#------------------------------------------------------------------------------ #$Date: 2019-06-12 07:24:17 +0300 (Wed, 12 Jun 2019) $ #$Revision: 215865 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021660.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_2021660 loop_ _publ_author_name 'Zhu, Jingyan' 'Yan, Shan' 'Xiao, Hongping' 'Jiang, Jun' 'Li, Xinhua' _publ_section_title ; Nickel(II) cluster-based mixed-cation coordination polymer synthesized from 2-mercaptobenzoic acid and its application ; _journal_coeditor_code YP3179 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619007368 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '[Ni8 Na Cl2 (O H)3 (C7 H4 O2 S)6]' _chemical_formula_sum 'C42 H27 Cl2 Na Ni8 O15 S6' _chemical_formula_weight 1527.56 _chemical_name_systematic Poly[hexakis[\m~4~-(2-carboxylatophenyl)sulfanido]di-\m~3~-chlorido-tri-\m~2~-hydroxido-octanickel(II)sodium(I)] _space_group_crystal_system hexagonal _space_group_IT_number 176 _space_group_name_Hall '-P 6c' _space_group_name_H-M_alt 'P 63/m' _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 13.2027(7) _cell_length_b 13.2027(7) _cell_length_c 18.3116(12) _cell_measurement_reflns_used 7580 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.1982 _cell_measurement_theta_min 2.8501 _cell_volume 2764.3(3) _computing_cell_refinement ; APEX3 (Bruker, 2014) ; _computing_data_collection ; APEX3 (Bruker, 2014) ; _computing_data_reduction ; APEX3 (Bruker, 2014) ; _computing_publication_material ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) and OLEX2 (Dolomanov et al., 2009) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEXIII area-detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 19761 _diffrn_reflns_theta_full 24.989 _diffrn_reflns_theta_max 24.989 _diffrn_reflns_theta_min 2.100 _exptl_absorpt_coefficient_mu 3.054 _exptl_absorpt_correction_T_max 0.2627 _exptl_absorpt_correction_T_min 0.1871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;(SADABS; Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10) ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.835 _exptl_crystal_description prism _exptl_crystal_F_000 1528 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.972 _refine_diff_density_min -2.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1679 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0683 _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^)+(0.1205P)^2^+36.4479P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2054 _refine_ls_wR_factor_ref 0.2134 _reflns_number_gt 1442 _reflns_number_total 1679 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yp3179sup1.cif _cod_data_source_block I _cod_database_code 2021660 _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 ; -2 1 0 343.097 12.7434 1 -2 1 0 370.360 14.7201 3 -1 -1 0 349.899 12.4751 1 -1 -1 0 339.827 12.1986 2 -1 -1 0 353.762 13.3651 3 -1 2 0 347.640 12.7268 1 -1 2 0 318.737 12.0170 2 1 -2 0 353.325 12.6164 1 1 -2 0 360.638 12.0934 2 1 1 0 356.361 12.4997 1 1 1 0 352.387 12.4652 2 1 1 0 356.987 13.5037 3 2 -1 0 345.118 12.7508 1 2 -1 0 355.415 15.0238 3 2 0 0 1867.44 60.0483 1 2 0 0 1862.31 59.4628 2 2 -2 0 1885.30 60.2051 1 2 -2 0 1813.25 59.0566 2 -2 0 0 1763.25 59.8245 1 -2 0 0 1859.79 59.1185 2 -2 0 0 1952.73 62.0636 3 -2 2 0 1784.08 60.1411 1 -2 2 0 1760.57 58.8248 2 -2 2 0 1906.93 61.5539 3 0 -2 0 1893.82 59.8992 1 0 -2 0 1752.17 59.4432 2 0 2 0 1846.81 60.0407 1 -1 -2 0 3482.02 107.902 1 -1 -2 0 3196.74 107.020 2 1 2 0 2981.51 107.424 2 1 2 0 3271.74 108.524 3 2 -3 0 3469.70 107.955 1 2 -3 0 3402.38 106.871 2 3 -1 0 3476.43 108.110 1 -3 1 0 3323.23 107.974 1 -3 1 0 3500.33 106.140 2 -3 1 0 3751.06 111.817 3 -2 3 0 3296.08 108.049 1 -2 3 0 3077.07 106.658 2 -1 -2 0 3337.30 107.561 1 3 -1 0 3608.96 112.251 3 3 -1 0 2919.67 106.492 2 -2 -1 0 3996.05 132.708 2 -2 -1 0 4113.79 133.381 1 -1 3 0 3763.16 132.987 2 -1 3 0 4052.90 133.816 1 2 1 0 4315.16 133.672 1 2 1 0 4062.47 133.362 2 3 -2 0 4208.57 133.949 1 3 -2 0 4258.07 132.290 2 3 -2 0 4193.38 136.800 3 -3 2 0 4192.11 131.758 