#------------------------------------------------------------------------------ #$Date: 2025-08-20 20:19:29 +0100 (Wed, 20 Aug 2025) $ #$Revision: 301836 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308422.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_4308422 loop_ _publ_author_name 'Gao, Jian' 'Reibenspies, Joseph H.' 'Zingaro, Ralph A.' 'Woolley, F. Ross' 'Martell, Arthur E.' 'Clearfield, Abraham' _publ_section_title ; Novel Chiral "Calixsalen" Macrocycle and Chiral Robson-type Macrocyclic Complexes ; _journal_coden_ASTM INOCAJ _journal_issue 2 _journal_name_full 'Inorganic Chemistry' _journal_page_first 232 _journal_page_last 241 _journal_paper_doi 10.1021/ic049181m _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C50 H45 Cl2 N6 Ni2 O10' _chemical_formula_weight 1078.24 _space_group_IT_number 78 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4cw' _symmetry_space_group_name_H-M 'P 43' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.2115(4) _cell_length_b 10.2115(4) _cell_length_c 43.848(3) _cell_measurement_reflns_used 8145 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.20 _cell_volume 4572.2(4) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_number 38628 _diffrn_reflns_theta_full 27.52 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_min 0.93 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_T_max 0.8077 _exptl_absorpt_correction_T_min 0.4860 _exptl_absorpt_correction_type none _exptl_crystal_colour dark_brown _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Diamond _exptl_crystal_F_000 2228 _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.558 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.181 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 636 _refine_ls_number_reflns 10482 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0458 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.1174 _reflns_number_gt 9782 _reflns_number_total 10482 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic049181msi20040623_010610.cif _cod_data_source_block am _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 2020-11-03 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_cell_volume 4572.3(4) _cod_original_formula_sum 'C66.67 H60 Cl2.67 N8 Ni2.67 O13.33' _cod_original_formula_units_Z 3 _cod_original_formula_weight 1437.65 _cod_database_code 