# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1563 data_NitmtaaS8 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.0406(6) _cell_length_b 13.8560(2) _cell_length_c 18.1661(6) _cell_angle_alpha 90 _cell_angle_beta 97.2162(5) _cell_angle_gamma 90 _cell_volume 4505.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123K _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1058.77 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H44 N8 Ni2 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2192.00 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 123K _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Enraf-Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 30310 _reflns_number_total 30310 _reflns_number_gt 4925 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 8 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 176 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 176 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) -0.25435(5) -0.03354(5) -0.21784(5) 0.0236(3) 1.000 . Uani d ? Ni(2) -0.23330(5) -0.34704(5) -0.10580(5) 0.0236(3) 1.000 . Uani d ? S(1) -0.2587(1) -0.0576(1) -0.4309(1) 0.0710(8) 1.000 . Uani d ? S(2) -0.1642(1) 0.0184(2) -0.4065(2) 0.085(1) 1.000 . Uani d ? S(3) -0.1497(1) 0.0889(2) -0.5004(2) 0.0753(9) 1.000 . Uani d ? S(4) -0.1834(2) 0.2292(2) -0.4927(2) 0.090(1) 1.000 . Uani d ? S(5) -0.2880(2) 0.2408(1) -0.5457(1) 0.081(1) 1.000 . Uani d ? S(6) -0.3605(1) 0.2297(2) -0.4692(2) 0.098(1) 1.000 . Uani d ? S(7) -0.3991(1) 0.0915(2) -0.4699(2) 0.0781(9) 1.000 . Uani d ? S(8) -0.3406(2) 0.0175(2) -0.3856(1) 0.088(1) 1.000 . Uani d ? N(1) -0.1820(3) -0.1259(3) -0.2334(3) 0.023(2) 1.000 . Uani d ? N(2) -0.1746(3) 0.0533(3) -0.2113(3) 0.025(2) 1.000 . Uani d ? N(3) -0.3258(3) 0.0595(3) -0.2047(3) 0.024(2) 1.000 . Uani d ? N(4) -0.3343(3) -0.1203(3) -0.2253(3) 0.023(2) 1.000 . Uani d ? N(5) -0.1573(3) -0.2691(3) -0.0583(3) 0.023(2) 1.000 . Uani d ? N(6) -0.2980(3) -0.2687(3) -0.0596(3) 0.022(2) 1.000 . Uani d ? N(7) -0.3091(3) -0.4265(3) -0.1523(3) 0.022(2) 1.000 . Uani d ? N(8) -0.1682(3) -0.4269(3) -0.1496(3) 0.023(2) 1.000 . Uani d ? C(1) -0.1104(4) -0.0952(4) -0.2055(3) 0.026(2) 1.000 . Uani d ? C(2) -0.0494(4) -0.1519(4) -0.1817(4) 0.030(2) 1.000 . Uani d ? C(3) 0.0156(4) -0.1107(5) -0.1452(4) 0.034(2) 1.000 . Uani d ? C(4) 0.0192(4) -0.0126(5) -0.1311(4) 0.037(2) 1.000 . Uani d ? C(5) -0.0419(4) 0.0459(4) -0.1539(4) 0.030(2) 1.000 . Uani d ? C(6) -0.1070(4) 0.0071(4) -0.1915(3) 0.022(2) 1.000 . Uani d ? C(7) -0.1830(4) 0.1474(4) -0.2287(4) 0.033(2) 1.000 . Uani d ? C(8) -0.2528(4) 0.1911(4) -0.2390(4) 0.032(2) 1.000 . Uani d ? C(9) -0.3200(4) 0.1525(4) -0.2254(4) 0.032(2) 1.000 . Uani d ? C(10) -0.3894(4) 0.0179(4) -0.1798(4) 0.026(2) 1.000 . Uani d ? C(11) -0.4390(4) 0.0625(4) -0.1387(4) 0.030(2) 1.000 . Uani d ? C(12) -0.4938(4) 0.0119(5) -0.1103(4) 0.038(2) 1.000 . Uani d ? C(13) -0.5003(4) -0.0869(5) -0.1229(4) 0.033(2) 1.000 . Uani d ? C(14) -0.4509(4) -0.1331(4) -0.1624(4) 0.029(2) 1.000 . Uani d ? C(15) -0.3942(3) -0.0829(4) -0.1917(3) 0.024(2) 1.000 . Uani d ? C(16) -0.3349(4) -0.2058(4) -0.2623(3) 0.025(2) 1.000 . Uani d ? C(17) -0.2705(4) -0.2409(4) -0.2872(3) 0.023(2) 1.000 . Uani d ? C(18) -0.1974(4) -0.2079(4) -0.2718(3) 0.026(2) 1.000 . Uani d ? C(19) -0.1174(4) 0.2087(4) -0.2429(4) 0.047(3) 1.000 . Uani d ? C(20) -0.3885(4) 0.2166(4) -0.2388(4) 0.043(2) 1.000 . Uani d ? C(21) -0.4051(4) -0.2620(4) -0.2806(4) 0.029(2) 1.000 . Uani d ? C(22) -0.1379(4) -0.2646(4) -0.3032(4) 0.036(2) 1.000 . Uani d ? C(23) -0.1865(4) -0.1781(4) -0.0388(3) 0.025(2) 1.000 . Uani d ? C(24) -0.1472(4) -0.0917(4) -0.0322(4) 0.029(2) 1.000 . Uani d ? C(25) -0.1843(4) -0.0069(4) -0.0216(4) 0.035(2) 1.000 . Uani d ? C(26) -0.2607(4) -0.0067(4) -0.0187(4) 0.032(2) 1.000 . Uani d ? C(27) -0.3001(4) -0.0925(4) -0.0281(4) 0.030(2) 1.000 . Uani d ? C(28) -0.2635(4) -0.1778(4) -0.0387(3) 0.026(2) 1.000 . Uani d ? C(29) -0.3627(4) -0.2986(4) -0.0412(4) 0.027(2) 1.000 . Uani d ? C(30) -0.3994(3) -0.3800(4) -0.0736(4) 0.027(2) 1.000 . Uani d ? C(31) -0.3757(4) -0.4378(4) -0.1294(4) 0.027(2) 1.000 . Uani d ? C(32) -0.2848(4) -0.4746(4) -0.2135(4) 0.023(2) 1.000 . Uani d ? C(33) -0.3288(4) -0.5104(4) -0.2749(4) 0.029(2) 1.000 . Uani d ? C(34) -0.2967(4) -0.5502(4) -0.3332(4) 0.032(2) 1.000 . Uani d ? C(35) -0.2208(4) -0.5532(4) -0.3318(4) 0.033(2) 1.000 . Uani d ? C(36) -0.1757(4) -0.5160(4) -0.2707(4) 0.030(2) 1.000 . Uani d ? C(37) -0.2062(4) -0.4764(4) -0.2111(4) 0.024(2) 1.000 . Uani d ? C(38) -0.0965(4) -0.4418(4) -0.1229(4) 0.028(2) 1.000 . Uani d ? C(39) -0.0608(4) -0.3831(4) -0.0671(4) 0.031(2) 1.000 . Uani d ? C(40) -0.0880(4) -0.2987(4) -0.0379(3) 0.024(2) 1.000 . Uani d ? C(41) -0.4004(4) -0.2489(4) 0.0186(4) 0.038(2) 1.000 . Uani d ? C(42) -0.4308(4) -0.5145(4) -0.1586(4) 0.038(2) 1.000 . Uani d ? C(43) -0.0506(4) -0.5228(4) -0.1474(4) 0.037(2) 1.000 . Uani d ? C(44) -0.0351(4) -0.2447(4) 0.0195(4) 0.032(2) 1.000 . Uani d ? H(1) -0.0517 -0.2196 -0.1901 0.036 1.000 . Uiso c ? H(2) 0.0578 -0.1502 -0.1300 0.041 1.000 . Uiso c ? H(3) 0.0635 0.0148 -0.1057 0.044 1.000 . Uiso c ? H(4) -0.0391 0.1132 -0.1436 0.036 1.000 . Uiso c ? H(5) -0.2543 0.2552 -0.2577 0.039 1.000 . Uiso c ? H(6) -0.4349 0.1300 -0.1300 0.036 1.000 . Uiso c ? H(7) -0.5274 0.0440 -0.0822 0.045 1.000 . Uiso c ? H(8) -0.5390 -0.1223 -0.1041 0.039 1.000 . Uiso c ? H(9) -0.4554 -0.2008 -0.1700 0.035 1.000 . Uiso c ? H(10) -0.2773 -0.2952 -0.3193 0.027 1.000 . Uiso c ? H(11) -0.0729 0.1715 -0.2347 0.057 1.000 . Uiso c ? H(12) -0.1243 0.2308 -0.2928 0.057 1.000 . Uiso c ? H(13) -0.1135 0.2625 -0.2103 0.057 1.000 . Uiso c ? H(14) -0.3818 0.2715 -0.2074 0.052 1.000 . Uiso c ? H(15) -0.3953 0.2369 -0.2892 0.052 1.000 . Uiso c ? H(16) -0.4312 0.1816 -0.2283 0.052 1.000 . Uiso c ? H(17) -0.4445 -0.2312 -0.2595 0.035 1.000 . Uiso c ? H(18) -0.4174 -0.2652 -0.3329 0.035 1.000 . Uiso c ? H(19) -0.3983 -0.3254 -0.2611 0.035 1.000 . Uiso c ? H(20) -0.1376 -0.3290 -0.2852 0.043 1.000 . Uiso c ? H(21) -0.1477 -0.2650 -0.3558 0.043 1.000 . Uiso c ? H(22) -0.0905 -0.2358 -0.2885 0.043 1.000 . Uiso c ? H(23) -0.0949 -0.0910 -0.0350 0.034 1.000 . Uiso c ? H(24) -0.1573 0.0520 -0.0162 0.042 1.000 . Uiso c ? H(25) -0.2858 0.0518 -0.0103 0.039 1.000 . Uiso c ? H(26) -0.3526 -0.0926 -0.0273 0.035 1.000 . Uiso c ? H(27) -0.4449 -0.3979 -0.0560 0.032 1.000 . Uiso c ? H(28) -0.3816 -0.5077 -0.2772 0.035 1.000 . Uiso c ? H(29) -0.3278 -0.5757 -0.3747 0.039 1.000 . Uiso c ? H(30) -0.1991 -0.5804 -0.3721 0.039 1.000 . Uiso c ? H(31) -0.1230 -0.5176 -0.2697 0.035 1.000 . Uiso c ? H(32) -0.0121 -0.4027 -0.0464 0.037 1.000 . Uiso c ? H(33) -0.3711 -0.1953 0.0374 0.046 1.000 . Uiso c ? H(34) -0.4486 -0.2273 -0.0018 0.046 1.000 . Uiso c ? H(35) -0.4050 -0.2931 0.0577 0.046 1.000 . Uiso c ? H(36) -0.4767 -0.4850 -0.1780 0.046 1.000 . Uiso c ? H(37) -0.4115 -0.5499 -0.1967 0.046 1.000 . Uiso c ? H(38) -0.4392 -0.5570 -0.1194 0.046 1.000 . Uiso c ? H(39) -0.0357 -0.5643 -0.1066 0.044 1.000 . Uiso c ? H(40) -0.0794 -0.5583 -0.1857 0.044 1.000 . Uiso c ? H(41) -0.0075 -0.4974 -0.1657 0.044 1.000 . Uiso c ? H(42) -0.0203 -0.2858 0.0605 0.039 1.000 . Uiso c ? H(43) 0.0078 -0.2250 -0.0020 0.039 1.000 . Uiso c ? H(44) -0.0596 -0.1895 0.0358 0.039 1.000 . Uiso c ? 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 Ni(1) 0.0220(5) 0.0197(4) 0.0289(6) -0.0008(4) 0.0019(4) -0.0003(4) Ni(2) 0.0226(5) 0.0227(4) 0.0253(5) 0.0013(4) 0.0026(4) -0.0019(4) S(1) 0.097(2) 0.039(1) 0.067(2) 0.000(1) -0.028(2) 0.000(1) S(2) 0.069(2) 0.071(2) 0.103(2) 0.011(1) -0.036(2) -0.019(1) S(3) 0.045(2) 0.070(1) 0.113(2) -0.009(1) 0.021(2) -0.040(1) S(4) 0.084(2) 0.056(1) 0.133(3) -0.031(1) 0.022(2) -0.019(1) S(5) 0.108(2) 0.047(1) 0.086(2) 0.007(1) 0.002(2) 0.020(1) S(6) 0.064(2) 0.053(1) 0.174(3) 0.026(1) 0.004(2) -0.043(2) S(7) 0.045(2) 0.087(2) 0.105(2) -0.008(1) 0.020(2) -0.022(2) S(8) 0.144(3) 0.084(2) 0.045(2) -0.047(2) 0.045(2) -0.016(1) N(1) 0.018(3) 0.021(3) 0.030(4) -0.004(2) 0.001(3) -0.001(2) N(2) 0.024(4) 0.018(3) 0.032(4) -0.002(2) 0.004(3) -0.001(2) N(3) 0.025(4) 0.017(3) 0.032(4) 0.003(2) 0.004(3) 0.000(2) N(4) 0.019(3) 0.020(3) 0.031(4) -0.001(2) -0.001(3) 0.002(2) N(5) 0.021(4) 0.023(3) 0.023(3) 0.002(2) 0.002(3) -0.002(2) N(6) 0.020(4) 0.023(3) 0.022(3) 0.004(2) 0.001(3) -0.001(2) N(7) 0.021(4) 0.017(3) 0.027(4) -0.002(2) 0.004(3) -0.001(2) N(8) 0.024(4) 0.024(3) 0.022(4) 0.000(2) 0.002(3) -0.003(2) C(1) 0.028(5) 0.029(4) 0.021(4) -0.001(3) 0.007(4) 0.000(3) C(2) 0.028(5) 0.029(4) 0.034(5) 0.006(3) 0.009(4) 0.003(3) C(3) 0.021(5) 0.047(4) 0.038(5) 0.009(3) 0.012(4) 0.001(3) C(4) 0.017(4) 0.058(5) 0.036(5) -0.010(4) 0.004(4) -0.005(4) C(5) 0.029(5) 0.030(4) 0.032(5) -0.003(3) 0.004(4) -0.003(3) C(6) 0.021(4) 0.023(3) 0.023(4) -0.001(3) 0.008(3) -0.001(3) C(7) 0.034(5) 0.026(4) 0.040(5) -0.009(3) 0.007(4) -0.002(3) C(8) 0.026(5) 0.013(3) 0.058(6) 0.000(3) 0.007(4) 0.003(3) C(9) 0.032(5) 0.030(4) 0.032(5) 0.006(3) 0.001(4) -0.008(3) C(10) 0.025(4) 0.020(3) 0.032(4) 0.002(3) 0.000(4) 0.002(3) C(11) 0.027(5) 0.026(3) 0.036(5) 0.005(3) 0.001(4) 0.000(3) C(12) 0.023(5) 0.051(4) 0.039(5) 0.011(4) 0.004(4) -0.002(4) C(13) 0.017(4) 0.050(4) 0.031(5) 0.000(3) 0.000(4) 0.000(3) C(14) 0.024(5) 0.034(4) 0.026(4) -0.004(3) -0.009(4) 0.002(3) C(15) 0.012(4) 