#------------------------------------------------------------------------------ #$Date: 2022-02-09 11:49:22 +0200 (Wed, 09 Feb 2022) $ #$Revision: 272871 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/45/8104551.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8104551 loop_ _publ_author_name 'Dey, Lucky' 'Rabi, Saswata' 'Begum, Zinnat A.' 'Takase, Tsugiko' 'Rahman, Ismail M.M.' 'Tiekink, Edward R.T.' 'Roy, Tapashi Ghosh' _publ_section_title ; Redetermination of the crystal structure of bis[N,N′-ethylenebis(acetylacetoniminato)nickel(II)] sodium perchlorate, C24H36ClN4NaNi2O8 ; _journal_issue 6 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 1147 _journal_page_last 1150 _journal_paper_doi 10.1515/ncrs-2021-0254 _journal_volume 236 _journal_year 2021 _chemical_formula_moiety 'C24 H36 Cl N4 Na Ni2 O8' _chemical_formula_sum 'C24 H36 Cl N4 Na Ni2 O8' _chemical_formula_weight 684.43 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 112.0320(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.5909(11) _cell_length_b 10.8023(6) _cell_length_c 14.5722(8) _cell_measurement_reflns_used 13693 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 27.59 _cell_measurement_theta_min 3.14 _cell_volume 2858.7(3) _computing_cell_refinement 'CrystalClear [2]' _computing_data_collection 'CrystalClear [2]' _computing_data_reduction 'CrystalClear [2]' _computing_molecular_graphics 'ORTEP-3 for Windows [5]' _computing_publication_material 'SHELXL-2018/3 [4]' _computing_structure_refinement 'SHELXL-2018/3 [4]' _computing_structure_solution 'SHELXS [3]' _diffrn_ambient_temperature 93(2) _diffrn_detector_area_resol_mean 7.111 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0246 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 14344 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.476 _diffrn_reflns_theta_min 3.373 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_T_max 0.732 _exptl_absorpt_correction_T_min 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB [1]' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.590 _exptl_crystal_description block _exptl_crystal_F_000 1424 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.400 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 3261 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0260 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+2.3767P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.0701 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3129 _reflns_number_total 3261 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_j_ncrs-2021-0254_suppl.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 8104551 _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_estimated_absorpt_t_min 0.756 _shelx_estimated_absorpt_t_max 0.756 _shelx_res_file ; TITL t6 shelx.res created by SHELXL-2018/3 at 10:04:32 on 17-Mar-2021 CELL 0.71075 19.5909 10.8023 14.5722 90.000 112.032 90.000 ZERR 4 0.0011 0.0006 0.0008 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H CL N NI O NA UNIT 96 144 4 16 8 32 4 MERG 2 FMAP 2 PLAN 5 SIZE 0.200 0.200 0.200 ACTA BOND $H CONF L.S. 18 TEMP -180 OMIT -1 1 6 WGHT 0.040900 2.376700 FVAR 0.39612 NI 5 0.674619 0.656125 0.826712 11.00000 0.01068 0.01916 = 0.01728 0.00103 0.00455 0.00022 O1 6 0.607876 0.724557 0.710324 11.00000 0.01454 0.02569 = 0.02128 0.00431 0.00588 0.00046 O2 6 0.589988 0.596403 0.839931 11.00000 0.01413 0.02656 = 0.02162 0.00461 0.00692 0.00100 N1 4 0.757574 0.715687 0.809153 11.00000 0.01367 0.01921 = 0.02468 0.00104 0.00647 0.00000 N2 4 0.738187 0.589257 0.945632 11.00000 0.01394 0.02071 = 0.01918 -0.00142 0.00466 0.00100 C1 1 0.624078 0.791987 0.647386 11.00000 0.02065 0.01993 = 0.02004 0.00132 0.00776 0.00226 C2 1 0.694226 0.822867 0.657286 11.00000 0.02316 0.02318 = 0.02821 0.00580 0.01304 0.00186 AFIX 43 H2 2 0.699881 0.874073 0.607606 11.00000 -1.20000 AFIX 0 C3 1 0.758979 0.784460 0.735756 11.00000 0.01869 0.01908 = 0.03070 0.00103 0.01231 -0.00025 C4 1 0.826982 0.666416 0.881104 11.00000 0.01321 0.03030 = 0.02971 0.00580 0.00519 0.00053 AFIX 23 H4A 2 0.866150 0.729908 0.896655 11.00000 -1.20000 H4B 2 0.842624 0.593109 0.853181 11.00000 -1.20000 AFIX 0 C5 1 0.814657 0.630910 0.973574 11.00000 0.01330 0.02500 = 0.02253 -0.00251 0.00257 0.00010 AFIX 23 H5A 2 0.848873 0.563636 1.008442 11.00000 -1.20000 H5B 2 0.824057 0.702938 1.018655 11.00000 -1.20000 AFIX 0 C6 1 0.720065 0.523472 1.008619 11.00000 0.01953 0.02214 = 0.01926 0.00001 0.00558 