#------------------------------------------------------------------------------
#$Date$
#$Revision$
#$URL$
#------------------------------------------------------------------------------
#
# 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_1a
loop_
_publ_author_name
'Jorge J. Carb\'o'
'Pascale Crochet'
'Miguel A. Esteruelas'
'Yves Jean'
'Agust\'i Lled\'os'
'Ana M. L\'opez'
'Enrique O\~nate'
_publ_section_title
;
 Two- and Four-Electron Alkyne Ligands in Osmium-Cyclopentadienyl
 Chemistry: Consequences of the \p⊥\\rightarrow M Interaction
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              305
_journal_page_last               314
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         ?
_chemical_formula_structural
;
Os(\h^5^C~5~H~5~)Cl(\m^2^-HCC(OH)Ph~2~)(P^i^Pr~3~)
;
_chemical_formula_sum            'C29 H38 Cl O Os P'
_chemical_formula_weight         659.21
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic
; 
 ? 
;
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   13.924(2)
_cell_length_b                   17.670(2)
_cell_length_c                   22.157(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     5451.4(12)
_computing_cell_refinement       'xscans (Bruker-Siemens)'
_computing_data_collection       'xscans (Bruker-Siemens)'
_computing_data_reduction        'xscans (Bruker-Siemens)'
_computing_molecular_graphics    'xp, shelxtl v. 4.2 (Bruker-Siemens)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Siemens P4'
_diffrn_measurement_method       '\w\2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.854
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00008(5)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                3266
_reflns_number_total             4798
_reflns_threshold_expression     >2sigma(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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
Os Os 0.600695(17) 0.243230(11) 0.441106(11) 0.03868(11) Uani 1 1 d . . .
Cl Cl 0.77411(11) 0.23015(10) 0.45478(9) 0.0601(5) Uani 1 1 d . . .
P P 0.63280(12) 0.36285(9) 0.40001(9) 0.0433(4) Uani 1 1 d . . .
O O 0.7393(3) 0.2665(3) 0.5879(2) 0.0674(15) Uani 1 1 d . A .
H0 H 0.7547 0.2630 0.5523 0.101 Uiso 1 1 calc R . .
C1 C 0.5192(5) 0.3011(4) 0.5089(3) 0.0453(17) Uani 1 1 d . . .
H1 H 0.457(5) 0.314(3) 0.505(3) 0.07(2) Uiso 1 1 d . . .
C2 C 0.5890(4) 0.2750(3) 0.5351(3) 0.0401(15) Uani 1 1 d . A .
C3 C 0.6389(5) 0.2574(3) 0.5934(3) 0.0485(16) Uani 1 1 d D . .
C4 C 0.6158(5) 0.1740(3) 0.6112(3) 0.0430(16) Uani 1 1 d . A .
C5 C 0.5261(5) 0.1413(4) 0.6024(4) 0.061(2) Uani 1 1 d . . .
H5 H 0.4762 0.1704 0.5869 0.074 Uiso 1 1 calc . . .
C6 C 0.5102(6) 0.0665(4) 0.6162(4) 0.069(2) Uani 1 1 d . A .
H6 H 0.4488 0.0464 0.6123 0.083 Uiso 1 1 calc . . .
C7 C 0.5827(6) 0.0219(4) 0.6355(4) 0.068(2) Uani 1 1 d . . .
H7 H 0.5722 -0.0293 0.6426 0.082 Uiso 1 1 calc . . .
C8 C 0.6708(6) 0.0523(4) 0.6446(4) 0.073(2) Uani 1 1 d . A .
H8 H 0.7205 0.0221 0.6588 0.087 Uiso 1 1 calc . . .
C9 C 0.6876(5) 0.1285(4) 0.6328(4) 0.064(2) Uani 1 1 d . . .
H9 H 0.7483 0.1487 0.6396 0.076 Uiso 1 1 calc . . .
C10A C 0.6168(10) 0.3125(6) 0.6441(5) 0.041(5) Uiso 0.47(3) 1 d PGD A 1
C11A C 0.5203(10) 0.3267(7) 0.6553(5) 0.054(5) Uiso 0.47(3) 1 d PG A 1
C12A C 0.4940(10) 0.3798(7) 0.6985(5) 0.060(5) Uiso 0.47(3) 1 d PG A 1
C13A C 0.5642(12) 0.4188(5) 0.7305(4) 0.041(5) Uiso 0.47(3) 1 d PG A 1
C14A C 0.6608(11) 0.4045(6) 0.7193(5) 0.056(5) Uiso 0.47(3) 1 d PG A 1
C15A C 0.6871(9) 0.3514(6) 0.6761(5) 0.049(4) Uiso 0.47(3) 1 d PG A 1
C10B C 0.5889(10) 0.3121(6) 0.6422(5) 0.047(4) Uiso 0.53(3) 1 d PGD A 2
C11B C 0.4907(10) 0.3135(7) 0.6533(5) 0.076(5) Uiso 0.53(3) 1 d PG A 2
C12B C 0.4530(11) 0.3647(7) 0.6946(5) 0.079(6) Uiso 0.53(3) 1 d PG A 2
C13B C 0.5135(14) 0.4146(6) 0.7247(5) 0.070(5) Uiso 0.53(3) 1 d PG A 2
C14B C 0.6118(13) 0.4132(5) 0.7136(5) 0.060(5) Uiso 0.53(3) 1 d PG A 2
C15B C 0.6494(11) 0.3619(6) 0.6723(5) 0.067(5) Uiso 0.53(3) 1 d PG A 2
C16 C 0.6549(5) 0.4364(3) 0.4563(3) 0.0511(18) Uani 1 1 d . . .
H16 H 0.6058 0.4271 0.4871 0.061 Uiso 1 1 calc R . .