0.034(4) 0.022(4) 0.004(3) -0.008(3) 0.000(3) C(16) 0.023(5) 0.028(4) 0.024(4) -0.004(3) -0.004(4) 0.007(3) C(17) 0.025(5) 0.018(3) 0.025(4) -0.001(3) 0.006(4) 0.000(3) C(18) 0.029(5) 0.028(4) 0.023(4) -0.002(3) 0.006(4) 0.000(3) C(19) 0.040(5) 0.029(4) 0.074(6) -0.002(3) 0.014(5) 0.012(4) C(20) 0.039(5) 0.031(4) 0.061(6) 0.003(3) 0.012(4) 0.009(4) C(21) 0.027(5) 0.028(3) 0.032(5) -0.006(3) 0.000(4) -0.002(3) C(22) 0.033(5) 0.037(4) 0.040(5) 0.001(3) 0.012(4) -0.010(3) C(23) 0.025(5) 0.028(4) 0.021(4) 0.003(3) -0.003(3) 0.000(3) C(24) 0.032(5) 0.025(4) 0.029(5) -0.001(3) 0.002(4) -0.006(3) C(25) 0.045(6) 0.030(4) 0.028(5) -0.002(4) -0.003(4) -0.005(3) C(26) 0.045(5) 0.025(4) 0.025(4) 0.007(3) -0.001(4) -0.002(3) C(27) 0.029(5) 0.033(4) 0.026(5) 0.003(3) 0.001(4) -0.004(3) C(28) 0.038(5) 0.023(3) 0.015(4) 0.003(3) 0.001(4) 0.001(3) C(29) 0.026(5) 0.033(4) 0.020(4) 0.008(3) 0.001(4) 0.002(3) C(30) 0.018(4) 0.036(4) 0.028(5) -0.003(3) 0.007(3) 0.003(3) C(31) 0.025(5) 0.027(4) 0.028(5) 0.002(3) -0.002(4) 0.001(3) C(32) 0.024(4) 0.017(3) 0.027(4) 0.003(3) 0.000(4) 0.001(3) C(33) 0.026(5) 0.028(4) 0.033(5) -0.005(3) 0.006(4) 0.000(3) C(34) 0.027(5) 0.040(4) 0.029(5) -0.004(3) -0.002(4) -0.008(3) C(35) 0.042(5) 0.032(4) 0.025(5) 0.002(3) 0.004(4) -0.004(3) C(36) 0.028(5) 0.029(4) 0.031(5) 0.005(3) 0.003(4) 0.009(3) C(37) 0.025(5) 0.021(3) 0.026(5) 0.000(3) 0.005(4) -0.001(3) C(38) 0.030(5) 0.030(4) 0.026(5) 0.004(3) 0.011(4) 0.003(3) C(39) 0.021(4) 0.036(4) 0.035(5) 0.007(3) -0.004(4) 0.006(3) C(40) 0.024(5) 0.023(3) 0.025(4) -0.002(3) 0.000(3) 0.004(3) C(41) 0.033(5) 0.050(4) 0.033(5) 0.000(3) 0.003(4) -0.006(4) C(42) 0.037(5) 0.034(4) 0.047(5) -0.010(3) 0.016(4) -0.009(3) C(43) 0.031(5) 0.042(4) 0.035(5) 0.005(3) -0.005(4) -0.008(3) C(44) 0.027(5) 0.033(4) 0.036(5) 0.001(3) -0.002(4) 0.000(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4925 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_all 0.0535 _refine_ls_wR_factor_ref 0.0535 _refine_ls_goodness_of_fit_all 2.751 _refine_ls_goodness_of_fit_ref 2.751 _refine_ls_shift/su_max 0.0002 _refine_ls_shift/su_mean 0.0012 _refine_diff_density_min -0.74 _refine_diff_density_max 1.07 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag NI1 N1 1.874(5) . . yes NI1 N2 1.867(5) . . yes NI1 N3 1.860(5) . . yes NI1 N4 1.870(5) . . yes NI2 N5 1.870(5) . . yes NI2 N6 1.869(5) . . yes NI2 N7 1.873(5) . . yes NI2 N8 1.863(5) . . yes S1 S2 2.006(3) . . yes S1 S8 2.060(4) . . yes S2 S3 2.012(4) . . yes S3 S4 2.047(3) . . yes S4 S5 2.013(4) . . yes S5 S6 2.032(4) . . yes S6 S7 2.038(3) . . yes S7 S8 2.026(4) . . yes N1 C1 1.394(7) . . yes N1 C18 1.343(7) . . yes N2 C6 1.384(7) . . yes N2 C7 1.346(7) . . yes N3 C9 1.350(7) . . yes N3 C10 1.408(7) . . yes N4 C15 1.406(7) . . yes N4 C16 1.361(7) . . yes N5 C23 1.428(7) . . yes N5 C40 1.323(7) . . yes N6 C28 1.434(7) . . yes N6 C29 1.321(7) . . yes N7 C31 1.328(7) . . yes N7 C32 1.411(7) . . yes N8 C37 1.412(7) . . yes N8 C38 1.340(7) . . yes C1 C2 1.377(8) . . yes C1 C6 1.439(7) . . yes C2 C3 1.396(9) . . yes C2 H1 0.95 . . no C3 C4 1.383(8) . . yes C3 H2 0.95 . . no C4 C5 1.388(8) . . yes C4 H3 0.95 . . no C5 C6 1.392(8) . . yes C5 H4 0.95 . . no C7 C8 1.388(8) . . yes C7 C19 1.506(9) . . yes C8 C9 1.376(8) . . yes C8 H5 0.95 . . no C9 C20 1.516(9) . . yes C10 C11 1.382(9) . . yes C10 C15 1.414(7) . . yes C11 C12 1.365(9) . . yes C11 H6 0.95 . . no C12 C13 1.390(8) . . yes C12 H7 0.95 . . no C13 C14 1.370(9) . . yes C13 H8 0.95 . . no C14 C15 1.396(8) . . yes C14 H9 0.95 . . no C16 C17 1.388(8) . . yes C16 C21 1.488(8) . . yes C17 C18 1.391(8) . . yes C17 H10 0.95 . . no C18 C22 1.500(9) . . yes C19 H11 0.95 . . no C19 H12 0.95 . . no C19 H13 0.95 . . no C20 H14 0.95 . . no C20 H15 0.95 . . no C20 H16 0.95 . . no C21 H17 0.95 . . no C21 H18 0.95 . . no C21 H19 0.95 . . no C22 H20 0.95 . . no C22 H21 0.95 . . no C22 H22 0.95 . . no C23 C24 1.389(7) . . yes C23 C28 1.389(8) . . yes C24 C25 1.378(8) . . yes C24 H23 0.95 . . no C25 C26 1.386(9) . . yes C25 H24 0.95 . . no C26 C27 1.384(8) . . yes C26 H25 0.95 . . no C27 C28 1.380(8) . . yes C27 H26 0.95 . . no C29 C30 1.400(8) . . yes C29 C41 1.517(9) . . yes C30 C31 1.401(8) . . yes C30 H27 0.95 . . no C31 C42 1.506(8) . . yes C32 C33 1.378(8) . . yes C32 C37 1.413(8) . . yes C33 C34 1.383(9) . . yes C33 H28 0.95 . . no C34 C35 1.368(9) . . yes C34 H29 0.95 . . no C35 C36 1.391(9) . . yes C35 H30 0.95 . . no C36 C37 1.387(8) . . yes C36 H31 0.95 . . no C38 C39 1.393(8) . . yes C38 C43 1.495(8) . . yes C39 C40 1.398(8) . . yes C39 H32 0.95 . . no C40 C44 1.519(8) . . yes C41 H33 0.95 . . no C41 H34 0.95 . . no C41 