0.0166(14) 0.0319(14) 0.0069(11) -0.0021(13) 0.0056(15)
C1 0.020(2) 0.0351(19) 0.0262(14) 0.0090(13) 0.0011(13) -0.0004(17)
C2 0.017(2) 0.041(2) 0.0364(16) 0.0125(15) -0.0011(14) -0.0087(19)
C3 0.017(2) 0.0267(19) 0.0466(18) 0.0057(15) -0.0042(14) -0.0080(19)
C4 0.013(2) 0.0218(17) 0.0373(16) -0.0007(13) -0.0020(13) 0.0003(15)
C5 0.0084(18) 0.0178(15) 0.0287(13) 0.0034(11) -0.0015(11) 0.0039(14)
C6 0.0169(18) 0.0154(14) 0.0211(12) -0.0015(10) -0.0004(11) 0.0025(14)
C7 0.0061(16) 0.0135(14) 0.0237(12) -0.0006(10) 0.0003(10) 0.0009(13)
C8 0.0124(17) 0.0177(15) 0.0209(11) -0.0034(11) 0.0022(11) 0.0008(15)
C9 0.0079(16) 0.0132(14) 0.0211(11) 0.0015(10) 0.0011(10) 0.0007(13)
C10 0.0074(16) 0.0173(15) 0.0220(12) 0.0011(11) -0.0008(10) 0.0014(14)
C11 0.0153(18) 0.0184(15) 0.0202(12) 0.0031(11) -0.0013(11) -0.0003(15)
C12 0.0172(18) 0.0133(13) 0.0206(12) 0.0006(9) -0.0011(11) -0.0003(15)
C13 0.018(2) 0.0167(14) 0.0161(11) -0.0034(10) -0.0013(11) 0.0002(15)
C14 0.0119(16) 0.0151(14) 0.0181(11) -0.0005(10) -0.0024(10) -0.0015(14)
C15 0.0135(17) 0.0170(15) 0.0170(11) 0.0015(10) -0.0036(10) 0.0046(14)
C16 0.0123(17) 0.0153(14) 0.0172(11) 0.0024(10) -0.0009(10) 0.0040(14)
C17 0.0151(18) 0.0210(16) 0.0190(12) 0.0038(10) -0.0009(10) 0.0052(15)
C18 0.0111(18) 0.0209(16) 0.0240(13) 0.0045(11) -0.0007(11) 0.0031(14)
C19 0.026(2) 0.0143(14) 0.0209(12) 0.0000(10) -0.0036(12) -0.0055(17)
C20 0.019(2) 0.0250(19) 0.0299(15) -0.0109(13) 0.0012(13) -0.0014(18)
C21 0.024(2) 0.0177(17) 0.0366(17) 0.0046(13) 0.0117(15) 0.0050(17)
C22 0.017(2) 0.038(2) 0.0367(18) 0.0019(15) -0.0056(15) 0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/00/00/1000007.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1000007
loop_
_publ_author_name
'Thompson, R. M.'
'Downs, R. T.'
_publ_section_title
;
 The crystal structure of diopside at pressure to 10 GPa
 Locality: DeKalb, New York
 Sample: P = 1 atm
;
_journal_name_full               'American Mineralogist'
_journal_page_first              177
_journal_page_last               186
_journal_paper_doi               10.2138/am.2008.2684
_journal_volume                  93
_journal_year                    2008
_chemical_formula_structural     CaMg(Si2O6)
_chemical_formula_sum            'Ca Mg O6 Si2'
_chemical_name_mineral           Diopside
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 105.86600
_cell_angle_gamma                90.00000
_cell_length_a                   9.73970
_cell_length_b                   8.91740
_cell_length_c                   5.25030
_diffrn_ambient_pressure         100
_exptl_crystal_density_diffrn    3.279
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'Ca Mg Si2 O6'
_cod_database_code               1000007
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
Mg Mg 0.00000 0.90808 0.25000 Uiso 0.00393
Ca Ca 0.00000 0.30148 0.25000 Uiso 0.00823
Si Si 0.28619 0.09319 0.22936 Uiso 0.00431
O1 O 0.11554 0.08690 0.14186 Uiso 0.00697
O2 O 0.36094 0.25019 0.31776 Uiso 0.00785
O3 O 0.35073 0.01744 0.99543 Uiso 0.00709



data_p21c

_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C34 H24 Al F36 Ga O4'
_chemical_formula_weight          1277.23

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ga'  'Ga'   0.2307   1.6083
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                    10.5086(3)
_cell_length_b                    20.9035(5)
_cell_length_c                    20.5072(5)
_cell_angle_alpha                 90
_cell_angle_beta                  94.1300(10)
_cell_angle_gamma                 90
_cell_volume                      4493.0(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.888
_exptl_crystal_F_000              2512
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.990
_exptl_crystal_size_mid           0.110
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.821
_shelx_estimated_absorpt_T_min    0.497
_shelx_estimated_absorpt_T_max    0.922
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             42245
_diffrn_reflns_av_unetI/netI      0.0585
_diffrn_reflns_av_R_equivalents   0.0504
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -25
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          1.943
_diffrn_reflns_theta_max          28.120
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.983
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.983
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.983
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              10786
_reflns_number_gt                 7085
_reflns_threshold_expression      'I > 2\s(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .

_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          10786
_refine_ls_number_parameters      945
_refine_ls_number_restraints      1924
_refine_ls_R_factor_all           0.0794
_refine_ls_R_factor_gt            0.0400
_refine_ls_wR_factor_ref          0.1008
_refine_ls_wR_factor_gt           0.0860
_refine_ls_goodness_of_fit_ref    1.015
_refine_ls_restrained_S_all       0.947
_refine_ls_shift/su_max           0.034
_refine_ls_shift/su_mean          0.002