2 2 1 0 4054.44 135.648 3 -2 -1 0 4339.62 135.492 3 1 -3 0 4311.53 133.601 1 1 -3 0 4038.96 132.835 2 -3 2 0 4527.65 137.160 3 -3 2 0 4083.30 133.939 1 0 -3 0 2634.23 85.3246 2 3 -3 0 2765.83 86.4564 1 0 -3 0 2705.47 85.8875 1 -3 0 0 2506.64 85.7605 1 -3 0 0 2573.33 84.5847 2 3 -3 0 2694.75 84.8767 2 3 0 0 2644.35 86.0934 1 0 3 0 2342.28 85.6103 2 3 0 0 2690.66 90.0935 3 -3 3 0 2457.48 84.2824 2 -3 3 0 2753.49 88.5552 3 3 0 0 2752.76 85.3911 2 -3 3 0 2600.92 86.3813 1 -3 0 0 2823.37 89.1872 3 0 3 0 2652.35 86.1917 1 -3 4 0 2172.92 71.3915 1 4 -1 0 2176.80 71.0851 1 3 -4 0 2175.63 69.6146 2 -1 -3 0 2240.82 70.7915 1 -1 -3 0 2154.58 69.9310 2 -4 1 0 2047.00 70.7120 1 -4 1 0 2049.59 68.4721 2 3 -4 0 2186.22 70.8626 1 4 -1 0 2180.62 69.5531 2 4 -1 0 2229.88 76.4799 3 -3 4 0 2187.19 72.4485 3 -3 4 0 1956.80 69.1766 2 -4 1 0 2209.36 75.0815 3 -1 -3 0 2134.02 70.5390 1 1 3 0 2013.50 70.6185 2 1 3 0 2113.26 71.4729 3 -2 -2 0 23.9403 2.40340 2 -2 4 0 22.4164 2.61106 2 -4 2 0 14.8224 1.48313 2 -4 2 0 17.0729 1.48006 2 2 2 0 16.2804 2.56469 1 2 2 0 19.2809 2.68788 2 -2 4 0 21.0747 3.05329 1 -2 -2 0 15.0210 2.46914 1 2 -4 0 17.8458 2.32712 2 2 2 0 19.5674 3.69172 3 2 -4 0 18.8318 2.70513 1 -4 2 0 16.3794 2.72663 1 4 -2 0 15.3633 4.63214 3 -4 2 0 19.7886 4.71669 3 4 -2 0 17.5363 2.84877 1 1 -4 0 1354.63 44.0194 2 4 -3 0 1340.50 45.3419 1 4 -3 0 1314.48 48.6310 3 -1 4 0 1259.86 44.3285 2 -4 3 0 1253.48 45.1808 1 4 -3 0 1351.07 43.3380 2 -3 -1 0 1280.51 44.4586 1 -3 -1 0 1349.86 43.4654 2 3 1 0 1354.21 44.6044 2 -4 3 0 1266.73 42.3216 2 1 -4 0 1356.89 44.6388 1 3 1 0 1279.42 48.2862 3 -1 4 0 1299.01 45.0860 1 3 1 0 1364.18 44.9973 1 -4 3 0 1334.60 48.6326 3 -3 -1 0 1329.16 47.2924 3 -4 0 0 73.5597 8.94159 3 0 -4 0 74.4319 4.78946 2 0 4 0 71.9092 5.25622 2 4 -4 0 72.1053 5.66958 1 4 -4 0 77.8495 4.40473 2 -4 4 0 67.6328 5.48164 1 0 -4 0 75.9870 5.21499 1 -4 4 0 69.4101 3.59563 2 -4 0 0 76.0544 3.87395 2 4 0 0 69.8133 8.66611 3 -4 4 0 63.7689 7.73569 3 4 0 0 71.3849 4.70822 2 4 0 0 79.2442 5.67135 1 -4 0 0 78.1159 5.16583 1 5 -1 0 1622.53 53.6167 2 5 -1 0 1637.05 61.8133 3 -1 -4 0 1611.12 54.6333 1 -5 1 0 1597.46 54.8887 1 -5 1 0 1533.59 51.9305 2 -4 5 0 1624.56 55.7168 1 5 -1 0 1661.36 55.5066 1 -4 5 0 1669.77 57.6916 3 1 4 0 1547.35 54.9544 2 -1 -4 0 1649.25 54.7171 1 -4 5 0 1562.17 53.0483 2 1 4 0 1594.92 55.6262 3 4 -5 0 1610.17 53.4597 2 3 -5 0 36.1173 4.73432 1 -5 2 0 30.2403 6.99157 3 -3 5 0 37.3209 4.53059 1 -3 5 0 39.9566 3.55372 2 -5 2 0 48.8250 2.15315 2 5 -2 0 36.4624 4.92061 1 2 3 0 47.9695 4.38860 2 5 -2 0 46.4416 8.00314 3 -5 2 0 31.0140 3.94570 1 3 -5 0 43.2185 3.75471 2 2 3 0 46.9697 6.02752 3 -2 -3 0 52.0345 4.12746 2 -3 -2 0 155.248 7.52870 1 -5 3 0 139.737 12.2492 3 2 -5 0 146.342 7.18190 2 3 2 0 167.151 8.20852 1 3 2 0 137.202 10.1084 3 2 -5 0 145.845 7.97836 1 5 -3 0 139.301 11.9147 3 -5 3 0 134.746 8.01482 1 -3 -2 0 138.379 10.4278 3 5 -3 0 107.839 8.03072 1 -2 5 0 133.453 8.03492 1 -2 5 0 137.480 7.29080 2 -3 -2 0 132.794 6.54823 2 3 2 0 140.217 7.85546 2 -5 3 0 129.055 4.82956 2 5 -4 0 299.508 17.5528 3 -1 5 0 329.301 14.6773 1 1 -5 0 326.567 14.0002 1 4 1 0 355.481 19.1257 3 -4 -1 0 308.687 13.7715 1 5 -4 0 329.356 12.8962 2 -5 4 0 308.648 14.7158 1 -1 5 0 357.382 14.4669 2 -5 4 0 316.823 18.7203 3 -4 -1 0 366.013 12.7710 2 4 1 0 380.155 14.6027 2 -5 4 0 350.812 11.6828 2 4 1 0 319.610 14.5259 1 0 -5 0 1676.95 53.7712 1 -5 0 0 1554.82 53.6306 1 0 5 0 1553.90 54.3056 1 -5 5 0 1567.77 54.9106 1 -5 5 0 1556.70 51.4371 2 -5 5 0 1571.86 58.0923 3 -5 0 0 1552.36 51.2339 2 0 5 0 1560.41 54.2071 2 5 0 0 1541.80 53.1639 2 5 0 0 1477.99 54.1163 1 5 -5 0 1616.28 52.5015 2 5 0 0 1597.54 60.3059 3 -1 -5 0 1.67843 2.74801 1 -1 -5 0 4.92597 2.43615 1 -6 1 0 8.77189 1.39566 2 1 5 0 11.1927 3.06696 2 6 -1 0 5.70691 5.83796 3 5 -6 0 9.32447 2.87466 2 -6 1 0 11.7773 2.84910 1 -5 6 0 8.85155 2.89652 1 -5 6 0 9.35605 2.26066 2 -5 6 0 10.2217 5.71365 3 1 5 0 10.2038 3.69385 3 6 -1 0 6.38687 2.43218 2 -4 6 0 42.0465 6.35402 3 2 4 0 33.5891 5.61797 3 -6 2 0 41.2887 5.12286 1 -2 -4 0 39.0634 4.48012 