4308422 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.12509(7) 0.83006(7) 0.234438(15) 0.01662(15) Uani 1 1 d . . . Ni2 Ni 0.23925(7) 0.79125(7) 0.292207(15) 0.01424(14) Uani 1 1 d . . . N1 N 0.1434(5) 0.7563(5) 0.19653(10) 0.0156(10) Uani 1 1 d . . . N2 N 0.0026(5) 0.9415(4) 0.21869(9) 0.0124(9) Uani 1 1 d . . . N3 N 0.2087(4) 0.8532(4) 0.33059(9) 0.0113(9) Uani 1 1 d . . . N4 N 0.3721(4) 0.6906(4) 0.30738(9) 0.0118(9) Uani 1 1 d . . . O1 O 0.2565(4) 0.7332(4) 0.25260(8) 0.0170(8) Uani 1 1 d . . . O2 O 0.1104(4) 0.8909(4) 0.27373(8) 0.0166(8) Uani 1 1 d . . . C1 C 0.0456(5) 0.8030(5) 0.17444(11) 0.0135(11) Uani 1 1 d . . . H1 H -0.0306 0.7414 0.1750 0.016 Uiso 1 1 calc R . . C2 C 0.0964(5) 0.8085(5) 0.14155(12) 0.0147(11) Uani 1 1 d . . . C3 C 0.0367(6) 0.7381(6) 0.11850(12) 0.0170(11) Uani 1 1 d . . . H3 H -0.0363 0.6836 0.1229 0.020 Uiso 1 1 calc R . . C4 C 0.0836(6) 0.7473(6) 0.08899(13) 0.0236(14) Uani 1 1 d . . . H4 H 0.0418 0.6990 0.0732 0.028 Uiso 1 1 calc R . . C5 C 0.1915(6) 0.8264(6) 0.08188(12) 0.0235(13) Uani 1 1 d . . . H5 H 0.2227 0.8325 0.0615 0.028 Uiso 1 1 calc R . . C6 C 0.2524(6) 0.8964(5) 0.10547(13) 0.0204(12) Uani 1 1 d . . . H6 H 0.3263 0.9498 0.1012 0.024 Uiso 1 1 calc R . . C7 C 0.2052(6) 0.8876(5) 0.13482(13) 0.0193(12) Uani 1 1 d . . . H7 H 0.2467 0.9356 0.1507 0.023 Uiso 1 1 calc R . . C8 C -0.0025(5) 0.9379(5) 0.18482(12) 0.0143(11) Uani 1 1 d . . . H8 H 0.0604 1.0048 0.1769 0.017 Uiso 1 1 calc R . . C9 C -0.2449(6) 0.8917(6) 0.17820(13) 0.0209(12) Uani 1 1 d . . . H9 H -0.2341 0.8128 0.1894 0.025 Uiso 1 1 calc R . . C10 C -0.3665(7) 0.9263(6) 0.16754(14) 0.0266(14) Uani 1 1 d . . . H10 H -0.4406 0.8742 0.1725 0.032 Uiso 1 1 calc R . . C11 C -0.3813(7) 1.0369(7) 0.14960(14) 0.0284(15) Uani 1 1 d . . . H11 H -0.4640 1.0559 0.1407 0.034 Uiso 1 1 calc R . . C12 C -0.2781(7) 1.1186(7) 0.14467(14) 0.0287(15) Uani 1 1 d . . . H12 H -0.2901 1.1974 0.1335 0.034 Uiso 1 1 calc R . . C13 C -0.1536(6) 1.0865(5) 0.15614(12) 0.0202(12) Uani 1 1 d . . . H13 H -0.0810 1.1427 0.1526 0.024 Uiso 1 1 calc R . . C14 C -0.1378(6) 0.9717(6) 0.17266(12) 0.0163(12) Uani 1 1 d . . . C15 C -0.0604(5) 1.0275(5) 0.23366(12) 0.0128(10) Uani 1 1 d . . . H15 H -0.1211 1.0793 0.2225 0.015 Uiso 1 1 calc R . . C16 C -0.0493(5) 1.0546(5) 0.26593(12) 0.0121(11) Uani 1 1 d . . . C17 C -0.1260(5) 1.1547(5) 