0.00270 C7 1 0.646636 0.484407 0.988149 11.00000 0.02228 0.02844 = 0.02115 0.00478 0.00880 0.00019 AFIX 43 H7 2 0.638224 0.430687 1.034448 11.00000 -1.20000 AFIX 0 C8 1 0.587142 0.518605 0.906517 11.00000 0.01859 0.02543 = 0.02268 0.00061 0.01112 -0.00009 C9 1 0.559151 0.836257 0.559459 11.00000 0.02463 0.03272 = 0.02384 0.00605 0.00684 0.00420 AFIX 137 H9A 2 0.520992 0.772111 0.539704 11.00000 -1.50000 H9B 2 0.574860 0.853528 0.504330 11.00000 -1.50000 H9C 2 0.539327 0.911954 0.577096 11.00000 -1.50000 AFIX 0 C10 1 0.831174 0.825801 0.731896 11.00000 0.02029 0.03241 = 0.04767 0.01292 0.01599 -0.00075 AFIX 137 H10A 2 0.855965 0.881642 0.787464 11.00000 -1.50000 H10B 2 0.822188 0.869280 0.669411 11.00000 -1.50000 H10C 2 0.862402 0.753415 0.736296 11.00000 -1.50000 AFIX 0 C11 1 0.777441 0.484043 1.106011 11.00000 0.02356 0.03543 = 0.02345 0.00769 0.00406 0.00281 AFIX 137 H11A 2 0.810566 0.423580 1.094259 11.00000 -1.50000 H11B 2 0.753314 0.446412 1.147139 11.00000 -1.50000 H11C 2 0.805829 0.556444 1.140091 11.00000 -1.50000 AFIX 0 C12 1 0.512347 0.464343 0.886145 11.00000 0.01939 0.04142 = 0.03034 0.00752 0.01045 -0.00404 AFIX 137 H12A 2 0.475258 0.530180 0.865340 11.00000 -1.50000 H12B 2 0.511615 0.425025 0.946377 11.00000 -1.50000 H12C 2 0.501329 0.402391 0.833417 11.00000 -1.50000 AFIX 0 NA1 7 0.500000 0.737699 0.750000 10.50000 0.01221 0.02593 = 0.02705 0.00000 0.00527 0.00000 CL1 3 0.500000 1.022550 0.750000 10.50000 0.01918 0.03139 = 0.02886 0.00000 0.00717 0.00000 O3 6 0.548123 0.942323 0.826272 11.00000 0.02247 0.04446 = 0.03753 0.00214 -0.00053 0.00405 O4 6 0.542173 1.095858 0.709700 11.00000 0.06281 0.05788 = 0.06068 0.00318 0.02910 -0.02936 HKLF 4 REM t6 REM wR2 = 0.0701, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0260 for 3129 Fo > 4sig(Fo) and 0.0269 for all 3261 data REM 186 parameters refined using 0 restraints END WGHT 0.0405 2.3992 REM Highest difference peak 0.400, deepest hole -0.783, 1-sigma level 0.066 Q1 1 0.6991 0.6515 0.9015 11.00000 0.05 0.40 Q2 1 0.8188 0.6454 0.9225 11.00000 0.05 0.38 Q3 1 0.6759 0.5671 0.8323 11.00000 0.05 0.35 Q4 1 0.6477 0.6550 0.7501 11.00000 0.05 0.34 Q5 1 0.5926 0.8074 0.5969 11.00000 0.05 0.33 ; _shelx_res_checksum 20025 _shelx_hkl_file ; 0 0 3 -0.11 0.58 0 0 3 1.17 0.40 0 0 3 1.58 0.40 0 0 4 22.05 0.88 0 0 4 22.82 1.57 0 0 5 0.88 0.97 0 0 5 1.68 0.47 0 0 6 4107.46 203.50 0 0 6 4046.16 196.17 0 0 7 0.30 0.96 0 0 7 0.80 0.62 0 0 -7 1.71 0.71 0 0 8 306.26 8.75 0 0 8 308.23 9.90 0 0 -8 313.10 9.31 0 0 9 0.57 1.13 0 0 9 0.72 0.57 0 0 -9 3.06 0.80 0 0 10 225.14 8.09 0 0 10 219.35 6.47 0 0 -10 232.26 7.52 0 0 11 -0.73 0.67 0 0 11 -0.72 1.30 0 0 -11 1.18 0.86 0 0 12 2335.27 107.60 0 0 -12 2207.53 98.78 0 0 13 0.82 2.00 0 0 -13 -0.02 0.88 0 0 14 1203.82 50.17 0 0 15 0.64 1.74 0 0 16 58.19 5.52 0 0 17 1.36 1.98 0 2 0 18.00 0.87 0 2 0 19.32 1.02 0 2 0 18.96 0.76 0 -2 0 19.79 0.80 0 -2 0 22.00 0.85 0 -2 0 20.60 1.06 0 2 1 7773.35 449.10 0 2 -1 7847.52 453.45 0 -2 1 7167.93 413.53 0 -2 -1 7026.66 405.99 0 2 -2 8259.47 495.49 0 -2 2 8017.66 476.98 0 -2 2 8687.25 519.66 0 2 3 24.97 1.43 0 2 -3 22.40 0.81 0 2 -3 24.78 1.28 0 -2 3 23.15 1.44 0 -2 -3 24.41 1.12 0 -2 -3 29.67 1.68 0 -2 -3 26.28 0.94 0 2 4 91.17 2.88 0 2 -4 87.69 1.88 0 2 -4 107.29 3.46 0 -2 4 94.91 3.09 0 -2 -4 91.49 2.88 0 -2 -4 87.28 2.31 0 2 5 1230.64 44.29 0 2 5 1052.98 36.81 0 2 5 1198.71 42.63 0 2 -5 1266.70 45.82 0 -2 5 1204.88 43.05 0 -2 -5 1213.70 42.16 0 2 -6 213.61 6.88 0 2 6 208.34 6.17 0 2 6 218.99 7.31 0 -2 6 207.02 6.27 0 -2 -6 213.41 5.79 0 2 7 2972.40 134.85 0 2 -7 3002.54 137.80 0 2 7 2951.78 135.98 0 -2 -7 3085.22 138.57 0 -2 7 3047.36 140.60 0 2 8 818.77 28.96 0 2 8 795.13 27.09 0 2 -8 808.11 28.36 0 -2 8 837.28 30.09 0 -2 -8 824.64 27.30 0 2 -9 273.14 9.26 0 2 9 261.63 8.30 0 2 9 272.49 9.31 0 -2 9 285.25 10.31 0 -2 -9 271.41 7.85 0 2 10 225.57 8.17 0 2 10 225.26 7.17 0 2 -10 219.37 7.80 0 -2 10 229.15 8.10 0 -2 -10 225.27 6.63 0 2 11 64.62 3.75 0 2 -11 73.37 3.60 0 2 11 70.41 3.19 0 -2 -11 68.43 2.49 0 -2 11 81.01 3.95 0 2 -12 19.29 2.23 0 2 12 21.51 2.48 0 2 12 14.11 1.49 0 -2 12 18.12 3.11 0 2 13 739.34 28.83 0 2 -13 783.30 29.63 0 -2 13 822.21 33.14 0 2 14 4.19 1.95 0 2 -14 2.60 1.65 0 -2 14 3.60 1.92 0 2 15 236.03 10.43 0 -2 15 263.05 12.26 0 2 16 4.80 2.99 0 -2 16 4.26 2.24 0 2 17 37.20 4.66 0 -2 17 44.36 5.09 0 4 0 21.77 1.36 0 4 0 23.10 1.47 0 -4 0 19.28 1.47 0 4 1 234.50 6.72 0 4 1 224.01 6.37 0 4 -1 227.52 6.47 0 4 -1 237.72 7.26 0 -4 -1 214.74 