H35 0.95 . . no C42 H36 0.95 . . no C42 H37 0.95 . . no C42 H38 0.95 . . no C43 H39 0.95 . . no C43 H40 0.95 . . no C43 H41 0.95 . . no C44 H42 0.95 . . no C44 H43 0.95 . . no C44 H44 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 NI1 N2 84.5(2) . . . yes N1 NI1 N3 178.6(2) . . . yes N1 NI1 N4 95.5(2) . . . yes N2 NI1 N3 94.9(2) . . . yes N2 NI1 N4 179.5(2) . . . yes N3 NI1 N4 85.1(2) . . . yes N5 NI2 N6 85.4(2) . . . yes N5 NI2 N7 179.2(2) . . . yes N5 NI2 N8 94.3(2) . . . yes N6 NI2 N7 94.7(2) . . . yes N6 NI2 N8 178.5(2) . . . yes N7 NI2 N8 85.5(2) . . . yes S2 S1 S8 106.2(1) . . . yes S1 S2 S3 105.3(1) . . . yes S2 S3 S4 109.4(2) . . . yes S3 S4 S5 108.2(1) . . . yes S4 S5 S6 108.2(2) . . . yes S5 S6 S7 108.4(1) . . . yes S6 S7 S8 109.0(2) . . . yes S1 S8 S7 106.6(1) . . . yes NI1 N1 C1 111.5(4) . . . yes NI1 N1 C18 123.6(4) . . . yes C1 N1 C18 124.6(5) . . . yes NI1 N2 C6 111.4(3) . . . yes NI1 N2 C7 123.1(4) . . . yes C6 N2 C7 125.3(5) . . . yes NI1 N3 C9 123.1(4) . . . yes NI1 N3 C10 111.3(3) . . . yes C9 N3 C10 125.1(5) . . . yes NI1 N4 C15 111.1(4) . . . yes NI1 N4 C16 123.6(4) . . . yes C15 N4 C16 125.2(5) . . . yes NI2 N5 C23 110.6(4) . . . yes NI2 N5 C40 124.2(4) . . . yes C23 N5 C40 124.7(5) . . . yes NI2 N6 C28 110.7(4) . . . yes NI2 N6 C29 123.6(4) . . . yes C28 N6 C29 125.2(5) . . . yes NI2 N7 C31 124.4(4) . . . yes NI2 N7 C32 110.6(4) . . . yes C31 N7 C32 125.0(5) . . . yes NI2 N8 C37 110.9(4) . . . yes NI2 N8 C38 124.6(4) . . . yes C37 N8 C38 124.2(5) . . . yes N1 C1 C2 127.4(5) . . . yes N1 C1 C6 112.5(5) . . . yes C2 C1 C6 119.5(6) . . . yes C1 C2 C3 120.4(5) . . . yes C1 C2 H1 119.8 . . . no C3 C2 H1 119.8 . . . no C2 C3 C4 120.5(6) . . . yes C2 C3 H2 119.8 . . . no C4 C3 H2 119.8 . . . no C3 C4 C5 120.1(6) . . . yes C3 C4 H3 119.9 . . . no C5 C4 H3 119.9 . . . no C4 C5 C6 120.7(5) . . . yes C4 C5 H4 119.7 . . . no C6 C5 H4 119.7 . . . no N2 C6 C1 113.1(5) . . . yes N2 C6 C5 127.6(5) . . . yes C1 C6 C5 118.8(6) . . . yes N2 C7 C8 121.8(6) . . . yes N2 C7 C19 121.3(6) . . . yes C8 C7 C19 116.7(5) . . . yes C7 C8 C9 127.7(5) . . . yes C7 C8 H5 116.2 . . . no C9 C8 H5 116.2 . . . no N3 C9 C8 121.4(6) . . . yes N3 C9 C20 120.9(6) . . . yes C8 C9 C20 117.5(6) . . . yes N3 C10 C11 126.8(5) . . . yes N3 C10 C15 113.1(6) . . . yes C11 C10 C15 119.5(6) . . . yes C10 C11 C12 121.6(6) . . . yes C10 C11 H6 119.2 . . . no C12 C11 H6 119.2 . . . no C11 C12 C13 119.6(6) . . . yes C11 C12 H7 120.2 . . . no C13 C12 H7 120.2 . . . no C12 C13 C14 119.9(6) . . . yes C12 C13 H8 120.0 . . . no C14 C13 H8 120.0 . . . no C13 C14 C15 121.5(6) . . . yes C13 C14 H9 119.2 . . . no C15 C14 H9 119.2 . . . no N4 C15 C10 113.2(6) . . . yes N4 C15 C14 128.5(6) . . . yes C10 C15 C14 117.9(6) . . . yes N4 C16 C17 120.8(6) . . . yes N4 C16 C21 121.3(6) . . . yes C17 C16 C21 117.9(5) . . . yes C16 C17 C18 129.1(6) . . . yes C16 C17 H10 115.4 . . . no C18 C17 H10 115.4 . . . no N1 C18 C17 120.7(6) . . . yes N1 C18 C22 122.0(6) . . . yes C17 C18 C22 117.2(5) . . . yes C7 C19 H11 109.5 . . . no C7 C19 H12 109.5 . . . no C7 C19 H13 109.5 . . . no H11 C19 H12 109.5 . . . no H11 C19 H13 109.4 . . . no H12 C19 H13 109.5 . . . no C9 C20 H14 109.5 . . . no C9 C20 H15 109.5 . . . no C9 C20 H16 109.5 . . . no H14 C20 H15 109.5 . . . no H14 C20 H16 109.5 . . . no H15 C20 H16 109.5 . . . no C16 C21 H17 109.5 . . . no C16 C21 H18 109.5 . . . no C16 C21 H19 109.5 . . . no H17 C21 H18 109.5 . . . no H17 C21 H19 109.5 . . . no H18 C21 H19 109.5 . . . no C18 C22 H20 109.5 . . . no C18 C22 H21 109.5 . . . no C18 C22 H22 109.5 . . . no H20 C22 H21 109.5 . . . no H20 C22 H22 109.5 . . . no H21 C22 H22 109.5 . . . no N5 C23 C24 125.6(6) . . . yes N5 C23 C28 113.7(5) . . . yes C24 C23 C28 119.9(5) . . . yes C23 C24 C25 119.6(6) . . . yes C23 C24 H23 120.2 . . . no C25 C24 H23 120.2 . . . no C24 C25 C26 120.7(6) . . . yes C24 C25 H24 119.6 . . . no C26 C25 H24 119.6 . . . no C25 C26 C27 119.4(6) . . . yes C25 C26 H25 120.3 . . . no C27 C26 H25 120.3 . . . no C26 C27 C28 120.4(6) . . . yes C26 C27 H26 119.8 . . . no C28 C27 H26 119.8 . . . no N6 C28 C23 113.5(5) . . . yes N6 C28 C27 126.2(6) . . . yes C23 C28 C27 119.9(5) . . . yes N6 C29 C30 122.2(6) . . . yes N6 C29 C41 121.9(6) . . . yes C30 C29 C41 115.9(6) . . . yes C29 C30 C31 126.4(6) . . . yes C29 C30 H27 116.8 . . . no C31 C30 H27 116.8 . . . no N7 C31 C30 122.0(6) . . . yes N7 C31 C42 123.8(6) . . . yes C30 C31 C42 114.1(6) . . . yes N7 C32 C33 127.1(6) . . . yes N7 C32 C37 113.2(5) . . . yes C33 C32 C37 119.5(6) . . . yes C32 C33 C34 120.6(6) . . . yes C32 C33 H28 119.7 . . . no C34 C33 H28 119.7 . . . no C33 C34 C35 120.9(6) . . . yes