C17 C 0.7505(6) 0.4267(4) 0.4909(4) 0.074(2) Uani 1 1 d . . .
H17A H 0.8032 0.4386 0.4647 0.112 Uiso 1 1 calc R . .
H17B H 0.7563 0.3753 0.5046 0.112 Uiso 1 1 calc R . .
H17C H 0.7514 0.4601 0.5250 0.112 Uiso 1 1 calc R . .
C18 C 0.6410(6) 0.5209(4) 0.4398(4) 0.087(3) Uani 1 1 d . . .
H18A H 0.6542 0.5517 0.4746 0.131 Uiso 1 1 calc R . .
H18B H 0.5761 0.5291 0.4269 0.131 Uiso 1 1 calc R . .
H18C H 0.6843 0.5343 0.4078 0.131 Uiso 1 1 calc R . .
C19 C 0.7425(5) 0.3662(4) 0.3516(3) 0.0531(17) Uani 1 1 d . . .
H19 H 0.7969 0.3631 0.3795 0.064 Uiso 1 1 calc R . .
C20 C 0.7528(7) 0.2985(5) 0.3094(3) 0.085(3) Uani 1 1 d . . .
H20A H 0.7028 0.2999 0.2796 0.127 Uiso 1 1 calc R . .
H20B H 0.7481 0.2526 0.3323 0.127 Uiso 1 1 calc R . .
H20C H 0.8142 0.3006 0.2897 0.127 Uiso 1 1 calc R . .
C21 C 0.7565(6) 0.4396(4) 0.3167(3) 0.081(3) Uani 1 1 d . . .
H21A H 0.8132 0.4359 0.2922 0.122 Uiso 1 1 calc R . .
H21B H 0.7633 0.4809 0.3445 0.122 Uiso 1 1 calc R . .
H21C H 0.7017 0.4484 0.2913 0.122 Uiso 1 1 calc R . .
C22 C 0.5374(5) 0.4041(4) 0.3520(4) 0.068(2) Uani 1 1 d . . .
H22 H 0.5596 0.4549 0.3409 0.081 Uiso 1 1 calc R . .
C23 C 0.4441(5) 0.4158(4) 0.3895(4) 0.087(3) Uani 1 1 d . . .
H23A H 0.4000 0.4467 0.3672 0.130 Uiso 1 1 calc R . .
H23B H 0.4596 0.4402 0.4270 0.130 Uiso 1 1 calc R . .
H23C H 0.4151 0.3675 0.3976 0.130 Uiso 1 1 calc R . .
C24 C 0.5154(6) 0.3639(5) 0.2929(4) 0.089(3) Uani 1 1 d . . .
H24A H 0.4977 0.3124 0.3011 0.134 Uiso 1 1 calc R . .
H24B H 0.5712 0.3649 0.2676 0.134 Uiso 1 1 calc R . .
H24C H 0.4633 0.3892 0.2729 0.134 Uiso 1 1 calc R . .
C25 C 0.6115(6) 0.1324(4) 0.3928(4) 0.071(2) Uani 1 1 d . . .
H25 H 0.6700 0.1107 0.3823 0.085 Uiso 1 1 calc . . .
C26 C 0.5600(6) 0.1815(4) 0.3563(4) 0.066(2) Uani 1 1 d . . .
H26 H 0.5766 0.1977 0.3178 0.079 Uiso 1 1 calc . . .
C27 C 0.4778(5) 0.2018(4) 0.3890(4) 0.068(2) Uani 1 1 d . . .
H27 H 0.4301 0.2351 0.3763 0.082 Uiso 1 1 calc . . .
C28 C 0.4803(6) 0.1625(4) 0.4451(4) 0.064(2) Uani 1 1 d . . .
H28 H 0.4337 0.1650 0.4751 0.077 Uiso 1 1 calc . . .
C29 C 0.5638(7) 0.1198(4) 0.4477(4) 0.077(3) Uani 1 1 d . . .
H29 H 0.5840 0.0891 0.4793 0.093 Uiso 1 1 calc . . .
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
Os 0.03579(15) 0.03346(15) 0.04678(17) -0.00264(12) 0.00025(12) -0.00089(11)
Cl 0.0385(9) 0.0651(11) 0.0768(13) 0.0045(9) 0.0003(8) 0.0111(8)
P 0.0360(9) 0.0429(9) 0.0509(12) 0.0072(8) -0.0002(9) -0.0018(7)
O 0.048(3) 0.092(4) 0.062(3) 0.020(3) -0.013(3) -0.024(3)
C1 0.036(4) 0.048(4) 0.052(5) 0.001(3) 0.005(4) 0.000(3)
C2 0.036(4) 0.037(3) 0.047(4) 0.001(3) 0.001(3) -0.009(3)
C3 0.046(4) 0.049(4) 0.050(4) -0.001(3) -0.006(3) -0.008(3)
C4 0.044(4) 0.046(3) 0.039(4) 0.002(3) 0.003(3) 0.000(3)
C5 0.049(4) 0.063(5) 0.072(5) 0.016(4) -0.007(4) 0.000(4)
C6 0.066(5) 0.061(5) 0.081(6) 0.012(4) -0.004(5) -0.010(4)
C7 0.087(6) 0.053(4) 0.066(6) 0.012(4) 0.008(5) -0.006(4)
C8 0.075(6) 0.058(5) 0.085(6) 0.018(4) 0.007(5) 0.029(4)
C9 0.055(5) 0.065(5) 0.071(5) -0.002(4) -0.005(4) 0.001(4)
C16 0.049(4) 0.042(4) 0.062(5) 0.009(3) 0.006(4) -0.009(3)
C17 0.089(6) 0.060(5) 0.074(6) -0.015(4) -0.015(5) -0.014(5)
C18 0.102(7) 0.045(4) 0.114(8) 0.013(5) 0.008(6) -0.005(4)
C19 0.046(4) 0.064(4) 0.049(4) 0.006(4) 0.009(4) -0.001(4)
C20 0.084(6) 0.096(6) 0.074(6) 0.004(5) 0.030(5) 0.005(5)
C21 0.081(6) 0.088(6) 0.075(6) 0.025(5) 0.017(5) -0.015(5)
C22 0.044(4) 0.071(5) 0.088(6) 0.036(5) -0.020(4) -0.007(4)
C23 0.040(5) 0.094(6) 0.126(9) 0.044(6) -0.010(5) 0.011(4)
C24 0.084(7) 0.102(7) 0.082(6) 0.027(6) -0.041(5) -0.012(5)
C25 0.067(6) 0.044(4) 0.102(7) -0.034(4) -0.004(5) 0.001(4)
C26 0.078(6) 0.058(5) 0.062(5) -0.027(4) 0.000(5) -0.007(4)
C27 0.053(5) 0.060(5) 0.091(7) -0.022(5) -0.014(5) -0.013(4)
C28 0.068(5) 0.053(4) 0.071(6) -0.007(4) 0.003(5) -0.026(4)
C29 0.103(7) 0.040(4) 0.089(7) -0.002(4) -0.004(6) -0.005(4)
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'
P P 0.1023 0.0942 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 Os C2 33.0(2) . . ?