1 -4 6 0 42.0968 5.06293 1 4 -6 0 39.8782 4.57736 2 -2 -4 0 29.3552 4.20558 1 6 -2 0 39.8100 8.80861 3 3 3 0 545.454 24.3683 3 -3 6 0 532.618 20.7895 2 -3 -3 0 537.190 20.8611 1 3 3 0 521.941 21.6848 2 -6 3 0 539.362 21.9559 1 3 3 0 550.595 21.3109 1 -3 6 0 558.792 22.2467 1 6 -3 0 531.105 27.2747 3 -2 6 0 950.664 35.2360 2 2 -6 0 997.274 35.4253 1 6 -4 0 996.596 41.5523 3 -4 -2 0 1003.68 33.7849 2 4 2 0 995.584 40.5592 3 4 2 0 1010.41 35.7627 1 -6 4 0 939.830 36.1492 1 -6 4 0 982.959 31.7212 2 -2 6 0 1007.89 36.4952 1 4 2 0 955.218 35.5861 2 -4 -2 0 962.017 34.8234 1 5 1 0 111.237 7.52500 2 -5 -1 0 104.021 7.08398 1 -1 6 0 107.231 7.87804 1 6 -5 0 108.010 6.38504 2 -5 -1 0 107.850 5.71210 2 5 1 0 109.666 8.73278 1 -6 5 0 91.6445 4.75277 2 -6 5 0 104.568 7.88787 1 -1 6 0 106.347 7.63979 2 1 -6 0 108.412 7.59223 1 5 1 0 96.0767 11.5164 3 -6 0 0 1201.32 43.6923 1 -6 6 0 1300.55 41.5986 2 6 0 0 1205.99 51.5518 3 0 6 0 1207.07 44.5053 2 0 6 0 1233.40 44.6564 1 0 -6 0 1272.84 43.7719 1 6 -6 0 1239.99 42.6788 2 -6 0 0 1253.41 40.9559 2 6 0 0 1205.35 43.4813 2 -6 6 0 1203.55 45.1629 1 -6 7 0 1400.54 48.4871 2 1 6 0 1461.04 51.9403 2 -6 7 0 1441.86 52.3843 1 -7 1 0 1401.13 50.6992 1 -1 -6 0 1434.97 50.2004 1 1 6 0 1453.83 51.8660 3 -1 -6 0 1428.11 50.6279 1 -7 1 0 1432.85 46.7064 2 6 -7 0 1401.59 49.4884 2 7 -1 0 1417.98 49.5821 2 7 -1 0 1438.00 60.6558 3 -5 7 0 1429.40 50.2769 2 2 5 0 1495.60 54.1163 3 -5 7 0 1452.49 54.9977 3 2 5 0 1460.65 52.9591 2 -2 -5 0 1492.40 51.3277 1 -2 -5 0 1488.92 51.6113 1 -7 2 0 1470.40 47.4111 2 -7 2 0 1487.22 52.3950 1 7 -2 0 1465.23 61.0820 3 -5 7 0 1476.15 53.2797 1 3 4 0 428.762 18.3838 2 -7 3 0 397.450 17.9525 1 3 4 0 385.148 20.3018 3 -3 -4 0 397.395 16.9211 1 -3 -4 0 408.283 17.8497 1 7 -3 0 378.893 23.9960 3 -4 7 0 385.181 18.2090 1 -4 7 0 379.457 16.4859 2 -3 7 0 127.192 7.94899 2 4 3 0 115.401 8.92729 1 -4 -3 0 108.935 7.32310 1 4 3 0 113.524 8.47864 2 4 3 0 108.482 11.1904 3 -7 4 0 102.025 8.14689 1 -3 7 0 121.550 8.69252 1 7 -4 0 113.681 12.5970 3 5 2 0 125.888 13.4162 3 5 2 0 131.765 10.0503 1 -7 5 0 128.205 8.95470 1 -5 -2 0 125.686 8.03117 1 7 -5 0 147.895 13.5391 3 -2 7 0 110.013 9.19862 1 5 2 0 140.764 9.14557 2 -6 -1 0 39.1894 4.97108 1 -7 6 0 32.8393 5.73504 1 7 -6 0 35.4668 5.10812 2 6 1 0 33.4177 5.14855 2 6 1 0 33.7912 8.42982 3 -1 7 0 46.8106 6.39609 1 -7 0 0 120.380 6.31188 2 -7 7 0 133.839 7.12826 2 -7 7 0 118.969 10.1352 1 7 0 0 125.717 16.3867 3 7 -7 0 111.189 8.64874 2 0 7 0 154.890 10.0755 1 -7 0 0 126.830 8.62250 1 0 7 0 109.917 9.27783 2 7 0 0 127.860 8.99983 2 -1 -7 0 578.650 24.0941 1 8 -1 0 601.314 35.3281 3 1 7 0 588.650 26.2576 2 1 7 0 546.039 25.0441 3 -7 8 0 555.876 22.0012 2 8 -1 0 560.964 23.1911 2 -7 8 0 566.658 26.0839 1 -8 1 0 573.308 19.9004 2 -8 1 0 546.927 23.9844 1 -6 8 0 19.6613 3.71920 2 -8 2 0 16.2899 2.24731 2 -8 2 0 8.28737 3.66674 1 2 6 0 12.8934 4.81648 3 -2 -6 0 13.9098 3.55784 1 -2 -6 0 10.1446 4.56975 1 2 6 0 21.3150 5.63942 2 -6 8 0 11.2931 4.44359 1 8 -2 0 12.2860 9.17375 3 8 -3 0 2.55833 7.77407 3 -5 8 0 4.87629 2.65511 2 -8 3 0 3.14701 3.19299 1 -5 8 0 5.76440 3.57697 1 -3 -5 0 0.75004 2.65388 1 3 5 0 2.36103 4.64258 3 -3 -5 0 1.47063 4.26882 1 3 5 0 5.62673 3.97485 2 -5 8 0 16.1069 6.69001 3 4 4 0 518.269 22.7823 1 4 4 0 544.556 23.7677 2 4 4 0 563.085 27.3564 3 -4 8 0 554.487 22.5316 2 -4 8 0 557.501 24.1722 1 -8 4 0 532.347 23.5451 1 -4 -4 0 529.394 21.6618 1 8 -4 0 501.447 30.4067 3 5 3 0 -0.7821 5.52529 3 -3 8 0 1.80910 3.08892 1 8 -5 0 2.48718 6.16871 3 -8 5 0 -3.2692 3.10621 1 -3 8 0 2.95083 3.20349 2 5 3 0 2.37237 3.61173 2 -5 -3 0 7.75914 2.69573 1 -8 6 0 438.872 14.9698 2 6 2 0 424.754 19.5451 2 -6 -2 0 407.081 18.0228 1 -2 8 0 409.048 19.7850 1 -8 6 0 426.197 20.4301 1 6 2 0 413.590 26.0028 3 -2 8 0 396.556 19.1589 2 -7 -1 0 106.891 8.24994 1 -8 7 0 108.466 10.2701 1 -8 7 0 129.076 6.52382 2 7 1 0 109.498 9.58241 2 8 -7 0 101.721 8.31419 2 -1 8 0 116.864 10.4176 2 7 1 0 111.777 16.4311 3 -1 8 0 100.704 9.60257 1 -8 0 0 74.4355 7.54544 1 -8 0 0 67.1182 5.48944 2 0 8 0 72.0071 8.50057 1 -8 8 0 71.5114 9.05294 1 -8 8 0 64.3681 5.78765 2 8 0 0 56.5152 13.8535 3 8 0 0 48.8977 7.04637 2 8 -8 0 54.9212 7.05596 2 9 -1 0 2216.50 75.6211 2 -9 1 0 2147.97 76.3994 1 1 8 0 2193.77 77.8120 3 -8 9 0 2291.37 74.3285 2 9 -1 0 2145.75 90.4112 3 1 8 0 2202.08 79.0603 2 -8 9 0 2108.81 78.9343 1 -1 -8 0 2169.91 76.1133 1 -9 1 0 2206.17 71.5994 2 2 7 0 11.8140 5.64366 3 -9 2 0 8.81494 4.36142 1 2 7 0 16.0169 6.40666 2 9 -2 0 3.16435 10.3250 3 -9 2 0 11.6925 2.15478 2 -2 -7 0 5.81615 3.87466 1 -7 9 0 17.0428 5.81027 1 -7 9 0 25.4597 4.40342 2 9 -3 0 6062.31 206.093 3 -3 -6 0 5854.81 192.004 1 -6 9 0 5846.27 195.283 1 -6 9 0 5761.05 191.795 2 -9 3 0 5936.28 194.042 1 3 6 0 6108.86 197.402 3 3 6 0 5705.63 194.882 2 4 5 0 387.868 23.0378 3 -4 -5 0 384.243 17.3957 1 -5 9 0 363.619 20.0806 1 -9 4 0 377.496 19.6016 1 -5 9 0 398.648 18.3626 2 9 -4 0 360.920 27.9446 3 4 5 0 437.260 20.9355 2 -4 9 0 781.592 31.8337 2 -5 -4 0 762.969 30.3285 1 5 4 0 838.404 33.6533 2 -9 5 0 809.184 33.2288 1 9 -5 0 791.315 41.9490 3 -4 9 0 808.776 33.7363 1 5 4 0 804.773 38.8054 3 6 3 0 804.169 32.6633 2 -6 -3 0 767.528 30.1328 1 -9 6 0 787.110 33.1958 1 9 -6 0 776.903 40.3877 3 6 3 0 826.997 40.3697 3 -3 9 0 761.610 33.0183 1 -7 -2 0 149.840 9.87000 1 7 2 0 153.215 11.7062 2 7 2 0 196.193 20.4831 3 -9 7 0 147.308 12.5264 1 -2 9 0 119.529 11.4489 2 -9 7 0 146.601 7.12337 2 -2 9 0 161.364 12.0959 1 -8 -1 0 595.645 25.4078 1 8 1 0 552.834 36.6806 3 8 1 0 610.108 26.8874 2 9 -8 0 618.123 24.8531 2 -9 8 0 562.954 27.6466 1 -1 9 0 637.521 28.5940 2 -9 8 0 662.235 22.7221 2 -1 9 0 580.721 26.9457 1 0 9 0 1354.61 48.7378 3 -9 0 0 1253.38 47.5303 1 9 0 0 1263.25 48.1380 2 0 9 0 1267.31 50.9049 2 -9 9 0 1223.51 50.5253 1 9 0 0 1236.14 61.5503 3 -9 9 0 1310.39 44.8093 2 1 9 0 567.232 29.4579 2 10 -1 0 598.596 25.8662 2 -1 -9 0 613.666 26.1735 1 -10 1 0 529.764 26.0382 1 10 -1 0 582.291 41.6410 3 1 9 0 633.434 28.2831 3 -10 1 0 561.948 21.7141 2 -9 10 0 566.925 29.2922 1 -9 10 0 614.210 24.0802 2 2 8 0 527.192 28.0333 2 10 -2 0 549.153 39.4898 3 -2 -8 0 564.195 24.4084 1 -8 10 0 588.895 24.0431 2 -10 2 0 539.651 25.7539 1 -10 2 0 547.384 19.8104 2 -8 10 0 551.037 27.9993 1 2 8 0 575.449 28.4004 3 -3 -7 0 67.1034 7.69834 1 3 7 0 55.0224 9.84761 3 -7 10 0 36.8732 7.76310 1 10 -3 0 56.6756 15.5407 3 -7 10 0 52.0718 8.14907 2 -10 3 0 53.8846 8.14514 1 3 7 0 67.9982 10.3246 2 -6 10 0 11.8673 6.13202 1 -4 -6 0 17.9758 3.78839 1 4 6 0 15.4867 6.60427 2 10 -4 0 3.70618 9.63697 3 -10 4 0 6.20508 4.82346 1 4 6 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23 37.2687 20.2186 2 -4 -1 23 58.5765 18.5823 1 -5 4 23 94.4436 24.6717 2 1 -5 23 104.510 21.7740 1 -5 4 23 77.1796 15.6563 1 5 -4 23 48.8748 17.5238 1 4 1 23 52.4040 20.0287 2 -5 5 23 -0.9563 11.6782 1 5 -5 23 8.53730 15.0655 1 -5 0 23 4.81070 14.8872 1 5 0 23 -1.8042 17.5303 2 -5 5 23 -2.4452 19.1029 2 0 -5 23 38.3917 17.8209 1 0 0 24 1397.07 75.0890 2 0 0 24 1230.67 60.7753 1 0 1 24 17.1856 13.2996 1 0 1 24 54.4790 23.6605 2 1 -1 24 42.0649 22.5209 2 1 0 24 53.1827 23.0204 2 -1 0 24 2.07483 13.8057 1 1 0 24 -2.9843 13.6767 1 -1 1 24 0.71317 13.2548 1 -1 1 24 17.6578 20.0234 2 1 -1 24 31.2422 14.6324 1 0 -1 24 -12.349 13.6583 1 -2 1 24 -32.184 19.2505 2 1 -2 24 26.4465 15.2384 1 2 -1 24 25.6038 15.4443 1 1 1 24 90.9875 25.1093 2 -1 2 24 31.7630 13.8173 1 2 -1 24 20.7556 22.4741 2 1 1 24 -1.9812 13.1758 1 -2 1 24 8.23367 13.6720 1 -1 -1 24 16.3475 14.7675 1 -2 2 24 149.004 20.3315 1 0 2 24 128.839 27.6648 2 2 -2 24 157.518 22.1874 1 -2 0 24 112.421 19.2659 1 0 2 24 132.999 19.2101 1 -2 2 24 71.4090 25.3912 2 0 -2 24 138.398 21.9066 1 2 0 24 203.096 26.7342 1 2 0 24 189.689 29.6719 2 3 -1 24 78.0298 17.3532 1 -2 3 24 64.7588 14.7639 1 -3 1 24 44.7333 16.2538 1 1 2 24 58.2926 14.5305 1 2 -3 24 56.5596 17.6218 1 -1 -2 24 59.5668 17.8329 1 3 -2 24 -4.1833 14.0209 1 -2 -1 24 -7.9643 14.1274 1 -1 3 24 -10.334 11.1802 1 -3 2 24 11.7333 13.1991 1 1 -3 24 9.34880 14.8892 1 2 1 24 39.0688 13.8627 1 0 0 0 0.00 0.00 0 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.2627 _exptl_absorpt_correction_T_min 0.1871 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 13.186 13.197 18.298 90.002 90.102 120.027 ) ; _shelx_hkl_checksum 51060 _shelx_res_file ; TITL ZNZ1252_NiO_0m_a.res in P6(3)/m znz1252_nio_0m_sq.res created by SHELXL-2018/3 at 09:41:21 on 28-Jan-2019 REM Old TITL ZNZ1252_NiO_0m in P6(3)/m REM SHELXT solution in P6(3)/m REM R1 0.172, Rweak 0.008, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C21 Ni4 O8 S4 CELL 0.71073 13.2027 13.2027 18.3116 90.000 90.000 120.000 ZERR 2 0.0007 0.0007 0.0012 0.000 0.000 0.000 LATT 1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, 1/2+Z SYMM Y, -X+Y, 1/2+Z SYMM X-Y, X, 1/2+Z SFAC C H NI O S Cl Na UNIT 84 54 16 30 12 4 2 OMIT -1 4 2 OMIT -1 2 2 OMIT 0 2 1 OMIT -2 4 0 OMIT -1 2 0 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173 L.S. 5 0 11 BOND $H ACTA CONF HTAB OMIT -3 50 FMAP 2 PLAN 20 ACTA ABIN WGHT 0.120500 36.447922 FVAR 0.25065 0.86759 NI1 3 0.000000 0.000000 0.664155 10.33333 0.04463 0.04463 = 0.03122 0.00000 0.00000 0.02231 NA1 7 0.000000 0.000000 0.500000 10.16667 0.02102 0.02102 = 0.01085 0.00000 0.00000 0.01051 O1 4 0.031289 0.142396 0.590515 11.00000 0.02880 0.02708 = 0.02904 -0.01299 -0.00941 0.01606 C1 1 0.163441 0.522597 0.466715 11.00000 0.02855 0.03012 = 0.02595 0.00396 -0.00227 0.00590 AFIX 43 H1 2 0.189294 0.584615 0.432392 11.00000 -1.20000 AFIX 0 S1 5 0.043954 0.474865 0.671574 11.00000 0.03668 0.02552 = 0.01679 -0.00102 -0.00234 0.01983 NI2 3 0.022840 0.346983 0.750000 10.50000 0.04750 0.02314 = 0.01579 0.00000 0.00000 0.02167 O2 4 0.006246 0.234833 0.681309 11.00000 0.07277 0.02523 = 0.01602 -0.00156 -0.00060 0.02827 C2 1 0.156652 0.417213 0.446607 11.00000 0.03977 0.05253 = 0.02224 -0.00697 0.00345 0.01810 AFIX 43 H2 2 0.180219 0.407978 0.399222 11.00000 -1.20000 AFIX 0 DFIX 0.85 0.001 O3 H3a O3 4 -0.110437 0.016677 0.750000 10.50000 0.02454 0.02308 = 0.07997 0.00000 0.00000 0.01301 AFIX 3 H3A 2 -0.080237 0.090589 0.750000 10.50000 -1.50000 AFIX 0 NI3 3 0.189900 0.574257 0.750000 10.50000 0.02988 0.02743 = 0.02273 0.00000 0.00000 0.01393 CL3 6 0.333333 0.666667 0.825751 10.33333 0.03557 0.03557 = 0.02411 0.00000 0.00000 0.01778 C3 1 0.115835 0.327950 0.495785 11.00000 0.02993 0.03118 = 0.02916 -0.00684 0.00447 0.01103 AFIX 43 H3 2 0.109301 0.255836 0.481263 11.00000 -1.20000 AFIX 0 C4 1 0.082994 0.338363 0.567205 11.00000 0.02320 0.03001 = 0.01841 -0.00730 -0.00826 0.01246 C7 1 0.039365 0.234761 0.615144 11.00000 0.02821 0.02060 = 0.02747 -0.00505 -0.01143 0.01321 C6 1 0.132518 0.536536 0.536575 11.00000 0.02857 0.03040 = 0.02522 -0.00229 -0.00744 0.01580 AFIX 43 H6 2 0.139475 0.609197 0.550159 11.00000 -1.20000 AFIX 0 C5 1 0.091564 0.446474 0.587143 11.00000 0.02578 0.02829 = 0.01552 -0.00242 -0.00594 0.01505 HKLF 4 REM ZNZ1252_NiO_0m_a.res in P6(3)/m REM wR2 = 0.213424, GooF = S = 1.02078, Restrained GooF = 1.02047 for all data REM R1 = 0.068254 for 1442 Fo > 4sig(Fo) and 0.076677 for all 1679 data REM 118 parameters refined using 1 restraints END WGHT 0.1108 32.7040 REM Instructions for potential hydrogen bonds HTAB O3 O2 EQIV $2 x, y, -z+3/2 HTAB O3 O2_$2 REM Highest difference peak 2.972, deepest hole -2.100, 1-sigma level 0.206 Q1 1 0.0891 0.3869 0.7500 10.50000 0.05 2.97 Q2 1 0.1215 0.5179 0.6710 11.00000 0.05 1.49 Q3 1 -0.2136 0.0057 0.7275 11.00000 0.05 0.86 Q4 1 0.0710 0.2676 0.6784 11.00000 0.05 0.75 Q5 1 0.3333 0.6667 0.7660 10.33333 0.05 0.65 Q6 1 -0.1313 0.0140 0.7197 11.00000 0.05 0.61 Q7 1 0.1096 0.3390 0.5302 11.00000 0.05 0.55 Q8 1 0.0749 0.1466 0.5732 11.00000 0.05 0.54 Q9 1 0.1576 0.4644 0.4588 11.00000 0.05 0.54 Q10 1 0.0888 0.3860 0.5784 11.00000 0.05 0.52 Q11 1 0.0323 0.1654 0.5564 11.00000 0.05 0.50 Q12 1 0.0000 0.0000 0.7256 10.33333 0.05 0.50 Q13 1 0.2586 0.5383 0.7500 10.50000 0.05 0.49 Q14 1 0.0731 0.1736 0.6039 11.00000 0.05 0.49 Q15 1 -0.0157 0.2633 0.6787 11.00000 0.05 0.49 Q16 1 0.0889 0.3048 0.5996 11.00000 0.05 0.48 Q17 1 -0.1973 -0.0601 0.7500 10.50000 0.05 0.47 Q18 1 0.2312 0.5842 0.6894 11.00000 0.05 0.46 Q19 1 0.0396 0.0987 0.6872 11.00000 