#------------------------------------------------------------------------------
#$Date: 2022-09-01 05:10:09 +0300 (Thu, 01 Sep 2022) $
#$Revision: 277534 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244155.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2244155
loop_
_publ_author_name
'Bettinger, Reuben T.'
'Squattrito, Philip J.'
'Aulakh, Darpandeep'
'Gianopoulos, Christopher G.'
_publ_section_title
;
Crystal structures of two new divalent transition-metal salts of
carboxybenzenesulfonate anions
;
_journal_coeditor_code MW2190
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 961
_journal_page_last 965
_journal_paper_doi 10.1107/S2056989022008295
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac '[Ni (H2 O1)6] (C7 H5 O6 S)2, 2H2 O'
_chemical_formula_moiety 'H12 Ni O6 2+, 2(C7 H5 O6 S -), 2(H2 O)'
_chemical_formula_sum 'C14 H26 Ni O20 S2'
_chemical_formula_weight 637.18
_chemical_name_common
;
Hexaaquanickel(II) bis(3-carboxy-4-hydroxybenzenesulfonate) dihydrate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 74.1712(14)
_cell_angle_beta 88.6035(14)
_cell_angle_gamma 77.9200(13)
_cell_formula_units_Z 1
_cell_length_a 6.5986(7)
_cell_length_b 7.4183(8)
_cell_length_c 13.2847(14)
_cell_measurement_reflns_used 4943
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 28.31
_cell_measurement_theta_min 2.92
_cell_volume 611.41(11)
_computing_cell_refinement 'SAINT (Bruker, 2015)'
_computing_data_collection 'APEX3 (Bruker, 2015)'
_computing_data_reduction 'SAINT (Bruker, 2015)'
_computing_molecular_graphics 'CrystalMaker (Palmer, 2014)'
_computing_structure_refinement 'SHELXL2018/3 (Sheldrick, 2015b)'
_computing_structure_solution 'SHELXT2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker Duo with APEXII CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0193
_diffrn_reflns_av_unetI/netI 0.0209
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 8656
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 28.403
_diffrn_reflns_theta_min 2.919
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 1.057
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.6699
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Krause et al., 2015)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.731
_exptl_crystal_description block
_exptl_crystal_F_000 330
_exptl_crystal_size_max 0.220
_exptl_crystal_size_mid 0.160
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.326
_refine_diff_density_min -0.413
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 209
_refine_ls_number_reflns 3047
_refine_ls_number_restraints 10
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0259
_refine_ls_R_factor_gt 0.0228
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0578
_refine_ls_wR_factor_ref 0.0592
_reflns_number_gt 2779
_reflns_number_total 3047
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file mw2190sup1.cif
_cod_data_source_block I
_cod_database_code 2244155
_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.
;
_shelx_hkl_file
;
-1 0 0 1195.08 19.70
-1 0 0 1205.78 19.90
1 0 0 1211.58 19.90
1 0 0 1205.48 19.80
-2 0 0 9976.80 163.78
2 0 0 9779.92 167.38
2 0 0 9999.00 165.48
-3 0 0 886.31 16.30
-3 0 0 873.71 17.20
3 0 0 882.51 17.00
3 0 0 831.02 16.70
-4 0 0 3285.37 54.29
-4 0 0 3279.27 55.89
4 0 0 3250.87 55.39
4 0 0 3191.28 55.09
-5 0 0 12.10 2.20
-5 0 0 9.80 2.50
5 0 0 10.50 2.50
5 0 0 15.30 2.80
-6 0 0 132.89 7.10
6 0 0 130.29 6.70
6 0 0 122.99 6.50
-7 0 0 475.55 15.20
7 0 0 469.25 14.40
-8 0 0 55.29 6.90
8 0 0 69.69 7.00
8 -1 0 233.18 10.80
-8 1 0 220.88 10.80
7 -1 0 43.20 5.30
-7 1 0 48.30 5.70
6 -1 0 45.70 4.80
6 -1 0 35.10 4.20
-6 1 0 45.80 4.70
-6 1 0 51.39 5.20
5 -1 0 1363.86 27.10
5 -1 0 1314.07 26.40
-5 1 0 1330.97 27.20
-5 1 0 1322.57 26.70
4 -1 0 209.48 7.10
4 -1 0 208.18 6.90
-4 1 0 210.88 7.10
-4 1 0 207.08 7.10
3 -1 0 3.50 1.50
3 -1 0 2.40 1.30
-3 1 0 3.30 1.30
-3 1 0 1.90 1.30
2 -1 0 106.49 3.60
2 -1 0 101.29 3.80
-2 1 0 106.89 3.60
-2 1 0 109.89 4.20
1 -1 0 872.01 15.40
1 -1 0 888.91 15.20
-1 1 0 854.31 15.90
-1 1 0 899.51 14.90
0 -1 0 849.02 14.40
0 -1 0 876.61 14.00
0 1 0 837.52 14.60
0 1 0 851.81 14.40
-1 -1 0 2492.65 41.40
1 1 0 2477.25 39.50
1 1 0 2405.06 40.10