C1 Os C27 96.6(3) . . ?
C2 Os C27 122.4(3) . . ?
C1 Os C28 83.0(3) . . ?
C2 Os C28 94.1(3) . . ?
C27 Os C28 37.9(3) . . ?
C1 Os C25 142.1(3) . . ?
C2 Os C25 133.9(3) . . ?
C27 Os C25 60.5(3) . . ?
C28 Os C25 60.2(3) . . ?
C1 Os C26 133.2(3) . . ?
C2 Os C26 155.9(3) . . ?
C27 Os C26 36.8(3) . . ?
C28 Os C26 61.8(3) . . ?
C25 Os C26 36.0(3) . . ?
C1 Os C29 107.3(3) . . ?
C2 Os C29 99.9(3) . . ?
C27 Os C29 62.0(3) . . ?
C28 Os C29 36.3(3) . . ?
C25 Os C29 36.5(3) . . ?
C26 Os C29 61.6(3) . . ?
C1 Os P 86.73(18) . . ?
C2 Os P 98.89(16) . . ?
C27 Os P 104.2(2) . . ?
C28 Os P 138.1(2) . . ?
C25 Os P 126.2(3) . . ?
C26 Os P 99.3(2) . . ?
C29 Os P 160.8(2) . . ?
C1 Os Cl 118.8(2) . . ?
C2 Os Cl 88.82(17) . . ?
C27 Os Cl 143.7(2) . . ?
C28 Os Cl 133.3(2) . . ?
C25 Os Cl 84.8(2) . . ?
C26 Os Cl 107.9(2) . . ?
C29 Os Cl 97.3(3) . . ?
P Os Cl 86.85(6) . . ?
C16 P C22 103.5(3) . . ?
C16 P C19 103.4(3) . . ?
C22 P C19 104.1(3) . . ?
C16 P Os 114.1(2) . . ?
C22 P Os 116.2(2) . . ?
C19 P Os 114.1(2) . . ?
C3 O H0 109.5 . . ?
C2 C1 Os 74.4(4) . . ?
C2 C1 H1 154(5) . . ?
Os C1 H1 125(5) . . ?
C1 C2 C3 148.8(7) . . ?
C1 C2 Os 72.6(5) . . ?
C3 C2 Os 137.8(5) . . ?
O C3 C2 111.2(6) . . ?
O C3 C10A 101.0(7) . . ?
C2 C3 C10A 114.2(7) . . ?
O C3 C4 109.5(5) . . ?
C2 C3 C4 108.6(5) . . ?
C10A C3 C4 112.1(7) . . ?
O C3 C10B 114.7(7) . . ?
C2 C3 C10B 104.7(7) . . ?
C10A C3 C10B 14.0(6) . . ?
C4 C3 C10B 107.9(6) . . ?
C9 C4 C5 117.4(6) . . ?
C9 C4 C3 119.5(6) . . ?
C5 C4 C3 122.9(6) . . ?
C6 C5 C4 120.8(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C7 C6 C5 120.8(7) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 119.5(7) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C7 C8 C9 120.6(7) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C4 C9 C8 120.8(7) . . ?
C4 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11A C10A C15A 120.0 . . ?
C11A C10A C3 116.4(7) . . ?
C15A C10A C3 123.5(7) . . ?
C12A C11A C10A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C12A C13A C14A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C14A C15A C10A 120.0 . . ?
C11B C10B C15B 120.0 . . ?
C11B C10B C3 123.8(7) . . ?
C15B C10B C3 116.2(7) . . ?
C12B C11B C10B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C12B C13B C14B 120.0 . . ?
C13B C14B C15B 120.0 . . ?
C14B C15B C10B 120.0 . . ?
C18 C16 C17 109.4(6) . . ?
C18 C16 P 120.2(5) . . ?
C17 C16 P 113.9(5) . . ?
C18 C16 H16 103.8 . . ?
C17 C16 H16 103.8 . . ?
P C16 H16 103.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C20 110.1(6) . . ?
C21 C19 P 115.1(5) . . ?
C20 C19 P 113.9(5) . . ?
C21 C19 H19 105.6 . . ?
C20 C19 H19 105.6 . . ?
P C19 H19 105.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C23 110.7(7) . . ?
C24 C22 P 117.1(6) . . ?
C23 C22 P 110.1(5) . . ?
C24 C22 H22 106.1 . . ?
C23 C22 H22 106.1 . . ?