0.27887(11) 0.0159(11) Uani 1 1 d . . . H17 H -0.1878 1.1982 0.2663 0.019 Uiso 1 1 calc R . . C18 C -0.1158(5) 1.1929(6) 0.30908(11) 0.0154(11) Uani 1 1 d . . . C19 C -0.0249(5) 1.1244(5) 0.32743(11) 0.0127(11) Uani 1 1 d . . . H19 H -0.0149 1.1496 0.3482 0.015 Uiso 1 1 calc R . . C20 C 0.0512(5) 1.0205(5) 0.31617(11) 0.0119(10) Uani 1 1 d . . . C21 C 0.0398(5) 0.9864(5) 0.28503(11) 0.0133(10) Uani 1 1 d . . . C22 C -0.1996(6) 1.2998(6) 0.32261(12) 0.0190(12) Uani 1 1 d . . . H22A H -0.1963 1.3773 0.3095 0.028 Uiso 1 1 calc R . . H22B H -0.1666 1.3224 0.3429 0.028 Uiso 1 1 calc R . . H22C H -0.2902 1.2692 0.3242 0.028 Uiso 1 1 calc R . . C23 C 0.1316(5) 0.9496(6) 0.33732(12) 0.0128(11) Uani 1 1 d . . . H23 H 0.1279 0.9757 0.3581 0.015 Uiso 1 1 calc R . . C24 C 0.2754(5) 0.7705(5) 0.35449(11) 0.0136(10) Uani 1 1 d . . . H24 H 0.2185 0.6926 0.3584 0.016 Uiso 1 1 calc R . . C25 C 0.2999(5) 0.8363(5) 0.38460(11) 0.0142(11) Uani 1 1 d . . . H25 H 0.2231 0.8951 0.3810 0.017 Uiso 1 1 calc R . . C26 C 0.3828(5) 0.9467(6) 0.38656(12) 0.0156(11) Uani 1 1 d . . . H26 H 0.4216 0.9817 0.3686 0.019 Uiso 1 1 calc R . . C27 C 0.4077(6) 1.0040(6) 0.41469(13) 0.0204(13) Uani 1 1 d . . . H27 H 0.4645 1.0775 0.4160 0.024 Uiso 1 1 calc R . . C28 C 0.3500(6) 0.9543(6) 0.44107(12) 0.0229(14) Uani 1 1 d . . . H28 H 0.3683 0.9932 0.4603 0.028 Uiso 1 1 calc R . . C29 C 0.2653(6) 0.8475(6) 0.43929(12) 0.0208(13) Uani 1 1 d . . . H29 H 0.2241 0.8141 0.4571 0.025 Uiso 1 1 calc R . . C30 C 0.2423(6) 0.7904(6) 0.41077(12) 0.0185(11) Uani 1 1 d . . . H30 H 0.1848 0.7175 0.4095 0.022 Uiso 1 1 calc R . . C31 C 0.4030(5) 0.7213(5) 0.34016(11) 0.0126(11) Uani 1 1 d . . . H31 H 0.4668 0.7956 0.3403 0.015 Uiso 1 1 calc R . . C32 C 0.4644(5) 0.6094(5) 0.35722(11) 0.0121(11) Uani 1 1 d . . . C33 C 0.5915(5) 0.6229(6) 0.36725(12) 0.0176(11) Uani 1 1 d . . . H33 H 0.6363 0.7032 0.3639 0.021 Uiso 1 1 calc R . . C34 C 0.6550(6) 0.5218(6) 0.38206(14) 0.0232(13) Uani 1 1 d . . . H34 H 0.7435 0.5318 0.3883 0.028 Uiso 1 1 calc R . . C35 C 0.5890(6) 0.4056(6) 0.38772(13) 0.0224(13) Uani 1 1 d . . . H35 H 0.6312 0.3364 0.3984 0.027 Uiso 1 1 calc R . . C36 C 0.4632(6) 0.3914(6) 0.37784(13) 0.0230(13) Uani 1 1 d . . . H36 H 0.4184 0.3112 0.3813 0.028 Uiso 1 1 calc R . . C37 C 0.4000(5) 0.4924(6) 0.36282(13) 0.0205(13) Uani 1 1 d . . . H37 H 0.3120 0.4815 0.3563 0.025 