#------------------------------------------------------------------------------ #$Date: 2008-02-07 18:04:49 +0000 (Thu, 07 Feb 2008) $ #$Revision: 98 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000098.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_4000098 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_name_systematic ; Bis(1,3-diphenyl-1,3-propanediono)bis(2-methylpyridine)nickel(II), metastable f ; _chemical_name_common Bis(dibenzoylmethanato)bis(2-methylpyridine)ni _chemical_formula_moiety [Ni(2-MePy)2(DBM)2] _chemical_formula_sum 'C42 H36 N2 Ni O4' _chemical_formula_weight 691.44 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7680(10) _cell_length_b 35.910(5) _cell_length_c 12.000(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.970(10) _cell_angle_gamma 90.00 _cell_volume 3528.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 'all data' _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41746 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.74 _reflns_number_total 9135 _reflns_number_gt 7106 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.5157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9135 _refine_ls_number_parameters 574 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.04482(2) 0.122223(5) 0.302727(14) 0.02842(6) Uani 1 d . . . O1 O -0.03902(13) 0.17073(3) 0.33882(8) 0.0341(2) Uani 1 d . . . C1 C -0.08822(17) 0.19815(4) 0.26876(12) 0.0294(3) Uani 1 d . . . C11 C -0.13132(18) 0.23218(4) 0.32406(13) 0.0330(3) Uani 1 d . . . C12 C -0.0936(2) 0.23261(5) 0.44704(14) 0.0435(4) Uani 1 d . . . H12 H -0.0335 0.2126 0.4942 0.052 Uiso 1 calc R . . C13 C -0.1426(3) 0.26184(6) 0.50162(17) 0.0593(5) Uani 1 d . . . H13 H -0.1157 0.2618 0.5857 0.071 Uiso 1 calc R . . C14 C -0.2307(3) 0.29105(6) 0.43384(19) 0.0663(6) Uani 1 d . . . H14 H -0.2657 0.3110 0.4710 0.080 Uiso 1 calc R . . C15 C -0.2675(3) 0.29124(5) 0.31232(19) 0.0612(5) Uani 1 d . . . H15 H -0.3273 0.3114 0.2658 0.073 Uiso 1 calc R . . C16 C -0.2180(2) 0.26217(4) 0.25748(16) 0.0466(4) Uani 1 d . . . H16 H -0.2434 0.2627 0.1736 0.056 Uiso 1 calc R . . C2 C -0.1105(2) 0.19796(4) 0.14752(13) 0.0359(3) Uani 1 d . . . H2 H -0.1347 0.2210 0.1060 0.043 Uiso 1 calc R . . O3 O -0.05413(13) 0.13417(3) 0.12595(8) 0.0330(2) Uani 1 d . . . C3 C -0.09991(17) 0.16609(4) 0.08241(12) 0.0308(3) Uani 1 d . . . C31 C -0.14533(19) 0.16934(4) -0.05065(12) 0.0356(3) Uani 1 d . . . C32 C -0.2458(3) 0.19756(5) -0.11752(15) 0.0573(5) Uani 1 d . . . H32 H -0.2907 0.2153 -0.0792 