C33 C34 H29 119.6 . . . no C35 C34 H29 119.6 . . . no C34 C35 C36 119.1(6) . . . yes C34 C35 H30 120.5 . . . no C36 C35 H30 120.5 . . . no C35 C36 C37 121.4(6) . . . yes C35 C36 H31 119.3 . . . no C37 C36 H31 119.3 . . . no N8 C37 C32 113.6(6) . . . yes N8 C37 C36 127.4(6) . . . yes C32 C37 C36 118.6(6) . . . yes N8 C38 C39 120.7(6) . . . yes N8 C38 C43 123.6(6) . . . yes C39 C38 C43 115.6(6) . . . yes C38 C39 C40 127.8(6) . . . yes C38 C39 H32 116.1 . . . no C40 C39 H32 116.1 . . . no N5 C40 C39 121.2(6) . . . yes N5 C40 C44 121.9(5) . . . yes C39 C40 C44 116.9(6) . . . yes C29 C41 H33 109.5 . . . no C29 C41 H34 109.5 . . . no C29 C41 H35 109.5 . . . no H33 C41 H34 109.5 . . . no H33 C41 H35 109.5 . . . no H34 C41 H35 109.5 . . . no C31 C42 H36 109.5 . . . no C31 C42 H37 109.5 . . . no C31 C42 H38 109.5 . . . no H36 C42 H37 109.5 . . . no H36 C42 H38 109.5 . . . no H37 C42 H38 109.5 . . . no C38 C43 H39 109.5 . . . no C38 C43 H40 109.5 . . . no C38 C43 H41 109.5 . . . no H39 C43 H40 109.5 . . . no H39 C43 H41 109.5 . . . no H40 C43 H41 109.5 . . . no C40 C44 H42 109.5 . . . no C40 C44 H43 109.5 . . . no C40 C44 H44 109.5 . . . no H42 C44 H43 109.5 . . . no H42 C44 H44 109.5 . . . no H43 C44 H44 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S1 C29 3.250(6) . 4_544 no S1 N6 3.368(5) . 4_544 no S1 C30 3.501(7) . 4_544 no S3 C38 3.250(7) . 4_544 no S3 N8 3.503(5) . 4_544 no S3 C43 3.517(7) . 4_544 no S3 C39 3.559(6) . 4_544 no S5 C9 3.563(7) . 4_554 no S7 C30 3.483(6) . 4_544 no S7 C42 3.567(7) . 4_544 no S8 N3 3.315(5) . . no S8 C9 3.441(7) . . no S8 N4 3.471(5) . . no N2 C25 3.571(9) . . no N3 C26 3.556(8) . . no N4 C28 3.559(8) . . no N4 C27 3.579(8) . . no N5 C2 3.541(8) . . no N7 C21 3.552(8) . . no C1 C24 3.298(9) . . no C2 C40 3.449(9) . . no C2 C24 3.519(9) . . no C4 C36 3.53(1) . 2_554 no C6 C24 3.362(9) . . no C6 C25 3.549(9) . . no C10 C27 3.378(9) . . no C10 C26 3.516(9) . . no C13 C33 3.555(9) . 2_454 no C14 C29 3.428(8) . . no C14 C27 3.465(9) . . no C15 C27 3.235(8) . . no C17 C32 3.526(7) . . no C26 C35 3.480(9) . 4_545 no C26 C34 3.60(1) . 4_545 no #------------------------------------------------------------------------------ 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #=END data_cutmtaas8 #------------------------------------------------------------------------------ _audit_creation_date '1999-03-02' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.1070(6) _cell_length_b 13.8543(3) _cell_length_c 18.0489(5) _cell_angle_alpha 90 _cell_angle_beta 96.791(1) _cell_angle_gamma 90 _cell_volume 4496.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123K _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'cube' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1068.46 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H44 Cu2 N8 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2200.00 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 123K _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Enraf-Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 49455 _reflns_number_total 49455 _reflns_number_gt 4621 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.160 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 30.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 8 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 176 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 176 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu1 0.23588(7) 0.15245(8) 0.10648(7) 0.0155(4) 1.000 . Uani d ? Cu2 0.25383(7) 0.46268(8) 0.20941(7) 0.0147(3) 1.000 . Uani d ? S1 0.2534(3) 0.0645(2) -0.0724(2) 0.086(2) 1.000 . Uani d ? S2 0.1621(2) -0.0130(3) -0.0994(3) 0.089(2) 1.000 . Uani d ? S3 0.1473(2) -0.0854(3) -0.0060(2) 0.072(1) 1.000 . Uani d ? S4 0.1811(3) -0.2249(3) -0.0138(3) 0.090(2) 1.000 . Uani d ? S5 0.2847(3) -0.2375(2) 0.0385(2) 0.086(2) 1.000 . Uani d ? S6 0.3576(2) -0.2215(3) -0.0386(4) 0.125(2) 1.000 . Uani d ? S7 0.3945(2) -0.0829(3) -0.0346(3) 0.084(2) 1.000 . Uani d ? S8 0.3357(3) -0.0068(3) -0.1183(2) 0.108(2) 1.000 . Uani d ? N1 0.3028(5) 0.2332(5) 0.0584(4) 0.014(3) 1.000 . Uani d ? N2 0.1585(5) 0.2338(5) 0.0576(4) 0.015(3) 1.000 . Uani d ? N3 0.1689(5) 0.0696(5) 0.1516(4) 0.013(2) 1.000 . Uani d ? N4 0.3123(5) 0.0690(5) 0.1530(4) 0.015(3) 1.000 . Uani d ? N5 0.3277(4) 0.5580(5) 0.1969(4) 0.014(2) 1.000 . Uani d ? N6 0.1720(4) 0.5520(5) 0.2034(4) 0.018(3) 1.000 . Uani d ? N7 0.1792(4) 0.3684(5) 0.2263(4) 0.013(2) 1.000 . Uani d ? N8 0.3366(4) 0.3735(5) 0.2183(4) 0.013(2) 1.000 . Uani d ? C1 0.2669(6) 0.3215(7) 0.0361(5) 0.020(3) 1.000 . Uani d ? C2 0.3037(6) 0.4074(7) 0.0240(5) 0.022(3) 