1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
131
132
133
134
135
136
137
138
139
140
141
142
143
144
145
146
147
148
149
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
171
172
173
174
175
176
177
|
data_RAMM013_publ
_journal_coeditor_code VN2124
_journal_date_accepted 2017-01-04
_journal_date_recd_electronic 2017-01-02
_journal_issue 2
_journal_name_full 'Acta Crystallographica, Section E'
_journal_page_first 133
_journal_page_last 136
_journal_paper_category GI
_journal_paper_doi 10.1107/S2056989017000135
_journal_volume 73
_journal_year 2017
_chemical_formula_analytical 'C6 H7 Cs O7'
_chemical_formula_iupac 'Cs +, C6 H7 O7 -'
_chemical_formula_moiety 'Cs +, C6 H7 O7 -'
_chemical_formula_structural 'Cs H2 C6 H5 O7'
_chemical_formula_sum 'C6 H7 Cs O7'
_chemical_formula_weight 323.97
_chemical_name_common 'cesium dihydrogen citrate'
_chemical_name_systematic 'cesium dihydrogen citrate'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_audit_creation_method 'from EXP file using GSAS2CIF'
_cell_angle_alpha 90.0
_cell_angle_beta 90.0
_cell_angle_gamma 90.0
_cell_formula_units_Z 4
_cell_length_a 8.7362(2)
_cell_length_b 20.53510(16)
_cell_length_c 5.1682(5)
_cell_measurement_temperature 300
_cell_volume 927.17(9)
_computing_data_collection
;
<i>DIFFRAC.Measurement</i> (Bruker, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Crystal Impact, 2015)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
(GSAS, Larson & Von Dreele, 2004)
;
_diffrn_ambient_temperature 300
_diffrn_measurement_device_type 'Bruker D2 Phaser'
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 1.00000
_exptl_absorpt_process_details
; GSAS Absorption/surface roughness correction: function number 3
Surface roughness abs. correction (Suortti)
Terms = 0.0000 0.0000
Correction is not refined.
;
_exptl_crystal_density_diffrn 2.321
_pd_block_id 2015-05-30T10:16|RAMM013|James_A._Kaduk|D2
_pd_calc_method 'Rietveld Refinement'
_pd_char_colour white
_pd_meas_2theta_range_inc 0.02021
_pd_meas_2theta_range_max 70.00603
_pd_meas_2theta_range_min 4.9978
_pd_meas_number_of_points 3217
_pd_meas_scan_method step
_pd_phase_name 'Cs (H2 C6 H5 O7)'
_pd_prep_temperature 295
_pd_proc_2theta_range_inc 0.02021
_pd_proc_2theta_range_max 70.05003
_pd_proc_2theta_range_min 5.0418
_pd_proc_info_datetime 2015-05-30T10:16:47
_pd_proc_ls_background_function
; GSAS Background function number 1 with 6 terms.
Shifted Chebyshev function of 1st kind
1: 1098.70 2: -707.295 3: 219.700 4: -87.7806
5: 41.2782 6: -44.6612
;
_pd_proc_ls_peak_cutoff 0.01000
_pd_proc_ls_profile_function
;
CW Profile function number 4 with 18 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl.
Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
Microstrain broadening by P.W. Stephens, (1999). J. Appl.
Cryst.,32,281-289.
#1(GU) = 1.718 #2(GV) = 0.000 #3(GW) = 4.751
#4(GP) = 0.000 #5(LX) = 2.847 #6(ptec) = 0.00
#7(trns) = 1.83 #8(shft) = 5.2787 #9(sfec) = 0.00
#10(S/L) = 0.0315 #11(H/L) = 0.0005 #12(eta) = 0.9000
#13(S400) = 1.7E-04 #14(S040) = 5.1E-06 #15(S004) = 1.4E-02
#16(S220) = -4.1E-05 #17(S202) = 5.1E-02 #18(S022) = 4.5E-04
Peak tails are ignored where the intensity is below 0.0100 times the peak
Aniso. broadening axis 0.0 0.0 1.0
;
_pd_proc_ls_prof_R_factor 0.0675
_pd_proc_ls_prof_wR_expected 0.0264
_pd_proc_ls_prof_wR_factor 0.0889
_pd_proc_number_of_points 3217
_pd_spec_mounting 'standard holder'
_pd_spec_mount_mode reflection
_pd_spec_shape flat_sheet
_pd_spec_size_axial 24
_pd_spec_size_equat 24
_pd_spec_size_thick 3
_refine_ls_goodness_of_fit_all 3.43
_refine_ls_hydrogen_treatment refU
_refine_ls_matrix_type full
_refine_ls_number_parameters 57
_refine_ls_number_restraints 29
_refine_ls_shift/su_max 0.05
_refine_ls_shift/su_mean 0.01
_refine_ls_weighting_scheme sigma
_reflns_number_total 476
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,+z+1/2
3 +x+1/2,-y+1/2,+z
4 -x,-y,+z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.1876(17) 0.0459(9) 0.281(8) 0.065(4) Uiso 1.0 4
C C2 0.347(2) 0.0446(9) 0.166(6) 0.009(9) Uiso 1.0 4
C C3 0.4423(18) 0.0965(6) 0.304(5) 0.009(9) Uiso 1.0 4
C C4 0.609(2) 0.0896(10) 0.212(7) 0.009(9) Uiso 1.0 4
C C5 0.706(2) 0.1464(9) 0.317(6) 0.065(4) Uiso 1.0 4
C C6 0.380(3) 0.1665(7) 0.241(6) 0.065(4) Uiso 1.0 4
O O7 0.130(2) -0.0065(11) 0.333(9) 0.065(4) Uiso 1.0 4
O O8 0.107(2) 0.0874(9) 0.223(13) 0.065(4) Uiso 1.0 4
O O9 0.371(5) 0.1862(12) 0.010(7) 0.065(4) Uiso 1.0 4
O O10 0.351(4) 0.2037(12) 0.418(7) 0.065(4) Uiso 1.0 4
O O11 0.716(3) 0.1978(11) 0.185(7) 0.065(4) Uiso 1.0 4
O O12 0.730(3) 0.1503(12) 0.552(7) 0.065(4) Uiso 1.0 4
O O13 0.436(3) 0.0847(9) 0.577(5) 0.065(4) Uiso 1.0 4
H H14 0.39911 -0.00564 0.19584 0.012(11) Uiso 1.0 4
H H15 0.34027 0.05603 -0.04959 0.012(11) Uiso 1.0 4
H H16 0.31496 0.11870 0.64320 0.085(6) Uiso 1.0 4
H H17 0.65810 0.04163 0.28558 0.012(11) Uiso 1.0 4
H H18 0.61212 0.09008 -0.00850 0.012(11) Uiso 1.0 4
Cs Cs19 0.0454(3) 0.20017(14) 0.7594 0.0505(15) Uiso 1.0 4
H H20 0.06940 -0.05097 0.56860 0.05 Uiso 1.0 4
H H21 0.67528 0.24300 0.25240 0.05 Uiso 1.00 4
loop_
_pd_proc_ls_weight
_pd_proc_intensity_bkg_calc
_pd_calc_intensity_total
_pd_meas_counts_total
. . . 8727.0
# trimmed for brevity
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_pd_refln_wavelength_id
_refln_observed_status
_refln_F_squared_meas
_refln_F_squared_calc
_refln_phase_calc
_refln_d_spacing
_gsas_i100_meas
1 1 0 1 o -81.317 2.109 0.00 8.03896 0.00
# trimmed for brevity
|