6.54 0 -4 1 253.38 7.28 0 4 2 7.05 0.96 0 4 2 8.04 0.92 0 4 -2 5.28 0.75 0 4 -2 5.91 0.94 0 -4 2 6.03 1.09 0 -4 -2 5.12 0.87 0 4 3 42.12 1.64 0 4 -3 38.54 1.50 0 4 3 38.64 1.73 0 4 -3 40.99 2.32 0 -4 -3 37.97 1.67 0 -4 3 46.95 2.09 0 4 -4 1664.44 66.40 0 4 4 1612.40 63.86 0 4 4 1873.52 72.65 0 4 -4 1727.46 66.18 0 -4 4 1830.97 72.28 0 -4 -4 1678.15 66.82 0 4 5 2461.59 106.42 0 4 -5 2582.87 112.45 0 4 -5 2106.60 90.89 0 4 -5 2627.90 110.28 0 -4 5 2662.32 115.51 0 -4 -5 2379.32 101.49 0 -4 -5 2561.68 111.64 0 -4 -5 2560.25 108.70 0 4 -6 3653.28 174.41 0 4 6 3528.92 167.41 0 4 -6 3543.98 162.52 0 4 -6 2845.72 133.38 0 -4 -6 3595.73 170.26 0 -4 -6 3214.92 150.85 0 -4 -6 3453.42 160.55 0 -4 6 3739.01 177.99 0 4 7 1751.32 69.86 0 4 -7 1657.51 67.67 0 -4 7 1844.19 73.71 0 -4 -7 1621.21 62.26 0 -4 -7 1456.42 56.55 0 4 8 3352.53 159.48 0 4 8 3237.64 153.74 0 4 -8 3257.61 155.46 0 -4 8 3237.41 154.37 0 -4 -8 3061.58 142.59 0 4 9 710.34 24.94 0 4 9 701.54 25.05 0 4 -9 724.63 26.19 0 -4 9 700.13 24.69 0 -4 -9 608.22 19.53 0 4 -10 274.55 10.52 0 4 10 267.99 10.83 0 4 10 263.54 9.33 0 -4 10 282.89 10.93 0 4 11 184.49 8.39 0 4 11 171.85 6.56 0 4 -11 182.81 7.65 0 -4 11 182.87 8.04 0 4 12 32.16 2.58 0 4 12 32.44 2.92 0 4 -12 33.40 3.28 0 -4 12 32.57 2.98 0 4 13 517.82 19.38 0 4 13 544.03 21.02 0 4 -13 534.79 20.92 0 -4 13 557.02 21.44 0 4 14 97.38 5.57 0 4 -14 96.14 5.51 0 -4 14 105.61 6.64 0 4 15 156.32 7.72 0 4 -15 150.89 7.42 0 -4 15 170.20 9.16 0 4 16 22.52 2.93 0 4 -16 13.20 2.73 0 -4 16 24.19 2.82 0 6 0 2658.73 117.75 0 6 0 2563.24 112.71 0 -6 0 2617.90 115.73 0 6 1 425.97 13.38 0 6 -1 399.94 12.54 0 6 1 396.07 12.41 0 6 -1 399.87 12.62 0 -6 1 367.32 11.94 0 -6 -1 379.10 12.20 0 6 -2 2.92 1.09 0 6 2 6.22 1.01 0 6 2 4.24 1.41 0 6 -2 3.44 1.00 0 -6 2 4.16 1.18 0 -6 -2 2.71 1.26 0 6 3 205.94 6.61 0 6 3 219.73 6.84 0 6 -3 217.24 6.45 0 6 -3 210.64 6.92 0 -6 -3 213.47 7.06 0 -6 3 225.17 7.22 0 6 4 513.21 16.37 0 6 -4 523.46 17.56 0 6 4 516.89 17.02 0 6 -4 544.24 17.01 0 -6 4 509.92 17.17 0 -6 -4 515.56 17.17 0 6 -5 851.66 28.52 0 6 5 854.37 29.01 0 6 5 795.96 28.23 0 6 -5 808.40 30.00 0 -6 5 874.26 30.99 0 -6 -5 779.40 27.37 0 6 6 936.53 35.01 0 6 -6 993.02 34.23 0 6 -6 967.75 35.82 0 -6 6 937.27 34.90 0 -6 -6 985.17 36.53 0 -6 -6 905.23 31.80 0 6 7 1254.88 48.88 0 6 -7 1201.95 43.53 0 6 -7 1275.20 50.55 0 -6 7 1216.71 47.52 0 -6 -7 1075.78 39.66 0 -6 -7 1239.53 47.31 0 6 8 21.23 2.55 0 6 -8 19.93 2.87 0 -6 8 22.22 2.49 0 -6 -8 19.80 2.11 0 6 9 151.54 5.85 0 6 9 154.51 6.21 0 6 -9 155.33 6.35 0 -6 9 170.83 7.05 0 6 10 17.59 2.53 0 6 10 17.77 3.08 0 6 -10 16.45 2.34 0 -6 10 17.08 2.10 0 6 11 39.09 3.23 0 6 11 36.48 3.32 0 6 -11 41.42 3.92 0 -6 11 38.27 3.74 0 6 -12 831.72 33.83 0 6 12 794.37 31.69 0 6 12 799.82 31.36 0 -6 12 840.45 34.23 0 6 -13 90.36 5.78 0 6 13 82.93 4.93 0 6 13 97.19 5.38 0 -6 13 87.34 5.99 0 6 14 417.43 16.90 0 6 14 505.87 21.30 0 6 -14 462.53 19.42 0 -6 14 499.32 20.95 0 6 15 19.05 2.85 0 6 -15 14.97 2.43 0 -6 15 17.60 3.54 0 8 0 19.85 2.17 0 8 0 20.19 2.18 0 -8 0 20.76 2.01 0 8 1 434.91 14.73 0 8 -1 433.33 15.11 0 8 1 420.32 13.97 0 8 -1 413.59 14.15 0 -8 1 438.67 14.75 0 -8 -1 403.46 13.76 0 8 2 35.89 2.28 0 8 2 35.08 2.29 0 8 -2 36.04 2.33 0 8 -2 31.65 2.84 0 -8 -2 31.89 2.42 0 -8 2 31.51 2.44 0 8 3 14.21 1.55 0 8 3 14.00 2.34 0 8 -3 14.40 1.59 0 8 -3 15.85 1.87 0 -8 -3 17.07 1.91 0 -8 3 12.79 1.97 0 8 4 341.25 11.74 0 8 4 328.97 10.64 0 8 -4 357.10 11.35 0 8 -4 334.79 11.85 0 -8 -4 329.53 11.59 0 -8 4 301.72 11.05 0 8 -5 750.51 27.86 0 8 5 777.56 27.30 0 8 5 733.60 27.13 0 8 -5 793.81 27.88 0 -8 5 758.84 27.82 0 -8 -5 778.06 28.59 0 8 6 115.78 4.07 0 8 6 126.00 6.10 0 8 -6 125.87 4.36 0 8 -6 132.47 6.35 0 -8 -6 115.84 4.60 0 -8 6 125.97 5.42 0 8 7 39.07 3.46 0 8 -7 35.70 3.74 0 -8 7 35.38 2.94 0 -8 -7 35.71 3.31 0 8 8 153.13 6.21 0 8 -8 164.18 6.89 0 -8 8 161.07 6.76 0 -8 -8 174.40 7.44 0 8 -9 2.47 1.70 0 8 9 2.04 2.08 0 -8 -9 1.79 1.48 0 -8 9 2.30 1.73 0 8 10 62.43 4.52 0 8 10 52.54 4.24 0 8 -10 46.77 3.67 0 -8 10 55.27 3.99 0 8 -11 321.34 14.30 0 8 11 329.91 13.70 0 8 11 340.25 13.10 0 -8 11 321.26 13.22 0 8 12 11.04 2.27 0 8 12 17.95 2.57 0 8 -12 15.41 2.69 0 -8 12 20.10 2.93 0 8 13 843.19 34.84 0 8 13 787.99 33.49 0 8 -13 873.72 37.47 0 -8 13 821.06 34.93 0 8 -14 16.78 3.37 0 8 14 11.40 2.91 0 8 14 13.14 3.49 0 -8 14 15.34 3.10 0 10 0 283.28 10.77 0 10 0 273.54 10.55 0 -10 0 255.10 9.40 0 10 1 86.31 5.03 0 10 1 96.16 4.80 0 10 -1 87.75 3.88 0 10 -1 89.22 5.06 0 -10 -1 87.71 4.25 0 -10 1 90.64 4.35 0 10 2 237.96 9.04 0 10 2 217.83 8.35 0 10 -2 220.32 8.50 0 10 -2 218.27 9.31 0 -10 -2 228.22 8.50 0 -10 2 216.85 8.23 0 10 3 153.81 6.13 0 10 -3 154.03 7.31 0 10 3 137.94 6.04 0 10 -3 156.91 6.07 0 -10 3 145.30 6.12 0 -10 -3 153.18 6.22 0 10 4 63.79 3.76 0 10 4 62.82 3.24 0 10 -4 65.76 3.37 0 10 -4 61.79 4.01 0 -10 4 60.79 3.79 0 -10 -4 63.53 3.87 0 10 5 331.76 12.29 0 10 -5 316.95 13.41 0 10 -5 337.52 11.67 0 -10 5 313.36 12.08 0 -10 -5 328.67 12.36 0 10 6 348.37 13.21 0 10 -6 366.33 15.14 0 -10 6 340.83 13.07 0 -10 -6 368.97 13.83 0 10 -7 183.92 8.74 0 10 7 176.54 8.58 0 -10 -7 176.83 6.96 0 -10 7 165.43 7.21 0 10 8 231.89 9.50 0 10 -8 235.73 11.06 0 -10 8 220.43 9.10 0 -10 -8 269.65 10.74 0 10 -9 -1.03 2.23 0 10 9 0.87 1.52 0 -10 -9 -1.29 1.87 0 -10 9 -1.33 1.54 0 10 -10 3.86 2.69 0 10 10 3.55 2.36 0 10 10 3.64 2.60 0 -10 10 4.21 1.94 0 10 11 0.23 1.58 0 10 11 1.29 1.61 0 10 -11 0.68 1.73 0 10 12 176.12 8.01 0 10 12 206.34 9.77 0 10 -12 170.54 8.62 0 12 0 409.91 16.52 0 12 0 383.38 15.53 0 -12 0 393.07 14.80 0 12 1 127.17 5.72 0 12 1 121.45 6.27 0 12 -1 118.91 6.52 0 12 -1 117.84 6.22 0 -12 1 112.63 5.35 0 -12 -1 117.89 5.47 0 12 2 34.27 3.88 0 12 2 30.70 3.11 0 12 -2 32.88 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11 1147.97 45.96 4 2 12 2.51 1.69 -4 2 -12 0.15 1.20 4 -2 12 1.99 2.14 4 2 13 124.76 6.31 4 -2 13 136.62 7.28 4 2 14 43.70 4.77 4 -2 14 44.04 4.61 4 2 15 185.31 8.75 4 -2 15 165.05 8.23 4 2 16 56.40 4.53 4 -2 16 55.34 5.42 4 4 -17 2.77 2.44 -4 4 17 7.44 3.08 -4 -4 17 6.52 3.34 4 4 -16 712.25 29.21 -4 4 16 649.76 27.05 -4 -4 16 602.13 25.77 4 4 -15 538.77 21.12 -4 4 15 490.97 19.86 -4 4 15 544.00 21.91 -4 -4 15 584.77 24.78 4 4 -14 794.24 32.31 -4 4 14 783.87 31.43 -4 4 14 755.24 30.00 -4 -4 14 829.58 34.70 4 4 -13 82.61 4.36 -4 4 13 82.79 4.64 -4 4 13 89.44 5.72 -4 -4 13 86.10 4.99 4 4 -12 209.25 8.16 -4 4 12 229.03 9.87 -4 4 12 213.01 8.42 -4 -4 12 234.20 10.30 4 4 -11 385.20 14.71 -4 4 11 380.74 13.66 -4 4 11 385.03 13.93 4 -4 -11 359.17 12.32 -4 -4 11 406.85 15.76 -4 4 10 487.62 17.44 4 4 -10 495.55 18.42 -4 4 10 477.49 16.70 4 -4 -10 473.75 16.10 -4 -4 10 481.69 17.30 4 4 -9 1467.24 58.57 -4 4 9 1465.14 58.12 4 4 -9 1197.27 45.14 -4 4 9 1438.37 56.73 -4 -4 9 1440.60 56.92 4 -4 -9 1330.94 51.41 -4 4 8 161.75 6.01 4 4 -8 139.97 4.16 4 4 -8 170.54 6.59 -4 4 8 150.38 5.87 4 -4 -8 151.35 5.03 -4 -4 8 175.25 6.72 -4 4 7 570.30 19.00 4 4 -7 533.28 18.07 4 4 -7 578.76 18.17 -4 4 7 577.39 19.69 4 -4 -7 563.73 18.39 -4 -4 7 589.02 19.69 -4 4 6 335.34 10.58 4 4 -6 309.43 9.24 4 4 -6 341.62 10.91 -4 4 6 340.73 11.30 4 -4 -6 337.61 10.68 -4 -4 6 343.78 11.04 -4 4 5 1985.20 81.70 4 4 -5 2058.24 84.43 4 4 -5 2043.46 85.07 -4 4 5 2020.15 84.90 4 -4 -5 1961.94 81.59 -4 -4 5 2181.37 91.56 4 4 -4 1425.07 53.12 4 4 -4 1388.51 52.44 -4 4 4 1377.40 52.44 -4 4 4 1352.20 50.08 -4 4 4 1290.29 48.99 -4 -4 4 1468.43 55.60 4 4 -3 2988.53 134.02 4 4 -3 2894.89 129.71 -4 4 3 3028.62 136.54 -4 4 3 2800.55 125.90 4 -4 -3 2753.25 121.85 -4 -4 3 2885.73 130.29 4 4 -2 4688.66 238.80 -4 4 2 4194.88 214.15 4 4 -2 4642.05 236.01 -4 4 2 4679.25 241.24 -4 4 2 4618.41 234.82 4 -4 -2 4455.83 223.52 -4 -4 2 5063.56 258.48 4 4 -1 78.93 2.74 4 4 -1 77.26 2.74 -4 4 1 76.49 2.88 -4 4 1 87.58 3.11 -4 -4 1 94.62 3.74 4 4 0 1569.04 59.86 -4 4 0 1398.92 51.79 4 4 0 1568.44 58.80 -4 4 0 1625.35 62.59 -4 4 0 1540.26 58.57 4 -4 0 1435.69 53.33 -4 -4 0 1722.20 66.67 4 4 1 91.54 2.60 -4 4 -1 83.30 2.68 4 4 1 80.08 2.82 -4 4 -1 80.71 3.05 -4 4 -1 79.88 2.00 4 -4 1 77.70 2.32 -4 -4 -1 90.80 3.81 4 4 2 103.91 2.80 4 4 2 105.15 3.60 -4 4 -2 99.24 2.93 -4 4 -2 110.08 4.43 4 -4 2 100.38 2.96 -4 -4 -2 109.93 3.85 -4 -4 -2 113.16 2.89 4 4 3 801.83 27.08 4 4 3 815.29 25.45 -4 4 -3 823.85 26.80 -4 4 -3 819.26 28.06 -4 -4 -3 847.43 29.68 4 -4 3 780.66 25.82 -4 -4 -3 710.67 22.34 4 4 4 516.76 16.47 -4 4 -4 495.13 14.88 -4 4 -4 497.88 16.27 -4 -4 -4 529.96 17.23 4 -4 4 533.52 16.60 -4 4 -5 5.57 1.52 4 4 5 5.17 1.41 -4 4 -5 5.02 0.57 -4 -4 -5 7.77 1.31 4 -4 5 6.23 0.98 4 4 6 128.05 4.68 -4 4 -6 120.40 4.37 4 -4 6 129.40 4.44 -4 -4 -6 133.46 4.87 4 4 7 310.15 10.47 -4 4 -7 314.96 11.09 4 -4 7 330.64 10.73 -4 -4 -7 278.20 9.86 4 4 8 480.25 16.62 -4 4 -8 470.66 16.85 4 -4 8 518.06 17.97 -4 -4 -8 462.24 16.55 4 4 9 846.05 33.53 4 4 9 850.94 31.54 -4 4 -9 839.69 32.12 4 -4 9 895.33 33.47 4 4 10 1719.58 72.28 4 4 10 1680.69 72.60 -4 4 -10 1706.41 73.35 4 -4 10 1807.74 77.38 4 4 11 509.15 