1.000 . Uani d ? C3 0.2642(6) 0.4933(7) 0.0141(5) 0.019(3) 1.000 . Uani d ? C4 0.1882(7) 0.4941(7) 0.0172(6) 0.028(4) 1.000 . Uani d ? C5 0.1507(6) 0.4089(7) 0.0287(5) 0.020(3) 1.000 . Uani d ? C6 0.1897(6) 0.3222(6) 0.0367(5) 0.017(3) 1.000 . Uani d ? C7 0.0892(6) 0.2035(6) 0.0385(5) 0.016(3) 1.000 . Uani d ? C8 0.0627(6) 0.1187(6) 0.0691(5) 0.021(3) 1.000 . Uani d ? C9 0.0976(6) 0.0571(6) 0.1235(5) 0.018(3) 1.000 . Uani d ? C10 0.2076(6) 0.0168(6) 0.2097(5) 0.014(3) 1.000 . Uani d ? C11 0.1771(5) -0.0241(6) 0.2703(6) 0.017(3) 1.000 . Uani d ? C12 0.2222(6) -0.0636(6) 0.3306(6) 0.022(3) 1.000 . Uani d ? C13 0.2972(6) -0.0616(6) 0.3323(6) 0.019(3) 1.000 . Uani d ? C14 0.3304(6) -0.0208(6) 0.2738(6) 0.018(3) 1.000 . Uani d ? C15 0.2866(6) 0.0177(6) 0.2118(5) 0.015(3) 1.000 . Uani d ? C16 0.3784(6) 0.0584(6) 0.1277(5) 0.019(3) 1.000 . Uani d ? C17 0.4012(6) 0.1195(7) 0.0726(6) 0.020(3) 1.000 . Uani d ? C18 0.3660(6) 0.2009(7) 0.0393(5) 0.018(3) 1.000 . Uani d ? C19 0.0372(6) 0.2543(7) -0.0198(5) 0.022(3) 1.000 . Uani d ? C20 0.0513(6) -0.0257(6) 0.1459(6) 0.026(3) 1.000 . Uani d ? C21 0.4324(6) -0.0206(7) 0.1543(6) 0.028(4) 1.000 . Uani d ? C22 0.4027(6) 0.2474(7) -0.0221(6) 0.027(3) 1.000 . Uani d ? C23 0.3202(6) 0.6504(7) 0.2198(5) 0.020(3) 1.000 . Uani d ? C24 0.2519(6) 0.6878(6) 0.2305(6) 0.021(3) 1.000 . Uani d ? C25 0.1813(6) 0.6444(7) 0.2228(6) 0.024(3) 1.000 . Uani d ? C26 0.1047(6) 0.5045(6) 0.1879(5) 0.013(3) 1.000 . Uani d ? C27 0.0394(6) 0.5442(6) 0.1519(5) 0.020(3) 1.000 . Uani d ? C28 -0.0224(6) 0.4871(7) 0.1301(5) 0.024(3) 1.000 . Uani d ? C29 -0.0185(6) 0.3875(7) 0.1447(5) 0.022(3) 1.000 . Uani d ? C30 0.0461(6) 0.3457(6) 0.1792(5) 0.018(3) 1.000 . Uani d ? C31 0.1080(6) 0.4019(6) 0.2015(5) 0.015(3) 1.000 . Uani d ? C32 0.1961(6) 0.2878(6) 0.2650(5) 0.015(3) 1.000 . Uani d ? C33 0.2695(6) 0.2543(6) 0.2789(5) 0.012(3) 1.000 . Uani d ? C34 0.3350(5) 0.2898(6) 0.2555(5) 0.010(3) 1.000 . Uani d ? C35 0.3966(5) 0.4130(7) 0.1863(5) 0.014(3) 1.000 . Uani d ? C36 0.4539(6) 0.3644(6) 0.1583(5) 0.019(3) 1.000 . Uani d ? C37 0.5043(6) 0.4091(7) 0.1199(6) 0.021(3) 1.000 . Uani d ? C38 0.4990(6) 0.5084(7) 0.1069(6) 0.026(4) 1.000 . Uani d ? C39 0.4431(6) 0.5601(6) 0.1344(6) 0.021(3) 1.000 . Uani d ? C40 0.3922(6) 0.5150(7) 0.1756(5) 0.017(3) 1.000 . Uani d ? C41 0.3882(6) 0.7145(7) 0.2349(6) 0.032(4) 1.000 . Uani d ? C42 0.1175(6) 0.7060(7) 0.2420(6) 0.033(4) 1.000 . Uani d ? C43 0.1384(6) 0.2313(7) 0.2998(6) 0.024(3) 1.000 . Uani d ? C44 0.4042(6) 0.2335(6) 0.2767(5) 0.017(3) 1.000 . Uani d ? H1 0.3559 0.4072 0.0225 0.026 1.000 . Uiso c ? H2 0.2894 0.5515 0.0052 0.023 1.000 . Uiso c ? H3 0.1615 0.5532 0.0114 0.034 1.000 . Uiso c ? H4 0.0986 0.4098 0.0311 0.024 1.000 . Uiso c ? H5 0.0136 0.1006 0.0497 0.025 1.000 . Uiso c ? H6 0.1246 -0.0250 0.2702 0.021 1.000 . Uiso c ? H7 0.2003 -0.0919 0.3706 0.027 1.000 . Uiso c ? H8 0.3274 -0.0883 0.3739 0.023 1.000 . Uiso c ? H9 0.3831 -0.0191 0.2761 0.021 1.000 . Uiso c ? H10 0.4472 0.1030 0.0556 0.024 1.000 . Uiso c ? H11 0.0611 0.3099 -0.0367 0.027 1.000 . Uiso c ? H12 0.0240 0.2120 -0.0607 0.027 1.000 . Uiso c ? H13 -0.0064 0.2733 0.0009 0.027 1.000 . Uiso c ? H14 0.0082 -0.0014 0.1649 0.031 1.000 . Uiso c ? H15 0.0367 -0.0651 0.1036 0.031 1.000 . Uiso c ? H16 0.0796 -0.0630 0.1833 0.031 1.000 . Uiso c ? H17 0.4125 -0.0579 0.1914 0.034 1.000 . Uiso c ? H18 0.4405 -0.0609 0.1135 0.034 1.000 . Uiso c ? H19 0.4782 0.0073 0.1748 0.034 1.000 . Uiso c ? H20 0.4516 0.2670 -0.0033 0.032 1.000 . Uiso c ? H21 0.4050 0.2024 -0.0615 0.032 1.000 . Uiso c ? H22 0.3746 0.3021 -0.0404 0.032 1.000 . Uiso c ? H23 0.2526 0.7535 0.2456 0.025 1.000 . Uiso c ? H24 0.0371 0.6115 0.1420 0.024 1.000 . Uiso c ? H25 -0.0667 0.5150 0.1056 0.029 1.000 . Uiso c ? H26 -0.0609 0.3482 0.1308 0.026 1.000 . Uiso c ? H27 0.0480 0.2780 0.1876 0.021 1.000 . Uiso c ? H28 0.2755 0.1981 0.3092 0.015 1.000 . Uiso c ? H29 0.4583 0.2967 0.1663 0.023 1.000 . Uiso c ? H30 0.5430 0.3730 0.1019 0.026 1.000 . Uiso c ? H31 0.5335 0.5400 0.0793 0.031 1.000 . Uiso c ? H32 0.4391 0.6275 0.1252 0.025 1.000 . Uiso c ? H33 0.4219 0.6869 0.2735 0.038 1.000 . Uiso c ? H34 0.4118 0.7202 0.1909 0.038 1.000 . Uiso c ? H35 0.3735 0.7766 0.2500 0.038 1.000 . Uiso c ? H36 0.1267 0.7259 0.2926 0.040 1.000 . Uiso c ? H37 0.1129 0.7611 0.2106 0.040 1.000 . Uiso c ? H38 0.0728 0.6695 0.2350 0.040 1.000 . Uiso c ? H39 0.0909 0.2599 0.2869 0.029 1.000 . Uiso c ? H40 0.1376 0.1667 0.2820 0.029 1.000 . Uiso c ? H41 0.1501 0.2315 0.3525 0.029 1.000 . Uiso c ? H42 0.3983 0.1702 0.2566 0.020 1.000 . Uiso c ? H43 0.4447 0.2645 0.2576 0.020 1.000 . Uiso c ? H44 0.4136 0.2298 0.3296 0.020 1.000 . Uiso c ? 