0.05 0.45 Q20 1 0.3262 0.7170 0.7823 11.00000 0.05 0.44 ; _shelx_res_checksum 69575 _shelx_fab_file ; -1 2 0 7.70 0.00 0 2 0 -32.13 0.00 -2 3 0 -5.66 0.00 -1 3 0 -7.81 0.00 0 3 0 41.37 0.00 -3 4 0 -1.27 0.00 -2 4 0 -0.77 0.00 -1 4 0 6.60 0.00 0 4 0 9.43 0.00 -4 5 0 -3.99 0.00 -3 5 0 -3.75 0.00 -2 5 0 -12.15 0.00 -1 5 0 -0.50 0.00 0 5 0 -10.22 0.00 -5 6 0 -1.08 0.00 -4 6 0 2.15 0.00 -3 6 0 -0.14 0.00 -2 6 0 -1.85 0.00 -1 6 0 2.42 0.00 0 6 0 -1.12 0.00 -6 7 0 0.24 0.00 -5 7 0 1.57 0.00 -4 7 0 3.62 0.00 -3 7 0 0.14 0.00 -2 7 0 5.53 0.00 -1 7 0 -1.50 0.00 0 7 0 -1.17 0.00 -7 8 0 1.44 0.00 -6 8 0 1.76 0.00 -5 8 0 0.56 0.00 -4 8 0 -0.77 0.00 -3 8 0 0.09 0.00 -2 8 0 0.39 0.00 -1 8 0 0.20 0.00 0 8 0 0.04 0.00 -8 9 0 3.03 0.00 -7 9 0 -0.29 0.00 -6 9 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17 -0.45 0.00 0 5 17 -0.11 0.00 -5 6 17 -0.30 0.00 -4 6 17 -0.20 0.00 -3 6 17 1.19 0.00 -2 6 17 1.57 0.00 -1 6 17 -0.80 0.00 0 6 17 -0.37 0.00 -6 7 17 -1.97 0.00 -5 7 17 -2.31 0.00 -4 7 17 -0.86 0.00 -3 7 17 -1.21 0.00 -2 7 17 -1.47 0.00 -1 7 17 -0.44 0.00 0 7 17 -0.82 0.00 -7 8 17 -0.41 0.00 -6 8 17 0.64 0.00 -5 8 17 1.08 0.00 -4 8 17 -0.11 0.00 -3 8 17 0.29 0.00 -2 8 17 -1.09 0.00 -1 8 17 0.32 0.00 0 8 17 0.50 0.00 -7 9 17 0.69 0.00 -6 9 17 1.96 0.00 -5 9 17 -0.01 0.00 -4 9 17 -0.07 0.00 -3 9 17 0.92 0.00 -2 9 17 2.58 0.00 0 0 18 -1.36 0.00 0 1 18 1.19 0.00 -1 2 18 -0.57 0.00 0 2 18 0.13 0.00 -2 3 18 -0.65 0.00 -1 3 18 -1.22 0.00 0 3 18 -0.30 0.00 -3 4 18 -0.17 0.00 -2 4 18 0.56 0.00 -1 4 18 0.23 0.00 0 4 18 1.04 0.00 -4 5 18 2.53 0.00 -3 5 18 0.02 0.00 -2 5 18 -1.53 0.00 -1 5 18 2.38 0.00 0 5 18 1.33 0.00 -5 6 18 -1.43 0.00 -4 6 18 -2.75 0.00 -3 6 18 -0.17 0.00 -2 6 18 -0.19 0.00 -1 6 18 -1.93 0.00 0 6 18 -1.05 0.00 -6 7 18 -0.13 0.00 -5 7 18 -0.25 0.00 -4 7 18 1.07 0.00 -3 7 18 -0.21 0.00 -2 7 18 -0.22 0.00 -1 7 18 -1.12 0.00 0 7 18 -0.53 0.00 -7 8 18 1.55 0.00 -6 8 18 1.30 0.00 -5 8 18 0.67 0.00 -4 8 18 1.71 0.00 -3 8 18 1.04 0.00 -2 8 18 0.51 0.00 -1 8 18 1.26 0.00 0 1 19 -1.81 0.00 -1 2 19 0.36 0.00 0 2 19 0.36 0.00 -2 3 19 -0.02 0.00 -1 3 19 0.71 0.00 0 3 19 0.25 0.00 -3 4 19 1.40 0.00 -2 4 19 1.98 0.00 -1 4 19 -0.82 0.00 0 4 19 0.29 0.00 -4 5 19 -0.54 0.00 -3 5 19 -2.79 0.00 -2 5 19 -0.65 0.00 -1 5 19 0.45 0.00 0 5 19 -0.18 0.00 -5 6 19 -0.19 0.00 -4 6 19 0.28 0.00 -3 6 19 -0.42 0.00 -2 6 19 -1.71 0.00 -1 6 19 0.48 0.00 0 6 19 0.28 0.00 -6 7 19 0.89 0.00 -5 7 19 2.56 0.00 -4 7 19 0.65 0.00 -3 7 19 0.75 0.00 -2 7 19 2.04 0.00 -1 7 19 -0.05 0.00 0 0 20 1.58 0.00 0 1 20 -0.97 0.00 -1 2 20 0.96 0.00 0 2 20 -0.38 0.00 -2 3 20 0.33 0.00 -1 3 20 0.29 0.00 0 3 20 -0.08 0.00 -3 4 20 0.72 0.00 -2 4 20 -0.65 0.00 -1 4 20 -0.04 0.00 0 4 20 -0.04 0.00 -4 5 20 -1.97 0.00 -3 5 20 -0.47 0.00 -2 5 20 1.72 0.00 -1 5 20 -1.51 0.00 0 5 20 -0.75 0.00 -4 6 20 1.70 0.00 -3 6 20 -0.27 0.00 -2 6 20 -0.23 0.00 0 1 21 1.64 0.00 -1 2 21 -0.48 0.00 0 2 21 -0.28 0.00 -2 3 21 0.68 0.00 -1 3 21 -0.05 0.00 0 3 21 -0.30 0.00 -2 4 21 -1.00 0.00 0 1 0 -18.86 0.00 0 0 2 -116.31 0.00 -13 14 3 -0.82 0.00 -1 14 3 -0.61 0.00 -11 15 4 0.46 0.00 -4 15 4 0.59 0.00 -12 14 6 -0.46 0.00 -2 14 6 -0.06 0.00 -9 15 6 0.86 0.00 -6 15 6 1.00 0.00 -10 14 9 1.32 0.00 -4 14 9 0.16 0.00 -11 13 10 0.61 0.00 -2 13 10 1.09 0.00 -8 14 10 -0.74 0.00 -7 14 10 -0.30 0.00 -6 14 10 0.51 0.00 -10 13 11 -0.53 0.00 -3 13 11 0.92 0.00 -8 13 12 -1.65 0.00 -5 13 12 -0.38 0.00 0 11 13 0.14 0.00 -10 11 14 0.34 0.00 -1 11 14 -0.92 0.00 -7 12 14 -0.14 0.00 -5 12 14 -0.45 0.00 0 10 15 0.10 0.00 -8 9 17 1.14 0.00 -1 9 17 0.30 0.00 -5 10 17 0.14 0.00 -5 9 18 -1.36 0.00 -4 9 18 -0.21 0.00 -5 6 20 1.01 0.00 -1 6 20 1.05 0.00 -3 4 21 -0.61 0.00 -1 4 21 0.72 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 201118) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 0.667 0.250 267 60 ' ' 2 -0.333 0.333 0.750 267 60 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 1 0 1.781 0 0 2 2.224 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL ZNZ1252_NiO_0m P 63/m R = 0.08 CELL 13.2027 13.2027 18.3116 90.00 90.00 120.00 SPGR P63/m # Solvent Accessible Volume = 537 # Electrons Found in S.A.V. = 120 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others Q101 0.704 0.094 0.247 ! 