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ga1 Ga 0.63951(3) 0.56174(2) 0.23776(2) 0.02486(8) Uani 1 1 d . . . . .
Al1 Al 0.06428(6) 0.26019(3) 0.47872(3) 0.01666(15) Uani 1 1 d D . . . .
O1 O 0.12047(15) 0.33657(7) 0.49413(7) 0.0205(4) Uani 1 1 d D . . . .
O2 O -0.09735(15) 0.26091(7) 0.48932(7) 0.0199(4) Uani 1 1 d . . . . .
F10 F -0.36256(13) 0.27826(7) 0.44777(6) 0.0312(3) Uani 1 1 d . . . . .
F11 F -0.40436(14) 0.25782(7) 0.54704(7) 0.0348(4) Uani 1 1 d . . . . .
F12 F -0.30142(14) 0.18957(7) 0.49253(7) 0.0324(3) Uani 1 1 d . . . . .
F13 F -0.17518(15) 0.20242(7) 0.61008(7) 0.0376(4) Uani 1 1 d . . . . .
F14 F -0.03152(13) 0.27554(7) 0.61664(6) 0.0347(4) Uani 1 1 d . . . . .
F15 F -0.22234(14) 0.29702(8) 0.64145(6) 0.0400(4) Uani 1 1 d . . . . .
F16 F -0.31328(14) 0.37729(7) 0.54057(7) 0.0339(4) Uani 1 1 d . . . . .
F17 F -0.18944(15) 0.37607(7) 0.46125(7) 0.0362(4) Uani 1 1 d . . . . .
F18 F -0.11040(14) 0.38667(7) 0.56007(7) 0.0354(4) Uani 1 1 d . . . . .
C5 C -0.1873(2) 0.28285(11) 0.52751(10) 0.0193(5) Uani 1 1 d . . . . .
C6 C -0.3160(2) 0.25167(12) 0.50399(11) 0.0248(5) Uani 1 1 d . . . . .
C7 C -0.1543(2) 0.26442(13) 0.60036(11) 0.0268(6) Uani 1 1 d . . . . .
C8 C -0.2011(2) 0.35676(12) 0.52218(12) 0.0268(6) Uani 1 1 d . . . . .
C1 C 0.2231(2) 0.37518(11) 0.50381(11) 0.0199(5) Uani 1 1 d . . . . .
C2 C 0.3258(2) 0.35914(12) 0.45611(12) 0.0269(6) Uani 1 1 d . . . . .
F1 F 0.29069(15) 0.37973(7) 0.39576(7) 0.0368(4) Uani 1 1 d . . . . .
F2 F 0.34279(14) 0.29634(7) 0.45200(7) 0.0351(4) Uani 1 1 d . . . . .
F3 F 0.43911(14) 0.38531(7) 0.47351(8) 0.0374(4) Uani 1 1 d . . . . .
C3 C 0.1789(2) 0.44511(11) 0.49260(12) 0.0252(6) Uani 1 1 d . . . . .
F4 F 0.10028(15) 0.44963(7) 0.43908(7) 0.0355(4) Uani 1 1 d . . . . .
F5 F 0.11602(14) 0.46625(7) 0.54273(7) 0.0328(3) Uani 1 1 d . . . . .
F6 F 0.27615(14) 0.48525(7) 0.48574(7) 0.0349(4) Uani 1 1 d . . . . .
C4 C 0.2822(2) 0.36863(12) 0.57553(12) 0.0282(6) Uani 1 1 d . . . . .
F7 F 0.35833(14) 0.41783(7) 0.59377(7) 0.0369(4) Uani 1 1 d . . . . .
F8 F 0.35189(14) 0.31520(7) 0.58280(7) 0.0383(4) Uani 1 1 d . . . . .
F9 F 0.19206(15) 0.36552(8) 0.61727(7) 0.0386(4) Uani 1 1 d . . . . .
C34 C 0.3697(2) 0.54873(11) 0.21320(12) 0.0247(5) Uani 1 1 d . . . . .
H34 H 0.340368 0.506496 0.203866 0.030 Uiso 1 1 calc R U . . .
C33 C 0.3806(2) 0.56954(12) 0.27790(11) 0.0244(5) Uani 1 1 d . . . . .
C32 C 0.4252(2) 0.63135(12) 0.29055(11) 0.0250(6) Uani 1 1 d . . . . .
H32 H 0.435587 0.645809 0.334526 0.030 Uiso 1 1 calc R U . . .
C35 C 0.4007(2) 0.58814(11) 0.16162(11) 0.0232(5) Uani 1 1 d . . . . .
C30 C 0.4438(2) 0.64985(11) 0.17637(11) 0.0238(5) Uani 1 1 d . . . . .
H30 H 0.466094 0.677168 0.141976 0.029 Uiso 1 1 calc R U . . .
C36 C 0.3837(3) 0.56513(13) 0.09209(11) 0.0342(7) Uani 1 1 d . . . . .
H36A H 0.294883 0.571492 0.075369 0.051 Uiso 1 1 calc R U . . .
H36B H 0.404980 0.519546 0.090375 0.051 Uiso 1 1 calc R U . . .
H36C H 0.440202 0.589360 0.065185 0.051 Uiso 1 1 calc R U . . .
C31 C 0.4548(2) 0.67245(12) 0.24067(12) 0.0260(6) Uani 1 1 d . . . . .
C37 C 0.3411(3) 0.52743(13) 0.33252(12) 0.0328(6) Uani 1 1 d . . . . .
H37A H 0.409049 0.526804 0.367870 0.049 Uiso 1 1 calc R U . . .
H37B H 0.326063 0.483871 0.316065 0.049 Uiso 1 1 calc R U . . .
H37C H 0.262663 0.544219 0.349164 0.049 Uiso 1 1 calc R U . . .
C38 C 0.4943(3) 0.74049(12) 0.25556(14) 0.0379(7) Uani 1 1 d . . . . .
H38A H 0.530123 0.759372 0.217156 0.057 Uiso 1 1 calc R U . . .
H38B H 0.558750 0.741073 0.292562 0.057 Uiso 1 1 calc R U . . .
H38C H 0.419731 0.765295 0.266654 0.057 Uiso 1 1 calc R U . . .
C21 C 0.7219(2) 0.44795(11) 0.16756(12) 0.0262(6) Uani 1 1 d . . . . .
C20 C 0.8383(2) 0.47476(12) 0.19037(12) 0.0273(6) Uani 1 1 d . . . . .
H20 H 0.894183 0.490749 0.159808 0.033 Uiso 1 1 calc R U . . .
C23 C 0.6734(3) 0.42917(11) 0.28051(12) 0.0263(6) Uani 1 1 d . . . . .
C25 C 0.8744(2) 0.47862(12) 0.25692(12) 0.0280(6) Uani 1 1 d . . . . .
C22 C 0.6410(2) 0.42569(11) 0.21311(12) 0.0278(6) Uani 1 1 d . . . . .
H22 H 0.561275 0.407572 0.198152 0.033 Uiso 1 1 calc R U . . .
C28 C 0.6857(3) 0.44354(13) 0.09530(12) 0.0380(7) Uani 1 1 d . . . . .
H28A H 0.672163 0.486642 0.077326 0.057 Uiso 1 1 calc R U . . .
H28B H 0.606897 0.418637 0.088035 0.057 Uiso 1 1 calc R U . . .
H28C H 0.754316 0.422459 0.073534 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5884(3) 0.40178(14) 0.32893(14) 0.0407(7) Uani 1 1 d . . . . .
H27A H 0.582419 0.431842 0.365247 0.061 Uiso 1 1 calc R U . . .
H27B H 0.623985 0.361147 0.345669 0.061 Uiso 1 1 calc R U . . .
H27C H 0.503252 0.394423 0.307573 0.061 Uiso 1 1 calc R U . . .
C24 C 0.7906(2) 0.45642(12) 0.30110(12) 0.0278(6) Uani 1 1 d . . . . .
H24 H 0.813753 0.459894 0.346610 0.033 Uiso 1 1 calc R U . . .
C26 C 1.0027(3) 0.50543(15) 0.28139(15) 0.0480(8) Uani 1 1 d . . . . .
H26A H 1.045652 0.523124 0.244548 0.072 Uiso 1 1 calc R U . . .
H26B H 1.055103 0.471240 0.302077 0.072 Uiso 1 1 calc R U . . .
H26C H 0.990498 0.539293 0.313390 0.072 Uiso 1 1 calc R U . . .
O1_1 O 0.158(2) 0.2094(6) 0.5279(9) 0.020(3) Uani 0.482(4) 1 d D U P A 1
C1_1 C 0.1989(8) 0.1495(5) 0.5435(4) 0.0198(19) Uani 0.482(4) 1 d D U P A 1
C2_1 C 0.2836(6) 0.1249(3) 0.4903(3) 0.0330(15) Uani 0.482(4) 1 d D U P A 1
F1_1 F 0.3556(18) 0.0749(6) 0.5105(9) 0.034(2) Uani 0.482(4) 1 d D U P A 1
F2_1 F 0.3595(7) 0.1706(4) 0.4715(4) 0.0399(16) Uani 0.482(4) 1 d D U P A 1
F3_1 F 0.2121(5) 0.10411(17) 0.43813(16) 0.0507(14) Uani 0.482(4) 1 d D U P A 1
C3_1 C 0.0865(6) 0.1035(3) 0.5496(4) 0.0395(17) Uani 0.482(4) 1 d D U P A 1
F4_1 F 0.1169(17) 0.0412(5) 0.5474(7) 0.056(4) Uani 0.482(4) 1 d D U P A 1
F5_1 F -0.0051(9) 0.1142(8) 0.5020(5) 0.056(3) Uani 0.482(4) 1 d D U P A 1
F6_1 F 0.0325(4) 0.1130(2) 0.6068(3) 0.0579(14) Uani 0.482(4) 1 d D U P A 1
C4_1 C 0.2805(6) 0.1528(3) 0.6099(2) 0.0297(13) Uani 0.482(4) 1 d D U P A 1
F7_1 F 0.2225(15) 0.1879(7) 0.6525(8) 0.044(3) Uani 0.482(4) 1 d D U P A 1
F8_1 F 0.2984(13) 0.0945(6) 0.6373(9) 0.037(2) Uani 0.482(4) 1 d D U P A 1
F9_1 F 0.3949(3) 0.17721(17) 0.6024(2) 0.0386(10) Uani 0.482(4) 1 d D U P A 1
O1_2 O 0.1412(19) 0.2070(6) 0.5329(8) 0.020(2) Uani 0.518(4) 1 d D U P A 2
C1_2 C 0.1825(8) 0.1467(5) 0.5459(4) 0.0219(18) Uani 0.518(4) 1 d D U P A 2
C2_2 C 0.1928(6) 0.1406(3) 0.6213(2) 0.0319(13) Uani 0.518(4) 1 d D U P A 2
F1_2 F 0.2452(14) 0.1928(7) 0.6492(8) 0.042(3) Uani 0.518(4) 1 d D U P A 2
F2_2 F 0.2638(12) 0.0903(6) 0.6420(9) 0.049(3) Uani 0.518(4) 1 d D U P A 2
F3_2 F 0.0786(4) 0.13192(19) 0.64353(18) 0.0458(10) Uani 0.518(4) 1 d D U P A 2
C3_2 C 0.0915(6) 0.0950(3) 0.5153(3) 0.0319(14) Uani 0.518(4) 1 d D U P A 2
F4_2 F 0.1079(4) 0.08545(15) 0.45255(15) 0.0425(10) Uani 0.518(4) 1 d D U P A 2
F5_2 F -0.0298(8) 0.1120(7) 0.5200(4) 0.043(2) Uani 0.518(4) 1 d D U P A 2
F6_2 F 0.1092(15) 0.0392(4) 0.5460(5) 0.042(3) Uani 0.518(4) 1 d D U P A 2
C4_2 C 0.3162(6) 0.1371(3) 0.5200(3) 0.0357(14) Uani 0.518(4) 1 d D U P A 2
F7_2 F 0.3192(7) 0.1575(4) 0.4581(3) 0.0434(17) Uani 0.518(4) 1 d D U P A 2
F8_2 F 0.3541(15) 0.0759(5) 0.5217(8) 0.040(3) Uani 0.518(4) 1 d D U P A 2
F9_2 F 0.4058(3) 0.16808(16) 0.5566(3) 0.0507(11) Uani 0.518(4) 1 d D U P A 2
O1_3 O 0.088(2) 0.2351(8) 0.4003(4) 0.024(3) Uani 0.559(5) 1 d D U P A 1
C1_3 C 0.0366(9) 0.2315(5) 0.3368(6) 0.021(2) Uani 0.559(5) 1 d . U P A 1
C2_3 C 0.1505(6) 0.2332(3) 0.2945(2) 0.0328(14) Uani 0.559(5) 1 d . U P A 1
F1_3 F 0.122(2) 0.2117(10) 0.2329(5) 0.038(2) Uani 0.559(5) 1 d . U P A 1
F2_3 F 0.2463(11) 0.1945(6) 0.3197(9) 0.037(2) Uani 0.559(5) 1 d . U P A 1
F3_3 F 0.1966(4) 0.2921(2) 0.29038(14) 0.0401(10) Uani 0.559(5) 1 d . U P A 1
C3_3 C -0.0528(6) 0.2887(3) 0.3184(2) 0.0319(14) Uani 0.559(5) 1 d . U P A 1
F4_3 F -0.0053(17) 0.3429(8) 0.3467(8) 0.0359(19) Uani 0.559(5) 1 d . U P A 1
F5_3 F -0.0674(11) 0.3011(7) 0.2537(5) 0.033(2) Uani 0.559(5) 1 d . U P A 1
F6_3 F -0.1692(4) 0.2798(2) 0.33928(18) 0.0404(11) Uani 0.559(5) 1 d . U P A 1
C4_3 C -0.0393(5) 0.1686(3) 0.3258(2) 0.0338(14) Uani 0.559(5) 1 d . U P A 1
F7_3 F -0.1142(15) 0.1582(5) 0.3731(5) 0.036(2) Uani 0.559(5) 1 d . U P A 1
F8_3 F -0.1123(18) 0.1686(8) 0.2681(5) 0.045(3) Uani 0.559(5) 1 d . U P A 1
F9_3 F 0.0414(5) 0.11871(17) 0.32486(19) 0.0424(10) Uani 0.559(5) 1 d . U P A 1
O1_4 O 0.075(2) 0.2355(9) 0.3996(5) 0.018(3) Uani 0.441(5) 1 d D U P A 2
C1_4 C 0.0285(11) 0.2346(5) 0.3369(7) 0.023(3) Uani 0.441(5) 1 d D U P A 2
C2_4 C 0.0188(8) 0.3026(3) 0.3076(3) 0.0359(17) Uani 0.441(5) 1 d D U P A 2
F1_4 F 0.1302(5) 0.3255(2) 0.29338(19) 0.0469(14) Uani 0.441(5) 1 d D U P A 2
F2_4 F -0.0571(17) 0.3008(10) 0.2528(7) 0.062(5) Uani 0.441(5) 1 d D U P A 2
F3_4 F -0.034(2) 0.3406(11) 0.3500(11) 0.050(5) Uani 0.441(5) 1 d D U P A 2
C3_4 C -0.1036(6) 0.2022(4) 0.3323(3) 0.0348(16) Uani 0.441(5) 1 d D U P A 2
F4_4 F -0.107(2) 0.1524(8) 0.3732(9) 0.059(5) Uani 0.441(5) 1 d D U P A 2
F5_4 F -0.1942(5) 0.2424(3) 0.3471(2) 0.0451(14) Uani 0.441(5) 1 d D U P A 2
F6_4 F -0.132(2) 0.1787(10) 0.2727(7) 0.048(4) Uani 0.441(5) 1 d D U P A 2
C4_4 C 0.1216(6) 0.1944(4) 0.2981(3) 0.0304(15) Uani 0.441(5) 1 d D U P A 2
F7_4 F 0.1125(6) 0.1321(2) 0.3114(2) 0.0433(13) Uani 0.441(5) 1 d D U P A 2
F8_4 F 0.100(3) 0.2004(12) 0.2340(6) 0.043(4) Uani 0.441(5) 1 d D U P A 2
F9_4 F 0.2417(12) 0.2112(8) 0.3142(11) 0.038(3) Uani 0.441(5) 1 d D U P A 2