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 Cu1 0.0139(8) 0.0165(6) 0.0161(7) -0.0018(6) 0.0015(6) 0.0024(5) Cu2 0.0111(8) 0.0119(6) 0.0203(8) 0.0006(6) -0.0008(6) 0.0009(5) S1 0.123(4) 0.043(2) 0.074(3) 0.002(2) -0.055(3) -0.001(2) S2 0.067(3) 0.074(3) 0.112(4) 0.011(2) -0.047(3) -0.020(3) S3 0.032(2) 0.078(3) 0.109(4) -0.014(2) 0.019(2) -0.052(2) S4 0.083(4) 0.063(3) 0.127(4) -0.040(2) 0.026(3) -0.019(3) S5 0.106(4) 0.045(2) 0.101(4) 0.003(2) -0.009(3) 0.027(2) S6 0.046(3) 0.054(3) 0.267(7) 0.024(2) -0.008(4) -0.084(3) S7 0.041(3) 0.093(3) 0.124(4) -0.020(2) 0.030(3) -0.048(3) S8 0.196(6) 0.101(3) 0.036(3) -0.086(4) 0.055(3) -0.021(2) N1 0.013(6) 0.011(4) 0.017(5) -0.001(4) 0.002(4) 0.006(4) N2 0.015(6) 0.019(5) 0.012(5) 0.004(4) 0.006(4) 0.004(4) N3 0.018(6) 0.017(4) 0.003(5) -0.001(4) 0.001(4) 0.002(3) N4 0.014(6) 0.013(4) 0.019(5) 0.000(4) 0.001(4) 0.001(4) N5 0.011(5) 0.014(5) 0.017(5) -0.004(4) 0.002(4) 0.005(3) N6 0.016(6) 0.007(4) 0.029(5) 0.003(4) -0.002(4) 0.007(4) N7 0.011(5) 0.009(4) 0.021(5) 0.000(4) 0.003(4) -0.002(4) N8 0.002(5) 0.016(4) 0.020(5) 0.002(4) -0.004(4) -0.005(4) C1 0.031(8) 0.022(6) 0.008(6) -0.008(5) 0.002(5) 0.000(4) C2 0.022(7) 0.031(6) 0.010(6) -0.005(5) -0.007(5) 0.007(5) C3 0.023(8) 0.024(6) 0.008(6) -0.009(5) -0.007(5) 0.004(4) C4 0.040(9) 0.019(6) 0.023(7) 0.004(5) -0.010(6) 0.007(5) C5 0.016(7) 0.025(6) 0.018(6) -0.001(5) 0.000(5) 0.009(5) C6 0.018(8) 0.016(6) 0.015(6) -0.004(5) 0.001(5) 0.005(4) C7 0.014(7) 0.023(6) 0.011(6) 0.004(5) 0.003(5) -0.001(5) C8 0.020(7) 0.022(6) 0.018(6) -0.009(5) -0.010(5) -0.002(5) C9 0.019(7) 0.020(6) 0.016(6) 0.001(5) 0.006(5) -0.006(5) C10 0.013(7) 0.014(5) 0.014(6) -0.002(4) -0.003(5) -0.004(4) C11 0.012(7) 0.021(6) 0.021(7) -0.002(5) 0.006(5) -0.003(5) C12 0.027(8) 0.021(6) 0.020(7) -0.005(5) 0.009(6) 0.001(5) C13 0.015(7) 0.023(6) 0.019(7) 0.000(5) -0.002(5) 0.004(5) C14 0.022(7) 0.011(5) 0.021(7) 0.006(5) 0.004(6) -0.006(5) C15 0.026(7) 0.006(5) 0.014(6) 0.000(4) 0.001(5) -0.003(4) C16 0.023(7) 0.013(6) 0.019(7) -0.001(5) -0.001(5) -0.005(4) C17 0.012(7) 0.028(6) 0.023(7) 0.001(5) 0.006(5) 0.001(5) C18 0.014(7) 0.027(6) 0.014(6) -0.008(5) 0.002(5) -0.005(5) C19 0.015(7) 0.030(6) 0.021(7) 0.000(5) -0.002(5) 0.003(5) C20 0.021(7) 0.022(6) 0.032(7) -0.007(5) -0.011(6) 0.005(5) C21 0.031(8) 0.025(6) 0.033(7) 0.009(5) 0.015(6) 0.006(5) C22 0.021(8) 0.035(6) 0.024(7) 0.003(5) 0.003(6) -0.001(5) C23 0.021(7) 0.019(6) 0.020(6) -0.003(5) 0.002(5) 0.001(5) C24 0.015(7) 0.007(5) 0.042(8) 0.004(5) 0.006(6) 0.001(5) C25 0.027(8) 0.021(6) 0.026(7) 0.016(6) 0.005(6) 0.010(5) C26 0.012(7) 0.015(5) 0.014(6) 0.003(5) 0.005(5) -0.001(4) C27 0.014(7) 0.019(5) 0.027(7) 0.008(5) 0.006(5) 0.004(5) C28 0.012(7) 0.048(7) 0.014(6) 0.005(5) 0.002(5) 0.005(5) C29 0.011(7) 0.035(6) 0.020(7) -0.010(5) 0.004(5) -0.001(5) C30 0.014(7) 0.020(5) 0.018(6) -0.003(5) 0.004(5) 0.004(5) C31 0.015(7) 0.024(6) 0.009(6) 0.002(5) 0.008(5) 0.002(4) C32 0.018(7) 0.015(5) 0.012(6) -0.004(5) 0.002(5) -0.006(4) C33 0.017(7) 0.006(5) 0.013(6) 0.005(4) 0.004(5) 0.002(4) C34 0.015(7) 0.004(5) 0.010(6) 0.005(4) -0.003(5) -0.003(4) C35 0.005(6) 0.025(6) 0.010(6) -0.009(5) -0.006(5) 0.003(5) C36 0.011(7) 0.021(6) 0.023(7) 0.001(5) -0.008(5) 0.000(5) C37 0.005(6) 0.030(6) 0.027(7) 0.002(5) -0.003(5) 0.001(5) C38 0.019(7) 0.035(7) 0.022(7) -0.008(5) -0.001(6) 0.002(5) C39 0.020(7) 0.016(6) 0.023(7) -0.007(5) -0.008(6) 0.006(5) C40 0.016(7) 0.021(6) 0.014(6) -0.003(5) -0.005(5) 0.003(4) C41 0.018(8) 0.027(6) 0.051(8) -0.002(5) 0.003(6) -0.007(5) C42 0.023(8) 0.019(6) 0.057(9) 0.002(5) 0.005(7) -0.010(5) C43 0.021(7) 0.023(6) 0.031(7) 0.001(5) 0.011(6) 0.008(5) C44 0.012(7) 0.017(5) 0.020(6) 0.003(5) 0.002(5) 0.002(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4621 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_all 0.0731 _refine_ls_wR_factor_ref 0.0731 _refine_ls_goodness_of_fit_all 3.310 _refine_ls_goodness_of_fit_ref 3.310 _refine_ls_shift/su_max 0.0001 _refine_ls_shift/su_mean 0.0009 _refine_diff_density_min -1.43 _refine_diff_density_max 2.00 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU1 N1 1.930(7) . . yes CU1 N2 1.928(8) . . yes CU1 N3 1.920(7) . . yes CU1 N4 1.918(8) . . yes CU2 N5 1.912(7) . . yes CU2 N6 1.923(7) . . yes CU2 N7 1.929(7) . . yes CU2 N8 1.934(7) . . yes S1 S2 1.982(6) . . yes S1 S8 2.043(7) . . yes S2 S3 2.007(7) . . yes S3 S4 2.037(5) . . yes S4 S5 2.005(7) . . yes S5 S6 2.039(7) . . yes S6 S7 2.031(5) . . yes S7 S8 2.037(7) . . yes N1 C1 1.42(1) . . yes N1 C18 1.31(1) . . yes N2 C6 1.42(1) . . yes N2 C7 1.33(1) . . yes N3 C9 1.34(1) . . yes N3 C10 