-2 -1 0 6575.34 102.99
-2 -1 0 6575.04 112.39
2 1 0 6117.89 108.89
2 1 0 6654.83 109.29
-3 -1 0 27.90 1.50
-3 -1 0 41.00 3.00
3 1 0 27.70 2.70
3 1 0 29.50 2.40
-4 -1 0 290.77 6.60
-4 -1 0 289.97 8.70
4 1 0 278.97 8.00
4 1 0 272.77 8.50
-5 -1 0 71.79 3.30
-5 -1 0 69.49 4.90
5 1 0 69.89 4.40
5 1 0 73.89 4.80
-6 -1 0 1168.48 26.50
6 1 0 1218.38 25.60
6 1 0 1252.97 26.70
-7 -1 0 24.20 4.40
7 1 0 31.90 4.40
7 1 0 23.20 4.30
-8 -1 0 8.20 3.60
8 1 0 14.30 3.60
8 -2 0 216.78 10.70
-8 2 0 215.78 10.70
7 -2 0 78.89 7.30
-7 2 0 89.69 6.80
6 -2 0 242.88 9.80
-6 2 0 238.28 9.60
-6 2 0 238.58 9.80
5 -2 0 16.80 3.20
5 -2 0 20.90 3.10
-5 2 0 13.70 3.00
-5 2 0 17.80 3.10
4 -2 0 2359.56 42.20
4 -2 0 2327.17 41.20
-4 2 0 2289.67 41.40
-4 2 0 2363.16 43.10
3 -2 0 348.17 8.90
3 -2 0 356.86 9.50
-3 2 0 354.06 10.30
-3 2 0 362.76 8.90
2 -2 0 522.25 10.90
2 -2 0 521.15 11.40
-2 2 0 530.15 10.50
-2 2 0 495.65 12.10
1 -2 0 2828.62 45.80
1 -2 0 2804.12 44.80
-1 2 0 2753.32 45.10
-1 2 0 2677.13 46.50
0 -2 0 990.60 16.30
0 -2 0 999.20 17.90
0 2 0 1011.20 17.80
0 2 0 1001.70 18.20
-1 -2 0 722.43 13.50
-1 -2 0 707.93 12.70
1 2 0 730.93 12.80
1 2 0 699.93 14.00
-2 -2 0 840.52 15.60
2 2 0 832.92 15.50
2 2 0 855.51 16.80
2 2 0 751.72 13.60
-3 -2 0 1817.62 32.80
3 2 0 1871.41 32.50
3 2 0 1861.81 33.80
-4 -2 0 119.49 5.40
4 2 0 115.99 5.00
4 2 0 113.39 5.70
-5 -2 0 37.40 4.00
5 2 0 36.80 4.10
5 2 0 40.90 3.80
-6 -2 0 12.10 3.00
6 2 0 18.30 3.20
6 2 0 15.60 3.30
-7 -2 0 270.37 11.20
7 2 0 276.67 10.40
7 2 0 268.57 11.10
-8 -2 0 56.79 6.70
8 2 0 48.10 6.20
8 2 0 71.39 6.70
7 -3 0 9.80 3.60
-7 3 0 9.80 3.60
6 -3 0 319.27 11.80
-6 3 0 301.07 11.00
-6 3 0 301.87 12.20
5 -3 0 239.68 9.50
-5 3 0 248.78 8.80
-5 3 0 250.17 10.30
4 -3 0 310.17 10.10
4 -3 0 299.67 8.90
-4 3 0 286.97 10.60
-4 3 0 287.97 8.70
3 -3 0 16.20 2.40
3 -3 0 13.00 2.50
-3 3 0 12.80 2.60
-3 3 0 16.80 2.10
2 -3 0 1244.88 23.10
2 -3 0 1223.08 23.80
-2 3 0 1223.68 21.70
-2 3 0 1257.07 25.30
1 -3 0 1101.59 21.00
1 -3 0 1077.29 18.40
-1 3 0 1115.39 20.30
-1 3 0 1084.69 21.90
0 -3 0 731.23 12.60
0 -3 0 759.52 15.10
0 3 0 754.32 15.40
0 3 0 727.23 14.80
-1 -3 0 4.00 1.40
-1 -3 0 3.20 1.00
1 3 0 4.90 1.40
1 3 0 3.20 1.50
-2 -3 0 608.94 13.10
-2 -3 0 618.64 12.40
2 3 0 588.64 11.30
2 3 0 600.74 14.00
-3 -3 0 15.70 2.20
3 3 0 17.70 2.30
3 3 0 16.00 2.60
-4 -3 0 398.86 10.80
4 3 0 378.76 10.40
4 3 0 390.46 11.80
-5 -3 0 1196.28 25.20
5 3 0 1186.08 26.30
5 3 0 1192.58 24.50
-6 -3 0 30.30 4.20
6 3 0 24.50 4.10
6 3 0 30.60 4.00
-7 -3 0 4.30 2.80
7 3 0 1.20 2.60
7 3 0 6.70 2.80
-8 -3 0 215.08 10.80
8 3 0 221.08 10.00
7 -4 0 155.88 9.30
-7 4 0 131.99 9.30
6 -4 0 59.99 6.50
-6 4 0 49.70 6.40
5 -4 0 2.00 2.40
-5 4 0 2.90 2.80
4 -4 0 212.38 8.80
-4 4 0 230.18 10.10
3 -4 0 397.36 10.80
3 -4 0 417.66 11.90
-3 4 0 400.06 10.40
-3 4 0 379.16 12.90
2 -4 0 16.90 2.80
-2 4 0 12.70 2.20
-2 4 0 8.50 2.60
-2 4 0 15.60 1.70
1 -4 0 771.02 13.30
-1 4 0 721.93 17.60
-1 4 0 775.32 16.00
0 -4 0 2221.08 38.60
0 -4 0 2126.49 34.90
0 4 0 2206.38 38.30
0 4 0 2115.99 39.10
-1 -4 0 1563.34 29.70
-1 -4 0 1642.64 27.20
1 4 0 1608.14 29.50
1 4 0 1635.24 30.30
-2 -4 0 24.80 2.40
-2 -4 0 26.20 3.10
2 4 0 24.30 2.40
2 4 0 24.50 3.20
-3 -4 0 163.48 6.40
-3 -4 0 165.18 5.90
3 4 0 157.18 7.00
3 4 0 161.18 4.20
-4 -4 0 2.20 1.70
4 4 0 4.40 2.00
4 4 0 3.10 2.00
-5 -4 0 110.49 6.00
5 4 0 114.09 5.90
5 4 0 105.59 6.80
-6 -4 0 702.83 18.50
6 4 0 698.33 19.60
6 4 0 698.43 17.70
-7 -4 0 145.89 8.40
7 4 0 142.69 8.80
7 4 0 162.98 8.10
-8 -4 0 61.99 7.10
8 4 0 66.09 7.90
8 4 0 65.29 6.70
6 -5 0 5.60 3.10
-6 5 0 0.80 3.30
5 -5 0 407.56 14.50
-5 5 0 437.96 16.40
4 -5 0 119.39 7.30
-4 5 0 125.09 8.40
3 -5 0 22.90 3.80
3 -5 0 24.30 3.50
-3 5 0 16.40 3.70
2 -5 0 357.16 11.50
-2 5 0 375.16 13.00
-2 5 0 379.46 10.40
1 -5 0 6.30 2.20
-1 5 0 8.10 2.70
-1 5 0 3.80 1.80
0 -5 0 16.10 2.90
0 -5 0 13.90 1.50
0 5 0 15.30 2.70
0 5 0 10.70 2.60
-1 -5 0 1801.22 33.50
-1 -5 0 1768.22 29.70
1 5 0 1731.33 33.20
1 5 0 1734.73 33.70
-2 -5 0 808.52 16.10
-2 -5 0 794.72 18.40
2 5 0 833.82 19.40
2 5 0 821.22 17.20
-3 -5 0 16.80 2.50
-3 -5 0 13.10 2.60
3 5 0 16.50 3.30
-4 -5 0 48.90 4.00
-4 -5 0 44.70 4.50
4 5 0 38.70 4.70
-5 -5 0 780.42 18.80
-5 -5 0 799.22 19.40