P C22 H22 106.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C29 111.1(7) . . ?
C26 C25 Os 72.3(4) . . ?
C29 C25 Os 72.1(4) . . ?
C26 C25 H25 124.5 . . ?
C29 C25 H25 124.5 . . ?
Os C25 H25 122.7 . . ?
C25 C26 C27 106.4(8) . . ?
C25 C26 Os 71.7(4) . . ?
C27 C26 Os 69.4(4) . . ?
C25 C26 H26 126.8 . . ?
C27 C26 H26 126.8 . . ?
Os C26 H26 123.8 . . ?
C26 C27 C28 107.8(7) . . ?
C26 C27 Os 73.8(4) . . ?
C28 C27 Os 71.6(4) . . ?
C26 C27 H27 126.1 . . ?
C28 C27 H27 126.1 . . ?
Os C27 H27 120.4 . . ?
C29 C28 C27 108.8(7) . . ?
C29 C28 Os 73.5(4) . . ?
C27 C28 Os 70.6(4) . . ?
C29 C28 H28 125.6 . . ?
C27 C28 H28 125.6 . . ?
Os C28 H28 121.9 . . ?
C28 C29 C25 106.0(8) . . ?
C28 C29 Os 70.2(4) . . ?
C25 C29 Os 71.4(4) . . ?
C28 C29 H29 127.0 . . ?
C25 C29 H29 127.0 . . ?
Os C29 H29 123.1 . . ?
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
Os C1 2.142(7) . ?
Os C2 2.163(6) . ?
Os C27 2.190(7) . ?
Os C28 2.203(7) . ?
Os C25 2.237(6) . ?
Os C26 2.246(7) . ?
Os C29 2.246(7) . ?
Os P 2.3444(17) . ?
Os Cl 2.4445(16) . ?
P C16 1.827(7) . ?
P C22 1.852(7) . ?
P C19 1.866(7) . ?
O C3 1.411(7) . ?
O H0 0.8200 . ?
C1 C2 1.222(8) . ?
C1 H1 0.89(6) . ?
C2 C3 1.499(9) . ?
C3 C10A 1.519(9) . ?
C3 C4 1.558(8) . ?
C3 C10B 1.609(9) . ?
C4 C9 1.369(9) . ?
C4 C5 1.390(9) . ?
C5 C6 1.375(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.350(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.354(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10A C11A 1.3900 . ?
C10A C15A 1.3900 . ?
C11A C12A 1.3900 . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C14A C15A 1.3900 . ?
C10B C11B 1.3900 . ?
C10B C15B 1.3900 . ?
C11B C12B 1.3900 . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C14B C15B 1.3900 . ?
C16 C18 1.550(8) . ?
C16 C17 1.546(9) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C21 1.524(8) . ?
C19 C20 1.525(9) . ?
C19 H19 0.9800 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C24 1.519(10) . ?
C22 C23 1.556(10) . ?
C22 H22 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.386(11) . ?
C25 C29 1.404(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.401(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.425(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.387(11) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
#------------------------------------------------------------------------------
#$Date$
#$Revision$
#$URL$
#------------------------------------------------------------------------------
#
# 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_2a
loop_
_publ_author_name
'Jorge J. Carb\'o'
'Pascale Crochet'
'Miguel A. Esteruelas'
'Yves Jean'
'Agust\'i Lled\'os'
'Ana M. L\'opez'
'Enrique O\~nate'
_publ_section_title
;
 Two- and Four-Electron Alkyne Ligands in Osmium-Cyclopentadienyl
 Chemistry: Consequences of the \p⊥\\rightarrow M Interaction
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              305
_journal_page_last               314
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         ?
_chemical_formula_structural
;
[Os(\h^5^C~5~H~5~)(\m^2^-HCC(OH)Ph~2~)(P^i^Pr~3~)]PF~6~
;
_chemical_formula_sum            'C29 H38 F6 O Os P2'
_chemical_formula_weight         768.73
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic
; 
 ? 
;
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21
_atom_sites_solution_hydrogens   geom
_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                   16.842(2)
_cell_length_b                   9.0770(10)
_cell_length_c                   19.643(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     3002.9(6)
_computing_cell_refinement       'xscans (Bruker-Siemens)'
_computing_data_collection       'xscans (Bruker-Siemens)'
_computing_data_reduction        'xscans (Bruker-Siemens)'
_computing_molecular_graphics    'xp, shelxtl v. 4.2 (Bruker-Siemens)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Siemens P4'
_diffrn_measurement_method       '\w\2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7844
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.426(10)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.318
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+5.0382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                4447
_reflns_number_total             5282
_reflns_threshold_expression     >2sigma(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
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
Os Os 0.911799(14) 0.92111(3) 1.00031(4) 0.03311(8) Uani 1 1 d . . .
P1 P 0.94480(12) 0.8203(2) 0.89041(10) 0.0329(5) Uani 1 1 d . . .
P2 P 0.72242(16) 0.3237(3) 0.87980(14) 0.0523(6) Uani 1 1 d . . .
