#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000118.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_4000118 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm010681c _journal_year 2002 _chemical_formula_moiety '[Ni(4-PhPy)2(DBM)2]*4(benzene)' _chemical_formula_sum 'C76 H64 N2 Ni O4' _chemical_formula_weight 1128.00 _chemical_name_common ; Bis(dibenzoylmethanato)bis- (4-phenylpyridine)nickel(II), clathrate with benzene 1:4 ; _chemical_name_systematic ; Bis(1,3-diphenyl-1,3-propanediono)bis(4-phenylpyridine)nickel(II), clathrate with benzene 1:4 ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 110.34(1) _cell_angle_beta 94.32(1) _cell_angle_gamma 117.73(1) _cell_formula_units_Z 1 _cell_length_a 11.565(2) _cell_length_b 12.354(2) _cell_length_c 13.205(2) _cell_measurement_reflns_used 'all data' _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.7 _cell_measurement_theta_min 1.7 _cell_volume 1500.6(4) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 18011 _diffrn_reflns_theta_max 28.73 _diffrn_reflns_theta_min 1.72 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_correction_T_min 0.7066 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'oblique block' _exptl_crystal_F_000 594 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 379 _refine_ls_number_reflns 7717 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.0963 _reflns_number_gt 5583 _reflns_number_total 7717 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4000118 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.0000 1.0000 0.02777(9) Uani 1 d S . . O1 O 0.17949(9) 0.02472(9) 1.06250(8) 0.0326(2) Uani 1 d . . . C1 C 0.20581(13) -0.06793(13) 1.03917(11) 0.0250(3) Uani 1 d . . . C11 C 0.35083(13) -0.02194(14) 1.09116(11) 0.0264(3) Uani 1 d . . . C12 C 0.44119(15) 0.11499(15) 1.16104(13) 0.0361(3) Uani 1 d . . . H12 H 0.4108 0.1768 1.1743 0.043 Uiso 1 calc R . . C13 C 0.57528(15) 0.16233(17) 1.21156(14) 0.0435(4) Uani 1 d . . . H13 H 0.6361 0.2562 1.2593 0.052 Uiso 1 calc R . . C14 C 0.62092(15) 0.07412(17) 1.19306(14) 0.0408(4) Uani 1 d . . . H14 H 0.7128 0.1067 1.2281 0.049 Uiso 1 calc R . . C15 C 0.53254(15) -0.06160(17) 1.12345(15) 0.0417(4) Uani 1 d . . . H15 H 0.5638 -0.1227 1.1099 0.050 Uiso 1 calc R . . C16 C 0.39838(14) -0.10962(15) 1.07303(13) 0.0345(3) Uani 1 d . . . H16 H 0.3382 -0.2036 1.0255 0.041 Uiso 1 calc R . . C2 C 0.11083(13) -0.20703(14) 0.97202(12) 0.0304(3) Uani 1 d . . . H2 H 0.1445 -0.2663 0.9570 0.036 Uiso 1 calc R . . O3 O -0.08947(9) -0.20209(9) 0.93143(8) 0.0300(2) Uani 1 d . . . C3 C -0.02830(13) -0.26566(13) 0.92558(11) 0.0240(3) Uani 1 d . . . C31 C -0.11893(13) -0.41772(13) 0.86308(11) 0.0249(3) Uani 1 d . . . C32 C -0.08041(14) -0.50617(14) 0.87112(12) 0.0313(3) Uani 1 d . . . H32 H 0.0091 -0.4708 0.9141 0.038 Uiso 1 calc R . . C33 C -0.17080(16) -0.64539(15) 0.81719(14) 0.0377(4) Uani 1 d . . . H33 H -0.1438 -0.7046 0.8249 0.045 Uiso 1 calc R . . C34 C -0.30010(16) -0.69824(15) 0.75225(14) 