5 5 0 774.12 20.90
-6 -5 0 6.20 2.70
6 5 0 2.80 2.60
6 5 0 3.40 2.80
-7 -5 0 11.40 3.70
7 5 0 5.80 3.70
7 5 0 4.60 2.80
-8 -5 0 277.27 12.30
8 5 0 252.67 12.70
8 5 0 260.07 11.30
5 -6 0 52.09 6.50
-5 6 0 61.29 7.70
4 -6 0 215.98 10.20
-4 6 0 205.38 11.40
3 -6 0 890.01 22.30
-3 6 0 876.71 24.30
2 -6 0 80.79 6.10
-2 6 0 87.29 6.90
-2 6 0 90.89 5.40
1 -6 0 152.18 7.50
-1 6 0 125.59 7.70
-1 6 0 136.49 6.60
0 -6 0 380.36 12.00
0 6 0 364.46 11.40
0 6 0 375.76 12.50
-1 -6 0 29.00 4.00
1 6 0 42.30 4.50
1 6 0 37.60 4.30
-2 -6 0 406.46 12.60
-2 -6 0 444.46 13.20
2 6 0 453.45 13.70
2 6 0 434.26 11.70
-3 -6 0 173.68 8.00
-3 -6 0 180.08 6.50
3 6 0 171.58 8.50
-4 -6 0 10.20 3.10
-4 -6 0 5.70 2.30
4 6 0 4.10 2.90
-5 -6 0 7.80 2.70
-5 -6 0 9.60 3.00
5 6 0 11.00 3.30
-6 -6 0 79.69 6.10
-6 -6 0 76.39 6.30
6 6 0 99.59 7.90
-7 -6 0 165.38 9.00
-7 -6 0 162.78 9.10
7 6 0 155.78 10.00
4 -7 0 67.09 7.40
-4 7 0 95.79 10.10
3 -7 0 126.69 8.20
-3 7 0 127.09 9.30
2 -7 0 307.67 12.30
-2 7 0 345.27 14.00
1 -7 0 55.39 6.10
-1 7 0 53.19 6.30
-1 7 0 46.40 5.10
0 -7 0 8.40 3.10
0 7 0 2.40 2.80
0 7 0 4.00 2.40
-1 -7 0 435.56 14.00
1 7 0 467.85 14.40
1 7 0 464.85 14.10
-2 -7 0 257.37 10.30
2 7 0 242.98 9.10
2 7 0 238.28 10.40
-3 -7 0 41.70 5.20
3 7 0 49.00 6.10
-4 -7 0 9.60 3.10
4 7 0 12.80 3.70
-5 -7 0 190.08 9.50
-5 -7 0 193.88 8.50
5 7 0 210.48 11.00
-6 -7 0 257.27 11.40
-6 -7 0 239.88 10.30
6 7 0 261.77 12.70
-7 -7 0 0.30 2.70
-7 -7 0 2.60 3.00
7 7 0 -0.70 2.70
3 -8 0 20.20 4.70
-3 8 0 18.20 5.20
2 -8 0 52.69 6.20
-2 8 0 51.39 7.30
1 -8 0 398.66 14.70
-1 8 0 418.16 13.70
-1 8 0 392.26 15.50
0 -8 0 196.08 9.90
0 8 0 201.38 9.60
0 8 0 200.38 10.30
-1 -8 0 0.50 2.50
1 8 0 0.30 2.50
1 8 0 0.20 2.30
-2 -8 0 57.49 6.30
2 8 0 53.19 6.20
-3 -8 0 229.58 10.70
3 8 0 242.58 11.50
-4 -8 0 3.20 3.00
4 8 0 -0.70 2.30
-5 -8 0 13.20 4.00
5 8 0 13.20 4.20
-6 -8 0 70.69 7.60
6 8 0 61.39 8.20
1 -9 0 21.70 4.70
-1 9 0 13.10 4.60
0 -9 0 5.30 3.60
0 9 0 0.20 2.70
0 9 0 4.10 3.60
1 9 0 596.64 18.90
1 9 0 593.34 22.60
-2 -9 0 278.77 12.80
2 9 0 314.57 13.50
-3 -9 0 117.09 8.50
3 9 0 150.58 9.80
-4 -9 0 86.39 8.50
4 9 0 97.29 9.70
4 9 -1 436.86 17.60
-4 -9 1 448.86 16.60
3 9 -1 123.39 9.20
-3 -9 1 106.59 8.40
2 9 -1 1.70 3.20
-2 -9 1 2.90 3.50
1 9 -1 86.29 8.60
-1 -9 1 60.79 6.90
0 9 -1 114.89 8.70
0 9 -1 116.89 8.50
0 -9 1 135.89 9.20
-6 -8 1 295.27 13.10
5 8 -1 72.79 8.10
-5 -8 1 82.29 8.00
4 8 -1 77.99 8.30
-4 -8 1 68.59 7.00
3 8 -1 2.50 3.00
-3 -8 1 7.00 3.40
2 8 -1 299.97 12.60
-2 -8 1 268.77 11.80
1 8 -1 62.19 6.90
1 8 -1 58.89 6.40
-1 -8 1 37.30 5.40
0 8 -1 17.80 4.00
0 8 -1 11.30 3.70
0 -8 1 16.60 4.10
-1 8 -1 35.30 5.10
-1 8 -1 19.90 4.70
1 -8 1 36.80 5.70
-2 8 -1 137.49 10.00
2 -8 1 150.78 9.40
7 7 -1 16.40 4.60
-7 -7 1 9.20 3.60
-7 -7 1 11.10 3.80
6 7 -1 1.90 3.30
-6 -7 1 3.70 2.70
-6 -7 1 0.70 2.70
5 7 -1 290.97 13.00
-5 -7 1 299.97 12.20
4 7 -1 213.38 10.90
-4 -7 1 227.88 10.30
3 7 -1 6.20 2.80
-3 -7 1 7.80 3.20
2 7 -1 13.00 3.30
2 7 -1 10.20 3.40
-2 -7 1 10.20 3.40
1 7 -1 415.06 13.60
1 7 -1 378.86 12.90
-1 -7 1 386.76 13.20
0 7 -1 549.85 16.20
0 7 -1 572.84 17.20
0 -7 1 569.54 16.60
-1 7 -1 123.59 8.20
-1 7 -1 123.09 7.10
1 -7 1 113.99 7.40
-2 7 -1 35.40 5.60
-2 7 -1 47.30 5.40
2 -7 1 35.70 5.00
-3 7 -1 76.89 8.30
3 -7 1 86.59 7.10
-4 7 -1 17.40 5.20
4 -7 1 16.20 4.30
7 6 -1 95.39 9.50
-7 -6 1 69.99 7.20
-7 -6 1 87.89 7.20
6 6 -1 182.88 10.30
-6 -6 1 166.38 9.10
-6 -6 1 176.88 8.50
5 6 -1 3.70 3.00
-5 -6 1 3.60 2.20
-5 -6 1 7.00 3.10
4 6 -1 90.69 6.70
-4 -6 1 87.79 5.10
-4 -6 1 91.09 6.30
3 6 -1 469.75 15.00
-3 -6 1 469.35 11.50
-3 -6 1 441.56 13.70
2 6 -1 96.19 5.30
2 6 -1 97.39 6.40
-2 -6 1 81.49 5.50
1 6 -1 707.13 18.00
1 6 -1 718.73 17.50
-1 -6 1 661.53 17.40
0 6 -1 22.10 3.90
0 6 -1 18.10 3.40
0 -6 1 14.90 3.10
-1 6 -1 2488.45 48.20
-1 6 -1 2458.75 46.00
1 -6 1 2456.85 46.70
-2 6 -1 225.58 8.60
-2 6 -1 204.08 10.10
2 -6 1 208.48 9.30
-3 6 -1 33.80 5.80
3 -6 1 31.00 4.70
-4 6 -1 104.19 8.60
4 -6 1 114.79 7.70
-5 6 -1 347.67 15.60
5 -6 1 328.97 13.50
8 5 -1 178.98 9.60
8 5 -1 178.38 10.70
-8 -5 1 174.68 10.00
7 5 -1 218.58 11.20
7 5 -1 223.88 10.10
-7 -5 1 230.18 10.50
6 5 -1 22.40 4.10
6 5 -1 20.70 4.30
-6 -5 1 25.10 4.10
5 5 -1 91.89 6.80
-5 -5 1 104.89 6.00