18.31 4 4 11 543.17 21.90 -4 4 -11 518.03 19.82 4 -4 11 536.25 20.59 4 4 12 630.00 25.68 4 4 12 576.66 21.41 -4 4 -12 588.20 22.90 4 -4 12 605.67 23.89 4 4 13 12.57 3.46 -4 4 -13 12.57 2.46 4 -4 13 16.83 2.97 4 4 14 262.48 11.35 4 -4 14 289.95 12.83 4 4 15 44.92 4.85 4 -4 15 36.68 4.13 4 6 -16 740.14 31.83 -4 6 16 690.56 30.61 -4 -6 16 709.74 32.36 4 6 -15 76.80 4.76 -4 6 15 83.04 6.12 -4 6 15 75.77 5.00 -4 -6 15 72.82 5.02 4 6 -14 307.70 12.43 -4 6 14 291.91 12.06 -4 6 14 333.18 14.26 -4 -6 14 286.68 12.31 4 6 -13 100.46 5.48 -4 6 13 106.56 5.89 -4 6 13 111.81 6.69 -4 -6 13 108.94 6.97 4 6 -12 10.83 3.11 -4 6 12 11.31 2.68 -4 6 12 11.47 2.80 -4 -6 12 7.29 2.35 4 6 -11 36.85 3.14 -4 6 11 39.23 3.52 -4 6 11 33.20 3.44 -4 -6 11 31.89 3.06 4 6 -10 1125.84 44.88 -4 6 10 1179.56 47.03 -4 6 10 1153.61 46.57 -4 -6 10 1181.00 47.71 4 -6 -10 1052.08 40.64 4 6 -9 8.27 2.07 4 6 -9 9.51 1.07 -4 6 9 11.65 2.57 -4 6 9 11.55 2.25 -4 -6 9 12.56 2.61 4 -6 -9 10.11 1.70 4 6 -8 1984.83 83.86 4 6 -8 2138.62 93.44 -4 6 8 2142.14 94.48 -4 6 8 2162.78 93.76 4 -6 -8 1982.11 85.39 -4 -6 8 2319.34 101.81 -4 6 7 10.51 1.79 4 6 -7 10.54 1.28 4 6 -7 10.52 1.89 -4 6 7 15.97 2.36 4 -6 -7 10.91 1.53 -4 -6 7 11.81 1.82 4 6 -6 28.15 1.58 4 6 -6 27.11 2.84 -4 6 6 28.84 2.16 4 -6 -6 27.13 2.03 -4 -6 6 27.11 2.17 4 6 -5 43.29 2.53 4 6 -5 42.80 2.12 -4 6 5 43.29 2.47 -4 6 5 40.51 3.03 -4 -6 5 47.35 3.23 4 -6 -5 43.31 2.08 -4 6 4 2121.24 90.00 4 6 -4 2068.04 87.56 4 6 -4 2087.25 87.71 -4 6 4 2056.20 87.22 4 -6 -4 2031.26 84.42 -4 -6 4 2282.94 97.68 -4 6 3 344.28 11.58 4 6 -3 340.73 11.16 4 6 -3 339.98 11.52 -4 6 3 339.05 10.91 4 -6 -3 336.16 10.20 -4 -6 3 393.03 13.41 4 6 -2 1314.59 50.05 4 6 -2 1333.34 50.17 -4 6 2 1358.38 51.52 -4 6 2 1383.20 53.31 -4 -6 2 1388.65 53.19 4 -6 -2 1243.26 45.95 4 6 -1 55.34 2.46 4 6 -1 59.50 2.62 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1148.92 45.49 -8 -4 10 1091.74 41.78 8 4 -9 702.37 25.03 -8 4 9 688.66 23.99 -8 4 9 694.82 25.05 -8 -4 9 679.99 25.49 8 -4 -9 583.35 22.16 -8 -4 9 724.22 24.86 8 4 -8 20.84 2.59 -8 4 8 20.18 1.72 -8 4 8 23.48 2.72 -8 -4 8 22.57 2.71 8 -4 -8 20.26 2.52 -8 -4 8 21.91 2.02 8 4 -7 321.21 10.81 -8 4 7 331.02 11.16 -8 4 7 319.30 9.84 8 -4 -7 320.04 11.48 -8 -4 7 358.67 11.78 -8 -4 7 327.68 11.10 8 4 -6 3.16 1.30 -8 4 6 5.36 1.41 -8 4 6 3.82 1.01 8 -4 -6 5.47 1.87 -8 -4 6 7.24 1.21 -8 -4 6 4.52 1.44 -8 4 5 3178.61 150.92 8 4 -5 3163.30 148.15 8 4 -5 3173.21 149.88 -8 4 5 3130.73 144.08 8 -4 -5 3396.10 160.79 -8 -4 5 3168.36 149.29 8 4 -4 237.76 8.28 8 4 -4 223.10 7.05 -8 4 4 230.10 7.53 -8 4 4 228.21 6.12 -8 -4 4 230.18 7.89 8 -4 -4 199.42 6.90 8 4 -3 1444.39 56.53 8 4 -3 1384.60 53.40 -8 4 3 1371.70 53.08 -8 4 3 1454.90 57.53 -8 -4 3 1494.20 58.77 8 4 -2 1994.03 83.16 8 4 -2 1973.86 81.39 -8 4 2 2011.98 84.12 -8 4 2 1994.67 83.47 -8 -4 2 1993.96 83.27 8 4 -1 231.61 7.87 8 4 -1 231.99 7.13 -8 4 1 223.56 7.69 -8 4 1 223.59 7.83 -8 -4 1 234.69 8.66 8 4 010282.25 666.42 8 4 010049.14 646.38 -8 4 0 9792.55 634.91 -8 4 0 9940.64 647.12 -8 -4 0 9980.44 646.60 8 4 1 3732.84 180.20 8 4 1 3741.64 185.81 -8 4 -1 3734.20 183.13 -8 4 -1 3872.94 192.20 -8 -4 -1 3815.33 189.17 8 4 2 2674.78 121.39 8 4 2 2787.78 122.68 -8 4 -2 2821.89 126.52 -8 4 -2 2851.17 131.19 -8 -4 -2 2865.83 130.03 8 -4 2 2626.72 115.12 8 4 3 977.92 35.43 8 4 3 958.09 32.15 -8 4 -3 1019.23 36.18 -8 4 -3 1008.13 36.94 -8 -4 -3 1000.54 36.57 8 -4 3 949.04 32.94 8 4 4 339.08 11.59 -8 4 -4 336.27 11.26 -8 4 -4 307.88 9.64 -8 -4 -4 327.95 11.09 8 -4 4 322.36 9.71 8 4 5 42.30 2.93 -8 4 -5 45.82 2.53 -8 4 -5 37.40 1.92 -8 -4 -5 43.49 3.59 8 -4 5 43.00 2.11 8 4 6 455.07 16.06 -8 4 -6 453.73 16.54 8 -4 6 451.08 15.37 -8 -4 -6 487.51 18.21 8 4 7 331.54 11.75 -8 4 -7 331.61 12.16 8 -4 7 319.48 10.89 -8 -4 -7 344.32 13.66 8 4 8 2.28 1.63 -8 4 -8 4.71 1.80 8 -4 8 4.39 1.39 -8 -4 -8 3.37 1.86 8 4 9 110.02 4.72 -8 4 -9 112.28 5.20 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555.24 22.83 -23 3 12 537.30 23.25 -23 -3 12 557.58 23.52 -23 -3 12 548.90 22.71 23 -3 -12 554.84 23.61 23 3 -11 38.45 3.71 -23 3 11 36.15 4.12 -23 -3 11 37.10 4.66 -23 -3 11 29.62 4.10 23 -3 -11 34.24 4.06 23 3 -10 54.15 5.20 -23 3 10 38.71 4.33 -23 -3 10 50.36 4.06 -23 -3 10 46.64 4.27 23 -3 -10 44.02 4.32 23 3 -9 175.12 9.14 -23 3 9 163.00 8.50 -23 -3 9 167.79 7.86 -23 -3 9 160.16 7.58 23 -3 -9 184.36 10.05 23 3 -8 603.51 24.58 -23 3 8 572.28 25.40 -23 -3 8 552.81 23.30 -23 -3 8 521.79 20.89 23 -3 -8 556.12 22.56 23 3 -7 