0.069 Uiso 1 calc R . . C33 C -0.2807(3) 0.19995(6) -0.23957(16) 0.0739(7) Uani 1 d . . . H33 H -0.3483 0.2195 -0.2842 0.089 Uiso 1 calc R . . C34 C -0.2179(3) 0.17414(6) -0.29631(15) 0.0632(6) Uani 1 d . . . H34 H -0.2412 0.1760 -0.3798 0.076 Uiso 1 calc R . . C35 C -0.1209(2) 0.14552(5) -0.23190(14) 0.0504(4) Uani 1 d . . . H35 H -0.0788 0.1275 -0.2711 0.060 Uiso 1 calc R . . C36 C -0.0851(2) 0.14319(4) -0.10939(13) 0.0393(3) Uani 1 d . . . H36 H -0.0185 0.1234 -0.0654 0.047 Uiso 1 calc R . . O4 O 0.12592(13) 0.07249(3) 0.26821(8) 0.0322(2) Uani 1 d . . . C4 C 0.17398(16) 0.04556(4) 0.34028(12) 0.0287(3) Uani 1 d . . . C41 C 0.21569(17) 0.01069(4) 0.28815(12) 0.0310(3) Uani 1 d . . . C42 C 0.1668(2) 0.00788(5) 0.16503(14) 0.0497(4) Uani 1 d . . . H42 H 0.1058 0.0275 0.1161 0.060 Uiso 1 calc R . . C43 C 0.2060(3) -0.02320(6) 0.11277(16) 0.0631(6) Uani 1 d . . . H43 H 0.1696 -0.0250 0.0283 0.076 Uiso 1 calc R . . C44 C 0.2975(2) -0.05166(5) 0.18188(17) 0.0535(4) Uani 1 d . . . H44 H 0.3248 -0.0729 0.1456 0.064 Uiso 1 calc R . . C45 C 0.3484(3) -0.04894(5) 0.30361(17) 0.0572(5) Uani 1 d . . . H45 H 0.4130 -0.0682 0.3522 0.069 Uiso 1 calc R . . C46 C 0.3062(2) -0.01820(5) 0.35639(15) 0.0499(4) Uani 1 d . . . H46 H 0.3401 -0.0170 0.4409 0.060 Uiso 1 calc R . . C5 C 0.19254(19) 0.04656(4) 0.46137(12) 0.0360(3) Uani 1 d . . . H5 H 0.2145 0.0238 0.5044 0.043 Uiso 1 calc R . . O6 O 0.14650(14) 0.11125(3) 0.47837(8) 0.0371(2) Uani 1 d . . . C6 C 0.18083(18) 0.07905(4) 0.52318(12) 0.0333(3) Uani 1 d . . . C61 C 0.2172(2) 0.07691(4) 0.65506(13) 0.0383(3) Uani 1 d . . . C62 C 0.1677(3) 0.04701(6) 0.70695(15) 0.0540(5) Uani 1 d . . . H62 H 0.1133 0.0265 0.6593 0.065 Uiso 1 calc R . . C63 C 0.1980(3) 0.04713(6) 0.82938(17) 0.0666(6) Uani 1 d . . . H63 H 0.1618 0.0269 0.8645 0.080 Uiso 1 calc R . . C64 C 0.2790(3) 0.07608(6) 0.89894(15) 0.0667(6) Uani 1 d . . . H64 H 0.3006 0.0757 0.9824 0.080 Uiso 1 calc R . . C65 C 0.3302(3) 0.10605(6) 0.84815(16) 0.0693(6) Uani 1 d . . . H65 H 0.3877 0.1261 0.8968 0.083 Uiso 1 calc R . . C66 C 0.2968(3) 0.10662(5) 0.72623(14) 0.0542(5) Uani 1 d . . . H66 H 0.3287 0.1275 0.6911 0.065 Uiso 1 calc R . . N7 N -0.1816(3) 0.09096(7) 0.2779(2) 0.0310(5) Uani 0.672(3) d P A -1 C71 C -0.2297(6) 0.07057(12) 0.1760(4) 0.0365(8) Uani 0.672(3) d P A -1 H71 H -0.1743 0.0741 0.1217 0.044 Uiso 0.672(3) calc PR A -1 C72 C -0.3549(3) 0.04501(8) 0.1475(2) 0.0470(7) Uani 0.672(3) d P A -1 H72 H -0.3850 0.0312 0.0754 0.056 Uiso 0.672(3) calc PR A -1 C73 C -0.4361(3) 