F1A F 0.6319(10) 0.2965(19) 0.8831(10) 0.097(5) Uiso 0.493(4) 1 d P A 1
F2A F 0.7023(13) 0.449(3) 0.9294(13) 0.131(8) Uiso 0.493(4) 1 d P A 1
F3A F 0.7378(11) 0.198(2) 0.9312(10) 0.124(6) Uiso 0.493(4) 1 d P A 1
F4A F 0.7432(10) 0.215(2) 0.8180(9) 0.107(5) Uiso 0.493(4) 1 d P A 1
F5A F 0.7141(10) 0.4403(19) 0.8167(9) 0.100(5) Uiso 0.493(4) 1 d P A 1
F6A F 0.8157(10) 0.345(2) 0.8809(10) 0.096(6) Uiso 0.493(4) 1 d P A 1
F1B F 0.6345(9) 0.2989(16) 0.8477(8) 0.079(4) Uiso 0.507(4) 1 d P A 2
F2B F 0.7046(13) 0.496(3) 0.8966(12) 0.126(7) Uiso 0.507(4) 1 d P A 2
F3B F 0.7377(11) 0.160(2) 0.8578(11) 0.127(6) Uiso 0.507(4) 1 d P A 2
F4B F 0.6934(10) 0.277(2) 0.9538(8) 0.111(5) Uiso 0.507(4) 1 d P A 2
F5B F 0.7497(12) 0.366(2) 0.8067(9) 0.121(6) Uiso 0.507(4) 1 d P A 2
F6B F 0.8045(11) 0.360(2) 0.9113(10) 0.099(6) Uiso 0.507(4) 1 d P A 2
O O 0.8302(4) 0.8873(8) 1.1730(3) 0.0531(19) Uani 1 1 d . B .
H2 H 0.794(5) 0.901(10) 1.204(5) 0.04(3) Uiso 1 1 d . . .
C1 C 0.8358(5) 0.7531(10) 0.9983(11) 0.0496(18) Uani 1 1 d . . .
H1 H 0.824(4) 0.662(8) 0.973(3) 0.02(2) Uiso 1 1 d . . .
C2 C 0.8307(5) 0.8165(10) 1.0551(4) 0.041(2) Uani 1 1 d . B .
C3 C 0.7874(6) 0.8030(10) 1.1223(4) 0.042(2) Uani 1 1 d D . .
C4 C 0.7027(5) 0.8720(9) 1.1161(4) 0.039(2) Uani 1 1 d . B .
C5 C 0.6877(6) 0.9880(11) 1.0763(5) 0.048(2) Uani 1 1 d . . .
H5 H 0.7279 1.0260 1.0490 0.057 Uiso 1 1 calc R B .
C6 C 0.6138(7) 1.0522(11) 1.0751(5) 0.059(3) Uani 1 1 d . B .
H6 H 0.6046 1.1325 1.0468 0.070 Uiso 1 1 calc R . .
C7 C 0.5539(7) 0.9996(13) 1.1149(6) 0.067(3) Uani 1 1 d . . .
H7 H 0.5040 1.0434 1.1141 0.080 Uiso 1 1 calc R B .
C8 C 0.5686(6) 0.8814(13) 1.1562(6) 0.069(3) Uani 1 1 d . B .
H8 H 0.5279 0.8447 1.1833 0.083 Uiso 1 1 calc R . .
C9 C 0.6417(6) 0.8157(12) 1.1585(5) 0.056(3) Uani 1 1 d . . .
H9 H 0.6511 0.7362 1.1872 0.067 Uiso 1 1 calc R B .
C10A C 0.7889(8) 0.6431(7) 1.1466(7) 0.032(4) Uiso 0.526(4) 1 d PGD B 3
C11A C 0.7442(7) 0.5412(12) 1.1104(7) 0.050(5) Uiso 0.526(4) 1 d PG B 3
C12A C 0.7534(8) 0.3914(10) 1.1229(8) 0.065(6) Uiso 0.526(4) 1 d PG B 3
C13A C 0.8073(8) 0.3436(7) 1.1717(7) 0.042(4) Uiso 0.526(4) 1 d PG B 3
C14A C 0.8521(8) 0.4455(13) 1.2080(6) 0.074(7) Uiso 0.526(4) 1 d PG B 3
C15A C 0.8429(9) 0.5953(11) 1.1954(7) 0.059(6) Uiso 0.526(4) 1 d PG B 3
C10B C 0.7877(8) 0.6353(6) 1.1298(4) 0.035(6) Uiso 0.474(4) 1 d PGD B 4
C11B C 0.8301(8) 0.5731(12) 1.1833(4) 0.051(6) Uiso 0.474(4) 1 d PG B 4
C12B C 0.8243(8) 0.4229(12) 1.1961(5) 0.054(5) Uiso 0.474(4) 1 d PG B 4
C13B C 0.7761(11) 0.3349(6) 1.1555(5) 0.052(5) Uiso 0.474(4) 1 d PG B 4
C14B C 0.7338(9) 0.3971(12) 1.1019(5) 0.097(11) Uiso 0.474(4) 1 d PG B 4
C15B C 0.7396(5) 0.5473(11) 1.0891(4) 0.047(5) Uiso 0.474(4) 1 d PG B 4
C16 C 0.8595(5) 0.7397(11) 0.8434(3) 0.050(2) Uani 1 1 d G . .
H16 H 0.8440 0.6538 0.8705 0.060 Uiso 1 1 calc R . .
C17 C 0.7870(6) 0.8324(15) 0.8408(5) 0.060(3) Uani 1 1 d . . .
H17A H 0.7444 0.7773 0.8206 0.091 Uiso 1 1 calc R . .
H17B H 0.7972 0.9188 0.8141 0.091 Uiso 1 1 calc R . .
H17C H 0.7723 0.8609 0.8862 0.091 Uiso 1 1 calc R . .
C18 C 0.8799(6) 0.6754(13) 0.7724(4) 0.061(3) Uani 1 1 d . . .
H18A H 0.8870 0.7544 0.7405 0.092 Uiso 1 1 calc R . .
H18B H 0.8373 0.6130 0.7574 0.092 Uiso 1 1 calc R . .
H18C H 0.9279 0.6189 0.7754 0.092 Uiso 1 1 calc R . .
C19 C 0.9943(6) 0.9556(10) 0.8343(4) 0.046(2) Uani 1 1 d . . .
H19 H 1.0298 1.0124 0.8639 0.055 Uiso 1 1 calc R . .