0.0395(4) Uani 1 d . . . H34 H -0.3618 -0.7937 0.7146 0.047 Uiso 1 calc R . . C35 C -0.33934(15) -0.61171(15) 0.74228(14) 0.0408(4) Uani 1 d . . . H35 H -0.4280 -0.6477 0.6972 0.049 Uiso 1 calc R . . C36 C -0.24979(14) -0.47258(14) 0.79777(13) 0.0324(3) Uani 1 d . . . H36 H -0.2781 -0.4138 0.7912 0.039 Uiso 1 calc R . . N7 N 0.05408(11) 0.00121(12) 0.85018(10) 0.0315(3) Uani 1 d . . . C71 C 0.16502(14) 0.11031(14) 0.85340(13) 0.0330(3) Uani 1 d . . . H71 H 0.2143 0.1894 0.9230 0.040 Uiso 1 calc R . . C72 C 0.21051(14) 0.11248(15) 0.76010(13) 0.0342(3) Uani 1 d . . . H72 H 0.2891 0.1922 0.7663 0.041 Uiso 1 calc R . . C73 C 0.14171(14) -0.00166(14) 0.65710(12) 0.0315(3) Uani 1 d . . . C74 C 0.02473(15) -0.11298(15) 0.65374(13) 0.0364(4) Uani 1 d . . . H74 H -0.0277 -0.1927 0.5849 0.044 Uiso 1 calc R . . C75 C -0.01482(14) -0.10722(15) 0.75028(13) 0.0358(3) Uani 1 d . . . H75 H -0.0952 -0.1843 0.7457 0.043 Uiso 1 calc R . . C76 C 0.19177(15) -0.00409(15) 0.55673(13) 0.0342(3) Uani 1 d . . . C77 C 0.33147(17) 0.05794(16) 0.56861(14) 0.0416(4) Uani 1 d . . . H77 H 0.3938 0.0996 0.6408 0.050 Uiso 1 calc R . . C78 C 0.3799(2) 0.05918(18) 0.47617(16) 0.0509(5) Uani 1 d . . . H78 H 0.4751 0.1005 0.4849 0.061 Uiso 1 calc R . . C79 C 0.2908(2) 0.00095(18) 0.37166(17) 0.0547(5) Uani 1 d . . . H79 H 0.3246 0.0034 0.3086 0.066 Uiso 1 calc R . . C7X C 0.1522(2) -0.06125(19) 0.35840(15) 0.0520(5) Uani 1 d . . . H7X H 0.0907 -0.1014 0.2862 0.062 Uiso 1 calc R . . C7Y C 0.10287(18) -0.06525(17) 0.44994(14) 0.0432(4) Uani 1 d . . . H7Y H 0.0073 -0.1102 0.4399 0.052 Uiso 1 calc R . . C1A C 0.8238(2) 0.5855(2) 0.2269(2) 0.0665(6) Uani 1.0000(19) d . A 1 H1A H 0.9188 0.6310 0.2617 0.080 Uiso 1.0000(19) calc R A 1 C2A C 0.7772(3) 0.5455(3) 0.1153(2) 0.0791(8) Uani 1.0000(19) d . A 1 H2A H 0.8398 0.5647 0.0721 0.095 Uiso 1.0000(19) calc R A 1 C3A C 0.6406(3) 0.4777(3) 0.06449(19) 0.0872(9) Uani 1.0000(19) d . A 1 H3A H 0.6083 0.4490 -0.0140 0.105 Uiso 1.0000(19) calc R A 1 C4A C 0.5496(2) 0.4509(2) 0.1272(2) 0.0743(7) Uani 1.0000(19) d . A 1 H4A H 0.4544 0.4033 0.0923 0.089 Uiso 1.0000(19) calc R A 1 C5A C 0.5977(2) 0.4935(2) 0.23986(18) 0.0596(5) Uani 1.0000(19) d . A 1 H5A H 0.5360 0.4767 0.2841 0.072 Uiso 1.0000(19) calc R A 1 C6A C 0.7338(2) 0.5601(2) 0.28898(17) 0.0606(5) Uani 1.0000(19) d . A 1 H6A H 0.7666 0.5892 0.3675 0.073 Uiso 1.0000(19) calc R A 1 C1B C 0.5343(2) 0.40383(19) 0.48155(16) 0.0542(5) Uani 1.006(3) d P . 2 H1B H 0.5580 0.3372 0.4685 0.065 Uiso 1.006(3) calc PR . 2 C2B C 0.63380(19) 0.53945(19) 0.54024(15) 0.0512(5) Uani 1.006(3) d P . 2 H2B H 0.7256 0.5661 0.5680 0.061 Uiso 1.006(3) calc PR . 2 C3B C 0.5995(2) 0.63597(19) 0.55845(16) 0.0547(5) Uani 1.006(3) d P . 2 H3B H 0.6677 0.7296 0.5984 0.066 Uiso 1.006(3) calc PR . 2 C1C C -0.06335(18) 0.45522(19) 0.57393(15) 0.0507(5) Uani 1.010(3) d P . 3 H1C H -0.1072 0.4245 0.6249 0.061 Uiso 1.010(3) calc PR . 3 C2C C 0.0470(2) 0.5850(2) 0.61303(15) 0.0578(6) Uani 1.010(3) d P . 