3.64 eA-3 C102 0.708 0.391 0.744 ! 2.42 eA-3 Q103 0.264 0.922 0.254 ! 2.17 eA-3 Q104 0.718 0.672 0.251 ! 1.98 eA-3 Q105 0.768 0.764 0.282 ! 1.80 eA-3 Q106 0.608 0.123 0.169 ! 1.61 eA-3 Q107 1.003 0.359 0.749 ! 1.38 eA-3 Q108 0.984 0.703 0.241 ! 1.35 eA-3 C109 0.280 0.797 0.251 ! 1.23 eA-3 C110 0.403 0.766 0.250 ! 0.93 eA-3 Q111 0.984 0.254 0.815 ! 0.90 eA-3 C112 0.236 0.628 0.297 ! 0.78 eA-3 Q113 0.813 0.087 0.307 ! 0.76 eA-3 Q114 0.186 0.297 0.753 ! 0.70 eA-3 Q115 0.014 0.159 0.283 ! 0.68 eA-3 Q116 0.578 0.599 0.673 ! 0.67 eA-3 Q117 0.845 0.879 0.888 ! 0.66 eA-3 Q118 0.579 0.022 0.203 ! 0.66 eA-3 Q119 1.001 0.891 0.091 ! 0.64 eA-3 Q120 0.281 0.234 0.833 ! 0.63 eA-3 Q121 0.343 0.244 0.028 ! 0.60 eA-3 Q122 0.389 0.844 0.247 ! 0.58 eA-3 Q123 0.939 0.325 0.330 ! 0.58 eA-3 Q124 0.037 0.172 0.932 ! 0.58 eA-3 Q125 0.127 0.995 0.545 ! 0.57 eA-3 Q126 1.004 0.030 0.497 ! 0.57 eA-3 Q127 0.534 0.027 0.173 ! 0.55 eA-3 Q128 0.032 0.389 0.215 ! 0.55 eA-3 Q129 0.798 0.938 0.750 ! 0.54 eA-3 Q130 0.511 0.422 0.254 ! 0.53 eA-3 Q131 0.915 0.708 0.098 ! 0.52 eA-3 Q132 0.472 0.290 0.970 ! 0.52 eA-3 Q133 0.911 0.906 0.250 ! 0.51 eA-3 Q134 0.084 0.390 0.919 ! 0.51 eA-3 Q135 0.076 0.147 0.938 ! 0.51 eA-3 ) ; _shelx_fab_checksum 12439 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -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_adp_type _atom_site_calc_flag _atom_site_occupancy Ni Ni1 0.000000 0.000000 0.66416(11) 0.0402(6) Uani d 1 Na Na1 0.000000 0.000000 0.500000 0.0176(14) Uani d 1 O O1 0.0313(5) 0.1424(5) 0.5905(3) 0.0274(12) Uani d 1 C C1 0.1634(7) 0.5226(7) 0.4667(5) 0.0321(19) Uani d 1 H H1 0.189294 0.584615 0.432392 0.039 Uiso calc 1 S S1 0.04395(18) 0.47486(16) 0.67157(10) 0.0244(5) Uani d 1 Ni Ni2 0.02284(14) 0.34698(12) 0.750000 0.0270(5) Uani d 1 O O2 0.0062(6) 0.2348(5) 0.6813(3) 0.0363(15) Uani d 1 C C2 0.1567(8) 0.4172(9) 0.4466(5) 0.040(2) Uani d 1 H H2 0.180219 0.407978 0.399222 0.048 Uiso calc 1 O O3 -0.1104(7) 0.0167(7) 0.750000 0.042(2) Uani d 1 H H3A -0.080237 0.090589 0.750000 0.063 Uiso d 1 Ni Ni3 0.18990(13) 0.57426(12) 0.750000 0.0269(5) Uani d 1 Cl Cl3 0.333333 0.666667 0.82575(19) 0.0317(8) Uani d 1 C C3 0.1158(7) 0.3279(8) 0.4958(4) 0.0320(19) Uani d 1 H H3 0.109301 0.255836 0.481263 0.038 Uiso calc 1 C C4 0.0830(6) 0.3384(7) 0.5672(4) 0.0242(16) Uani d 1 C C7 0.0394(7) 0.2348(6) 0.6151(4) 0.0250(17) Uani d 1 C C6 0.1325(7) 0.5365(7) 0.5366(4) 0.0276(17) Uani d 1 H H6 0.139475 0.609197 0.550159 0.033 Uiso calc 1 C C5 0.0916(6) 0.4465(7) 0.5871(4) 0.0225(16) Uani 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 0.0446(8) 0.0446(8) 0.0312(12) 0.0223(4) 0.000 0.000 Na1 0.021(2) 0.021(2) 0.011(3) 0.0105(10) 0.000 0.000 O1 0.029(3) 0.027(3) 0.029(3) 0.016(2) -0.009(2) -0.013(2) C1 0.029(4) 0.030(4) 0.026(4) 0.006(3) -0.002(3) 0.004(3) S1 0.0367(11) 0.0255(10) 0.0168(10) 0.0198(9) -0.0023(8) -0.0010(7) Ni2 0.0475(10) 0.0231(8) 0.0158(7) 0.0217(7) 0.000 0.000 O2 0.073(4) 0.025(3) 0.016(3) 0.028(3) -0.001(3) -0.002(2) C2 0.040(5) 0.053(6) 0.022(4) 0.018(4) 0.003(4) -0.007(4) O3 0.025(4) 0.023(4) 0.080(7) 0.013(4) 0.000 0.000 Ni3 0.0299(8) 0.0274(8) 0.0227(8) 0.0139(6) 0.000 0.000 Cl3 0.0356(12) 0.0356(12) 0.0241(17) 0.0178(6) 0.000 0.000 C3 0.030(4) 0.031(4) 0.029(4) 0.011(4) 0.004(3) -0.007(3) C4 0.023(4) 0.030(4) 0.018(4) 0.012(3) -0.008(3) -0.007(3) C7 0.028(4) 0.021(4) 0.027(4) 0.013(3) -0.011(3) -0.005(3) C6 0.029(4) 0.030(4) 0.025(4) 0.016(3) -0.007(3) -0.002(3) C5 0.026(4) 0.028(4) 0.016(4) 0.015(3) -0.006(3) -0.002(3) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 O1 Ni1 O1 2 3 85.7(2) O1 Ni1 O1 2 . 85.7(2) O1 Ni1 O1 3 . 85.7(2) O1 Ni1 O3 2 3 172.3(2) O1 Ni1 O3 3 3 101.7(2) O1 Ni1 O3 . 3 96.7(2) O1 Ni1 O3 2 2 101.7(2) O1 Ni1 O3 3 2 96.7(2) O1 Ni1 O3 . 2 172.3(2) O3 Ni1 O3 3 2 75.7(2) O1 Ni1 O3 2 . 96.7(2) O1 Ni1 O3 3 . 172.3(2) O1 Ni1 O3 . . 101.7(2) O3 Ni1 O3 3 . 75.7(2) O3 Ni1 O3 2 . 75.7(2) O1 Ni1 Na1 2 . 51.76(14) O1 Ni1 Na1 3 . 