0.03998(9) 0.2264(3) 0.0525(7) Uani 0.672(3) d P A -1 H73 H -0.5210 0.0221 0.2104 0.063 Uiso 0.672(3) calc PR A -1 C74 C -0.3917(9) 0.0614(2) 0.3289(4) 0.0418(11) Uani 0.672(3) d P A -1 H74 H -0.4479 0.0588 0.3830 0.050 Uiso 0.672(3) calc PR A -1 C75 C -0.2639(3) 0.08669(6) 0.35218(19) 0.0345(6) Uani 0.672(3) d P A -1 C76 C -0.2178(6) 0.11022(11) 0.4622(3) 0.0450(9) Uani 0.672(3) d P A -1 H76A H -0.3167 0.1177 0.4765 0.067 Uiso 0.672(3) calc PR A -1 H76B H -0.1597 0.1325 0.4515 0.067 Uiso 0.672(3) calc PR A -1 H76C H -0.1469 0.0959 0.5307 0.067 Uiso 0.672(3) calc PR A -1 N7A N -0.1737(6) 0.10071(14) 0.3248(4) 0.0326(11) Uani 0.328(3) d P A -2 C71A C -0.1996(9) 0.1126(2) 0.4228(6) 0.0345(14) Uani 0.328(3) d P A -2 H71A H -0.1275 0.1309 0.4708 0.041 Uiso 0.328(3) calc PR A -2 C72A C -0.3232(7) 0.10006(15) 0.4584(5) 0.0422(13) Uani 0.328(3) d P A -2 H72A H -0.3366 0.1097 0.5280 0.051 Uiso 0.328(3) calc PR A -2 C73A C -0.4279(7) 0.07293(16) 0.3895(5) 0.0420(13) Uani 0.328(3) d P A -2 H73A H -0.5144 0.0634 0.4111 0.050 Uiso 0.328(3) calc PR A -2 C74A C -0.4027(18) 0.0601(4) 0.2875(7) 0.037(2) Uani 0.328(3) d P A -2 H74A H -0.4720 0.0415 0.2390 0.045 Uiso 0.328(3) calc PR A -2 C75A C -0.2758(6) 0.07468(14) 0.2575(4) 0.0351(12) Uani 0.328(3) d P A -2 C76A C -0.2578(14) 0.0618(3) 0.1468(9) 0.044(2) Uani 0.328(3) d P A -2 H76D H -0.2521 0.0833 0.0982 0.066 Uiso 0.328(3) calc PR A -2 H76E H -0.3519 0.0463 0.1020 0.066 Uiso 0.328(3) calc PR A -2 H76F H -0.1574 0.0471 0.1662 0.066 Uiso 0.328(3) calc PR A -2 N8 N 0.2657(3) 0.14669(7) 0.2946(2) 0.0338(5) Uani 0.830(3) d PD A -1 C81 C 0.3044(3) 0.13245(6) 0.2037(2) 0.0370(5) Uani 0.830(3) d PD A -1 H81 H 0.2396 0.1127 0.1583 0.044 Uiso 0.830(3) calc PR A -1 C82 C 0.4324(3) 0.14512(7) 0.17350(18) 0.0464(5) Uani 0.830(3) d PD A -1 H82 H 0.4576 0.1339 0.1104 0.056 Uiso 0.830(3) calc PR A -1 C83 C 0.5230(3) 0.17443(8) 0.2373(2) 0.0576(7) Uani 0.830(3) d PD A -1 H83 H 0.6101 0.1845 0.2171 0.069 Uiso 0.830(3) calc PR A -1 C84 C 0.4865(4) 0.18904(10) 0.3302(3) 0.0535(8) Uani 0.830(3) d PD A -1 H84 H 0.5490 0.2092 0.3751 0.064 Uiso 0.830(3) calc PR A -1 C85 C 0.3589(3) 0.17452(6) 0.35901(18) 0.0416(5) Uani 0.830(3) d PD A -1 C86 C 0.3240(4) 0.18956(8) 0.4633(2) 0.0586(8) Uani 0.830(3) d PD A -1 H86A H 0.4244 0.1999 0.5215 0.088 Uiso 0.830(3) calc PR A -1 H86B H 0.2836 0.1695 0.5007 0.088 Uiso 0.830(3) calc PR A -1 H86C H 0.2412 0.2092 0.4364 0.088 Uiso 0.830(3) calc PR A -1 N8A N 0.2736(13) 0.1542(3) 0.3330(8) 0.029(2) Uani 0.170(3) d PD A -2 C81A C 0.3045(12) 0.1782(2) 0.4255(7) 0.034(2) Uani 0.170(3) d PD A -2 H81A H 0.2458 0.1755 0.4780 0.041 Uiso 0.170(3) calc PR A -2 C82A C 0.4183(11) 0.2062(2) 0.4462(7) 0.046(3) Uani 0.170(3) d PD A -2 H82A H 0.4352 0.2233 0.5099 0.055 Uiso 0.170(3) calc PR A -2 C83A C 0.5066(11) 0.2087(3) 0.3725(9) 0.053(3) Uani 0.170(3) d PD A -2 H83A H 0.5825 0.2285 0.3826 0.064 Uiso 0.170(3) calc PR A -2 C84A C 0.4856(16) 0.1829(4) 0.2845(11) 0.037(3) Uani 0.170(3) d PD A -2 H84A H 0.5555 0.1828 0.2395 0.044 Uiso 0.170(3) calc PR A -2 C85A C 0.3611(9) 0.1569(2) 0.2615(6) 0.033(2) Uani 0.170(3) d PD A -2 C86A C 0.3323(14) 0.1297(3) 0.1627(8) 0.036(3) Uani 0.170(3) d PD A -2 H86D H 0.2408 0.1381 0.0926 0.055 Uiso 0.170(3) calc PR A -2 H86E H 0.3065 0.1053 0.1879 0.055 Uiso 0.170(3) calc PR A -2 H86F H 0.4308 0.1277 0.1423 0.055 Uiso 0.170(3) calc PR A -2 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 0.03576(10) 0.02745(9) 0.02239(9) 0.00132(6) 0.01084(7) 0.00207(7) O1 0.0444(6) 0.0326(5) 0.0273(5) 0.0021(4) 0.0152(4) 0.0067(4) C1 0.0302(7) 0.0277(7) 0.0304(7) -0.0004(5) 0.0110(5) -0.0011(5) C11 0.0328(7) 0.0293(7) 0.0358(7) -0.0043(5) 0.0108(6) -0.0021(6) C12 0.0494(9) 0.0403(8) 0.0374(8) -0.0069(6) 0.0115(7) 0.0044(7) C13 0.0736(13) 0.0553(11) 0.0457(10) -0.0191(8) 0.0175(9) 0.0082(10) C14 0.0721(14) 0.0517(11) 0.0689(13) -0.0261(10) 0.0176(11) 0.0143(10) C15 0.0694(13) 0.0377(9) 0.0654(12) -0.0075(8) 0.0107(10) 0.0162(9) C16 0.0538(10) 0.0350(8) 0.0456(9) -0.0027(7) 0.0112(8) 0.0051(7) C2 0.0492(9) 0.0277(7) 0.0307(7) 0.0037(5) 0.0141(6) 0.0027(6) O3 0.0438(6) 0.0283(5) 0.0254(4) 0.0015(4) 0.0104(4) 0.0014(4) C3 0.0343(7) 0.0322(7) 0.0260(6) 0.0019(5) 0.0108(5) -0.0020(6) C31 0.0445(8) 0.0335(7) 0.0263(6) 0.0013(5) 0.0096(6) -0.0019(6) C32 0.0802(14) 0.0524(11) 0.0322(8) 0.0030(7) 0.0114(8) 0.0227(10) C33 0.1095(18) 0.0638(13) 0.0322(9) 0.0096(8) 0.0058(10) 0.0282(13) C34 0.0963(16) 0.0622(12) 0.0250(8) 0.0027(7) 0.0145(9) 0.0049(11) C35 0.0699(12) 0.0513(10) 0.0300(8) -0.0046(7) 0.0181(8) -0.0014(9) C36 0.0496(9) 0.0366(8) 0.0299(7) 0.0001(6) 0.0120(6) 0.0000(7) O4 0.0414(6) 0.0295(5) 0.0259(5) 0.0022(4) 0.0124(4) 0.0024(4) C4 0.0285(7) 0.0281(6) 0.0288(6) 0.0003(5) 0.0093(5) -0.0007(5) C41 0.0318(7) 0.0289(7) 0.0322(7) -0.0018(5) 0.0115(6) -0.0023(5) C42 0.0625(11) 0.0499(10) 0.0324(8) -0.0042(7) 0.0116(7) 0.0152(8) C43 0.0825(15) 0.0621(12) 0.0398(9) -0.0135(8) 0.0160(9) 0.0187(11) C44 0.0656(12) 0.0396(9) 0.0587(11) -0.0131(8) 0.0266(9) 0.0046(8) C45 0.0796(14) 