C20 C 0.9365(7) 1.0679(12) 0.8038(6) 0.067(3) Uani 1 1 d . . .
H20A H 0.9046 1.0210 0.7696 0.101 Uiso 1 1 calc R . .
H20B H 0.9659 1.1474 0.7836 0.101 Uiso 1 1 calc R . .
H20C H 0.9027 1.1059 0.8390 0.101 Uiso 1 1 calc R . .
C21 C 1.0488(7) 0.8892(14) 0.7773(5) 0.075(4) Uani 1 1 d . . .
H21A H 1.0758 0.9675 0.7540 0.113 Uiso 1 1 calc R . .
H21B H 1.0168 0.8352 0.7455 0.113 Uiso 1 1 calc R . .
H21C H 1.0871 0.8243 0.7975 0.113 Uiso 1 1 calc R . .
C22 C 1.0162(6) 0.6685(10) 0.8970(6) 0.054(2) Uani 1 1 d . . .
H22 H 1.0328 0.6438 0.8506 0.064 Uiso 1 1 calc R . .
C23 C 0.9811(7) 0.5275(12) 0.9286(7) 0.076(4) Uani 1 1 d . . .
H23A H 0.9506 0.5527 0.9682 0.115 Uiso 1 1 calc R . .
H23B H 1.0234 0.4621 0.9413 0.115 Uiso 1 1 calc R . .
H23C H 0.9474 0.4797 0.8960 0.115 Uiso 1 1 calc R . .
C24 C 1.0910(5) 0.7119(12) 0.9362(6) 0.066(3) Uani 1 1 d . . .
H24A H 1.1289 0.6332 0.9339 0.098 Uiso 1 1 calc R . .
H24B H 1.0776 0.7305 0.9830 0.098 Uiso 1 1 calc R . .
H24C H 1.1134 0.7992 0.9165 0.098 Uiso 1 1 calc R . .
C25 C 1.0242(5) 1.0493(10) 1.0019(11) 0.066(3) Uani 1 1 d . . .
H25 H 1.0703 1.0182 0.9801 0.080 Uiso 1 1 calc R . .
C26 C 0.9651(6) 1.1377(10) 0.9745(5) 0.052(3) Uani 1 1 d . . .
H26 H 0.9649 1.1784 0.9310 0.062 Uiso 1 1 calc R . .
C27 C 0.9051(7) 1.1552(12) 1.0244(5) 0.065(3) Uani 1 1 d . . .
H27 H 0.8576 1.2061 1.0190 0.077 Uiso 1 1 calc R . .
C28 C 0.9296(6) 1.0833(11) 1.0825(5) 0.057(3) Uani 1 1 d . . .
H28 H 0.9021 1.0818 1.1235 0.069 Uiso 1 1 calc R . .
C29 C 1.0003(7) 1.0148(12) 1.0708(6) 0.063(3) Uani 1 1 d . . .
H29 H 1.0282 0.9564 1.1016 0.076 Uiso 1 1 calc R . .
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
Os 0.03532(13) 0.03676(14) 0.02726(12) -0.0001(3) 0.0029(3) -0.00526(13)
P1 0.0361(11) 0.0336(11) 0.0290(10) 0.0008(9) 0.0063(9) 0.0003(10)
P2 0.0496(15) 0.0577(17) 0.0495(14) -0.0029(13) -0.0010(12) 0.0104(14)
O 0.056(4) 0.070(5) 0.033(3) -0.005(3) 0.006(3) -0.020(4)
C1 0.063(5) 0.053(4) 0.033(4) -0.002(7) 0.019(7) -0.017(4)
C2 0.049(5) 0.047(5) 0.028(4) 0.006(4) 0.003(4) -0.015(4)
C3 0.053(6) 0.055(6) 0.018(4) -0.007(4) -0.002(4) -0.007(5)
C4 0.049(5) 0.034(5) 0.033(4) -0.005(4) 0.002(4) -0.009(4)
C5 0.054(6) 0.045(6) 0.044(5) 0.009(5) -0.004(4) -0.014(5)
C6 0.070(7) 0.052(7) 0.054(6) 0.004(5) -0.007(5) 0.010(5)
C7 0.058(7) 0.072(8) 0.071(7) -0.007(7) 0.006(6) 0.002(6)
C8 0.054(7) 0.075(8) 0.078(7) 0.002(6) 0.025(5) -0.002(6)
C9 0.049(6) 0.063(7) 0.055(5) 0.005(5) 0.013(5) 0.004(5)
C16 0.050(5) 0.065(7) 0.034(4) -0.009(5) 0.005(4) -0.019(5)
C17 0.039(6) 0.090(9) 0.052(7) -0.010(7) -0.013(5) 0.003(6)
C18 0.076(7) 0.072(7) 0.036(5) -0.018(5) 0.000(5) -0.011(6)
C19 0.055(5) 0.044(6) 0.039(5) 0.009(4) 0.013(4) -0.004(5)
C20 0.079(7) 0.055(7) 0.068(7) 0.024(6) 0.002(6) 0.004(6)
C21 0.084(8) 0.096(10) 0.046(6) 0.007(6) 0.037(6) -0.005(7)
C22 0.058(6) 0.035(5) 0.067(6) 0.000(5) -0.003(5) 0.006(5)
C23 0.067(7) 0.045(7) 0.116(10) 0.006(7) -0.003(7) 0.009(6)
C24 0.036(5) 0.060(7) 0.101(8) 0.014(6) 0.013(5) 0.016(5)
C25 0.045(4) 0.072(6) 0.083(6) -0.027(12) 0.025(10) -0.027(4)
C26 0.070(7) 0.035(5) 0.050(5) 0.004(4) 0.005(5) -0.021(5)
C27 0.072(7) 0.046(6) 0.075(8) -0.006(5) 0.012(6) -0.001(6)
C28 0.068(7) 0.063(7) 0.041(5) -0.011(5) 0.004(4) -0.028(6)
C29 0.071(7) 0.054(7) 0.065(7) 0.006(6) -0.032(6) -0.019(6)
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'
F F 0.0171 0.0103 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 Os C1 36.9(6) . . ?