Uiso 1 1 calc R . . C38 C 0.4383(5) 0.6050(5) 0.29226(12) 0.0132(10) Uani 1 1 d . . . H38 H 0.5048 0.5593 0.3031 0.016 Uiso 1 1 calc R . . C39 C 0.4212(5) 0.5717(5) 0.26038(12) 0.0125(11) Uani 1 1 d . . . C40 C 0.4958(6) 0.4718(6) 0.24753(13) 0.0176(11) Uani 1 1 d . . . H40 H 0.5571 0.4277 0.2602 0.021 Uiso 1 1 calc R . . C41 C 0.4857(6) 0.4334(6) 0.21768(12) 0.0183(12) Uani 1 1 d . . . C42 C 0.3943(6) 0.4972(6) 0.19982(14) 0.0196(13) Uani 1 1 d . . . H42 H 0.3843 0.4705 0.1792 0.023 Uiso 1 1 calc R . . C43 C 0.3160(6) 0.5992(5) 0.21075(12) 0.0146(11) Uani 1 1 d . . . C44 C 0.3301(5) 0.6376(5) 0.24168(11) 0.0119(10) Uani 1 1 d . . . C45 C 0.5672(7) 0.3233(7) 0.20525(14) 0.0290(15) Uani 1 1 d . . . H45A H 0.5616 0.2479 0.2190 0.043 Uiso 1 1 calc R . . H45B H 0.6586 0.3517 0.2036 0.043 Uiso 1 1 calc R . . H45C H 0.5345 0.2985 0.1850 0.043 Uiso 1 1 calc R . . C46 C 0.2223(5) 0.6604(6) 0.19046(11) 0.0153(11) Uani 1 1 d . . . H46 H 0.2182 0.6263 0.1703 0.018 Uiso 1 1 calc R . . Cl1 Cl 0.83750(15) 0.59344(15) 0.24261(3) 0.0256(3) Uani 1 1 d . . . O3 O 0.7491(5) 0.6775(6) 0.25759(12) 0.0480(14) Uani 1 1 d . . . O4 O 0.8186(4) 0.4596(4) 0.25174(10) 0.0323(11) Uani 1 1 d . . . O5 O 0.9684(5) 0.6296(5) 0.24893(17) 0.0653(19) Uani 1 1 d . . . O6 O 0.8149(7) 0.6016(5) 0.21056(10) 0.0548(18) Uani 1 1 d . . . Cl2 Cl 0.39451(15) 0.15956(17) 0.30961(4) 0.0297(3) Uani 1 1 d . . . O7 O 0.3050(4) 0.1867(5) 0.33410(11) 0.0346(11) Uani 1 1 d . . . O8 O 0.4546(6) 0.2761(6) 0.30047(13) 0.0623(18) Uani 1 1 d . . . O9 O 0.3242(5) 0.1034(5) 0.28451(11) 0.0426(13) Uani 1 1 d . . . O10 O 0.4910(6) 0.0672(6) 0.32002(12) 0.0570(18) Uani 1 1 d . . . C60 C 0.1349(7) 0.3769(6) 0.27578(14) 0.0279(14) Uani 1 1 d . . . H60A H 0.0622 0.3931 0.2617 0.042 Uiso 1 1 calc R . . H60B H 0.1375 0.2837 0.2811 0.042 Uiso 1 1 calc R . . H60C H 0.2175 0.4020 0.2660 0.042 Uiso 1 1 calc R . . C61 C 0.1164(6) 0.4541(7) 0.30333(15) 0.0258(14) Uani 1 1 d . . . N62 N 0.1029(5) 0.5089(6) 0.32538(13) 0.0310(13) Uani 1 1 d . . . C71 C 0.4319(7) 0.9739(7) 0.22482(15) 0.0306(15) Uani 1 1 d . . . C70 C 0.5332(8) 0.9423(8) 0.24621(17) 0.0421(19) Uani 1 1 d . . . H70A H 0.5720 0.8576 0.2408 0.063 Uiso 1 1 calc R . . H70B H 0.4959 0.9374 0.2668 0.063 Uiso 1 1 calc R . . H70C H 0.6009 1.0103 0.2456 0.063 Uiso 1 1 calc R . . N72 N 0.3490(7) 0.9989(6) 0.20775(13) 0.0380(15) 