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ga1 0.02411(16) 0.02509(16) 0.02491(14) 0.00000(11) -0.00158(11) 0.00159(12)
Al1 0.0161(4) 0.0198(4) 0.0137(3) -0.0001(3) -0.0022(3) 0.0012(3)
O1 0.0159(9) 0.0219(9) 0.0232(8) -0.0012(7) -0.0022(7) -0.0016(7)
O2 0.0170(9) 0.0260(9) 0.0167(7) -0.0042(6) 0.0004(7) 0.0007(7)
F10 0.0227(8) 0.0420(9) 0.0273(7) 0.0010(6) -0.0101(6) 0.0019(7)
F11 0.0206(8) 0.0489(10) 0.0356(8) -0.0016(7) 0.0054(7) -0.0023(7)
F12 0.0269(8) 0.0271(8) 0.0424(8) -0.0040(6) -0.0018(7) -0.0053(7)
F13 0.0403(10) 0.0437(10) 0.0285(8) 0.0132(7) 0.0012(7) 0.0038(8)
F14 0.0229(8) 0.0577(10) 0.0221(7) -0.0063(7) -0.0081(6) 0.0075(7)
F15 0.0325(9) 0.0682(11) 0.0196(7) -0.0071(7) 0.0037(6) 0.0158(8)
F16 0.0235(8) 0.0331(9) 0.0446(9) -0.0066(7) -0.0002(7) 0.0094(7)
F17 0.0457(10) 0.0283(8) 0.0349(8) 0.0060(6) 0.0045(7) 0.0019(7)
F18 0.0268(8) 0.0330(9) 0.0459(9) -0.0153(7) -0.0015(7) -0.0044(7)
C5 0.0175(13) 0.0224(12) 0.0176(11) -0.0003(9) -0.0020(9) 0.0012(10)
C6 0.0220(14) 0.0283(14) 0.0238(12) 0.0005(10) 0.0009(10) 0.0007(11)
C7 0.0202(14) 0.0375(16) 0.0224(12) -0.0018(11) -0.0003(10) 0.0060(12)
C8 0.0217(14) 0.0290(14) 0.0294(13) -0.0059(11) 0.0004(11) 0.0004(12)
C1 0.0156(12) 0.0222(13) 0.0211(11) 0.0010(9) -0.0035(9) -0.0005(10)
C2 0.0216(14) 0.0286(14) 0.0303(13) -0.0007(11) -0.0004(11) -0.0006(12)
F1 0.0394(10) 0.0464(10) 0.0253(7) 0.0020(7) 0.0075(7) -0.0033(8)
F2 0.0252(9) 0.0309(9) 0.0494(9) -0.0095(7) 0.0044(7) 0.0047(7)
F3 0.0175(8) 0.0435(9) 0.0514(10) -0.0054(7) 0.0037(7) -0.0064(7)
C3 0.0222(14) 0.0255(14) 0.0273(12) 0.0016(10) -0.0020(10) -0.0009(11)
F4 0.0371(9) 0.0327(9) 0.0346(8) 0.0078(6) -0.0123(7) 0.0073(7)
F5 0.0313(9) 0.0283(8) 0.0390(8) -0.0087(6) 0.0025(7) 0.0037(7)
F6 0.0330(9) 0.0249(8) 0.0465(9) 0.0051(7) 0.0009(7) -0.0068(7)
C4 0.0273(15) 0.0297(14) 0.0261(13) 0.0007(11) -0.0075(11) -0.0036(12)
F7 0.0345(9) 0.0395(9) 0.0340(8) -0.0037(7) -0.0152(7) -0.0099(7)
F8 0.0364(9) 0.0342(9) 0.0411(9) 0.0079(7) -0.0204(7) 0.0048(7)
F9 0.0414(10) 0.0538(10) 0.0202(7) 0.0022(7) 0.0000(7) -0.0093(8)
C34 0.0200(13) 0.0225(13) 0.0308(13) -0.0049(10) -0.0029(10) 0.0011(10)
C33 0.0160(13) 0.0324(15) 0.0243(12) 0.0013(10) -0.0020(10) 0.0041(11)
C32 0.0154(13) 0.0321(14) 0.0266(12) -0.0092(11) -0.0040(10) 0.0056(11)
C35 0.0178(13) 0.0285(13) 0.0223(11) -0.0016(10) -0.0058(10) 0.0028(11)
C30 0.0203(13) 0.0243(13) 0.0261(12) 0.0046(10) -0.0025(10) 0.0041(11)
C36 0.0430(18) 0.0360(16) 0.0226(12) -0.0027(11) -0.0039(12) 0.0002(13)
C31 0.0165(13) 0.0250(13) 0.0356(13) -0.0043(11) -0.0038(11) 0.0041(11)
C37 0.0265(15) 0.0435(17) 0.0284(13) 0.0016(12) 0.0020(11) -0.0043(13)
C38 0.0363(17) 0.0278(15) 0.0482(17) -0.0073(12) -0.0069(13) -0.0010(13)
C21 0.0290(15) 0.0229(13) 0.0262(12) -0.0035(10) -0.0015(11) 0.0071(11)
C20 0.0235(14) 0.0300(14) 0.0289(13) 0.0042(11) 0.0047(11) 0.0070(12)
C23 0.0301(15) 0.0195(13) 0.0297(13) 0.0033(10) 0.0033(11) 0.0051(11)
C25 0.0198(14) 0.0280(14) 0.0349(14) 0.0029(11) -0.0073(11) 0.0037(11)
C22 0.0269(15) 0.0216(13) 0.0342(13) -0.0007(11) -0.0033(11) 0.0018(11)
C28 0.0502(19) 0.0368(16) 0.0258(13) -0.0065(11) -0.0045(12) 0.0029(14)
C27 0.0426(18) 0.0406(17) 0.0394(16) 0.0085(13) 0.0064(14) -0.0020(15)
C24 0.0322(16) 0.0272(14) 0.0231(12) 0.0002(10) -0.0047(11) 0.0090(12)
C26 0.0288(17) 0.063(2) 0.0504(18) 0.0071(16) -0.0130(14) -0.0025(15)
O1_1 0.021(5) 0.019(3) 0.022(5) -0.002(3) -0.001(4) 0.006(3)
C1_1 0.019(4) 0.015(4) 0.024(4) 0.003(3) -0.004(3) -0.002(3)
C2_1 0.044(4) 0.026(3) 0.028(3) 0.002(3) 0.000(3) 0.009(3)
F1_1 0.047(5) 0.028(3) 0.027(3) -0.004(2) -0.001(3) 0.013(3)
F2_1 0.040(4) 0.037(3) 0.045(3) 0.007(2) 0.018(3) 0.012(2)
F3_1 0.080(4) 0.039(2) 0.0290(18) -0.0118(15) -0.021(2) 0.024(2)
C3_1 0.023(3) 0.031(3) 0.063(4) 0.014(4) -0.006(3) 0.001(3)
F4_1 0.034(6) 0.028(4) 0.105(8) 0.021(4) -0.008(5) -0.002(4)
F5_1 0.032(4) 0.036(3) 0.097(6) 0.009(5) -0.033(4) -0.009(4)
F6_1 0.041(3) 0.053(3) 0.084(3) 0.032(3) 0.031(3) 0.002(2)
C4_1 0.037(3) 0.027(3) 0.024(3) 0.006(2) -0.007(2) 0.008(3)
F7_1 0.066(6) 0.048(6) 0.016(3) 0.004(3) -0.005(4) 0.022(5)
F8_1 0.049(6) 0.031(3) 0.029(3) 0.012(2) -0.010(4) 0.013(3)
F9_1 0.028(2) 0.039(2) 0.045(2) -0.0040(18) -0.0189(17) 0.0020(15)
O1_2 0.022(5) 0.027(4) 0.013(3) 0.006(2) 0.000(3) 0.005(3)
C1_2 0.020(3) 0.024(4) 0.021(3) 0.000(3) -0.004(3) 0.008(3)
C2_2 0.042(3) 0.028(3) 0.024(2) 0.007(2) -0.008(2) 0.001(3)
F1_2 0.052(4) 0.039(4) 0.032(5) -0.005(3) -0.019(3) -0.005(3)
F2_2 0.060(6) 0.045(3) 0.041(4) 0.016(2) -0.015(5) 0.014(4)
F3_2 0.057(3) 0.049(2) 0.034(2) 0.0104(17) 0.0188(18) 0.0038(19)
C3_2 0.028(3) 0.031(3) 0.036(3) 0.000(3) -0.004(3) 0.002(2)
F4_2 0.053(3) 0.0385(19) 0.0338(16) -0.0126(14) -0.0096(16) 0.0063(18)
F5_2 0.023(3) 0.044(4) 0.063(4) -0.004(3) -0.006(2) -0.004(3)
F6_2 0.052(7) 0.025(4) 0.047(4) -0.002(3) -0.006(4) -0.003(4)
C4_2 0.032(3) 0.026(3) 0.050(4) 0.010(3) 0.007(3) 0.004(2)
F7_2 0.044(4) 0.044(4) 0.044(3) 0.016(3) 0.019(3) 0.014(3)
F8_2 0.030(4) 0.036(4) 0.054(7) 0.011(3) 0.007(4) 0.021(3)
F9_2 0.0225(19) 0.038(2) 0.090(3) 0.004(2) -0.007(2) -0.0032(15)
O1_3 0.018(5) 0.046(6) 0.009(4) -0.001(3) -0.002(3) 0.006(3)
C1_3 0.014(4) 0.030(4) 0.018(5) 0.002(4) -0.008(3) 0.006(3)
C2_3 0.040(4) 0.040(4) 0.018(2) -0.005(3) -0.003(2) 0.009(3)
F1_3 0.042(6) 0.059(5) 0.012(2) -0.0051(19) 0.001(2) 0.003(3)
F2_3 0.028(3) 0.053(5) 0.029(3) -0.003(4) -0.0033(18) 0.018(3)
F3_3 0.044(2) 0.048(2) 0.0286(15) 0.0019(15) 0.0056(14) -0.0126(19)
C3_3 0.034(4) 0.040(3) 0.020(2) -0.004(2) -0.006(3) 0.012(3)
F4_3 0.050(6) 0.027(3) 0.028(3) -0.004(2) -0.012(3) 0.013(3)
F5_3 0.042(4) 0.041(5) 0.016(4) 0.001(3) -0.005(3) 0.013(3)
F6_3 0.024(2) 0.065(3) 0.0314(16) 0.000(2) -0.0046(14) 0.017(2)
C4_3 0.033(3) 0.043(3) 0.024(2) -0.002(2) -0.011(2) -0.005(3)
F7_3 0.029(5) 0.051(4) 0.028(4) -0.003(3) 0.001(4) -0.019(3)
F8_3 0.054(7) 0.050(3) 0.028(3) 0.001(3) -0.022(4) -0.008(3)
F9_3 0.055(3) 0.0323(19) 0.038(2) -0.0075(14) -0.0107(19) 0.006(2)
O1_4 0.015(5) 0.020(6) 0.019(5) -0.005(4) -0.005(3) 0.004(4)
C1_4 0.023(5) 0.036(5) 0.011(5) -0.010(4) 0.000(4) 0.004(4)
C2_4 0.046(4) 0.041(4) 0.019(3) 0.000(3) -0.009(3) 0.006(3)
F1_4 0.062(3) 0.043(3) 0.035(2) 0.0083(19) -0.001(2) -0.012(3)
F2_4 0.078(8) 0.072(10) 0.031(6) 0.002(6) -0.028(6) 0.026(7)
F3_4 0.063(10) 0.044(6) 0.039(4) -0.008(4) -0.014(4) 0.026(6)
C3_4 0.028(3) 0.061(4) 0.015(3) -0.006(3) -0.004(2) -0.007(3)
F4_4 0.052(9) 0.072(7) 0.049(8) 0.017(6) -0.010(6) -0.021(6)
F5_4 0.020(2) 0.083(4) 0.031(2) -0.014(3) -0.0065(17) 0.007(3)
F6_4 0.035(5) 0.082(10) 0.025(3) -0.021(4) -0.006(3) -0.019(6)
C4_4 0.030(3) 0.045(4) 0.016(2) -0.005(3) -0.001(2) 0.011(3)
F7_4 0.057(4) 0.038(3) 0.034(2) -0.0058(18) 0.002(2) 0.019(3)
F8_4 0.043(8) 0.070(9) 0.017(3) -0.010(3) 0.003(3) 0.015(7)
F9_4 0.020(3) 0.065(8) 0.028(4) -0.003(5) 0.005(3) 0.017(4)