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3 -4 -14 3.80 2.70
-3 4 14 -0.20 3.20
2 -4 -14 111.29 7.60
-2 4 14 110.89 8.80
1 -4 -14 200.08 9.50
-1 4 14 224.28 11.70
0 -4 -14 11.80 3.20
0 4 14 9.10 4.10
-1 -4 -14 88.89 6.60
1 4 14 92.79 7.90
-2 -4 -14 266.07 11.20
2 4 14 284.97 11.40
2 4 14 263.87 12.60
-3 -4 -14 384.46 13.90
3 4 14 380.76 14.30
3 4 14 417.76 15.90
-4 -4 -14 20.20 4.20
4 4 14 16.80 4.80
4 4 14 18.50 4.70
-5 -4 -14 5.10 3.30
-5 -4 -14 4.10 3.20
5 4 14 6.40 4.20
3 -5 -14 220.58 11.10
-3 5 14 219.08 12.60
2 -5 -14 249.38 11.30
-2 5 14 292.37 14.10
1 -5 -14 3.10 2.60
-1 5 14 -2.00 2.80
0 -5 -14 223.78 10.30
0 5 14 213.18 11.40
-1 -5 -14 302.27 11.90
1 5 14 292.67 13.50
-2 -5 -14 18.50 3.90
2 5 14 20.00 4.70
2 5 14 16.10 3.90
-3 -5 -14 1.70 2.70
3 5 14 -0.90 2.80
3 5 14 -2.80 2.40
-4 -5 -14 369.86 14.20
4 5 14 409.26 15.70
4 5 14 394.26 15.40
-5 -5 -14 53.09 6.80
5 5 14 67.69 10.60
5 5 14 72.49 8.50
3 -6 -14 25.20 5.00
-3 6 14 17.80 5.30
2 -6 -14 1.50 3.10
-2 6 14 -1.60 3.00
1 -6 -14 611.54 18.70
-1 6 14 611.14 21.30
0 -6 -14 119.09 8.10
0 6 14 148.49 10.20
-1 -6 -14 1.70 2.80
1 6 14 -1.00 2.70
-2 -6 -14 376.06 14.20
2 6 14 406.66 16.10
-3 -6 -14 178.58 10.00
3 6 14 188.98 10.00
3 6 14 193.58 11.00
-4 -6 -14 5.00 3.00
4 6 14 3.60 3.30
4 6 14 12.50 4.20
1 -7 -14 -1.40 2.60
-1 7 14 -1.30 3.10
0 -7 -14 235.88 11.20
0 7 14 233.28 13.00
-1 -7 -14 265.97 11.90
1 7 14 259.87 13.40
-2 -7 -14 15.90 4.20
2 7 14 16.50 4.90
-3 -7 -14 31.70 5.20
3 7 14 31.40 5.90
-4 -7 -14 203.38 11.00
4 7 14 163.48 10.30
2 2 -15 64.79 7.30
-2 -2 15 69.79 7.70
1 2 -15 203.58 11.00
-1 -2 15 184.48 10.80
0 2 -15 421.36 16.80
0 -2 15 440.26 17.00
-1 2 -15 2.20 3.30
1 -2 15 7.00 4.00
3 1 -15 71.89 7.00
-3 -1 15 72.89 7.90
2 1 -15 87.79 8.50
-2 -1 15 71.99 7.40
1 1 -15 387.16 15.10
-1 -1 15 369.66 14.40
0 1 -15 30.80 5.50
0 -1 15 28.30 5.20
-1 1 -15 111.69 8.80
1 -1 15 117.19 9.00
-2 1 -15 272.87 13.50
2 -1 15 303.77 14.10
-3 1 -15 109.79 9.30
3 -1 15 118.39 11.60
4 0 -15 206.08 10.60
3 0 -15 72.59 6.90
-3 0 15 85.19 8.50
2 0 -15 23.90 4.30
-2 0 15 27.20 5.60
1 0 -15 8.50 3.70
1 0 -15 6.00 2.80
-1 0 15 6.50 3.10
0 0 -15 456.85 13.80
0 0 -15 426.66 16.20
0 0 15 463.45 15.80
-1 0 -15 37.90 6.20
1 0 15 48.10 6.60
-2 0 -15 8.50 3.80
2 0 15 3.60 3.40
-3 0 -15 303.77 14.30
3 0 15 304.87 14.40
4 -1 -15 26.30 5.10
-4 1 15 22.60 5.20
-3 1 15 1.80 3.10
2 -1 -15 571.64 17.20
-2 1 15 539.65 18.80
1 -1 -15 324.67 12.10
-1 1 15 349.17 14.80
0 -1 -15 125.89 7.20
0 -1 -15 105.19 8.20
0 1 15 120.89 7.60
-1 -1 -15 193.28 9.00
-1 -1 -15 205.08 10.90
1 1 15 208.58 10.40
-2 -1 -15 871.11 21.50
-2 -1 -15 848.32 24.50
2 1 15 865.91 24.10
-3 -1 -15 2.20 3.90
-3 -1 -15 4.90 3.50
3 1 15 -3.20 3.00
-4 -1 -15 11.40 4.40
4 1 15 18.60 5.20
4 -2 -15 100.39 7.80
-4 2 15 78.59 8.50
3 -2 -15 40.10 5.80
-3 2 15 45.50 6.70
2 -2 -15 6.40 3.30
-2 2 15 4.50 3.60
1 -2 -15 59.09 6.10
-1 2 15 64.99 7.70
0 -2 -15 303.97 11.50
0 2 15 259.37 13.50
0 2 15 272.67 13.20
-1 -2 -15 30.40 5.50
-1 -2 -15 39.20 5.20
1 2 15 52.49 6.10
-2 -2 -15 1.20 2.80
-2 -2 -15 2.40 2.30
2 2 15 2.70 3.30
-3 -2 -15 212.08 9.90
-3 -2 -15 210.18 11.30
3 2 15 216.28 11.40
-4 -2 -15 165.68 10.30
4 2 15 169.98 10.80
4 -3 -15 27.50 5.20
-4 3 15 22.50 5.50
3 -3 -15 24.30 4.70
-3 3 15 32.20 6.00
2 -3 -15 193.78 9.70
-2 3 15 184.08 11.10
1 -3 -15 -0.60 2.30
-1 3 15 2.50 3.50
0 -3 -15 160.58 8.70
0 3 15 176.48 10.50
-1 -3 -15 642.34 18.50
1 3 15 652.03 21.20
1 3 15 645.24 18.20
-2 -3 -15 252.47 12.10
-2 -3 -15 269.97 11.30
2 3 15 265.17 13.10
2 3 15 288.37 12.00
-3 -3 -15 46.30 6.60
-3 -3 -15 33.80 5.10
3 3 15 28.50 5.20
-4 -3 -15 6.40 3.10
-4 -3 -15 9.20 4.10
4 3 15 8.90 4.00
3 -4 -15 100.99 7.70
-3 4 15 111.09 9.30
2 -4 -15 105.19 7.50
-2 4 15 102.29 10.20
1 -4 -15 2.20 2.60
-1 4 15 3.50 3.60
0 -4 -15 211.88 10.20
0 4 15 211.78 11.90
-1 -4 -15 147.39 8.60
1 4 15 141.89 9.80
-2 -4 -15 10.60 3.50
2 4 15 9.60 3.50
2 4 15 15.30 4.70
-3 -4 -15 243.58 11.10
3 4 15 249.18 11.80
3 4 15 250.37 12.80
-4 -4 -15 275.87 12.10
4 4 15 268.47 13.30
4 4 15 280.67 13.20
3 -5 -15 39.30 6.30
-3 5 15 45.30 7.40
2 -5 -15 295.07 12.80
-2 5 15 282.87 14.30
1 -5 -15 32.50 5.40
-1 5 15 25.30 5.90
0 -5 -15 0.80 2.60
0 5 15 0.10 3.20