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 Ni1 0.0171(4) 0.0177(4) 0.0151(3) -0.0013(3) -0.0027(3) 0.0035(3) Ni2 0.0133(4) 0.0163(4) 0.0132(3) 0.0003(3) -0.0022(3) 0.0026(3) N1 0.016(2) 0.016(2) 0.014(2) -0.0005(19) 0.0009(18) -0.0040(19) N2 0.015(2) 0.011(2) 0.010(2) 0.0001(17) -0.0023(18) 0.0018(18) N3 0.013(2) 0.010(2) 0.012(2) 0.0024(17) -0.0055(17) -0.0019(18) N4 0.012(2) 0.009(2) 0.014(2) 0.0035(17) -0.0055(17) -0.0050(18) O1 0.022(2) 0.016(2) 0.0134(17) -0.0027(15) -0.0043(16) 0.0052(17) O2 0.019(2) 0.022(2) 0.0081(16) -0.0030(16) -0.0053(15) 0.0065(17) C1 0.014(3) 0.017(3) 0.009(2) 0.001(2) 0.001(2) 0.003(2) C2 0.017(3) 0.014(3) 0.013(2) 0.002(2) -0.001(2) 0.004(2) C3 0.019(3) 0.016(3) 0.015(2) -0.002(2) -0.002(2) 0.004(2) C4 0.030(3) 0.019(3) 0.021(3) -0.002(3) -0.010(3) 0.014(3) C5 0.035(4) 0.023(3) 0.013(2) 0.007(2) 0.001(2) 0.013(3) C6 0.020(3) 0.018(3) 0.023(3) 0.002(2) 0.006(2) 0.002(2) C7 0.026(3) 0.009(3) 0.023(3) 0.000(2) -0.004(2) 0.001(2) C8 0.016(3) 0.012(3) 0.014(2) -0.001(2) 0.003(2) 0.000(2) C9 0.022(3) 0.020(3) 0.021(3) 0.001(2) -0.006(2) 0.000(3) C10 0.027(4) 0.027(3) 0.026(3) -0.012(3) -0.006(3) 0.002(3) C11 0.030(4) 0.034(4) 0.021(3) -0.012(3) -0.016(3) 0.009(3) C12 0.039(4) 0.027(3) 0.020(3) -0.001(3) -0.003(3) 0.020(3) C13 0.030(3) 0.014(3) 0.017(3) -0.003(2) 0.007(2) 0.001(3) C14 0.025(3) 0.016(3) 0.008(2) -0.005(2) 0.000(2) 0.009(2) C15 0.007(2) 0.019(3) 0.013(2) 0.001(2) -0.003(2) 0.000(2) C16 0.012(2) 0.011(3) 0.013(2) -0.003(2) 0.000(2) 0.0005(19) C17 0.013(3) 0.018(3) 0.016(2) 0.000(2) 0.000(2) 0.001(2) C18 0.013(3) 0.018(3) 0.015(2) -0.003(2) -0.003(2) 0.002(2) C19 0.010(2) 0.017(3) 0.011(3) -0.006(2) 0.007(2) -0.002(2) C20 0.014(3) 0.012(3) 0.010(2) 0.001(2) -0.002(2) -0.004(2) C21 0.014(3) 0.014(3) 0.012(2) 0.000(2) -0.001(2) 0.000(2) C22 0.021(3) 0.018(3) 0.019(3) 0.001(2) 0.002(2) 0.004(2) C23 0.008(3) 0.020(3) 0.010(2) 0.002(2) -0.002(2) -0.002(2) C24 0.011(2) 0.014(2) 0.016(2) 0.005(2) -0.003(2) -0.001(2) C25 0.009(2) 0.019(3) 0.015(3) -0.004(2) -0.003(2) 0.007(2) C26 0.010(3) 0.020(3) 0.017(3) 0.000(2) 0.003(2) 0.002(2) C27 0.019(3) 0.019(3) 0.023(3) -0.001(2) -0.005(2) 0.001(2) C28 0.030(3) 0.033(3) 0.006(2) -0.006(2) -0.006(2) 0.009(3) C29 0.027(3) 0.025(3) 0.010(2) 0.000(2) 0.002(2) 0.005(3) C30 0.015(3) 0.021(3) 0.020(3) 0.003(2) 0.000(2) 0.003(2) C31 