3 H2C H 0.0800 0.6439 0.6913 0.069 Uiso 1.010(3) calc PR . 3 C3C C 0.11014(18) 0.63006(19) 0.53932(15) 0.0537(5) Uani 1.010(3) d P . 3 H3C H 0.1860 0.7201 0.5667 0.064 Uiso 1.010(3) calc PR . 3 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 0.02368(14) 0.02104(13) 0.03175(16) 0.00588(11) 0.00115(10) 0.01168(11) O1 0.0266(5) 0.0232(5) 0.0379(6) 0.0051(4) -0.0002(4) 0.0129(4) C1 0.0239(6) 0.0258(7) 0.0236(7) 0.0102(6) 0.0057(5) 0.0124(6) C11 0.0238(6) 0.0301(7) 0.0239(7) 0.0117(6) 0.0055(5) 0.0133(6) C12 0.0303(7) 0.0313(8) 0.0376(9) 0.0078(7) 0.0026(6) 0.0158(6) C13 0.0276(8) 0.0356(8) 0.0448(10) 0.0053(7) -0.0021(7) 0.0106(7) C14 0.0248(7) 0.0490(10) 0.0397(9) 0.0144(8) 0.0008(6) 0.0175(7) C15 0.0326(8) 0.0438(9) 0.0522(10) 0.0189(8) 0.0061(7) 0.0248(7) C16 0.0282(7) 0.0301(7) 0.0390(9) 0.0104(7) 0.0023(6) 0.0150(6) C2 0.0262(7) 0.0241(7) 0.0372(8) 0.0085(6) 0.0037(6) 0.0147(6) O3 0.0250(5) 0.0227(5) 0.0356(6) 0.0065(4) 0.0017(4) 0.0129(4) C3 0.0271(7) 0.0228(6) 0.0214(7) 0.0090(5) 0.0064(5) 0.0129(6) C31 0.0265(7) 0.0232(6) 0.0229(7) 0.0087(5) 0.0074(5) 0.0125(6) C32 0.0301(7) 0.0273(7) 0.0321(8) 0.0096(6) 0.0036(6) 0.0149(6) C33 0.0411(8) 0.0253(7) 0.0460(9) 0.0131(7) 0.0094(7) 0.0190(7) C34 0.0368(8) 0.0206(7) 0.0461(10) 0.0079(7) 0.0062(7) 0.0095(6) C35 0.0295(8) 0.0287(8) 0.0484(10) 0.0097(7) -0.0014(7) 0.0106(7) C36 0.0296(7) 0.0260(7) 0.0379(8) 0.0108(6) 0.0043(6) 0.0148(6) N7 0.0266(6) 0.0268(6) 0.0345(7) 0.0089(5) 0.0015(5) 0.0134(5) C71 0.0289(7) 0.0262(7) 0.0341(8) 0.0070(6) 0.0025(6) 0.0126(6) C72 0.0281(7) 0.0285(7) 0.0381(9) 0.0106(7) 0.0047(6) 0.0124(6) C73 0.0295(7) 0.0316(7) 0.0339(8) 0.0122(6) 0.0034(6) 0.0186(6) C74 0.0340(8) 0.0304(8) 0.0303(8) 0.0058(6) -0.0011(6) 0.0132(7) C75 0.0274(7) 0.0285(7) 0.0361(9) 0.0090(7) -0.0002(6) 0.0084(6) C76 0.0413(8) 0.0277(7) 0.0345(8) 0.0110(6) 0.0086(7) 0.0209(7) C77 0.0434(9) 0.0353(8) 0.0418(9) 0.0151(7) 0.0132(7) 0.0186(7) C78 0.0572(11) 0.0372(9) 0.0564(12) 0.0203(9) 0.0275(9) 0.0219(8) C79 0.0912(15) 0.0437(10) 0.0500(12) 0.0254(9) 0.0389(11) 0.0444(11) C7X 0.0809(14) 0.0560(11) 0.0349(10) 0.0170(8) 0.0152(9) 0.0496(11) C7Y 0.0524(10) 0.0464(9) 0.0374(9) 0.0136(8) 0.0088(8) 0.0345(9) C1A 0.0574(12) 0.0766(15) 0.0784(16) 0.0421(13) 0.0335(12) 0.0367(11) C2A 0.117(2) 0.127(2) 0.0852(18) 0.0763(17) 0.0741(17) 0.104(2) C3A 0.148(2) 0.129(2) 0.0433(13) 0.0376(14) 0.0293(15) 0.115(2) C4A 0.0718(15) 0.0860(17) 0.0649(15) 0.0267(13) 0.0074(12) 0.0472(13) C5A 0.0514(11) 0.0781(15) 0.0643(14) 0.0428(12) 0.0268(10) 0.0349(11) C6A 0.0595(12) 0.0716(14) 0.0472(11) 0.0254(10) 0.0206(10) 0.0315(11) C1B 0.0702(13) 0.0480(11) 0.0545(12) 0.0249(9) 0.0201(10) 0.0363(10) C2B 0.0519(10) 0.0555(11) 0.0462(11) 0.0260(9) 0.0126(8) 0.0256(9) C3B 0.0611(12) 0.0401(10) 0.0491(11) 0.0159(8) 0.0094(9) 0.0198(9) C1C 0.0506(11) 0.0573(11) 0.0418(10) 0.0217(9) 0.0150(8) 0.0262(9) C2C 0.0595(12) 0.0511(11) 0.0346(10) 0.0055(8) 0.0074(8) 0.0186(9) C3C 0.0470(10) 0.0430(10) 0.0479(11) 0.0112(8) 0.0076(8) 0.0137(8)