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 O1_4 1.714(10) . ?
Al1 O1_1 1.723(9) . ?
Al1 O1 1.7236(17) . ?
Al1 O1_3 1.727(8) . ?
Al1 O2 1.7279(17) . ?
Al1 O1_2 1.731(8) . ?
O1 C1 1.351(3) . ?
O2 C5 1.351(3) . ?
F10 C6 1.340(3) . ?
F11 C6 1.333(3) . ?
F12 C6 1.330(3) . ?
F13 C7 1.332(3) . ?
F14 C7 1.330(3) . ?
F15 C7 1.331(3) . ?
F16 C8 1.335(3) . ?
F17 C8 1.327(3) . ?
F18 C8 1.340(3) . ?
C5 C6 1.546(3) . ?
C5 C8 1.555(3) . ?
C5 C7 1.558(3) . ?
C1 C2 1.544(3) . ?
C1 C3 1.546(3) . ?
C1 C4 1.560(3) . ?
C2 F2 1.328(3) . ?
C2 F3 1.336(3) . ?
C2 F1 1.337(3) . ?
C3 F4 1.328(3) . ?
C3 F5 1.336(3) . ?
C3 F6 1.338(3) . ?
C4 F9 1.323(3) . ?
C4 F8 1.338(3) . ?
C4 F7 1.340(3) . ?
C34 C33 1.393(3) . ?
C34 C35 1.398(3) . ?
C34 H34 0.9500 . ?
C33 C32 1.393(3) . ?
C33 C37 1.506(3) . ?
C32 C31 1.388(3) . ?
C32 H32 0.9500 . ?
C35 C30 1.393(3) . ?
C35 C36 1.503(3) . ?
C30 C31 1.398(3) . ?
C30 H30 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C31 C38 1.507(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C21 C22 1.388(4) . ?
C21 C20 1.395(3) . ?
C21 C28 1.506(3) . ?
C20 C25 1.392(3) . ?
C20 H20 0.9500 . ?
C23 C24 1.394(4) . ?
C23 C22 1.402(3) . ?
C23 C27 1.496(4) . ?
C25 C24 1.388(4) . ?
C25 C26 1.512(4) . ?
C22 H22 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O1_1 C1_1 1.354(9) . ?
C1_1 C3_1 1.536(9) . ?
C1_1 C2_1 1.545(9) . ?
C1_1 C4_1 1.557(9) . ?
C2_1 F2_1 1.319(9) . ?
C2_1 F3_1 1.335(7) . ?
C2_1 F1_1 1.338(10) . ?
C3_1 F5_1 1.340(9) . ?
C3_1 F4_1 1.341(10) . ?
C3_1 F6_1 1.353(8) . ?
C4_1 F7_1 1.323(11) . ?
C4_1 F9_1 1.325(7) . ?
C4_1 F8_1 1.350(9) . ?
O1_2 C1_2 1.353(9) . ?
C1_2 C3_2 1.545(9) . ?
C1_2 C2_2 1.547(9) . ?
C1_2 C4_2 1.551(9) . ?
C2_2 F3_2 1.326(7) . ?
C2_2 F1_2 1.333(11) . ?
C2_2 F2_2 1.341(9) . ?
C3_2 F4_2 1.326(6) . ?
C3_2 F6_2 1.333(9) . ?
C3_2 F5_2 1.334(9) . ?
C4_2 F9_2 1.331(7) . ?
C4_2 F8_2 1.339(9) . ?
C4_2 F7_2 1.341(8) . ?
O1_3 C1_3 1.376(12) . ?
C1_3 C2_3 1.528(11) . ?
C1_3 C4_3 1.546(11) . ?
C1_3 C3_3 1.549(10) . ?
C2_3 F3_3 1.327(8) . ?
C2_3 F1_3 1.354(13) . ?
C2_3 F2_3 1.365(13) . ?
C3_3 F6_3 1.338(8) . ?
C3_3 F5_3 1.349(10) . ?
C3_3 F4_3 1.352(17) . ?
C4_3 F7_3 1.310(14) . ?
C4_3 F9_3 1.346(7) . ?
C4_3 F8_3 1.362(12) . ?
O1_4 C1_4 1.343(15) . ?
C1_4 C3_4 1.541(11) . ?
C1_4 C2_4 1.543(11) . ?
C1_4 C4_4 1.552(11) . ?
C2_4 F1_4 1.317(9) . ?
C2_4 F3_4 1.329(12) . ?
C2_4 F2_4 1.330(12) . ?
C3_4 F5_4 1.321(8) . ?
C3_4 F6_4 1.332(11) . ?
C3_4 F4_4 1.339(12) . ?
C4_4 F8_4 1.325(12) . ?
C4_4 F9_4 1.329(12) . ?
C4_4 F7_4 1.336(9) . ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1_4 Al1 O1 114.1(7) . . ?
O1_1 Al1 O1 106.8(6) . . ?
O1_1 Al1 O1_3 104.0(9) . . ?
O1 Al1 O1_3 112.5(6) . . ?
O1_4 Al1 O2 104.7(9) . . ?
O1_1 Al1 O2 117.3(8) . . ?
O1 Al1 O2 107.20(8) . . ?
O1_3 Al1 O2 109.2(7) . . ?
O1_4 Al1 O1_2 110.7(9) . . ?
O1 Al1 O1_2 109.9(6) . . ?
O2 Al1 O1_2 110.0(7) . . ?
C1 O1 Al1 147.14(15) . . ?
C5 O2 Al1 144.23(14) . . ?
O2 C5 C6 107.99(18) . . ?
O2 C5 C8 111.22(19) . . ?
C6 C5 C8 108.79(19) . . ?
O2 C5 C7 110.81(18) . . ?
C6 C5 C7 108.92(19) . . ?
C8 C5 C7 109.04(18) . . ?
F12 C6 F11 107.79(19) . . ?
F12 C6 F10 106.99(19) . . ?
F11 C6 F10 107.51(19) . . ?
F12 C6 C5 110.9(2) . . ?
F11 C6 C5 112.84(19) . . ?
F10 C6 C5 110.52(19) . . ?
F14 C7 F15 107.90(19) . . ?
F14 C7 F13 107.45(19) . . ?
F15 C7 F13 107.6(2) . . ?
F14 C7 C5 110.0(2) . . ?
F15 C7 C5 112.8(2) . . ?
F13 C7 C5 110.88(19) . . ?
F17 C8 F16 108.1(2) . . ?
F17 C8 F18 107.1(2) . . ?
F16 C8 F18 106.97(19) . . ?
F17 C8 C5 110.73(19) . . ?
F16 C8 C5 112.3(2) . . ?
F18 C8 C5 111.36(19) . . ?
O1 C1 C2 111.35(19) . . ?
O1 C1 C3 108.33(19) . . ?
C2 C1 C3 109.11(19) . . ?
O1 C1 C4 110.20(19) . . ?
C2 C1 C4 109.24(19) . . ?
C3 C1 C4 108.55(19) . . ?
F2 C2 F3 107.5(2) . . ?
F2 C2 F1 106.78(19) . . ?
F3 C2 F1 107.3(2) . . ?
F2 C2 C1 111.0(2) . . ?
F3 C2 C1 113.1(2) . . ?
F1 C2 C1 111.0(2) . . ?
F4 C3 F5 107.4(2) . . ?
F4 C3 F6 107.63(19) . . ?
F5 C3 F6 107.28(19) . . ?
F4 C3 C1 110.65(19) . . ?
F5 C3 C1 110.99(19) . . ?
F6 C3 C1 112.6(2) . . ?
F9 C4 F8 107.4(2) . . ?
F9 C4 F7 107.3(2) . . ?
F8 C4 F7 107.4(2) . . ?
F9 C4 C1 111.1(2) . . ?
F8 C4 C1 110.8(2) . . ?
F7 C4 C1 112.6(2) . . ?
C33 C34 C35 122.0(2) . . ?
C33 C34 H34 119.0 . . ?
C35 C34 H34 119.0 . . ?
C32 C33 C34 118.1(2) . . ?
C32 C33 C37 120.7(2) . . ?
C34 C33 C37 121.2(2) . . ?
C31 C32 C33 121.8(2) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C30 C35 C34 118.1(2) . . ?
C30 C35 C36 121.1(2) . . ?
C34 C35 C36 120.7(2) . . ?
C35 C30 C31 121.4(2) . . ?
C35 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C31 C30 118.6(2) . . ?
C32 C31 C38 120.5(2) . . ?
C30 C31 C38 120.9(2) . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C31 C38 H38A 109.5 . . ?
C31 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C31 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C22 C21 C20 118.3(2) . . ?
C22 C21 C28 121.2(2) . . ?
C20 C21 C28 120.5(2) . . ?
C25 C20 C21 121.5(2) . . ?
C25 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C24 C23 C22 117.8(2) . . ?
C24 C23 C27 120.8(2) . . ?
C22 C23 C27 121.3(2) . . ?
C24 C25 C20 118.7(2) . . ?
C24 C25 C26 120.0(2) . . ?
C20 C25 C26 121.3(3) . . ?
C21 C22 C23 121.9(2) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
C21 C28 H28A 109.5 . . ?
C21 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C21 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C24 C23 121.8(2) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1_1 O1_1 Al1 149.9(14) . . ?
O1_1 C1_1 C3_1 111.5(12) . . ?
O1_1 C1_1 C2_1 109.3(11) . . ?
C3_1 C1_1 C2_1 109.5(7) . . ?
O1_1 C1_1 C4_1 108.1(9) . . ?
C3_1 C1_1 C4_1 109.5(7) . . ?
C2_1 C1_1 C4_1 108.8(6) . . ?
F2_1 C2_1 F3_1 108.6(6) . . ?
F2_1 C2_1 F1_1 108.4(10) . . ?
F3_1 C2_1 F1_1 105.5(8) . . ?
F2_1 C2_1 C1_1 110.9(7) . . ?
F3_1 C2_1 C1_1 110.8(6) . . ?
F1_1 C2_1 C1_1 112.5(10) . . ?
F5_1 C3_1 F4_1 107.3(10) . . ?
F5_1 C3_1 F6_1 106.4(6) . . ?
F4_1 C3_1 F6_1 106.8(8) . . ?
F5_1 C3_1 C1_1 110.6(8) . . ?
F4_1 C3_1 C1_1 114.8(9) . . ?
F6_1 C3_1 C1_1 110.6(6) . . ?
F7_1 C4_1 F9_1 109.2(8) . . ?
F7_1 C4_1 F8_1 106.4(10) . . ?
F9_1 C4_1 F8_1 107.2(7) . . ?
F7_1 C4_1 C1_1 110.5(9) . . ?
F9_1 C4_1 C1_1 111.3(5) . . ?
F8_1 C4_1 C1_1 112.1(9) . . ?
C1_2 O1_2 Al1 148.6(13) . . ?
O1_2 C1_2 C3_2 113.0(10) . . ?
O1_2 C1_2 C2_2 105.8(9) . . ?
C3_2 C1_2 C2_2 110.2(6) . . ?
O1_2 C1_2 C4_2 109.8(11) . . ?
C3_2 C1_2 C4_2 108.6(6) . . ?
C2_2 C1_2 C4_2 109.4(6) . . ?
F3_2 C2_2 F1_2 108.6(7) . . ?
F3_2 C2_2 F2_2 106.3(7) . . ?
F1_2 C2_2 F2_2 107.6(10) . . ?
F3_2 C2_2 C1_2 110.8(5) . . ?
F1_2 C2_2 C1_2 111.0(9) . . ?
F2_2 C2_2 C1_2 112.2(9) . . ?
F4_2 C3_2 F6_2 107.7(6) . . ?
F4_2 C3_2 F5_2 107.5(6) . . ?
F6_2 C3_2 F5_2 107.5(9) . . ?
F4_2 C3_2 C1_2 112.3(5) . . ?
F6_2 C3_2 C1_2 111.0(8) . . ?
F5_2 C3_2 C1_2 110.6(8) . . ?
F9_2 C4_2 F8_2 104.6(8) . . ?
F9_2 C4_2 F7_2 108.4(5) . . ?
F8_2 C4_2 F7_2 107.6(9) . . ?
F9_2 C4_2 C1_2 111.4(6) . . ?
F8_2 C4_2 C1_2 112.9(9) . . ?
F7_2 C4_2 C1_2 111.5(6) . . ?
C1_3 O1_3 Al1 145.6(15) . . ?
O1_3 C1_3 C2_3 105.4(10) . . ?
O1_3 C1_3 C4_3 110.3(10) . . ?
C2_3 C1_3 C4_3 110.7(8) . . ?
O1_3 C1_3 C3_3 112.3(11) . . ?
C2_3 C1_3 C3_3 109.2(7) . . ?
C4_3 C1_3 C3_3 108.8(7) . . ?
F3_3 C2_3 F1_3 107.8(8) . . ?
F3_3 C2_3 F2_3 108.1(7) . . ?
F1_3 C2_3 F2_3 105.4(12) . . ?
F3_3 C2_3 C1_3 111.3(6) . . ?
F1_3 C2_3 C1_3 113.1(10) . . ?
F2_3 C2_3 C1_3 110.9(9) . . ?
F6_3 C3_3 F5_3 107.4(6) . . ?
F6_3 C3_3 F4_3 107.2(7) . . ?
F5_3 C3_3 F4_3 105.8(10) . . ?
F6_3 C3_3 C1_3 111.6(6) . . ?
F5_3 C3_3 C1_3 114.3(8) . . ?
F4_3 C3_3 C1_3 110.1(10) . . ?
F7_3 C4_3 F9_3 107.1(7) . . ?
F7_3 C4_3 F8_3 108.2(10) . . ?
F9_3 C4_3 F8_3 107.7(8) . . ?
F7_3 C4_3 C1_3 111.4(8) . . ?
F9_3 C4_3 C1_3 110.0(5) . . ?
F8_3 C4_3 C1_3 112.3(9) . . ?
C1_4 O1_4 Al1 150.0(17) . . ?
O1_4 C1_4 C3_4 109.2(14) . . ?
O1_4 C1_4 C2_4 111.8(12) . . ?
C3_4 C1_4 C2_4 110.3(8) . . ?
O1_4 C1_4 C4_4 107.4(11) . . ?
C3_4 C1_4 C4_4 109.2(8) . . ?
C2_4 C1_4 C4_4 108.9(8) . . ?
F1_4 C2_4 F3_4 110.2(12) . . ?
F1_4 C2_4 F2_4 108.2(10) . . ?
F3_4 C2_4 F2_4 108.5(14) . . ?
F1_4 C2_4 C1_4 112.8(7) . . ?
F3_4 C2_4 C1_4 108.3(13) . . ?
F2_4 C2_4 C1_4 108.8(11) . . ?
F5_4 C3_4 F6_4 109.0(11) . . ?
F5_4 C3_4 F4_4 107.2(11) . . ?
F6_4 C3_4 F4_4 105.8(13) . . ?
F5_4 C3_4 C1_4 111.5(7) . . ?
F6_4 C3_4 C1_4 111.2(12) . . ?
F4_4 C3_4 C1_4 111.7(11) . . ?
F8_4 C4_4 F9_4 108.2(13) . . ?
F8_4 C4_4 F7_4 106.5(12) . . ?
F9_4 C4_4 F7_4 106.8(9) . . ?
F8_4 C4_4 C1_4 112.9(13) . . ?
F9_4 C4_4 C1_4 110.6(11) . . ?
F7_4 C4_4 C1_4 111.6(7) . . ?

loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
O1_4 Al1 O1 C1 -74.8(9) . . . . ?
O1_1 Al1 O1 C1 43.3(8) . . . . ?
O1_3 Al1 O1 C1 -70.2(7) . . . . ?
O2 Al1 O1 C1 169.7(3) . . . . ?
O1_2 Al1 O1 C1 50.2(8) . . . . ?
O1_4 Al1 O2 C5 -163.4(7) . . . . ?
O1_1 Al1 O2 C5 78.1(7) . . . . ?
O1 Al1 O2 C5 -41.9(3) . . . . ?
O1_3 Al1 O2 C5 -164.0(6) . . . . ?
O1_2 Al1 O2 C5 77.6(7) . . . . ?
Al1 O2 C5 C6 -172.98(19) . . . . ?
Al1 O2 C5 C8 67.7(3) . . . . ?
Al1 O2 C5 C7 -53.8(3) . . . . ?
O2 C5 C6 F12 44.1(2) . . . . ?
C8 C5 C6 F12 164.88(18) . . . . ?
C7 C5 C6 F12 -76.4(2) . . . . ?
O2 C5 C6 F11 165.13(18) . . . . ?
C8 C5 C6 F11 -74.0(2) . . . . ?
C7 C5 C6 F11 44.7(3) . . . . ?
O2 C5 C6 F10 -74.5(2) . . . . ?
C8 C5 C6 F10 46.4(3) . . . . ?
C7 C5 C6 F10 165.12(19) . . . . ?
O2 C5 C7 F14 44.7(3) . . . . ?
C6 C5 C7 F14 163.38(19) . . . . ?
C8 C5 C7 F14 -78.0(2) . . . . ?
O2 C5 C7 F15 165.28(19) . . . . ?
C6 C5 C7 F15 -76.1(3) . . . . ?
C8 C5 C7 F15 42.5(3) . . . . ?
O2 C5 C7 F13 -74.0(2) . . . . ?
C6 C5 C7 F13 44.6(3) . . . . ?
C8 C5 C7 F13 163.24(19) . . . . ?
O2 C5 C8 F17 38.0(3) . . . . ?
C6 C5 C8 F17 -80.8(2) . . . . ?
C7 C5 C8 F17 160.5(2) . . . . ?
O2 C5 C8 F16 159.03(18) . . . . ?
C6 C5 C8 F16 40.2(2) . . . . ?
C7 C5 C8 F16 -78.5(2) . . . . ?
O2 C5 C8 F18 -81.0(2) . . . . ?
C6 C5 C8 F18 160.15(19) . . . . ?
C7 C5 C8 F18 41.5(3) . . . . ?
Al1 O1 C1 C2 41.7(3) . . . . ?
Al1 O1 C1 C3 161.7(2) . . . . ?
Al1 O1 C1 C4 -79.7(3) . . . . ?
O1 C1 C2 F2 -44.5(2) . . . . ?
C3 C1 C2 F2 -163.99(19) . . . . ?
C4 C1 C2 F2 77.5(2) . . . . ?
O1 C1 C2 F3 -165.32(18) . . . . ?
C3 C1 C2 F3 75.2(2) . . . . ?
C4 C1 C2 F3 -43.4(3) . . . . ?
O1 C1 C2 F1 74.1(2) . . . . ?
C3 C1 C2 F1 -45.4(3) . . . . ?
C4 C1 C2 F1 -163.95(19) . . . . ?
O1 C1 C3 F4 -44.6(3) . . . . ?
C2 C1 C3 F4 76.8(2) . . . . ?
C4 C1 C3 F4 -164.3(2) . . . . ?
O1 C1 C3 F5 74.6(2) . . . . ?
C2 C1 C3 F5 -164.04(18) . . . . ?
C4 C1 C3 F5 -45.1(3) . . . . ?
O1 C1 C3 F6 -165.12(18) . . . . ?
C2 C1 C3 F6 -43.7(2) . . . . ?
C4 C1 C3 F6 75.2(2) . . . . ?
O1 C1 C4 F9 -41.1(3) . . . . ?
C2 C1 C4 F9 -163.75(19) . . . . ?
C3 C1 C4 F9 77.4(2) . . . . ?
O1 C1 C4 F8 78.2(2) . . . . ?
C2 C1 C4 F8 -44.5(3) . . . . ?
C3 C1 C4 F8 -163.4(2) . . . . ?
O1 C1 C4 F7 -161.6(2) . . . . ?
C2 C1 C4 F7 75.8(3) . . . . ?
C3 C1 C4 F7 -43.1(3) . . . . ?
C35 C34 C33 C32 -0.7(4) . . . . ?
C35 C34 C33 C37 177.2(2) . . . . ?
C34 C33 C32 C31 1.9(4) . . . . ?
C37 C33 C32 C31 -176.1(2) . . . . ?
C33 C34 C35 C30 0.1(4) . . . . ?
C33 C34 C35 C36 -177.9(2) . . . . ?
C34 C35 C30 C31 -0.6(4) . . . . ?
C36 C35 C30 C31 177.4(2) . . . . ?
C33 C32 C31 C30 -2.4(4) . . . . ?
C33 C32 C31 C38 175.8(2) . . . . ?
C35 C30 C31 C32 1.7(4) . . . . ?
C35 C30 C31 C38 -176.5(2) . . . . ?
C22 C21 C20 C25 0.9(4) . . . . ?
C28 C21 C20 C25 -179.2(2) . . . . ?
C21 C20 C25 C24 -1.4(4) . . . . ?
C21 C20 C25 C26 177.7(2) . . . . ?
C20 C21 C22 C23 -0.4(4) . . . . ?
C28 C21 C22 C23 179.7(2) . . . . ?
C24 C23 C22 C21 0.5(4) . . . . ?
C27 C23 C22 C21 -176.6(2) . . . . ?
C20 C25 C24 C23 1.6(4) . . . . ?
C26 C25 C24 C23 -177.6(2) . . . . ?
C22 C23 C24 C25 -1.1(4) . . . . ?
C27 C23 C24 C25 176.1(2) . . . . ?
O1 Al1 O1_1 C1_1 -166(3) . . . . ?
O1_3 Al1 O1_1 C1_1 -46(4) . . . . ?
O2 Al1 O1_1 C1_1 74(3) . . . . ?
Al1 O1_1 C1_1 C3_1 -51(4) . . . . ?
Al1 O1_1 C1_1 C2_1 70(4) . . . . ?
Al1 O1_1 C1_1 C4_1 -171(3) . . . . ?
O1_1 C1_1 C2_1 F2_1 40.8(12) . . . . ?
C3_1 C1_1 C2_1 F2_1 163.2(7) . . . . ?
C4_1 C1_1 C2_1 F2_1 -77.1(8) . . . . ?
O1_1 C1_1 C2_1 F3_1 -79.8(11) . . . . ?
C3_1 C1_1 C2_1 F3_1 42.6(8) . . . . ?
C4_1 C1_1 C2_1 F3_1 162.3(6) . . . . ?
O1_1 C1_1 C2_1 F1_1 162.3(13) . . . . ?
C3_1 C1_1 C2_1 F1_1 -75.2(11) . . . . ?
C4_1 C1_1 C2_1 F1_1 44.5(11) . . . . ?
O1_1 C1_1 C3_1 F5_1 41.3(13) . . . . ?
C2_1 C1_1 C3_1 F5_1 -79.8(10) . . . . ?
C4_1 C1_1 C3_1 F5_1 160.9(8) . . . . ?
O1_1 C1_1 C3_1 F4_1 162.8(12) . . . . ?
C2_1 C1_1 C3_1 F4_1 41.8(10) . . . . ?
C4_1 C1_1 C3_1 F4_1 -77.5(10) . . . . ?
O1_1 C1_1 C3_1 F6_1 -76.3(11) . . . . ?
C2_1 C1_1 C3_1 F6_1 162.6(6) . . . . ?
C4_1 C1_1 C3_1 F6_1 43.3(8) . . . . ?
O1_1 C1_1 C4_1 F7_1 46.0(15) . . . . ?
C3_1 C1_1 C4_1 F7_1 -75.7(11) . . . . ?