117.36 6.00 -23 3 7 121.42 8.32 -23 -3 7 105.82 5.96 -23 -3 7 110.31 6.02 23 -3 -7 115.59 6.54 23 3 -6 416.40 16.90 -23 3 6 401.35 16.69 -23 -3 6 393.06 15.70 -23 -3 6 404.25 17.81 23 -3 -6 416.33 16.60 23 3 -5 135.63 6.90 -23 3 5 126.65 6.72 -23 -3 5 127.82 6.44 -23 -3 5 123.33 6.24 23 -3 -5 133.19 7.97 23 3 -4 17.52 2.84 -23 3 4 11.42 3.65 23 -3 -4 20.99 3.85 -23 -3 4 19.46 2.87 23 3 -3 20.37 2.77 -23 3 3 11.11 3.40 23 -3 -3 16.63 3.70 -23 -3 3 16.86 2.87 23 3 -2 482.61 20.18 -23 3 2 461.01 19.19 23 -3 -2 505.96 20.95 23 3 -1 4.20 2.86 -23 3 1 1.03 2.54 23 -3 -1 12.23 2.86 23 3 0 741.50 29.96 -23 3 0 580.54 26.29 23 -3 0 747.79 30.06 23 5 -10 35.98 4.38 -23 5 10 43.80 4.32 23 -5 -10 40.15 5.17 -23 -5 10 37.41 4.36 -23 5 9 20.01 3.78 23 5 -9 29.36 3.35 23 5 -9 28.51 3.02 23 -5 -9 24.42 4.58 -23 -5 9 25.14 2.90 -23 5 8 147.62 9.56 23 5 -8 149.73 7.39 23 5 -8 148.64 6.76 23 -5 -8 155.40 8.11 -23 -5 8 143.81 6.71 -23 5 7 565.03 25.43 23 5 -7 582.22 24.76 23 5 -7 590.81 23.78 23 -5 -7 610.54 24.75 -23 -5 7 543.96 22.52 -23 5 6 39.97 4.12 23 5 -6 41.85 4.97 23 5 -6 50.98 4.09 23 -5 -6 41.60 4.25 -23 -5 6 43.66 3.25 23 5 -5 127.88 7.46 -23 5 5 130.87 6.57 23 -5 -5 137.90 7.07 -23 -5 5 121.51 5.54 23 5 -4 25.34 3.02 -23 5 4 18.45 3.89 23 -5 -4 27.68 3.31 -23 -5 4 27.64 2.57 23 5 -3 32.31 3.36 -23 5 3 32.23 4.18 23 -5 -3 41.09 4.78 -23 -5 3 34.67 3.73 24 0 -12 13.73 3.12 -24 0 12 12.07 3.09 24 0 -11 -0.23 2.94 -24 0 11 -3.70 2.87 24 0 -10 249.59 12.25 -24 0 10 238.86 12.02 24 0 -9 2.24 1.94 -24 0 9 -4.95 2.49 24 0 -8 118.82 7.37 -24 0 8 112.36 6.13 24 0 -7 -0.66 1.94 -24 0 7 3.72 1.99 24 0 -6 10.33 3.12 -24 0 6 8.04 3.37 24 0 -5 0.70 1.57 -24 0 5 -1.06 2.26 24 0 -4 1073.95 45.13 -24 0 4 1022.46 44.43 24 0 -3 2.50 2.68 -24 0 3 2.33 2.94 24 0 -2 2684.72 132.63 -24 0 2 2618.73 130.63 -24 0 1 4.43 2.73 24 2 -11 153.60 8.95 -24 2 11 143.35 7.78 24 -2 -11 143.77 7.53 -24 -2 11 138.21 7.35 24 2 -10 103.27 6.00 -24 2 10 102.42 7.85 24 -2 -10 115.20 7.65 -24 -2 10 101.57 7.34 24 2 -9 517.72 21.77 -24 2 9 500.74 21.14 24 -2 -9 511.59 22.54 -24 -2 9 485.35 21.47 24 2 -8 47.71 4.99 -24 2 8 49.59 5.57 24 -2 -8 38.35 5.04 -24 -2 8 48.41 3.97 24 2 -7 79.74 5.70 -24 2 7 83.31 6.36 24 -2 -7 82.43 6.29 -24 -2 7 71.64 4.76 24 2 -6 16.07 3.30 -24 2 6 17.69 2.85 24 -2 -6 14.99 2.81 -24 -2 6 12.17 3.51 24 2 -5 85.99 5.34 -24 2 5 71.19 4.88 24 -2 -5 82.15 5.04 -24 -2 5 76.57 4.84 24 2 -4 124.06 6.28 -24 2 4 110.32 7.00 24 -2 -4 121.02 6.13 -24 -2 4 106.24 5.96 -24 2 3 379.10 16.68 24 -2 -3 407.14 17.06 -24 -2 3 361.28 14.95 24 2 -2 -0.64 1.54 -24 2 2 -0.78 1.93 24 -2 -2 1.27 1.46 24 4 -9 417.41 17.06 -24 4 9 436.11 19.11 -24 -4 9 412.01 17.13 -24 -4 9 409.49 17.44 24 -4 -9 437.99 19.90 24 4 -8 500.07 20.72 -24 4 8 517.20 23.57 -24 -4 8 454.96 18.84 -24 -4 8 457.39 18.87 24 -4 -8 497.64 20.69 24 4 -7 11.58 2.91 -24 4 7 6.14 2.73 24 -4 -7 10.10 3.64 -24 -4 7 7.73 2.64 24 4 -6 127.10 7.62 24 4 -6 140.55 7.15 -24 4 6 124.81 8.24 24 -4 -6 141.35 8.32 -24 -4 6 122.72 6.31 24 4 -5 30.35 3.41 24 4 -5 34.35 3.64 -24 4 5 34.59 4.60 24 -4 -5 40.75 4.69 -24 -4 5 31.70 3.45 24 4 -4 102.28 6.95 -24 4 4 104.33 7.03 24 -4 -4 122.69 6.41 -24 -4 4 114.57 6.15 25 1 -9 3.33 2.03 -25 1 9 0.32 2.69 25 -1 -9 -0.20 2.73 -25 -1 9 2.00 2.69 25 1 -8 1.31 2.23 -25 1 8 0.05 1.87 25 -1 -8 0.98 1.74 -25 -1 8 -2.88 1.80 25 1 -7 83.57 4.82 -25 1 7 88.35 6.52 25 -1 -7 81.01 6.28 -25 -1 7 79.03 5.22 25 1 -6 63.50 5.14 -25 1 6 57.19 5.63 25 -1 -6 75.23 5.56 -25 -1 6 64.96 4.37 25 1 -5 291.09 12.49 -25 1 5 289.20 13.40 25 -1 -5 291.41 12.88 -25 -1 5 258.56 11.00 25 1 -4 26.21 3.45 -25 1 4 15.44 3.08 25 -1 -4 26.29 3.80 -25 -1 4 16.66 3.08 ; _shelx_hkl_checksum 68666 loop_ _space_group_symop_operation_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' '-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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.67462(2) 0.65612(2) 0.82671(2) 0.01590(8) Uani 1 1 d . . . . . O1 O 0.60788(5) 0.72456(9) 0.71032(7) 0.0207(2) Uani 1 1 d . . . . . O2 O 0.58999(5) 0.59640(9) 0.83993(7) 0.0207(2) Uani 1 1 d . . . . . N1 N 0.75757(6) 0.71569(10) 0.80915(9) 0.0194(2) Uani 1 1 d . . . . . N2 N 0.73819(6) 0.58926(10) 0.94563(8) 0.0184(2) Uani 1 1 d . . . . . C1 C 0.62408(8) 0.79199(13) 0.64739(10) 0.0202(3) Uani 1 1 d . . . . . C2 C 0.69423(8) 0.82287(13) 0.65729(11) 0.0239(3) Uani 1 1 d . . . . . H2 H 0.699881 0.874073 0.607606 0.029 Uiso 1 1 calc R U . . . C3 C 0.75898(8) 0.78446(13) 0.73576(11) 0.0219(3) Uani 