C2 Os C27 108.2(4) . . ?
C1 Os C27 135.8(4) . . ?
C2 Os C28 90.9(4) . . ?
C1 Os C28 127.8(6) . . ?
C27 Os C28 36.6(4) . . ?
C2 Os C29 108.1(4) . . ?
C1 Os C29 137.9(6) . . ?
C27 Os C29 61.5(4) . . ?
C28 Os C29 36.0(4) . . ?
C2 Os C26 145.8(4) . . ?
C1 Os C26 159.0(6) . . ?
C27 Os C26 37.6(3) . . ?
C28 Os C26 61.4(4) . . ?
C29 Os C26 61.9(4) . . ?
C2 Os C25 146.2(6) . . ?
C1 Os C25 161.6(4) . . ?
C27 Os C25 62.0(4) . . ?
C28 Os C25 61.6(5) . . ?
C29 Os C25 38.1(6) . . ?
C26 Os C25 36.4(4) . . ?
C2 Os P1 117.6(3) . . ?
C1 Os P1 80.8(5) . . ?
C27 Os P1 125.2(3) . . ?
C28 Os P1 151.4(3) . . ?
C29 Os P1 123.6(3) . . ?
C26 Os P1 92.2(3) . . ?
C25 Os P1 90.9(5) . . ?
C22 P1 C19 104.2(4) . . ?
C22 P1 C16 104.3(5) . . ?
C19 P1 C16 108.3(4) . . ?
C22 P1 Os 111.9(4) . . ?
C19 P1 Os 112.7(3) . . ?
C16 P1 Os 114.6(3) . . ?
F2A P2 F1A 82.8(11) . . ?
F2A P2 F3A 99.8(12) . . ?
F1A P2 F3A 91.1(10) . . ?
F2A P2 F6B 77.6(11) . . ?
F1A P2 F6B 153.8(10) . . ?
F3A P2 F6B 75.5(9) . . ?
F2A P2 F5B 117.9(13) . . ?
F1A P2 F5B 111.7(10) . . ?
F3A P2 F5B 137.3(11) . . ?
F6B P2 F5B 93.0(10) . . ?
F2A P2 F3B 155.8(13) . . ?
F1A P2 F3B 91.2(10) . . ?
F3A P2 F3B 56.8(9) . . ?
F6B P2 F3B 99.6(10) . . ?
F5B P2 F3B 86.1(10) . . ?
F2A P2 F6A 96.9(11) . . ?
F1A P2 F6A 176.1(10) . . ?
F3A P2 F6A 85.1(10) . . ?
F6B P2 F6A 23.6(8) . . ?
F5B P2 F6A 71.9(10) . . ?
F3B P2 F6A 87.5(10) . . ?
F2A P2 F4B 63.1(11) . . ?
F1A P2 F4B 67.4(9) . . ?
F3A P2 F4B 42.2(8) . . ?
F6B P2 F4B 88.1(9) . . ?
F5B P2 F4B 178.6(10) . . ?
F3B P2 F4B 92.9(10) . . ?
F6A P2 F4B 108.9(9) . . ?
F2A P2 F4A 170.0(12) . . ?
F1A P2 F4A 98.5(10) . . ?
F3A P2 F4A 90.1(10) . . ?
F6B P2 F4A 103.9(10) . . ?
F5B P2 F4A 52.3(9) . . ?
F3B P2 F4A 34.2(8) . . ?
F6A P2 F4A 82.5(10) . . ?
F4B P2 F4A 126.6(10) . . ?
F2A P2 F2B 28.1(10) . . ?
F1A P2 F2B 87.9(10) . . ?
F3A P2 F2B 127.5(11) . . ?
F6B P2 F2B 83.0(10) . . ?
F5B P2 F2B 90.3(12) . . ?
F3B P2 F2B 175.6(12) . . ?
F6A P2 F2B 93.7(11) . . ?
F4B P2 F2B 90.7(11) . . ?
F4A P2 F2B 141.8(11) . . ?
F2A P2 F1B 98.5(10) . . ?
F1A P2 F1B 25.3(7) . . ?
F3A P2 F1B 107.6(9) . . ?
F6B P2 F1B 175.5(9) . . ?
F5B P2 F1B 86.8(9) . . ?
F3B P2 F1B 84.9(9) . . ?
F6A P2 F1B 157.9(9) . . ?
F4B P2 F1B 92.2(8) . . ?
F4A P2 F1B 79.6(8) . . ?
F2B P2 F1B 92.5(9) . . ?
F2A P2 F5A 89.0(11) . . ?
F1A P2 F5A 92.9(9) . . ?
F3A P2 F5A 170.7(10) . . ?
F6B P2 F5A 103.8(9) . . ?
F5B P2 F5A 33.5(8) . . ?
F3B P2 F5A 114.7(10) . . ?
F6A P2 F5A 91.0(9) . . ?
F4B P2 F5A 146.9(9) . . ?
F4A P2 F5A 81.0(9) . . ?
F2B P2 F5A 61.1(10) . . ?
F1B P2 F5A 73.6(8) . . ?
C3 O H2 102(6) . . ?
C2 C1 Os 71.1(6) . . ?
C2 C1 H1 145(4) . . ?
Os C1 H1 141(4) . . ?
C1 C2 C3 140.3(9) . . ?
C1 C2 Os 72.0(5) . . ?
C3 C2 Os 147.6(7) . . ?
O C3 C2 108.6(7) . . ?