C2_1 C1_1 C4_1 F7_1 164.6(9) . . . . ?
O1_1 C1_1 C4_1 F9_1 -75.5(12) . . . . ?
C3_1 C1_1 C4_1 F9_1 162.8(6) . . . . ?
C2_1 C1_1 C4_1 F9_1 43.1(8) . . . . ?
O1_1 C1_1 C4_1 F8_1 164.5(13) . . . . ?
C3_1 C1_1 C4_1 F8_1 42.8(10) . . . . ?
C2_1 C1_1 C4_1 F8_1 -76.9(10) . . . . ?
O1_4 Al1 O1_2 C1_2 -26(3) . . . . ?
O1 Al1 O1_2 C1_2 -153(3) . . . . ?
O2 Al1 O1_2 C1_2 89(3) . . . . ?
Al1 O1_2 C1_2 C3_2 -35(3) . . . . ?
Al1 O1_2 C1_2 C2_2 -156(3) . . . . ?
Al1 O1_2 C1_2 C4_2 86(3) . . . . ?
O1_2 C1_2 C2_2 F3_2 78.0(11) . . . . ?
C3_2 C1_2 C2_2 F3_2 -44.4(8) . . . . ?
C4_2 C1_2 C2_2 F3_2 -163.8(5) . . . . ?
O1_2 C1_2 C2_2 F1_2 -42.8(13) . . . . ?
C3_2 C1_2 C2_2 F1_2 -165.2(9) . . . . ?
C4_2 C1_2 C2_2 F1_2 75.4(10) . . . . ?
O1_2 C1_2 C2_2 F2_2 -163.3(12) . . . . ?
C3_2 C1_2 C2_2 F2_2 74.2(10) . . . . ?
C4_2 C1_2 C2_2 F2_2 -45.1(10) . . . . ?
O1_2 C1_2 C3_2 F4_2 80.7(12) . . . . ?
C2_2 C1_2 C3_2 F4_2 -161.2(6) . . . . ?
C4_2 C1_2 C3_2 F4_2 -41.4(8) . . . . ?
O1_2 C1_2 C3_2 F6_2 -158.6(12) . . . . ?
C2_2 C1_2 C3_2 F6_2 -40.6(9) . . . . ?
C4_2 C1_2 C3_2 F6_2 79.2(9) . . . . ?
O1_2 C1_2 C3_2 F5_2 -39.4(13) . . . . ?
C2_2 C1_2 C3_2 F5_2 78.7(8) . . . . ?
C4_2 C1_2 C3_2 F5_2 -161.5(7) . . . . ?
O1_2 C1_2 C4_2 F9_2 72.6(10) . . . . ?
C3_2 C1_2 C4_2 F9_2 -163.4(6) . . . . ?
C2_2 C1_2 C4_2 F9_2 -43.1(8) . . . . ?
O1_2 C1_2 C4_2 F8_2 -170.0(11) . . . . ?
C3_2 C1_2 C4_2 F8_2 -46.0(10) . . . . ?
C2_2 C1_2 C4_2 F8_2 74.3(10) . . . . ?
O1_2 C1_2 C4_2 F7_2 -48.6(11) . . . . ?
C3_2 C1_2 C4_2 F7_2 75.4(8) . . . . ?
C2_2 C1_2 C4_2 F7_2 -164.3(7) . . . . ?
O1_1 Al1 O1_3 C1_3 153(2) . . . . ?
O1 Al1 O1_3 C1_3 -92(2) . . . . ?
O2 Al1 O1_3 C1_3 27(3) . . . . ?
Al1 O1_3 C1_3 C2_3 150(2) . . . . ?
Al1 O1_3 C1_3 C4_3 -90(2) . . . . ?
Al1 O1_3 C1_3 C3_3 31(3) . . . . ?
O1_3 C1_3 C2_3 F3_3 -76.7(10) . . . . ?
C4_3 C1_3 C2_3 F3_3 164.0(6) . . . . ?
C3_3 C1_3 C2_3 F3_3 44.2(9) . . . . ?
O1_3 C1_3 C2_3 F1_3 161.8(13) . . . . ?
C4_3 C1_3 C2_3 F1_3 42.5(12) . . . . ?
C3_3 C1_3 C2_3 F1_3 -77.3(13) . . . . ?
O1_3 C1_3 C2_3 F2_3 43.7(12) . . . . ?
C4_3 C1_3 C2_3 F2_3 -75.6(10) . . . . ?
C3_3 C1_3 C2_3 F2_3 164.5(9) . . . . ?
O1_3 C1_3 C3_3 F6_3 -81.3(11) . . . . ?
C2_3 C1_3 C3_3 F6_3 162.1(6) . . . . ?
C4_3 C1_3 C3_3 F6_3 41.1(9) . . . . ?
O1_3 C1_3 C3_3 F5_3 156.5(12) . . . . ?
C2_3 C1_3 C3_3 F5_3 39.9(11) . . . . ?
C4_3 C1_3 C3_3 F5_3 -81.1(10) . . . . ?
O1_3 C1_3 C3_3 F4_3 37.6(14) . . . . ?
C2_3 C1_3 C3_3 F4_3 -79.0(11) . . . . ?
C4_3 C1_3 C3_3 F4_3 160.0(9) . . . . ?
O1_3 C1_3 C4_3 F7_3 46.4(13) . . . . ?
C2_3 C1_3 C4_3 F7_3 162.7(9) . . . . ?
C3_3 C1_3 C4_3 F7_3 -77.2(10) . . . . ?
O1_3 C1_3 C4_3 F9_3 -72.2(11) . . . . ?
C2_3 C1_3 C4_3 F9_3 44.1(9) . . . . ?
C3_3 C1_3 C4_3 F9_3 164.2(6) . . . . ?
O1_3 C1_3 C4_3 F8_3 167.8(12) . . . . ?
C2_3 C1_3 C4_3 F8_3 -75.8(11) . . . . ?
C3_3 C1_3 C4_3 F8_3 44.2(11) . . . . ?
O1 Al1 O1_4 C1_4 -81(3) . . . . ?
O2 Al1 O1_4 C1_4 36(3) . . . . ?
O1_2 Al1 O1_4 C1_4 154(3) . . . . ?
Al1 O1_4 C1_4 C3_4 -63(3) . . . . ?
Al1 O1_4 C1_4 C2_4 59(4) . . . . ?
Al1 O1_4 C1_4 C4_4 179(3) . . . . ?
O1_4 C1_4 C2_4 F1_4 76.1(14) . . . . ?
C3_4 C1_4 C2_4 F1_4 -162.2(7) . . . . ?
C4_4 C1_4 C2_4 F1_4 -42.4(11) . . . . ?
O1_4 C1_4 C2_4 F3_4 -46.1(19) . . . . ?
C3_4 C1_4 C2_4 F3_4 75.6(15) . . . . ?
C4_4 C1_4 C2_4 F3_4 -164.5(14) . . . . ?
O1_4 C1_4 C2_4 F2_4 -163.8(16) . . . . ?
C3_4 C1_4 C2_4 F2_4 -42.1(13) . . . . ?
C4_4 C1_4 C2_4 F2_4 77.7(13) . . . . ?
O1_4 C1_4 C3_4 F5_4 81.5(12) . . . . ?
C2_4 C1_4 C3_4 F5_4 -41.7(11) . . . . ?
C4_4 C1_4 C3_4 F5_4 -161.4(7) . . . . ?
O1_4 C1_4 C3_4 F6_4 -156.5(14) . . . . ?
C2_4 C1_4 C3_4 F6_4 80.2(13) . . . . ?
C4_4 C1_4 C3_4 F6_4 -39.5(14) . . . . ?
O1_4 C1_4 C3_4 F4_4 -38.5(16) . . . . ?
C2_4 C1_4 C3_4 F4_4 -161.7(12) . . . . ?
C4_4 C1_4 C3_4 F4_4 78.6(14) . . . . ?
O1_4 C1_4 C4_4 F8_4 -167.5(16) . . . . ?
C3_4 C1_4 C4_4 F8_4 74.2(14) . . . . ?
C2_4 C1_4 C4_4 F8_4 -46.3(15) . . . . ?
O1_4 C1_4 C4_4 F9_4 -46.1(16) . . . . ?
C3_4 C1_4 C4_4 F9_4 -164.3(11) . . . . ?
C2_4 C1_4 C4_4 F9_4 75.1(13) . . . . ?
O1_4 C1_4 C4_4 F7_4 72.6(13) . . . . ?
C3_4 C1_4 C4_4 F7_4 -45.6(10) . . . . ?
C2_4 C1_4 C4_4 F7_4 -166.2(7) . . . . ?