-1 -5 -15 251.17 11.40
1 5 15 248.08 12.90
-2 -5 -15 230.78 10.90
2 5 15 234.58 12.40
-3 -5 -15 -1.20 2.40
3 5 15 -0.30 2.90
3 5 15 -1.70 3.00
-4 -5 -15 16.40 4.30
4 5 15 15.60 4.60
4 5 15 37.80 6.40
2 -6 -15 56.29 7.00
-2 6 15 79.49 9.40
1 -6 -15 36.10 5.70
-1 6 15 21.50 5.80
0 -6 -15 583.84 18.50
0 6 15 565.54 20.70
-1 -6 -15 13.20 4.30
1 6 15 7.90 4.30
-2 -6 -15 0.40 2.80
2 6 15 -2.10 3.20
-3 -6 -15 164.48 9.70
3 6 15 158.38 10.50
-4 -6 -15 153.38 9.70
4 6 15 148.99 10.10
4 6 15 149.09 9.90
0 -7 -15 5.70 3.40
0 7 15 -2.40 2.90
-1 -7 -15 298.77 13.30
1 7 15 335.27 15.60
-2 -7 -15 226.88 11.50
2 7 15 219.28 12.60
2 1 -16 3.90 3.40
1 1 -16 440.36 16.80
-1 -1 16 418.06 16.00
0 1 -16 22.10 5.20
0 -1 16 12.20 4.40
-1 1 -16 8.20 4.20
1 -1 16 7.10 4.20
3 0 -16 46.30 5.80
-3 0 16 61.19 7.80
2 0 -16 286.17 11.70
-2 0 16 272.77 13.50
1 0 -16 46.10 5.90
1 0 -16 38.90 6.40
0 0 -16 -0.40 2.90
0 0 16 3.50 3.30
-1 0 -16 386.16 16.10
1 0 16 411.86 15.90
-2 0 -16 74.09 8.70
2 0 16 65.69 8.10
3 -1 -16 -4.20 2.40
-3 1 16 -1.40 3.00
2 -1 -16 22.00 4.40
-2 1 16 14.10 4.60
1 -1 -16 278.17 11.40
-1 1 16 269.47 13.60
0 -1 -16 1.10 3.10
0 -1 -16 1.30 2.50
0 1 16 2.50 2.80
-1 -1 -16 20.90 4.80
-1 -1 -16 29.50 4.70
1 1 16 29.60 5.50
-2 -1 -16 650.13 21.60
2 1 16 676.03 21.30
-3 -1 -16 454.75 17.70
3 1 16 436.16 17.60
3 -2 -16 467.65 16.50
-3 2 16 450.05 17.90
2 -2 -16 87.49 7.10
-2 2 16 109.09 9.00
1 -2 -16 50.29 5.90
-1 2 16 56.19 7.50
0 -2 -16 33.10 4.90
0 2 16 20.10 5.00
-1 -2 -16 302.77 13.90
-1 -2 -16 316.27 12.20
1 2 16 330.67 13.10
-2 -2 -16 1.90 2.70
-2 -2 -16 1.70 3.40
2 2 16 7.50 3.60
-3 -2 -16 10.30 4.40
-3 -2 -16 4.30 3.00
3 2 16 -1.20 3.10
3 -3 -16 55.49 6.90
-3 3 16 47.90 7.30
2 -3 -16 152.58 9.20
-2 3 16 162.68 10.90
1 -3 -16 195.68 9.90
-1 3 16 186.18 11.50
0 -3 -16 29.20 4.90
0 3 16 29.70 5.60
-1 -3 -16 10.40 3.50
1 3 16 3.90 3.20
-2 -3 -16 226.48 10.70
2 3 16 246.18 13.10
2 3 16 245.48 11.60
-3 -3 -16 211.68 10.50
-3 -3 -16 207.88 11.50
3 3 16 235.28 11.90
-4 -3 -16 4.60 3.70
4 3 16 6.90 3.80
2 -4 -16 3.50 3.00
-2 4 16 -1.70 3.40
1 -4 -16 6.10 3.20
-1 4 16 3.50 3.50
0 -4 -16 94.19 8.50
0 4 16 96.39 10.00
-1 -4 -16 131.49 8.40
1 4 16 115.99 9.10
-2 -4 -16 9.50 3.40
2 4 16 5.90 3.30
2 4 16 7.00 4.10
-3 -4 -16 26.50 4.60
3 4 16 38.00 6.70
3 4 16 23.80 4.90
2 -5 -16 23.50 5.10
-2 5 16 21.10 5.40
1 -5 -16 224.58 11.00
-1 5 16 188.48 12.20
0 -5 -16 9.90 3.50
0 5 16 9.80 4.60
-1 -5 -16 8.00 3.70
1 5 16 4.40 4.00
-2 -5 -16 231.28 11.20
2 5 16 260.27 13.50
-3 -5 -16 245.18 11.80
3 5 16 247.58 13.20
3 5 16 241.38 12.00
-1 6 16 -0.50 3.60
0 -6 -16 71.69 7.70
0 6 16 72.29 8.60
-1 -6 -16 24.20 5.10
1 6 16 30.20 6.20
-2 -6 -16 -1.80 2.40
2 6 16 -3.00 3.30
1 0 -17 67.19 8.00
0 0 -17 21.30 5.50
0 0 17 14.10 4.60
2 -1 -17 12.50 3.80
-2 1 17 10.00 4.50
1 -1 -17 35.20 5.20
-1 1 17 42.30 7.00
0 -1 -17 174.28 10.70
0 -1 -17 174.78 9.20
-1 -1 -17 58.39 8.20
1 1 17 55.09 7.30
2 -2 -17 257.67 12.10
-2 2 17 228.98 13.30
1 -2 -17 20.40 4.50
-1 2 17 22.10 5.40
0 -2 -17 7.70 3.50
0 2 17 1.10 3.10
-1 -2 -17 97.39 7.30
-1 -2 -17 109.69 8.90
1 2 17 82.09 8.10
1 2 17 98.89 10.50
-2 -2 -17 44.60 5.90
-2 -2 -17 30.20 6.30
2 2 17 33.10 5.70
2 -3 -17 6.60 3.80
-2 3 17 3.20 4.00
1 -3 -17 79.29 7.90
-1 3 17 59.09 8.40
0 -3 -17 101.89 7.60
0 3 17 84.79 9.50
-1 -3 -17 4.40 3.10
1 3 17 5.60 4.20
-2 -3 -17 16.90 4.40
2 3 17 17.70 4.70
2 3 17 17.80 5.60
1 -4 -17 17.50 4.50
-1 4 17 13.10 4.90
0 -4 -17 4.30 3.30
0 4 17 8.20 4.20
-1 -4 -17 258.27 12.00
1 4 17 258.57 13.80
-2 -4 -17 237.78 11.50
2 4 17 232.68 13.30
0 -5 -17 39.90 6.20
0 5 17 53.99 8.10
-1 -5 -17 3.60 3.30
1 5 17 0.40 4.10
;
_shelx_hkl_checksum 80308
_shelx_res_file
;
TITL RB303_0m_a.res in P-1
rb303_084_final.res
created by SHELXL-2018/3 at 14:13:09 on 17-Aug-2022
REM Old TITL RB303_0m in P-1
REM SHELXT solution in P-1
REM R1 0.055, Rweak 0.005, Alpha 0.048, Orientation as input
REM Formula found by SHELXT: C14 Ni O20 S2
CELL 0.71073 6.5986 7.4183 13.2847 74.1712 88.6035 77.9200
ZERR 1 0.0007 0.0008 0.0014 0.0014 0.0014 0.0013
LATT 1
SFAC C H Ni O S
UNIT 14 26 1 20 2
ACTA 52
L.S. 32
PLAN 20
TEMP -123
BOND $H
CONF
LIST 6
FMAP 2
dfix 0.84 0.01 o1w h11 o1w h12 o2w h21 o2w h22 o3w h31 o3w h32 o4w h41 o4w h42