1 1 d . . . . . C4 C 0.82698(8) 0.66642(14) 0.88110(12) 0.0252(3) Uani 1 1 d . . . . . H4A H 0.866150 0.729908 0.896655 0.030 Uiso 1 1 calc R U . . . H4B H 0.842624 0.593109 0.853181 0.030 Uiso 1 1 calc R U . . . C5 C 0.81466(7) 0.63091(14) 0.97357(11) 0.0215(3) Uani 1 1 d . . . . . H5A H 0.848873 0.563636 1.008442 0.026 Uiso 1 1 calc R U . . . H5B H 0.824057 0.702938 1.018655 0.026 Uiso 1 1 calc R U . . . C6 C 0.72007(8) 0.52347(13) 1.00862(10) 0.0208(3) Uani 1 1 d . . . . . C7 C 0.64664(8) 0.48441(14) 0.98815(11) 0.0238(3) Uani 1 1 d . . . . . H7 H 0.638224 0.430687 1.034448 0.029 Uiso 1 1 calc R U . . . C8 C 0.58714(8) 0.51861(13) 0.90652(10) 0.0212(3) Uani 1 1 d . . . . . C9 C 0.55915(9) 0.83626(14) 0.55946(12) 0.0277(3) Uani 1 1 d . . . . . H9A H 0.520992 0.772111 0.539704 0.042 Uiso 1 1 calc R U . . . H9B H 0.574860 0.853528 0.504330 0.042 Uiso 1 1 calc R U . . . H9C H 0.539327 0.911954 0.577096 0.042 Uiso 1 1 calc R U . . . C10 C 0.83117(9) 0.82580(15) 0.73190(14) 0.0325(4) Uani 1 1 d . . . . . H10A H 0.855965 0.881642 0.787464 0.049 Uiso 1 1 calc R U . . . H10B H 0.822188 0.869280 0.669411 0.049 Uiso 1 1 calc R U . . . H10C H 0.862402 0.753415 0.736296 0.049 Uiso 1 1 calc R U . . . C11 C 0.77744(8) 0.48404(15) 1.10601(11) 0.0289(3) Uani 1 1 d . . . . . H11A H 0.810566 0.423580 1.094259 0.043 Uiso 1 1 calc R U . . . H11B H 0.753314 0.446412 1.147139 0.043 Uiso 1 1 calc R U . . . H11C H 0.805829 0.556444 1.140091 0.043 Uiso 1 1 calc R U . . . C12 C 0.51235(8) 0.46434(16) 0.88615(12) 0.0301(3) Uani 1 1 d . . . . . H12A H 0.475258 0.530180 0.865340 0.045 Uiso 1 1 calc R U . . . H12B H 0.511615 0.425025 0.946377 0.045 Uiso 1 1 calc R U . . . H12C H 0.501329 0.402391 0.833417 0.045 Uiso 1 1 calc R U . . . Na1 Na 0.500000 0.73770(7) 0.750000 0.02234(17) Uani 1 2 d S T P . . Cl1 Cl 0.500000 1.02255(5) 0.750000 0.02701(12) Uani 1 2 d S T P . . O3 O 0.54812(6) 0.94232(12) 0.82627(9) 0.0382(3) Uani 1 1 d . . . . . O4 O 0.54217(9) 1.09586(15) 0.70970(12) 0.0587(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01068(11) 0.01916(11) 0.01728(11) 0.00103(6) 0.00455(8) 0.00022(5) O1 0.0145(4) 0.0257(5) 0.0213(5) 0.0043(4) 0.0059(4) 0.0005(4) O2 0.0141(4) 0.0266(5) 0.0216(5) 0.0046(4) 0.0069(4) 0.0010(4) N1 0.0137(5) 0.0192(5) 0.0247(6) 0.0010(4) 0.0065(4) 0.0000(4) N2 0.0139(5) 0.0207(5) 0.0192(5) -0.0014(4) 0.0047(4) 0.0010(4) C1 0.0206(6) 0.0199(6) 0.0200(6) 0.0013(5) 0.0078(5) 0.0023(5) C2 0.0232(7) 0.0232(7) 0.0282(7) 0.0058(6) 0.0130(6) 0.0019(5) C3 0.0187(6) 0.0191(6) 0.0307(7) 0.0010(5) 0.0123(6) -0.0003(5) C4 0.0132(6) 0.0303(7) 0.0297(8) 0.0058(6) 0.0052(6) 0.0005(5) C5 0.0133(6) 0.0250(6) 0.0225(7) -0.0025(5) 0.0026(5) 0.0001(5) C6 0.0195(6) 0.0221(6) 0.0193(6) 0.0000(5) 0.0056(5) 0.0027(5) C7 0.0223(7) 0.0284(7) 0.0212(7) 0.0048(5) 0.0088(6) 0.0002(5) C8 0.0186(6) 0.0254(7) 0.0227(7) 0.0006(5) 0.0111(5) -0.0001(5) C9 0.0246(8) 0.0327(8) 0.0238(8) 0.0060(6) 0.0068(6) 0.0042(6) C10 0.0203(7) 0.0324(8) 0.0477(10) 0.0129(7) 0.0160(7) -0.0007(6) C11 0.0236(7) 0.0354(8) 0.0235(7) 0.0077(6) 0.0041(6) 0.0028(6) C12 0.0194(7) 0.0414(9) 0.0303(8) 0.0075(6) 0.0105(6) -0.0040(6) Na1 0.0122(3) 0.0259(4) 0.0271(4) 0.000 0.0053(3) 0.000 Cl1 0.0192(2) 0.0314(3) 0.0289(3) 0.000 0.00717(19) 0.000 O3 0.0225(6) 0.0445(7) 0.0375(7) 0.0021(5) -0.0005(5) 0.0041(5) O4 0.0628(10) 0.0579(9) 0.0607(10) 0.0032(8) 0.0291(8) -0.0294(8) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 Ni O2 178.17(5) . . N1 Ni N2 87.02(5) . . O2 Ni N2 94.61(5) . . N1 Ni O1 95.10(5) . . O2 Ni O1 83.29(4) . . N2 Ni O1 177.38(4) . . N1 Ni Na1 135.48(4) . . O2 Ni Na1 43.43(3) . . N2 Ni Na1 131.85(4) . . O1 Ni Na1 45.58(3) . . C1 O1 Ni 126.22(9) . . C1 O1 Na1 127.44(8) . . Ni O1 Na1 100.68(4) . . C8 O2 Ni 126.32(9) . . C8 O2 Na1 127.46(8) . . Ni O2 Na1 103.36(4) . . C3 N1 C4 119.34(12) . . C3 N1 Ni 126.69(10) . . C4 N1 Ni 113.60(9) . . C6 N2 C5 119.23(12) . . C6 N2 Ni 126.92(10) . . C5 N2 Ni 113.36(9) . . O1 C1 C2 124.30(13) . . O1 C1 C9 115.24(12) . . C2 C1 C9 120.46(13) . . C1 C2 C3 125.06(13) . . C1 C2 H2 117.5 . . C3 C2 H2 117.5 . . N1 C3 C2 122.60(12) . . N1 C3 C10 120.43(13) . . C2 C3 C10 116.96(13) . . N1 C4 C5 108.34(12) . . N1 C4 H4A 110.0 . . C5 C4 H4A 110.0 . . N1 C4 H4B 110.0 . . C5 C4 H4B 110.0 . . H4A C4 H4B 108.4 . . N2 C5 C4 108.64(11) . . N2 C5 H5A 110.0 . . C4 C5 H5A 110.0 . . N2 C5 H5B 110.0 . . C4 C5 H5B 110.0 . . H5A C5 H5B 108.3 . . N2 C6 C7 122.24(13) . . N2 C6 C11 120.76(13) . . C7 C6 C11 