0.010(3) 0.011(3) 0.017(3) 0.002(2) -0.002(2) 0.000(2) C32 0.012(2) 0.015(3) 0.009(2) 0.002(2) -0.002(2) 0.003(2) C33 0.012(3) 0.019(3) 0.021(3) 0.002(2) -0.001(2) -0.003(2) C34 0.013(3) 0.027(3) 0.029(3) 0.006(3) -0.008(3) 0.001(3) C35 0.020(3) 0.022(3) 0.026(3) 0.005(2) -0.005(2) 0.006(3) C36 0.030(3) 0.016(3) 0.023(3) 0.009(2) -0.001(3) -0.005(3) C37 0.012(3) 0.020(3) 0.030(3) 0.001(2) -0.007(2) -0.003(2) C38 0.009(2) 0.014(3) 0.017(2) 0.001(2) -0.001(2) 0.001(2) C39 0.011(2) 0.014(3) 0.013(2) 0.007(2) -0.003(2) -0.004(2) C40 0.014(3) 0.017(3) 0.022(3) 0.001(2) -0.002(2) 0.005(2) C41 0.022(3) 0.018(3) 0.015(3) 0.000(2) -0.001(2) 0.001(2) C42 0.022(3) 0.015(3) 0.022(3) -0.001(2) 0.003(3) -0.001(2) C43 0.020(3) 0.009(2) 0.015(3) 0.000(2) 0.001(2) 0.000(2) C44 0.010(2) 0.013(3) 0.013(2) -0.001(2) 0.007(2) 0.002(2) C45 0.035(4) 0.029(4) 0.023(3) -0.004(3) 0.003(3) 0.007(3) C46 0.018(3) 0.020(3) 0.008(2) -0.004(2) 0.001(2) -0.001(2) Cl1 0.0241(7) 0.0220(7) 0.0309(8) 0.0067(6) 0.0046(6) 0.0024(6) O3 0.045(3) 0.048(3) 0.051(3) -0.023(3) 0.005(3) 0.017(3) O4 0.025(2) 0.029(2) 0.043(3) 0.018(2) -0.005(2) -0.008(2) O5 0.026(3) 0.032(3) 0.138(6) 0.030(3) -0.008(3) -0.009(2) O6 0.102(5) 0.041(3) 0.021(2) 0.010(2) 0.013(3) 0.018(3) Cl2 0.0212(8) 0.0314(9) 0.0364(8) 0.0138(7) -0.0033(7) -0.0047(6) O7 0.026(2) 0.034(3) 0.044(3) -0.009(2) -0.001(2) -0.004(2) O8 0.064(4) 0.059(4) 0.064(4) 0.032(3) -0.014(3) -0.035(3) O9 0.032(3) 0.052(3) 0.044(3) -0.012(3) -0.004(2) -0.005(3) O10 0.043(3) 0.079(5) 0.049(3) 0.040(3) 0.016(3) 0.026(3) C60 0.028(4) 0.028(3) 0.028(3) -0.003(3) -0.002(3) -0.001(3) C61 0.017(3) 0.025(3) 0.036(4) 0.004(3) -0.004(3) -0.010(3) N62 0.021(3) 0.033(3) 0.039(3) -0.005(3) -0.011(3) 0.001(2) C71 0.032(4) 0.032(4) 0.029(3) 0.000(3) 0.007(3) -0.009(3) C70 0.043(5) 0.047(5) 0.035(4) 0.008(4) 0.001(4) -0.004(4) N72 0.038(4) 0.037(3) 0.040(3) 0.005(3) 0.002(3) -0.006(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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 89.0(2) . . ? N2 Ni1 O2 95.07(17) . . ? N1 Ni1 O2 175.30(19) . . ? N2 Ni1 O1 173.68(19) . . ? N1 Ni1 O1 95.54(18) . . ? O2 Ni1 O1 80.56(15) . . ? N2 Ni1 Ni2 135.34(13) . . ? N1 Ni1 Ni2 135.63(15) . . ? O2 Ni1 Ni2 40.36(12) . . ? O1 Ni1 Ni2 40.21(11) . . ? N3 Ni2 N4 89.21(19) . . ? N3 Ni2 O1 175.31(19) . . ? N4 Ni2 O1 95.22(18) . . ? N3 Ni2 O2 