0.0371(9) 0.0557(11) 0.0037(8) 0.0251(10) 0.0194(9) C46 0.0733(12) 0.0385(9) 0.0371(8) 0.0034(7) 0.0187(8) 0.0145(8) C5 0.0476(9) 0.0318(7) 0.0290(7) 0.0055(5) 0.0141(6) 0.0056(6) O6 0.0521(6) 0.0335(5) 0.0252(5) 0.0030(4) 0.0133(4) 0.0084(5) C6 0.0370(8) 0.0373(8) 0.0257(6) 0.0045(5) 0.0114(6) 0.0065(6) C61 0.0474(9) 0.0420(8) 0.0267(7) 0.0056(6) 0.0147(6) 0.0162(7) C62 0.0719(13) 0.0589(11) 0.0349(8) 0.0064(8) 0.0235(8) 0.0016(9) C63 0.0994(17) 0.0686(13) 0.0414(10) 0.0173(9) 0.0369(11) 0.0125(12) C64 0.1060(17) 0.0697(13) 0.0277(8) 0.0094(8) 0.0278(10) 0.0328(12) C65 0.1191(19) 0.0532(11) 0.0307(8) -0.0024(8) 0.0208(10) 0.0203(12) C66 0.0898(14) 0.0418(9) 0.0309(8) 0.0011(7) 0.0214(9) 0.0115(9) N7 0.0362(12) 0.0288(12) 0.0293(13) -0.0007(9) 0.0133(11) -0.0006(10) C71 0.037(2) 0.037(2) 0.035(2) -0.0074(14) 0.0115(16) -0.0048(15) C72 0.0445(15) 0.0449(14) 0.0497(15) -0.0118(11) 0.0147(12) -0.0062(12) C73 0.0434(15) 0.0471(16) 0.0677(19) -0.0040(15) 0.0206(14) -0.0146(12) C74 0.041(2) 0.0475(19) 0.042(3) 0.009(3) 0.020(3) 0.0002(15) C75 0.0385(13) 0.0362(12) 0.0317(11) 0.0083(9) 0.0161(9) 0.0068(10) C76 0.057(2) 0.0527(18) 0.0337(19) -0.0013(15) 0.0268(16) 0.0038(15) N7A 0.036(2) 0.032(2) 0.026(2) -0.0036(18) 0.006(2) 0.0020(19) C71A 0.039(3) 0.037(3) 0.029(3) 0.001(3) 0.015(3) 0.000(2) C72A 0.045(3) 0.049(3) 0.040(3) 0.006(2) 0.023(2) 0.002(2) C73A 0.035(3) 0.051(3) 0.040(3) 0.010(2) 0.013(2) -0.005(2) C74A 0.032(3) 0.046(4) 0.032(5) 0.000(5) 0.010(5) -0.009(2) C75A 0.033(3) 0.036(2) 0.030(2) -0.0007(18) 0.0047(19) 0.005(2) C76A 0.042(5) 0.048(5) 0.041(5) -0.019(3) 0.012(4) -0.015(3) N8 0.0357(10) 0.0313(11) 0.0315(14) 0.0000(9) 0.0085(10) -0.0017(7) C81 0.0381(12) 0.0397(11) 0.0348(13) 0.0046(10) 0.0149(9) 0.0003(9) C82 0.0380(11) 0.0614(14) 0.0419(11) 0.0112(9) 0.0169(9) 0.0025(10) C83 0.0381(13) 0.0706(18) 0.0625(17) 0.0162(13) 0.0159(11) -0.0086(12) C84 0.0416(14) 0.0436(17) 0.065(3) -0.0011(16) 0.0068(15) -0.0112(13) C85 0.0371(11) 0.0345(10) 0.0434(11) 0.0003(8) 0.0023(9) -0.0001(9) C86 0.0574(17) 0.0536(18) 0.0541(18) -0.0266(12) 0.0068(14) -0.0084(13) N8A 0.038(5) 0.029(6) 0.017(5) -0.003(4) 0.007(4) 0.002(4) C81A 0.043(6) 0.027(5) 0.026(6) -0.006(4) 0.006(5) -0.006(4) C82A 0.047(6) 0.032(5) 0.047(6) -0.011(4) 0.004(4) -0.008(4) C83A 0.030(5) 0.053(7) 0.073(8) 0.001(6) 0.014(5) -0.016(5) C84A 0.042(6) 0.037(7) 0.045(9) -0.010(5) 0.031(7) -0.011(5) C85A 0.028(4) 0.039(5) 0.029(4) 0.010(3) 0.006(3) 0.001(4) C86A 0.037(6) 0.046(6) 0.034(6) 0.001(4) 0.022(4) 0.001(5)