O C3 C10A 106.2(8) . . ?
C2 C3 C10A 110.0(9) . . ?
O C3 C10B 117.3(8) . . ?
C2 C3 C10B 99.4(7) . . ?
C10A C3 C10B 12.8(6) . . ?
O C3 C4 107.2(7) . . ?
C2 C3 C4 109.8(7) . . ?
C10A C3 C4 114.8(8) . . ?
C10B C3 C4 114.1(9) . . ?
C5 C4 C9 119.3(9) . . ?
C5 C4 C3 122.3(8) . . ?
C9 C4 C3 118.1(8) . . ?
C4 C5 C6 121.1(9) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 120.8(10) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C6 118.7(11) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 121.7(10) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C4 118.4(10) . . ?
C8 C9 H9 120.8 . . ?
C4 C9 H9 120.8 . . ?
C11A C10A C15A 120.0 . . ?
C11A C10A C3 117.6(9) . . ?
C15A C10A C3 121.5(9) . . ?
C12A C11A C10A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C14A C15A C10A 120.0 . . ?
C11B C10B C15B 120.0 . . ?
C11B C10B C3 118.6(8) . . ?
C15B C10B C3 121.0(9) . . ?
C10B C11B C12B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C12B C13B C14B 120.0 . . ?
C15B C14B C13B 120.0 . . ?
C14B C15B C10B 120.0 . . ?
C17 C16 C18 111.4(7) . . ?
C17 C16 P1 115.4(8) . . ?
C18 C16 P1 115.2(6) . . ?
C17 C16 H16 104.4 . . ?
C18 C16 H16 104.4 . . ?
P1 C16 H16 104.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C21 110.4(8) . . ?
C20 C19 P1 112.9(7) . . ?
C21 C19 P1 115.8(7) . . ?
C20 C19 H19 105.6 . . ?
C21 C19 H19 105.6 . . ?
P1 C19 H19 105.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C23 109.1(9) . . ?
C24 C22 P1 112.5(7) . . ?
C23 C22 P1 113.7(7) . . ?
C24 C22 H22 107.1 . . ?
C23 C22 H22 107.1 . . ?
P1 C22 H22 107.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C29 106.8(10) . . ?
C26 C25 Os 71.7(5) . . ?
C29 C25 Os 70.3(5) . . ?
C26 C25 H25 126.6 . . ?
C29 C25 H25 126.6 . . ?
Os C25 H25 123.0 . . ?
C25 C26 C27 107.9(10) . . ?
C25 C26 Os 71.9(5) . . ?
C27 C26 Os 69.7(6) . . ?
C25 C26 H26 126.0 . . ?
C27 C26 H26 126.0 . . ?
Os C26 H26 124.0 . . ?
C28 C27 C26 107.8(10) . . ?
C28 C27 Os 72.7(6) . . ?
C26 C27 Os 72.7(6) . . ?
C28 C27 H27 126.1 . . ?
C26 C27 H27 126.1 . . ?
Os C27 H27 120.3 . . ?
C29 C28 C27 109.9(10) . . ?
C29 C28 Os 72.0(6) . . ?
C27 C28 Os 70.7(6) . . ?
C29 C28 H28 125.1 . . ?
C27 C28 H28 125.1 . . ?
Os C28 H28 123.8 . . ?
C28 C29 C25 107.5(9) . . ?
C28 C29 Os 72.0(6) . . ?
C25 C29 Os 71.5(6) . . ?
C28 C29 H29 126.2 . . ?
C25 C29 H29 126.2 . . ?
Os C29 H29 121.9 . . ?
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
Os C2 1.981(8) . ?
Os C1 1.992(9) . ?
Os C27 2.180(11) . ?
Os C28 2.205(9) . ?
Os C29 2.205(10) . ?
Os C26 2.220(9) . ?
Os C25 2.222(7) . ?
Os P1 2.410(2) . ?
P1 C22 1.833(9) . ?
P1 C19 1.849(8) . ?
P1 C16 1.858(9) . ?
P2 F2A 1.54(2) . ?
P2 F1A 1.546(17) . ?
P2 F3A 1.547(19) . ?
P2 F6B 1.551(18) . ?
P2 F5B 1.555(19) . ?
P2 F3B 1.57(2) . ?
P2 F6A 1.583(18) . ?
P2 F4B 1.590(17) . ?
P2 F4A 1.604(17) . ?
P2 F2B 1.63(2) . ?
P2 F1B 1.625(15) . ?
P2 F5A 1.636(17) . ?
O C3 1.448(10) . ?
O H2 0.86(9) . ?
C1 C2 1.26(2) . ?
C1 H1 0.98(7) . ?
C2 C3 1.513(11) . ?
C3 C10A 1.528(10) . ?
C3 C10B 1.530(10) . ?
C3 C4 1.563(13) . ?
C4 C5 1.336(12) . ?
C4 C9 1.419(12) . ?
C5 C6 1.374(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.363(15) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(15) . ?
C7 H7 0.9300 . ?
C8 C9 1.368(14) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10A C11A 1.3900 . ?
C10A C15A 1.3900 . ?
C11A C12A 1.3900 . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C14A C15A 1.3900 . ?
C10B C11B 1.3900 . ?
C10B C15B 1.3900 . ?
C11B C12B 1.3900 . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C14B C15B 1.3900 . ?
C16 C17 1.484(14) . ?
C16 C18 1.549(11) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.532(13) . ?
C19 C21 1.568(12) . ?
C19 H19 0.9800 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C24 1.528(13) . ?
C22 C23 1.541(14) . ?
C22 H22 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.387(15) . ?
C25 C29 1.45(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.418(13) . ?
C26 H26 0.9300 . ?
C27 C28 1.377(14) . ?
C27 H27 0.9300 . ?
C28 C29 1.363(15) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?