95.26(18) . . ? N4 Ni2 O2 175.35(18) . . ? O1 Ni2 O2 80.35(15) . . ? N3 Ni2 Ni1 135.23(14) . . ? N4 Ni2 Ni1 135.54(13) . . ? O1 Ni2 Ni1 40.32(11) . . ? O2 Ni2 Ni1 40.04(11) . . ? C46 N1 C1 122.1(5) . . ? C46 N1 Ni1 124.1(4) . . ? C1 N1 Ni1 113.2(3) . . ? C15 N2 C8 121.0(4) . . ? C15 N2 Ni1 125.6(4) . . ? C8 N2 Ni1 112.7(3) . . ? C23 N3 C24 122.8(4) . . ? C23 N3 Ni2 125.3(4) . . ? C24 N3 Ni2 111.7(3) . . ? C38 N4 C31 121.5(4) . . ? C38 N4 Ni2 125.7(4) . . ? C31 N4 Ni2 112.7(3) . . ? C44 O1 Ni2 129.3(3) . . ? C44 O1 Ni1 130.7(3) . . ? Ni2 O1 Ni1 99.46(17) . . ? C21 O2 Ni1 130.6(3) . . ? C21 O2 Ni2 129.4(3) . . ? Ni1 O2 Ni2 99.60(17) . . ? N1 C1 C8 108.3(4) . . ? N1 C1 C2 113.7(4) . . ? C8 C1 C2 110.8(4) . . ? C3 C2 C7 119.6(5) . . ? C3 C2 C1 121.3(5) . . ? C7 C2 C1 119.1(5) . . ? C2 C3 C4 119.7(6) . . ? C3 C4 C5 121.3(5) . . ? C6 C5 C4 118.6(5) . . ? C7 C6 C5 120.1(5) . . ? C6 C7 C2 120.7(5) . . ? N2 C8 C14 112.1(4) . . ? N2 C8 C1 107.9(4) . . ? C14 C8 C1 113.0(4) . . ? C10 C9 C14 120.1(6) . . ? C9 C10 C11 120.1(6) . . ? C12 C11 C10 120.3(6) . . ? C11 C12 C13 120.0(6) . . ? C14 C13 C12 119.3(6) . . ? C13 C14 C9 119.8(6) . . ? C13 C14 C8 118.7(5) . . ? C9 C14 C8 121.4(5) . . ? N2 C15 C16 126.7(5) . . ? C17 C16 C21 118.4(5) . . ? C17 C16 C15 119.3(5) . . ? C21 C16 C15 122.3(5) . . ? C18 C17 C16 123.3(5) . . ? C17 C18 C19 117.0(5) . . ? C17 C18 C22 122.5(5) . . ? C19 C18 C22 120.5(4) . . ? C20 C19 C18 122.5(5) . . ? C19 C20 C21 118.7(5) . . ? C19 C20 C23 118.1(5) . . ? C21 C20 C23 123.2(5) . . ? O2 C21 C20 120.2(5) . . ? O2 C21 C16 119.7(4) . . ? C20 C21 C16 120.1(5) . . ? N3 C23 C20 125.8(5) . . ? C25 C24 N3 115.9(4) . . ? C25 C24 C31 111.4(4) . . ? N3 C24 C31 106.4(4) . . ? C30 C25 C26 118.6(5) . . ? C30 C25 C24 120.7(5) . . ? C26 C25 C24 120.7(5) . . ? C27 C26 C25 120.0(5) . . ? C26 C27 C28 120.4(6) . . ? C29 C28 C27 120.1(5) . . ? C28 C29 C30 118.7(5) . . ? C25 C30 C29 122.2(6) . . ? C32 C31 N4 113.9(4) . . ? C32 C31 C24 113.6(4) . . ? N4 C31 C24 106.4(4) . . ? C33 C32 C37 118.4(5) . . ? C33 C32 C31 118.4(5) . . ? C37 C32 C31 123.1(5) . . ? C32 C33 C34 121.2(5) . . ? C33 C34 C35 119.7(5) . . ? C36 C35 C34 119.4(5) . . ? C35 C36 C37 120.8(5) . . ? C36 C37 C32 120.4(5) . . ? N4 C38 C39 126.3(5) . . ? C40 C39 C44 118.4(5) . . ? C40 C39 C38 119.7(5) . . ? C44 C39 C38 121.9(5) . . ? C41 C40 C39 123.7(5) . . ? C40 C41 C42 