_refine_diff_density_max    0.406
_refine_diff_density_min   -0.689
_refine_diff_density_rms    0.073

_shelx_res_file
;
TITL p21c in P2(1)/c
    p21c.res
    created by SHELXL-2018/3 at 13:19:54 on 08-Aug-2019
CELL 0.71073 10.5086 20.9035 20.5072 90 94.13 90
ZERR 4 0.0003 0.0005 0.0005 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC  C  H  O  F  AL  GA
UNIT 136 96 16 144 4 4
REM Restraints for Fragment oc(cf3)3, Nonafluoro-tert-butoxy, [(CF3)3CO]-
REM from: TURBOMOLE V6.0 B-P86/def-SV(P). Please cite
REM https://doi.org/10.1107/S1600576718004508
SADI_CCF3 0.02 C1 C2 C1 C3 C1 C4
SADI_CCF3 0.02 F1 C2 F2 C2 F3 C2 F4 C3 F5 C3 F6 C3 F7 C4 F8 C4 F9 C4
SADI_CCF3 0.04 C2 C3 C3 C4 C2 C4
SADI_CCF3 0.04 O1 C2 O1 C3 O1 C4
SADI_CCF3 0.04 F1 F2 F2 F3 F3 F1 F4 F5 F5 F6 F6 F4 F7 F8 F8 F9 F9 F7
SADI_CCF3 0.02 O1 C1
SADI_CCF3 0.1 F1 C1 F2 C1 F3 C1 F4 C1 F5 C1 F6 C1 F7 C1 F8 C1 F9 C1
SIMU_CCF3 O1 > F9
RIGU_CCF3 O1 > F9
SAME_CCF3 O1 > F9
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
ACTA
CONF
L.S.  1
PLAN  20
SADI Al1 O1_*
TEMP -173.18
BOND $H
SIZE 0.11 0.10 0.99
fmap 2
SIMU 0.03 0.06 1
REM REM DSR REPLACE OC(CF3)3 WITH O1 C1 C4 ON O2 C5 C7 OCC 11 RESI CCF3
WGHT    0.049300
FVAR       0.08684   0.48166   0.55902
GA1   6    0.639513    0.561736    0.237758    11.00000    0.02411    0.02509 =
         0.02491    0.00000   -0.00158    0.00159
AL1   5    0.064281    0.260190    0.478724    11.00000    0.01606    0.01976 =
         0.01369   -0.00007   -0.00220    0.00124
O1    3    0.120467    0.336570    0.494130    11.00000    0.01593    0.02187 =
         0.02317   -0.00115   -0.00225   -0.00160
O2    3   -0.097354    0.260914    0.489317    11.00000    0.01700    0.02602 =
         0.01665   -0.00417    0.00040    0.00073
F10   4   -0.362563    0.278257    0.447769    11.00000    0.02265    0.04196 =
         0.02735    0.00097   -0.01014    0.00190
F11   4   -0.404361    0.257815    0.547038    11.00000    0.02062    0.04885 =
         0.03555   -0.00163    0.00538   -0.00228
F12   4   -0.301423    0.189571    0.492526    11.00000    0.02691    0.02714 =
         0.04239   -0.00400   -0.00180   -0.00535
F13   4   -0.175183    0.202424    0.610080    11.00000    0.04034    0.04365 =
         0.02848    0.01315    0.00120    0.00379
F14   4   -0.031518    0.275541    0.616640    11.00000    0.02288    0.05771 =
         0.02207   -0.00630   -0.00811    0.00749
F15   4   -0.222344    0.297022    0.641449    11.00000    0.03254    0.06818 =
         0.01960   -0.00712    0.00369    0.01577
F16   4   -0.313278    0.377295    0.540565    11.00000    0.02354    0.03308 =
         0.04458   -0.00660   -0.00017    0.00939
F17   4   -0.189442    0.376065    0.461252    11.00000    0.04569    0.02834 =
         0.03492    0.00598    0.00448    0.00192
F18   4   -0.110398    0.386667    0.560069    11.00000    0.02680    0.03300 =
         0.04594   -0.01528   -0.00147   -0.00436
C5    1   -0.187321    0.282851    0.527506    11.00000    0.01747    0.02239 =
         0.01764   -0.00030   -0.00196    0.00122
C6    1   -0.315963    0.251671    0.503988    11.00000    0.02202    0.02833 =
         0.02384    0.00047    0.00088    0.00067
C7    1   -0.154299    0.264421    0.600364    11.00000    0.02018    0.03755 =
         0.02243   -0.00178   -0.00027    0.00597
C8    1   -0.201069    0.356755    0.522178    11.00000    0.02168    0.02902 =
         0.02940   -0.00587    0.00039    0.00035
C1    1    0.223139    0.375179    0.503814    11.00000    0.01563    0.02218 =
         0.02106    0.00104   -0.00347   -0.00051
C2    1    0.325770    0.359140    0.456114    11.00000    0.02162    0.02860 =
         0.03030   -0.00068   -0.00039   -0.00063
F1    4    0.290695    0.379726    0.395762    11.00000    0.03938    0.04638 =
         0.02532    0.00201    0.00753   -0.00334
F2    4    0.342786    0.296339    0.451998    11.00000    0.02516    0.03092 =
         0.04945   -0.00951    0.00445    0.00466
F3    4    0.439106    0.385305    0.473513    11.00000    0.01746    0.04354 =
         0.05143   -0.00543    0.00374   -0.00641
C3    1    0.178864    0.445110    0.492597    11.00000    0.02221    0.02551 =
         0.02731    0.00163   -0.00199   -0.00088
F4    4    0.100278    0.449626    0.439084    11.00000    0.03712    0.03267 =
         0.03459    0.00784   -0.01231    0.00733
F5    4    0.116024    0.466252    0.542727    11.00000    0.03131    0.02826 =
         0.03896   -0.00874    0.00246    0.00367
F6    4    0.276147    0.485252    0.485743    11.00000    0.03304    0.02488 =
         0.04649    0.00509    0.00086   -0.00681
C4    1    0.282171    0.368632    0.575530    11.00000    0.02733    0.02969 =
         0.02610    0.00067   -0.00750   -0.00362
F7    4    0.358327    0.417827    0.593769    11.00000    0.03452    0.03947 =
         0.03403   -0.00366   -0.01521   -0.00995
F8    4    0.351892    0.315202    0.582799    11.00000    0.03636    0.03419 =
         0.04108    0.00793   -0.02040    0.00475
F9    4    0.192063    0.365523    0.617272    11.00000    0.04144    0.05384 =
         0.02015    0.00217    0.00000   -0.00931
C34   1    0.369703    0.548728    0.213201    11.00000    0.02002    0.02249 =
         0.03079   -0.00487   -0.00290    0.00113
AFIX  43
H34   2    0.340368    0.506496    0.203866    11.00000   -1.20000
AFIX   0
C33   1    0.380575    0.569536    0.277905    11.00000    0.01599    0.03244 =
         0.02433    0.00128   -0.00203    0.00415
C32   1    0.425173    0.631355    0.290545    11.00000    0.01543    0.03210 =
         0.02656   -0.00924   -0.00400    0.00558
AFIX  43
H32   2    0.435587    0.645809    0.334526    11.00000   -1.20000
AFIX   0
C35   1    0.400676    0.588144    0.161618    11.00000    0.01782    0.02848 =
         0.02229   -0.00165   -0.00583    0.00284
C30   1    0.443758    0.649851    0.176371    11.00000    0.02026    0.02429 =
         0.02614    0.00456   -0.00252    0.00409
AFIX  43
H30   2    0.466094    0.677168    0.141976    11.00000   -1.20000
AFIX   0
C36   1    0.383709    0.565133    0.092086    11.00000    0.04297    0.03599 =
         0.02259   -0.00274   -0.00392    0.00016
AFIX 137
H36A  2    0.294883    0.571492    0.075369    11.00000   -1.50000
H36B  2    0.404980    0.519546    0.090375    11.00000   -1.50000
H36C  2    0.440202    0.589360    0.065185    11.00000   -1.50000
AFIX   0
C31   1    0.454835    0.672445    0.240675    11.00000    0.01654    0.02497 =
         0.03564   -0.00430   -0.00380    0.00410
C37   1    0.341145    0.527432    0.332519    11.00000    0.02650    0.04351 =
         0.02841    0.00163    0.00199   -0.00427
AFIX 137
H37A  2    0.409049    0.526804    0.367870    11.00000   -1.50000
H37B  2    0.326063    0.483871    0.316065    11.00000   -1.50000
H37C  2    0.262663    0.544219    0.349164    11.00000   -1.50000
AFIX   0
C38   1    0.494310    0.740494    0.255563    11.00000    0.03632    0.02783 =
         0.04824   -0.00734   -0.00686   -0.00104
AFIX 137
H38A  2    0.530123    0.759372    0.217156    11.00000   -1.50000
H38B  2    0.558750    0.741073    0.292562    11.00000   -1.50000
H38C  2    0.419731    0.765295    0.266654    11.00000   -1.50000
AFIX   0

C21   1    0.721927    0.447952    0.167561    11.00000    0.02895    0.02287 =
         0.02623   -0.00352   -0.00154    0.00705
C20   1    0.838294    0.474763    0.190372    11.00000    0.02348    0.02997 =
         0.02889    0.00415    0.00468    0.00696
AFIX  43
H20   2    0.894183    0.490749    0.159808    11.00000   -1.20000
AFIX   0
C23   1    0.673450    0.429166    0.280511    11.00000    0.03008    0.01946 =
         0.02967    0.00331    0.00335    0.00508
C25   1    0.874370    0.478621    0.256918    11.00000    0.01977    0.02800 =
         0.03489    0.00295   -0.00733    0.00368
C22   1    0.641003    0.425694    0.213106    11.00000    0.02685    0.02164 =
         0.03419   -0.00071   -0.00333    0.00175
AFIX  43
H22   2    0.561275    0.407572    0.198152    11.00000   -1.20000
AFIX   0
C28   1    0.685659    0.443537    0.095305    11.00000    0.05025    0.03680 =
         0.02585   -0.00651   -0.00449    0.00286
AFIX 137
H28A  2    0.672163    0.486642    0.077326    11.00000   -1.50000
H28B  2    0.606897    0.418637    0.088035    11.00000   -1.50000
H28C  2    0.754316    0.422459    0.073534    11.00000   -1.50000
AFIX   0
C27   1    0.588442    0.401782    0.328927    11.00000    0.04255    0.04060 =
         0.03940    0.00848    0.00638   -0.00202
AFIX 137
H27A  2    0.582419    0.431842    0.365247    11.00000   -1.50000
H27B  2    0.623985    0.361147    0.345669    11.00000   -1.50000
H27C  2    0.503252    0.394423    0.307573    11.00000   -1.50000
AFIX   0
C24   1    0.790628    0.456425    0.301104    11.00000    0.03217    0.02718 =
         0.02312    0.00019   -0.00473    0.00901
AFIX  43
H24   2    0.813753    0.459894    0.346610    11.00000   -1.20000
AFIX   0
C26   1    1.002697    0.505428    0.281386    11.00000    0.02884    0.06250 =
         0.05037    0.00713   -0.01300   -0.00248
AFIX 137
H26A  2    1.045652    0.523124    0.244548    11.00000   -1.50000
H26B  2    1.055103    0.471240    0.302077    11.00000   -1.50000
H26C  2    0.990498    0.539293    0.313390    11.00000   -1.50000
AFIX   0