dfix 0.84 0.01 o4 h4 o6 h6a
WGHT 0.028400 0.222300
FVAR 0.97637
NI1 3 0.500000 1.000000 0.000000 10.50000 0.01121 0.01190 =
0.00927 -0.00113 -0.00053 -0.00301
O1W 4 0.402371 0.994216 0.147331 11.00000 0.01843 0.01725 =
0.01103 -0.00254 -0.00040 -0.00208
H11 2 0.342424 1.095257 0.159973 11.00000 0.03905
H12 2 0.488141 0.938574 0.196639 11.00000 0.04083
O2W 4 0.662697 0.722302 0.050400 11.00000 0.01402 0.01446 =
0.01992 0.00053 -0.00200 -0.00349
H22 2 0.596496 0.642231 0.084597 11.00000 0.04774
H21 2 0.778865 0.700580 0.079469 11.00000 0.03716
O3W 4 0.235001 0.913810 -0.026632 11.00000 0.01685 0.02263 =
0.01286 -0.00427 0.00026 -0.00945
H32 2 0.219999 0.883865 -0.081642 11.00000 0.03695
H31 2 0.182238 0.839755 0.019951 11.00000 0.03285
S1 5 0.782000 0.523271 0.798242 11.00000 0.01103 0.01454 =
0.01148 -0.00112 0.00037 -0.00312
O1 4 0.841939 0.706944 0.786584 11.00000 0.01935 0.01831 =
0.01753 -0.00542 0.00350 -0.00789
O2 4 0.567467 0.529704 0.831701 11.00000 0.01220 0.02051 =
0.01717 -0.00089 0.00324 -0.00304
O3 4 0.925765 0.359615 0.864399 11.00000 0.01498 0.02075 =
0.01466 0.00006 -0.00245 -0.00100
O6 4 0.730621 0.396143 0.381414 11.00000 0.02388 0.02494 =
0.01736 -0.00928 -0.00055 -0.00682
H6A 2 0.703984 0.502501 0.335490 11.00000 0.05067
O5 4 0.683772 0.762834 0.301567 11.00000 0.02105 0.02513 =
0.01315 -0.00240 -0.00277 -0.00399
O4 4 0.723364 0.948067 0.404560 11.00000 0.03060 0.01587 =
0.01419 0.00072 -0.00032 -0.00400
H4 2 0.726819 1.025038 0.345379 11.00000 0.04156
C1 1 0.784476 0.489049 0.671543 11.00000 0.01035 0.01605 =
0.01323 -0.00208 -0.00020 -0.00305
C6 1 0.800571 0.303812 0.661251 11.00000 0.01301 0.01526 =
0.01739 -0.00055 0.00081 -0.00381
AFIX 43
H6 2 0.823672 0.197124 0.721651 11.00000 -1.20000
AFIX 0
C5 1 0.782956 0.275680 0.563499 11.00000 0.01574 0.01540 =
0.02148 -0.00579 0.00145 -0.00503
AFIX 43
H5 2 0.793317 0.149826 0.556807 11.00000 -1.20000
AFIX 0
C4 1 0.749807 0.432731 0.474196 11.00000 0.01007 0.02189 =
0.01660 -0.00620 0.00045 -0.00420
C3 1 0.738727 0.618770 0.484378 11.00000 0.01042 0.01689 =
0.01338 -0.00148 0.00019 -0.00271
C7 1 0.712870 0.781952 0.389325 11.00000 0.01117 0.01916 =
0.01488 -0.00136 0.00010 -0.00116
C2 1 0.755939 0.644957 0.584050 11.00000 0.01240 0.01412 =
0.01455 -0.00241 0.00035 -0.00289
AFIX 43
H2 2 0.747996 0.769976 0.591539 11.00000 -1.20000
AFIX 0
O4W 4 0.777814 1.179562 0.218154 11.00000 0.01602 0.01638 =
0.01776 -0.00387 -0.00085 -0.00441
H42 2 0.674410 1.269422 0.203985 11.00000 0.03518
H41 2 0.878825 1.230054 0.219930 11.00000 0.03858
EQIV $2 -x+1, -y+2, -z+1
HTAB O1W O1_$2
HTAB O1W O5
EQIV $3 -x+1, -y+1, -z+1
HTAB O2W O2_$3
EQIV $4 -x+2, -y+1, -z+1
HTAB O2W O3_$4
EQIV $1 -x+1, -y+2, -z
HTAB O3W O4W_$1
HTAB O3W O3_$3
HTAB O6 O5
HTAB O4 O4W
EQIV $5 x, y-1, z
HTAB O4W O2_$2
EQIV $6 -x+2, -y+2, -z+1
HTAB O4W O1_$6
HKLF 4
REM RB303_0m_a.res in P-1
REM wR2 = 0.0592, GooF = S = 1.082, Restrained GooF = 1.081 for all data
REM R1 = 0.0228 for 2779 Fo > 4sig(Fo) and 0.0259 for all 3047 data
REM 209 parameters refined using 10 restraints
END
WGHT 0.0284 0.2223
REM Highest difference peak 0.326, deepest hole -0.413, 1-sigma level 0.059
Q1 1 0.7846 0.5048 0.7205 11.00000 0.05 0.33
Q2 1 0.7776 0.3556 0.5188 11.00000 0.05 0.30
Q3 1 0.7491 0.6895 0.4413 11.00000 0.05 0.29
Q4 1 0.7255 0.5345 0.4761 11.00000 0.05 0.26
Q5 1 0.7551 0.6400 0.5288 11.00000 0.05 0.26
Q6 1 0.7878 0.5656 0.6295 11.00000 0.05 0.26
Q7 1 0.8292 0.4026 0.6652 11.00000 0.05 0.25
Q8 1 0.8174 0.6243 0.8005 11.00000 0.05 0.24
Q9 1 0.8266 0.2986 0.6062 11.00000 0.05 0.22
Q10 1 0.8554 0.4329 0.8394 11.00000 0.05 0.21
Q11 1 0.5671 0.5310 0.8754 11.00000 0.05 0.20
Q12 1 0.4971 0.5828 0.8040 11.00000 0.05 0.20
Q13 1 0.6189 0.5966 0.8012 11.00000 0.05 0.19
Q14 1 0.5289 0.5352 0.8014 11.00000 0.05 0.18
Q15 1 0.6552 0.5385 0.8249 11.00000 0.05 0.17
Q16 1 0.5041 0.6091 0.9010 11.00000 0.05 0.16
Q17 1 0.5332 0.4427 0.8588 11.00000 0.05 0.16
Q18 1 0.9716 0.5295 0.6046 11.00000 0.05 0.16
Q19 1 0.5202 0.7083 0.2689 11.00000 0.05 0.16
Q20 1 1.0228 0.3593 0.8411 11.00000 0.05 0.15
;
_shelx_res_checksum 43234
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.500000 1.000000 0.000000 0.01105(7) Uani d 1 . .