117.2(5) . . ? C40 C41 C45 121.3(5) . . ? C42 C41 C45 121.4(5) . . ? C41 C42 C43 122.9(5) . . ? C42 C43 C44 118.4(5) . . ? C42 C43 C46 119.3(5) . . ? C44 C43 C46 122.3(5) . . ? O1 C44 C39 121.1(5) . . ? O1 C44 C43 119.5(5) . . ? C39 C44 C43 119.4(5) . . ? N1 C46 C43 127.7(5) . . ? O3 Cl1 O5 110.8(4) . . ? O3 Cl1 O6 108.7(3) . . ? O5 Cl1 O6 109.3(4) . . ? O3 Cl1 O4 111.3(3) . . ? O5 Cl1 O4 108.7(3) . . ? O6 Cl1 O4 108.0(3) . . ? O8 Cl2 O9 109.9(3) . . ? O8 Cl2 O10 110.4(4) . . ? O9 Cl2 O10 108.9(4) . . ? O8 Cl2 O7 109.2(4) . . ? O9 Cl2 O7 109.4(3) . . ? O10 Cl2 O7 109.0(3) . . ? N62 C61 C60 176.9(7) . . ? N72 C71 C70 179.3(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.826(4) . ? Ni1 N1 1.835(5) . ? Ni1 O2 1.838(4) . ? Ni1 O1 1.848(4) . ? Ni1 Ni2 2.8165(9) . ? Ni2 N3 1.825(4) . ? Ni2 N4 1.828(4) . ? Ni2 O1 1.843(3) . ? Ni2 O2 1.850(4) . ? N1 C46 1.295(7) . ? N1 C1 1.471(7) . ? N2 C15 1.272(7) . ? N2 C8 1.486(6) . ? N3 C23 1.295(7) . ? N3 C24 1.508(6) . ? N4 C38 1.288(7) . ? N4 C31 1.505(6) . ? O1 C44 1.322(6) . ? O2 C21 1.311(7) . ? C1 C8 1.532(7) . ? C1 C2 1.534(7) . ? C2 C3 1.382(7) . ? C2 C7 1.405(8) . ? C3 C4 1.383(8) . ? C4 C5 1.401(9) . ? C5 C6 1.403(8) . ? C6 C7 1.377(8) . ? C8 C14 1.521(8) . ? C9 C10 1.373(8) . ? C9 C14 1.386(8) . ? C10 C11 1.385(9) . ? C11 C12 1.362(10) . ? C12 C13 1.406(9) . ? C13 C14 1.388(8) . ? C15 C16 1.446(7) . ? C16 C17 1.407(7) . ? C16 C21 1.419(7) . ? C17 C18 1.385(7) . ? C18 C19 1.413(8) . ? C18 C22 1.508(8) . ? C19 C20 1.404(7) . ? C20 C21 1.414(7) . ? C20 C23 1.434(7) . ? C24 C25 1.502(7) . ? C24 C31 1.532(7) . ? C25 C30 1.372(7) . ? C25 C26 1.412(8) . ? C26 C27 1.389(7) . ? C27 C28 1.394(8) . ? C28 C29 1.393(9) . ? C29 C30 1.399(7) . ? C31 C32 1.502(7) . ? C32 C33 1.378(7) . ? C32 C37 1.385(8) . ? C33 C34 1.381(8) . ? C34 C35 1.387(9) . ? C35 C36 1.364(8) . ? C36 C37 1.384(8) . ? C38 C39 1.449(7) . ? C39 C40 1.393(8) . ? C39 C44 1.410(7) . ? C40 C41 1.370(7) . ? C41 C42 1.381(8) . ? C41 C45 1.500(8) . ? C42 C43 1.398(8) . ? C43 C44 1.419(7) . ? C43 C46 1.449(7) . ? Cl1 O3 1.408(5) . ? Cl1 O5 1.415(6) . ? Cl1 O6 1.427(5) . ? Cl1 O4 1.438(4) . ? Cl2 O8 1.398(5) . ? Cl2 O9 1.434(5) . ? Cl2 O10 1.438(5) . ? Cl2 O7 1.437(5) . ? C60 C61 1.455(9) . ? C61 N62 1.125(8) . ? C71 N72 1.159(9) . ? C71 C70 1.433(10) . ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168337010