RESI 1 CCF3
PART 1 21
O1    3    0.158116    0.209440    0.527868    21.00000    0.02050    0.01868 =
         0.02168   -0.00158   -0.00103    0.00599
C1    1    0.198917    0.149539    0.543482    21.00000    0.01946    0.01474 =
         0.02428    0.00294   -0.00450   -0.00247
C2    1    0.283612    0.124886    0.490301    21.00000    0.04444    0.02582 =
         0.02820    0.00177   -0.00017    0.00923
F1    4    0.355607    0.074917    0.510523    21.00000    0.04680    0.02789 =
         0.02715   -0.00410   -0.00120    0.01279
F2    4    0.359474    0.170557    0.471489    21.00000    0.04020    0.03683 =
         0.04494    0.00719    0.01805    0.01211
F3    4    0.212121    0.104106    0.438134    21.00000    0.08032    0.03917 =
         0.02899   -0.01184   -0.02126    0.02445
C3    1    0.086523    0.103451    0.549644    21.00000    0.02256    0.03133 =
         0.06315    0.01391   -0.00639    0.00098
F4    4    0.116911    0.041210    0.547418    21.00000    0.03360    0.02764 =
         0.10523    0.02060   -0.00819   -0.00168
F5    4   -0.005096    0.114171    0.501983    21.00000    0.03159    0.03579 =
         0.09659    0.00890   -0.03322   -0.00876
F6    4    0.032525    0.113022    0.606778    21.00000    0.04081    0.05296 =
         0.08383    0.03214    0.03061    0.00247
C4    1    0.280511    0.152811    0.609857    21.00000    0.03674    0.02719 =
         0.02379    0.00582   -0.00734    0.00815
F7    4    0.222458    0.187887    0.652499    21.00000    0.06642    0.04760 =
         0.01612    0.00373   -0.00471    0.02228
F8    4    0.298382    0.094478    0.637285    21.00000    0.04914    0.03141 =
         0.02861    0.01155   -0.00999    0.01290
F9    4    0.394940    0.177208    0.602404    21.00000    0.02817    0.03932 =
         0.04517   -0.00403   -0.01888    0.00199
PART 0
RESI 0

RESI 2 CCF3
PART 2 -21
O1    3    0.141152    0.206954    0.532906   -21.00000    0.02154    0.02660 =
         0.01301    0.00605    0.00036    0.00536
C1    1    0.182476    0.146664    0.545905   -21.00000    0.01959    0.02444 =
         0.02081   -0.00004   -0.00354    0.00830
C2    1    0.192791    0.140574    0.621295   -21.00000    0.04239    0.02784 =
         0.02407    0.00709   -0.00750    0.00144
F1    4    0.245159    0.192794    0.649228   -21.00000    0.05192    0.03851 =
         0.03219   -0.00503   -0.01878   -0.00515
F2    4    0.263844    0.090264    0.641963   -21.00000    0.05995    0.04467 =
         0.04097    0.01619   -0.01453    0.01435
F3    4    0.078612    0.131920    0.643533   -21.00000    0.05666    0.04942 =
         0.03368    0.01037    0.01876    0.00378
C3    1    0.091502    0.094998    0.515319   -21.00000    0.02772    0.03062 =
         0.03627   -0.00034   -0.00447    0.00208
F4    4    0.107888    0.085451    0.452550   -21.00000    0.05337    0.03851 =
         0.03375   -0.01256   -0.00957    0.00632
F5    4   -0.029823    0.112021    0.519982   -21.00000    0.02255    0.04371 =
         0.06271   -0.00443   -0.00584   -0.00350
F6    4    0.109204    0.039177    0.546028   -21.00000    0.05249    0.02459 =
         0.04717   -0.00159   -0.00648   -0.00348
C4    1    0.316177    0.137057    0.519953   -21.00000    0.03160    0.02632 =
         0.04985    0.00988    0.00709    0.00422
F7    4    0.319204    0.157497    0.458120   -21.00000    0.04428    0.04449 =
         0.04363    0.01637    0.01909    0.01368
F8    4    0.354086    0.075879    0.521731   -21.00000    0.02978    0.03600 =
         0.05355    0.01144    0.00725    0.02068
F9    4    0.405829    0.168081    0.556633   -21.00000    0.02253    0.03777 =
         0.09009    0.00410   -0.00673   -0.00316
PART 0
RESI 0

RESI 3 CF3
PART 1 31
O1    3    0.088009    0.235057    0.400323    31.00000    0.01783    0.04573 =
         0.00869   -0.00148   -0.00187    0.00579
C1    1    0.036601    0.231526    0.336795    31.00000    0.01439    0.03007 =
         0.01760    0.00177   -0.00796    0.00601
C2    1    0.150456    0.233233    0.294475    31.00000    0.03966    0.04027 =
         0.01784   -0.00484   -0.00299    0.00885
F1    4    0.121813    0.211741    0.232851    31.00000    0.04217    0.05907 =
         0.01186   -0.00513    0.00126    0.00289
F2    4    0.246268    0.194482    0.319706    31.00000    0.02770    0.05345 =
         0.02902   -0.00349   -0.00330    0.01753
F3    4    0.196637    0.292061    0.290376    31.00000    0.04429    0.04775 =
         0.02860    0.00194    0.00559   -0.01265
C3    1   -0.052758    0.288678    0.318386    31.00000    0.03433    0.03997 =
         0.02019   -0.00381   -0.00608    0.01194
F4    4   -0.005252    0.342910    0.346674    31.00000    0.05005    0.02721 =
         0.02838   -0.00388   -0.01218    0.01289
F5    4   -0.067350    0.301071    0.253701    31.00000    0.04237    0.04063 =
         0.01580    0.00072   -0.00455    0.01324
F6    4   -0.169163    0.279844    0.339280    31.00000    0.02397    0.06496 =
         0.03144   -0.00006   -0.00465    0.01722
C4    1   -0.039324    0.168633    0.325780    31.00000    0.03251    0.04328 =
         0.02358   -0.00223   -0.01144   -0.00482
F7    4   -0.114204    0.158182    0.373065    31.00000    0.02874    0.05075 =
         0.02800   -0.00309    0.00085   -0.01888
F8    4   -0.112337    0.168639    0.268132    31.00000    0.05439    0.04951 =
         0.02843    0.00051   -0.02203   -0.00828
F9    4    0.041390    0.118709    0.324856    31.00000    0.05483    0.03231 =
         0.03803   -0.00747   -0.01069    0.00558
RESI 0
PART 0

REM rem dsr put oc(cf3)3 with o1 c1 c2 c3 c4 on O1_3 c1_3 q6 Q4 q7 resi ccf3 =

RESI CCF3 4
PART 2  -31
O1    3    0.075037    0.235472    0.399642   -31.00000    0.01483    0.01988 =
         0.01936   -0.00537   -0.00515    0.00401
C1    1    0.028467    0.234636    0.336927   -31.00000    0.02276    0.03631 =
         0.01088   -0.01024   -0.00014    0.00360
C2    1    0.018823    0.302575    0.307550   -31.00000    0.04584    0.04118 =
         0.01895   -0.00004   -0.00887    0.00579
F1    4    0.130216    0.325520    0.293384   -31.00000    0.06165    0.04315 =
         0.03523    0.00834   -0.00132   -0.01151
F2    4   -0.057099    0.300843    0.252783   -31.00000    0.07766    0.07178 =
         0.03090    0.00192   -0.02837    0.02572
F3    4   -0.033762    0.340595    0.350034   -31.00000    0.06341    0.04441 =
         0.03875   -0.00805   -0.01440    0.02592
C3    1   -0.103615    0.202225    0.332317   -31.00000    0.02811    0.06081 =
         0.01472   -0.00626   -0.00374   -0.00662
F4    4   -0.107376    0.152443    0.373201   -31.00000    0.05208    0.07245 =
         0.04910    0.01735   -0.01033   -0.02066
F5    4   -0.194206    0.242390    0.347085   -31.00000    0.01951    0.08324 =
         0.03137   -0.01427   -0.00645    0.00711
F6    4   -0.132273    0.178712    0.272707   -31.00000    0.03515    0.08244 =
         0.02549   -0.02100   -0.00626   -0.01881
C4    1    0.121559    0.194396    0.298133   -31.00000    0.02977    0.04522 =
         0.01581   -0.00537   -0.00066    0.01105
F7    4    0.112457    0.132062    0.311376   -31.00000    0.05692    0.03833 =
         0.03446   -0.00577    0.00171    0.01875
F8    4    0.099919    0.200371    0.233993   -31.00000    0.04332    0.07022 =
         0.01665   -0.01039    0.00323    0.01545
F9    4    0.241722    0.211230    0.314172   -31.00000    0.02020    0.06500 =
         0.02837   -0.00278    0.00498    0.01667
PART 0
RESI 0
HKLF 4




REM  p21c in P2(1)/c
REM wR2 = 0.100809, GooF = S = 1.01523, Restrained GooF = 0.94652 for all data
REM R1 = 0.039983 for 7085 Fo > 4sig(Fo) and 0.079441 for all 10786 data
REM 945 parameters refined using 1924 restraints

END

WGHT      0.0493      0.0000

REM Highest difference peak  0.406,  deepest hole -0.689,  1-sigma level  0.073
Q1    1   0.6918  0.6019  0.2176  11.00000  0.05    0.41
Q2    1   0.7506  0.5647  0.2192  11.00000  0.05    0.36
Q3    1   0.6807  0.5285  0.2072  11.00000  0.05    0.36
Q4    1   0.7401  0.4707  0.0667  11.00000  0.05    0.35
Q5    1   0.2756  0.3717  0.4871  11.00000  0.05    0.33
Q6    1   0.6860  0.3929  0.0901  11.00000  0.05    0.33
Q7    1   0.5918  0.5882  0.2737  11.00000  0.05    0.32
Q8    1   0.6394  0.4370  0.3132  11.00000  0.05    0.31
Q9    1  -0.1802  0.3161  0.5156  11.00000  0.05    0.31
Q10   1   0.1829  0.3571  0.4989  11.00000  0.05    0.31
Q11   1  -0.1286  0.2540  0.4775  11.00000  0.05    0.30
Q12   1   0.5863  0.6685  0.2340  11.00000  0.05    0.30
Q13   1   0.5938  0.5394  0.2789  11.00000  0.05    0.30
Q14   1   0.1385  0.3033  0.4745  11.00000  0.05    0.30
Q15   1  -0.1350  0.2674  0.5111  11.00000  0.05    0.29
Q16   1   0.5874  0.5160  0.2606  11.00000  0.05    0.29
Q17   1   0.3484  0.5659  0.2460  11.00000  0.05    0.29
Q18   1   0.8795  0.5410  0.3472  11.00000  0.05    0.28
Q19   1  -0.1713  0.2796  0.5595  11.00000  0.05    0.28
Q20   1   0.1928  0.4095  0.5090  11.00000  0.05    0.27
;
_shelx_res_checksum   64461