O O1W 0.40237(15) 0.99422(14) 0.14733(7) 0.0161(2) Uani d 1 . .
H H11 0.342(3) 1.095(2) 0.1600(16) 0.039(6) Uiso d 1 . .
H H12 0.488(3) 0.939(3) 0.1966(12) 0.041(6) Uiso d 1 . .
O O2W 0.66270(15) 0.72230(14) 0.05040(8) 0.0171(2) Uani d 1 . .
H H22 0.596(3) 0.642(3) 0.0846(16) 0.048(6) Uiso d 1 . .
H H21 0.7789(19) 0.701(3) 0.0795(15) 0.037(6) Uiso d 1 . .
O O3W 0.23500(15) 0.91381(15) -0.02663(8) 0.0168(2) Uani d 1 . .
H H32 0.220(3) 0.884(3) -0.0816(11) 0.037(6) Uiso d 1 . .
H H31 0.182(3) 0.840(2) 0.0200(12) 0.033(5) Uiso d 1 . .
S S1 0.78200(5) 0.52327(5) 0.79824(2) 0.01278(8) Uani d 1 . .
O O1 0.84194(15) 0.70694(14) 0.78658(8) 0.0177(2) Uani d 1 . .
O O2 0.56747(14) 0.52970(14) 0.83170(8) 0.0176(2) Uani d 1 . .
O O3 0.92577(15) 0.35961(14) 0.86440(8) 0.0181(2) Uani d 1 . .
O O6 0.73062(17) 0.39614(16) 0.38141(8) 0.0211(2) Uani d 1 . .
H H6A 0.704(4) 0.503(2) 0.3355(14) 0.051(7) Uiso d 1 . .
O O5 0.68377(16) 0.76283(15) 0.30157(8) 0.0204(2) Uani d 1 . .
O O4 0.72336(17) 0.94807(15) 0.40456(8) 0.0213(2) Uani d 1 . .
H H4 0.727(3) 1.025(3) 0.3454(10) 0.042(6) Uiso d 1 . .
C C1 0.78448(19) 0.48905(19) 0.67154(10) 0.0135(2) Uani d 1 . .
C C6 0.8006(2) 0.30381(19) 0.66125(11) 0.0159(3) Uani d 1 . .
H H6 0.823672 0.197124 0.721651 0.019 Uiso calc 1 . .
C C5 0.7830(2) 0.2757(2) 0.56350(11) 0.0171(3) Uani d 1 . .
H H5 0.793317 0.149826 0.556807 0.021 Uiso calc 1 . .
C C4 0.7498(2) 0.4327(2) 0.47420(11) 0.0159(3) Uani d 1 . .
C C3 0.7387(2) 0.61877(19) 0.48438(10) 0.0141(3) Uani d 1 . .
C C7 0.7129(2) 0.7820(2) 0.38932(11) 0.0160(3) Uani d 1 . .
C C2 0.7559(2) 0.64496(19) 0.58405(10) 0.0140(2) Uani d 1 . .
H H2 0.747996 0.769976 0.591539 0.017 Uiso calc 1 . .
O O4W 0.77781(16) 1.17956(14) 0.21815(8) 0.0167(2) Uani d 1 . .
H H42 0.674(2) 1.269(2) 0.2040(16) 0.035(6) Uiso d 1 . .
H H41 0.879(2) 1.230(3) 0.2199(17) 0.039(6) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 0.01121(12) 0.01190(12) 0.00927(12) -0.00301(8) -0.00053(8) -0.00113(8)
O1W 0.0184(5) 0.0172(5) 0.0110(4) -0.0021(4) -0.0004(4) -0.0025(4)
O2W 0.0140(5) 0.0145(5) 0.0199(5) -0.0035(4) -0.0020(4) 0.0005(4)
O3W 0.0168(5) 0.0226(5) 0.0129(5) -0.0095(4) 0.0003(4) -0.0043(4)
S1 0.01103(15) 0.01454(16) 0.01148(15) -0.00312(11) 0.00037(11) -0.00112(12)
O1 0.0193(5) 0.0183(5) 0.0175(5) -0.0079(4) 0.0035(4) -0.0054(4)
O2 0.0122(4) 0.0205(5) 0.0172(5) -0.0030(4) 0.0032(4) -0.0009(4)
O3 0.0150(5) 0.0208(5) 0.0147(5) -0.0010(4) -0.0024(4) 0.0001(4)
O6 0.0239(5) 0.0249(6) 0.0174(5) -0.0068(4) -0.0005(4) -0.0093(4)
O5 0.0211(5) 0.0251(5) 0.0132(5) -0.0040(4) -0.0028(4) -0.0024(4)
O4 0.0306(6) 0.0159(5) 0.0142(5) -0.0040(4) -0.0003(4) 0.0007(4)
C1 0.0103(6) 0.0161(6) 0.0132(6) -0.0030(5) -0.0002(4) -0.0021(5)
C6 0.0130(6) 0.0153(6) 0.0174(6) -0.0038(5) 0.0008(5) -0.0005(5)
C5 0.0157(6) 0.0154(6) 0.0215(7) -0.0050(5) 0.0015(5) -0.0058(5)
C4 0.0101(6) 0.0219(7) 0.0166(6) -0.0042(5) 0.0004(5) -0.0062(5)
C3 0.0104(6) 0.0169(6) 0.0134(6) -0.0027(5) 0.0002(5) -0.0015(5)
C7 0.0112(6) 0.0192(7) 0.0149(6) -0.0012(5) 0.0001(5) -0.0014(5)
C2 0.0124(6) 0.0141(6) 0.0145(6) -0.0029(5) 0.0004(5) -0.0024(5)
O4W 0.0160(5) 0.0164(5) 0.0178(5) -0.0044(4) -0.0009(4) -0.0039(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'
Ni Ni 0.3393 1.1124 '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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1W Ni1 O1W 2_675 . 180.0 ?