116.99(12) . . C8 C7 C6 124.64(13) . . C8 C7 H7 117.7 . . C6 C7 H7 117.7 . . O2 C8 C7 124.23(13) . . O2 C8 C12 114.63(12) . . C7 C8 C12 121.12(13) . . C1 C9 H9A 109.5 . . C1 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C1 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C3 C10 H10A 109.5 . . C3 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C3 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C6 C11 H11A 109.5 . . C6 C11 H11B 109.5 . . H11A C11 H11B 109.5 . . C6 C11 H11C 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . C8 C12 H12A 109.5 . . C8 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C8 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . O2 Na1 O2 98.08(6) . 2_656 O2 Na1 O1 112.06(4) . 2_656 O2 Na1 O1 63.04(3) 2_656 2_656 O2 Na1 O1 63.04(3) . . O2 Na1 O1 112.06(4) 2_656 . O1 Na1 O1 173.20(6) 2_656 . O2 Na1 O3 155.69(4) . 2_656 O2 Na1 O3 104.49(4) 2_656 2_656 O1 Na1 O3 86.55(4) 2_656 2_656 O1 Na1 O3 99.51(4) . 2_656 O2 Na1 O3 104.49(4) . . O2 Na1 O3 155.69(4) 2_656 . O1 Na1 O3 99.51(4) 2_656 . O1 Na1 O3 86.55(4) . . O3 Na1 O3 55.25(6) 2_656 . O2 Na1 Cl1 130.96(3) . . O2 Na1 Cl1 130.96(3) 2_656 . O1 Na1 Cl1 93.40(3) 2_656 . O1 Na1 Cl1 93.40(3) . . O3 Na1 Cl1 27.62(3) 2_656 . O3 Na1 Cl1 27.62(3) . . O2 Na1 Ni 33.21(2) . . O2 Na1 Ni 119.08(4) 2_656 . O1 Na1 Ni 143.12(3) 2_656 . O1 Na1 Ni 33.74(2) . . O3 Na1 Ni 123.97(3) 2_656 . O3 Na1 Ni 85.13(3) . . Cl1 Na1 Ni 105.509(14) . . O2 Na1 Ni 119.08(4) . 2_656 O2 Na1 Ni 33.21(2) 2_656 2_656 O1 Na1 Ni 33.74(2) 2_656 2_656 O1 Na1 Ni 143.12(3) . 2_656 O3 Na1 Ni 85.13(3) 2_656 2_656 O3 Na1 Ni 123.97(3) . 2_656 Cl1 Na1 Ni 105.508(14) . 2_656 Ni Na1 Ni 148.98(3) . 2_656 O4 Cl1 O4 112.25(15) . 2_656 O4 Cl1 O3 109.84(9) . . O4 Cl1 O3 109.21(9) 2_656 . O4 Cl1 O3 109.21(9) . 2_656 O4 Cl1 O3 109.84(9) 2_656 2_656 O3 Cl1 O3 106.32(11) . 2_656 O4 Cl1 Na1 123.87(8) . . O4 Cl1 Na1 123.87(8) 2_656 . O3 Cl1 Na1 53.16(5) . . O3 Cl1 Na1 53.16(5) 2_656 . Cl1 O3 Na1 99.22(6) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni N1 1.8527(11) . Ni O2 1.8552(9) . Ni N2 1.8592(12) . Ni O1 1.8625(10) . Ni Na1 3.2954(3) . O1 C1 1.3003(16) . O1 Na1 2.3953(9) . O2 C8 1.3006(17) . O2 Na1 2.3285(11) . N1 C3 1.3110(18) . N1 C4 1.4704(18) . N2 C6 1.3107(18) . N2 C5 1.4680(17) . C1 C2 1.368(2) . C1 C9 1.505(2) . C2 C3 1.414(2) . C2 H2 0.9500 . C3 C10 1.5042(19) . C4 C5 1.505(2) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 H5A 0.9900 . C5 H5B 0.9900 . C6 C7 1.419(2) . C6 C11 1.5041(19) . C7 C8 1.367(2) . C7 H7 0.9500 . C8 C12 1.5008(19) . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . Na1 O3 2.4948(15) 2_656 Na1 O3 2.4948(15) . Na1 Cl1 3.0771(9) . Cl1 O4 1.4208(14) . Cl1 O4 1.4208(14) 2_656 Cl1 O3 1.4454(12) . Cl1 O3 1.4454(12) 2_656 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N1 Ni O1 C1 -1.35(11) . . . . O2 Ni O1 C1 179.53(11) . . . . Na1 Ni O1 C1 154.82(13) . . . . N1 Ni O1 Na1 -156.17(5) . . . . O2 Ni O1 Na1 24.71(5) . . . . N2 Ni O2 C8 -9.18(12) . . . . O1 Ni O2 C8 172.39(12) . . . . Na1 Ni O2 C8 -161.87(13) . . . . N2 Ni O2 Na1 152.69(5) . . . . O1 Ni O2 Na1 -25.74(5) . . . . N2 Ni N1 C3 -177.20(12) . . . . O1 Ni N1 C3 1.27(12) . . . . Na1 Ni N1 C3 -23.03(15) . . . . N2 Ni N1 C4 9.93(10) . . . . O1 Ni N1 C4 -171.60(10) . . . . Na1 Ni N1 C4 164.10(8) . . . . N1 Ni N2 C6 -178.75(12) . . . . O2 Ni N2 C6 0.41(12) . . . . Na1 Ni N2 C6 25.46(14) . . . . N1 Ni N2 C5 9.45(9) . . . . O2 Ni N2 C5 -171.38(9) . . . . Na1 Ni N2 C5 -146.33(8) . . . . Ni O1 C1 C2 0.4(2) . . . . Na1 O1 C1 C2 148.59(12) . . . . Ni O1 C1 C9 -179.62(9) . . . . Na1 O1 C1 C9 -31.40(17) . . . . O1 C1 C2 C3 1.2(2) . . . . C9 C1 C2 C3 -178.77(14) . . . . C4 N1 C3 C2 172.27(13) . . . . Ni N1 C3 C2 -0.2(2) . . . . C4 N1 C3 C10 -7.5(2) . . . . Ni N1 C3 C10 179.96(11) . . . . C1 C2 C3 N1 -1.3(2) . . . . C1 C2 C3 C10 178.50(15) . . . . C3 N1 C4 C5 160.54(12) . . . . Ni N1 C4 C5 -26.01(14) . . . . C6 N2 C5 C4 161.82(12) . . . . Ni N2 C5 C4 -25.69(14) . . . . N1 C4 C5 N2 32.10(15) . . . . C5 N2 C6 C7 177.39(13) . . . . Ni N2 C6 C7 6.0(2) . . . . C5 N2 C6 C11 -3.74(19) . . . . Ni N2 C6 C11 -175.10(10) . . . . N2 C6 C7 C8 -5.6(2) . . . . C11 C6 C7 C8 175.45(14) . . . . Ni O2 C8 C7 11.8(2) . . . . Na1 O2 C8 C7 -145.82(12) . . . . Ni O2 C8 C12 -166.67(10) . . . . Na1 O2 C8 C12 35.75(17) . . . . C6 C7 C8 O2 -3.7(2) . . . . C6 C7 C8 C12 174.66(14) . . . . O4 Cl1 O3 Na1 -118.04(8) . . . . O4 Cl1 O3 Na1 118.45(9) 2_656 . . . O3 Cl1 O3 Na1 0.002(1) 2_656 . . .