51.76(14) O1 Ni1 Na1 . . 51.76(14) O3 Ni1 Na1 3 . 134.86(15) O3 Ni1 Na1 2 . 134.86(15) O3 Ni1 Na1 . . 134.86(15) O1 Na1 O1 7_556 9_556 76.9(2) O1 Na1 O1 7_556 3 103.1(2) O1 Na1 O1 9_556 3 180.0(2) O1 Na1 O1 7_556 8_556 76.9(2) O1 Na1 O1 9_556 8_556 76.9(2) O1 Na1 O1 3 8_556 103.1(2) O1 Na1 O1 7_556 2 103.1(2) O1 Na1 O1 9_556 2 103.1(2) O1 Na1 O1 3 2 76.9(2) O1 Na1 O1 8_556 2 180.0 O1 Na1 O1 7_556 . 180.0 O1 Na1 O1 9_556 . 103.1(2) O1 Na1 O1 3 . 76.9(2) O1 Na1 O1 8_556 . 103.1(2) O1 Na1 O1 2 . 76.9(2) O1 Na1 Ni1 7_556 7_556 45.91(14) O1 Na1 Ni1 9_556 7_556 45.91(14) O1 Na1 Ni1 3 7_556 134.09(14) O1 Na1 Ni1 8_556 7_556 45.91(14) O1 Na1 Ni1 2 7_556 134.09(14) O1 Na1 Ni1 . 7_556 134.09(14) O1 Na1 Ni1 7_556 . 134.09(14) O1 Na1 Ni1 9_556 . 134.09(14) O1 Na1 Ni1 3 . 45.91(14) O1 Na1 Ni1 8_556 . 134.09(14) O1 Na1 Ni1 2 . 45.91(14) O1 Na1 Ni1 . . 45.91(14) Ni1 Na1 Ni1 7_556 . 180.0 C7 O1 Ni1 . . 120.3(5) C7 O1 Na1 . . 156.2(5) Ni1 O1 Na1 . . 82.32(18) C6 C1 C2 . . 120.0(8) C6 C1 H1 . . 120.0 C2 C1 H1 . . 120.0 C5 S1 Ni2 . . 109.9(3) C5 S1 Ni3 . . 113.1(3) Ni2 S1 Ni3 . . 76.34(8) O2 Ni2 O2 . 10_557 84.5(3) O2 Ni2 S1 . 10_557 179.2(2) O2 Ni2 S1 10_557 10_557 95.24(17) O2 Ni2 S1 . . 95.24(17) O2 Ni2 S1 10_557 . 179.2(2) S1 Ni2 S1 10_557 . 84.98(11) O2 Ni2 Ni3 . . 126.1(2) O2 Ni2 Ni3 10_557 . 126.1(2) S1 Ni2 Ni3 10_557 . 53.55(6) S1 Ni2 Ni3 . . 53.55(6) C7 O2 Ni2 . . 136.7(5) C3 C2 C1 . . 119.2(8) C3 C2 H2 . . 120.4 C1 C2 H2 . . 120.4 Ni1 O3 Ni1 . 10_557 89.7(3) Ni1 O3 H3A . . 99.1 Ni1 O3 H3A 10_557 . 99.1 Cl3 Ni3 Cl3 . 10_557 79.68(15) Cl3 Ni3 S1 . 10_557 100.02(9) Cl3 Ni3 S1 10_557 10_557 178.18(9) Cl3 Ni3 S1 . . 178.18(9) Cl3 Ni3 S1 10_557 . 100.02(9) S1 Ni3 S1 10_557 . 80.22(11) Cl3 Ni3 Ni2 . . 128.77(7) Cl3 Ni3 Ni2 10_557 . 128.77(7) S1 Ni3 Ni2 10_557 . 50.11(6) S1 Ni3 Ni2 . . 50.11(6) Cl3 Ni3 Ni3 . 3_565 48.32(5) Cl3 Ni3 Ni3 10_557 3_565 48.32(5) S1 Ni3 Ni3 10_557 3_565 132.64(7) S1 Ni3 Ni3 . 3_565 132.64(7) Ni2 Ni3 Ni3 . 3_565 174.64(8) Cl3 Ni3 Ni3 . 2_665 48.32(5) Cl3 Ni3 Ni3 10_557 2_665 48.32(5) S1 Ni3 Ni3 10_557 2_665 130.25(7) S1 Ni3 Ni3 . 2_665 130.25(7) Ni2 Ni3 Ni3 . 2_665 114.64(8) Ni3 Ni3 Ni3 3_565 2_665 59.9990(10) Ni3 Cl3 Ni3 3_565 2_665 83.36(11) Ni3 Cl3 Ni3 3_565 . 83.36(11) Ni3 Cl3 Ni3 2_665 . 83.36(11) C2 C3 C4 . . 122.6(8) C2 C3 H3 . . 118.7 C4 C3 H3 . . 118.7 C3 C4 C5 . . 117.6(7) C3 C4 C7 . . 117.3(7) C5 C4 C7 . . 125.1(7) O1 C7 O2 . . 118.4(7) O1 C7 C4 . . 119.4(7) O2 C7 C4 . . 122.2(7) C1 C6 C5 . . 121.2(8) C1 C6 H6 . . 119.4 C5 C6 H6 . . 119.4 C6 C5 C4 . . 119.4(7) C6 C5 S1 . . 115.3(6) C4 C5 S1 . . 125.2(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Ni1 O1 2 2.179(6) Ni1 O1 3 2.179(6) Ni1 O1 . 2.179(6) Ni1 O3 3 2.229(6) Ni1 O3 2 2.229(6) Ni1 O3 . 2.229(6) Ni1 Na1 . 3.006(2) Na1 O1 7_556 2.382(5) Na1 O1 9_556 2.382(5) Na1 O1 3 2.382(5) Na1 O1 8_556 2.382(5) Na1 O1 2 2.382(5) Na1 O1 . 2.382(5) O1 C7 . 1.254(9) C1 C6 . 1.383(12) C1 C2 . 1.398(13) C1 H1 . 0.9500 S1 C5 . 1.778(8) S1 Ni2 . 2.126(2) S1 Ni3 . 2.229(2) Ni2 O2 . 1.870(5) Ni2 O2 10_557 1.870(5) Ni2 Ni3 . 2.693(2) O2 C7 . 1.288(10) C2 C3 . 1.362(13) C2 H2 . 0.9500 O3 H3A . 0.8498 Ni3 Cl3 . 2.165(2) Ni3 Cl3 10_557 2.165(2) Ni3 Ni3 3_565 2.880(3) Ni3 Ni3 2_665 2.880(3) C3 C4 . 1.406(11) C3 H3 . 0.9500 C4 C5 . 1.422(11) C4 C7 . 1.478(11) C6 C5 . 1.386(11) C6 H6 . 0.9500 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 O2 Ni2 O2 C7 10_557 -152.7(7) S1 Ni2 O2 C7 . 26.6(8) Ni3 Ni2 O2 C7 . -21.3(9) C6 C1 C2 C3 . 2.1(13) C1 C2 C3 C4 . -1.8(14) C2 C3 C4 C5 . 1.1(12) C2 C3 C4 C7 . 179.6(8) Ni1 O1 C7 O2 . -13.5(9) Na1 O1 C7 O2 . 146.1(10) Ni1 O1 C7 C4 . 168.2(5) Na1 O1 C7 C4 . -32.1(17) Ni2 O2 C7 O1 . 165.9(6) Ni2 O2 C7 C4 . -15.8(13) C3 C4 C7 O1 . -1.3(11) C5 C4 C7 O1 . 177.1(7) C3 C4 C7 O2 . -179.5(8) C5 C4 C7 O2 . -1.1(12) C2 C1 C6 C5 . -1.7(12) C1 C6 C5 C4 . 1.0(11) C1 C6 C5 S1 . -174.8(6) C3 C4 C5 C6 . -0.7(11) C7 C4 C5 C6 . -179.1(7) C3 C4 C5 S1 . 174.7(6) C7 C4 C5 S1 . -3.7(11) Ni2 S1 C5 C6 . -166.7(5) Ni3 S1 C5 C6 . -83.5(6) Ni2 S1 C5 C4 . 17.8(7) Ni3 S1 C5 C4 . 100.9(6) _cod_database_fobs_code 2021660