O1W Ni1 O2W 2_675 2_675 91.26(4) ?
O1W Ni1 O2W . 2_675 88.74(4) ?
O1W Ni1 O2W 2_675 . 88.74(4) ?
O1W Ni1 O2W . . 91.26(4) ?
O2W Ni1 O2W 2_675 . 180.0 ?
O1W Ni1 O3W 2_675 . 92.03(4) ?
O1W Ni1 O3W . . 87.97(4) ?
O2W Ni1 O3W 2_675 . 88.06(4) ?
O2W Ni1 O3W . . 91.94(4) ?
O1W Ni1 O3W 2_675 2_675 87.97(4) ?
O1W Ni1 O3W . 2_675 92.03(4) ?
O2W Ni1 O3W 2_675 2_675 91.94(4) ?
O2W Ni1 O3W . 2_675 88.06(4) ?
O3W Ni1 O3W . 2_675 180.0 ?
Ni1 O1W H11 . . 119.4(15) ?
Ni1 O1W H12 . . 117.2(15) ?
H11 O1W H12 . . 106(2) ?
Ni1 O2W H22 . . 116.1(16) ?
Ni1 O2W H21 . . 118.9(15) ?
H22 O2W H21 . . 109(2) ?
Ni1 O3W H32 . . 119.8(15) ?
Ni1 O3W H31 . . 122.3(14) ?
H32 O3W H31 . . 106(2) ?
O3 S1 O1 . . 113.84(6) ?
O3 S1 O2 . . 111.87(6) ?
O1 S1 O2 . . 111.57(6) ?
O3 S1 C1 . . 106.97(6) ?
O1 S1 C1 . . 106.29(6) ?
O2 S1 C1 . . 105.69(6) ?
C4 O6 H6A . . 107.2(16) ?
C7 O4 H4 . . 107.2(15) ?
C2 C1 C6 . . 120.45(12) ?
C2 C1 S1 . . 120.22(10) ?
C6 C1 S1 . . 119.17(10) ?
C5 C6 C1 . . 120.19(12) ?
C5 C6 H6 . . 119.9 ?
C1 C6 H6 . . 119.9 ?
C6 C5 C4 . . 120.03(13) ?
C6 C5 H5 . . 120.0 ?
C4 C5 H5 . . 120.0 ?
O6 C4 C5 . . 117.16(13) ?
O6 C4 C3 . . 123.10(12) ?
C5 C4 C3 . . 119.74(12) ?
C2 C3 C4 . . 119.51(12) ?
C2 C3 C7 . . 121.27(12) ?
C4 C3 C7 . . 119.21(12) ?
O5 C7 O4 . . 122.61(13) ?
O5 C7 C3 . . 121.89(13) ?
O4 C7 C3 . . 115.49(12) ?
C1 C2 C3 . . 120.05(12) ?
C1 C2 H2 . . 120.0 ?
C3 C2 H2 . . 120.0 ?
H42 O4W H41 . . 106(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1W 2_675 2.0376(10) ?
Ni1 O1W . 2.0376(10) ?
Ni1 O2W 2_675 2.0498(10) ?
Ni1 O2W . 2.0498(10) ?
Ni1 O3W . 2.0526(10) ?
Ni1 O3W 2_675 2.0526(10) ?
O1W H11 . 0.829(9) ?
O1W H12 . 0.832(10) ?
O2W H22 . 0.838(10) ?
O2W H21 . 0.832(9) ?
O3W H32 . 0.833(9) ?
O3W H31 . 0.831(9) ?
S1 O3 . 1.4570(10) ?
S1 O1 . 1.4644(10) ?
S1 O2 . 1.4685(10) ?
S1 C1 . 1.7685(14) ?
O6 C4 . 1.3466(17) ?
O6 H6A . 0.843(10) ?
O5 C7 . 1.2364(17) ?
O4 C7 . 1.3179(18) ?
O4 H4 . 0.839(9) ?
C1 C2 . 1.3821(18) ?
C1 C6 . 1.3996(19) ?
C6 C5 . 1.3816(19) ?
C6 H6 . 0.9500 ?
C5 C4 . 1.4016(19) ?
C5 H5 . 0.9500 ?
C4 C3 . 1.4098(19) ?
C3 C2 . 1.4003(18) ?
C3 C7 . 1.4762(19) ?
C2 H2 . 0.9500 ?
O4W H42 . 0.832(9) ?
O4W H41 . 0.834(10) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H11 O1 2_676 0.829(9) 1.979(11) 2.7895(14) 165(2) yes
O1W H12 O5 . 0.832(10) 1.924(11) 2.7432(14) 168(2) yes
O2W H22 O2 2_666 0.838(10) 1.944(10) 2.7802(14) 176(2) yes
O2W H21 O3 2_766 0.832(9) 2.020(10) 2.8476(14) 174(2) yes
O3W H32 O4W 2_675 0.833(9) 1.993(10) 2.8208(14) 172(2) yes
O3W H31 O3 2_666 0.831(9) 2.050(10) 2.8790(14) 175(2) yes
O6 H6A O5 . 0.843(10) 1.836(15) 2.5904(16) 148(2) yes
O4 H4 O4W . 0.839(9) 1.833(10) 2.6656(14) 171(2) yes
O4W H42 O2 2_676 0.832(9) 1.910(10) 2.7420(14) 178(2) yes
O4W H41 O1 2_776 0.834(10) 1.988(11) 2.8029(14) 165(2) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 S1 C1 C2 . . . . -147.25(11) ?
O1 S1 C1 C2 . . . . -25.29(12) ?
O2 S1 C1 C2 . . . . 93.39(11) ?
O3 S1 C1 C6 . . . . 37.34(12) ?
O1 S1 C1 C6 . . . . 159.30(10) ?
O2 S1 C1 C6 . . . . -82.02(11) ?
C2 C1 C6 C5 . . . . -1.6(2) ?
S1 C1 C6 C5 . . . . 173.82(10) ?
C1 C6 C5 C4 . . . . 0.3(2) ?
C6 C5 C4 O6 . . . . -178.94(12) ?
C6 C5 C4 C3 . . . . 1.3(2) ?
O6 C4 C3 C2 . . . . 178.67(12) ?
C5 C4 C3 C2 . . . . -1.56(19) ?
O6 C4 C3 C7 . . . . -2.41(19) ?
C5 C4 C3 C7 . . . . 177.36(12) ?
C2 C3 C7 O5 . . . . -175.12(12) ?
C4 C3 C7 O5 . . . . 5.97(19) ?
C2 C3 C7 O4 . . . . 5.01(18) ?
C4 C3 C7 O4 . . . . -173.89(12) ?
C6 C1 C2 C3 . . . . 1.29(19) ?
S1 C1 C2 C3 . . . . -174.06(10) ?
C4 C3 C2 C1 . . . . 0.28(19) ?
C7 C3 C2 C1 . . . . -178.62(12) ?
_cod_database_fobs_code 2244155