1.40(1) . . yes N4 C15 1.40(1) . . yes N4 C16 1.34(1) . . yes N5 C23 1.36(1) . . yes N5 C40 1.41(1) . . yes N6 C25 1.33(1) . . yes N6 C26 1.38(1) . . yes N7 C31 1.39(1) . . yes N7 C32 1.33(1) . . yes N8 C34 1.34(1) . . yes N8 C35 1.40(1) . . yes C1 C2 1.39(1) . . yes C1 C6 1.40(1) . . yes C2 C3 1.39(1) . . yes C2 H1 0.95 . . no C3 C4 1.38(1) . . yes C3 H2 0.95 . . no C4 C5 1.39(1) . . yes C4 H3 0.95 . . no C5 C6 1.39(1) . . yes C5 H4 0.95 . . no C7 C8 1.41(1) . . yes C7 C19 1.50(1) . . yes C8 C9 1.39(1) . . yes C8 H5 0.95 . . no C9 C20 1.50(1) . . yes C10 C11 1.40(1) . . yes C10 C15 1.43(1) . . yes C11 C12 1.39(1) . . yes C11 H6 0.95 . . no C12 C13 1.35(1) . . yes C12 H7 0.95 . . no C13 C14 1.40(1) . . yes C13 H8 0.95 . . no C14 C15 1.40(1) . . yes C14 H9 0.95 . . no C16 C17 1.40(1) . . yes C16 C21 1.51(1) . . yes C17 C18 1.40(1) . . yes C17 H10 0.95 . . no C18 C22 1.50(1) . . yes C19 H11 0.95 . . no C19 H12 0.95 . . no C19 H13 0.95 . . no C20 H14 0.95 . . no C20 H15 0.95 . . no C20 H16 0.95 . . no C21 H17 0.95 . . no C21 H18 0.95 . . no C21 H19 0.95 . . no C22 H20 0.95 . . no C22 H21 0.95 . . no C22 H22 0.95 . . no C23 C24 1.38(1) . . yes C23 C41 1.52(1) . . yes C24 C25 1.40(1) . . yes C24 H23 0.95 . . no C25 C42 1.51(1) . . yes C26 C27 1.39(1) . . yes C26 C31 1.44(1) . . yes C27 C28 1.39(1) . . yes C27 H24 0.95 . . no C28 C29 1.40(1) . . yes C28 H25 0.95 . . no C29 C30 1.39(1) . . yes C29 H26 0.95 . . no C30 C31 1.38(1) . . yes C30 H27 0.95 . . no C32 C33 1.40(1) . . yes C32 C43 1.50(1) . . yes C33 C34 1.39(1) . . yes C33 H28 0.95 . . no C34 C44 1.49(1) . . yes C35 C36 1.38(1) . . yes C35 C40 1.43(1) . . yes C36 C37 1.36(1) . . yes C36 H29 0.95 . . no C37 C38 1.40(1) . . yes C37 H30 0.95 . . no C38 C39 1.38(1) . . yes C38 H31 0.95 . . no C39 C40 1.40(1) . . yes C39 H32 0.95 . . no C41 H33 0.95 . . no C41 H34 0.95 . . no C41 H35 0.95 . . no C42 H36 0.95 . . no C42 H37 0.95 . . no C42 H38 0.95 . . no C43 H39 0.95 . . no C43 H40 0.95 . . no C43 H41 0.95 . . no C44 H42 0.95 . . no C44 H43 0.95 . . no C44 H44 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 CU1 N2 85.2(3) . . . yes N1 CU1 N3 178.2(3) . . . yes N1 CU1 N4 95.0(3) . . . yes N2 CU1 N3 94.7(3) . . . yes N2 CU1 N4 178.5(3) . . . yes N3 CU1 N4 85.0(3) . . . yes N5 CU2 N6 95.3(3) . . . yes N5 CU2 N7 177.6(3) . . . yes N5 CU2 N8 84.6(3) . . . yes N6 CU2 N7 84.0(3) . . . yes N6 CU2 N8 178.5(3) . . . yes N7 CU2 N8 96.0(3) . . . yes S2 S1 S8 105.4(2) . . . yes S1 S2 S3 104.8(2) . . . yes S2 S3 S4 110.2(2) . . . yes S3 S4 S5 108.8(2) . . . yes S4 S5 S6 108.3(3) . . . yes S5 S6 S7 108.4(2) . . . yes S6 S7 S8 108.8(3) . . . yes S1 S8 S7 107.0(2) . . . yes CU1 N1 C1 109.6(7) . . . yes CU1 N1 C18 122.2(6) . . . yes C1 N1 C18 127.1(8) . . . yes CU1 N2 C6 109.6(6) . . . yes CU1 N2 C7 123.1(6) . . . yes C6 N2 C7 126.7(8) . . . yes CU1 N3 C9 123.0(6) . . . yes CU1 N3 C10 110.2(6) . . . yes C9 N3 C10 126.3(8) . . . yes CU1 N4 C15 110.5(6) . . . yes CU1 N4 C16 123.0(7) . . . yes C15 N4 C16 126.4(8) . . . yes CU2 N5 C23 121.4(7) . . . yes CU2 N5 C40 110.8(6) . . . yes C23 N5 C40 126.8(8) . . . yes CU2 N6 C25 122.0(7) . . . yes CU2 N6 C26 111.1(6) . . . yes C25 N6 C26 126.2(8) . . . yes CU2 N7 C31 111.3(6) . . . yes CU2 N7 C32 121.8(7) . . . yes C31 N7 C32 126.4(8) . . . yes CU2 N8 C34 122.1(6) . . . yes CU2 N8 C35 110.3(6) . . . yes C34 N8 C35 127.4(8) . . . yes N1 C1 C2 125(1) . . . yes N1 C1 C6 115.3(8) . . . yes C2 C1 C6 119.4(9) . . . yes C1 C2 C3 120(1) . . . yes C1 C2 H1 119.9 . . . no C3 C2 H1 119.8 . . . no C2 C3 C4 120.0(9) . . . yes C2 C3 H2 120.0 . . . no C4 C3 H2 120.0 . . . no C3 C4 C5 120.3(9) . . . yes C3 C4 H3 119.9 . . . no C5 C4 H3 119.9 . . . no C4 C5 C6 119.9(9) . . . yes C4 C5 H4 120.0 . . . no C6 C5 H4 120.1 . . . no N2 C6 C1 115.2(8) . . . yes N2 C6 C5 124.0(9) . . . yes C1 C6 C5 120.0(9) . . . yes N2 C7 C8 121.2(9) . . . yes N2 C7 C19 121.8(9) . . . yes C8 C7 C19 116.9(9) . . . yes C7 C8 C9 129.8(9) . . . yes C7 C8 H5 115.1 . . . no C9 C8 H5 115.1 . . . no N3 C9 C8 121.6(9) . . . yes N3 C9 C20 122.6(9) . . . yes C8 C9 C20 115.8(9) . . . yes N3 C10 C11 126.0(9) . . . yes N3 C10 C15 115.3(9) . . . yes C11 C10 C15 118.0(9) . . . yes C10 C11 C12 121.3(9) . . . yes C10 C11 H6 119.4 . . . no C12 C11 H6 119.4 . . . no C11 C12 C13 120.3(9) . . . yes C11 C12 H7 119.9 . . . no C13 C12 H7 119.9 . . . no C12 C13 C14 120.8(9) . . . yes C12 C13 H8 119.6 . . . no C14 C13 H8 119.6 . . . no C13 C14 C15 120(1) . . . yes C13 C14 H9 119.8 . . . no C15 C14 H9 119.9 . . . no N4 C15 C10 114.0(8) . . . yes N4 C15 C14 126(1) . . . yes C10 C15 C14 119.4(9) . . . yes N4 C16 C17 121.6(9) . . . yes N4 C16 C21 122.9(9) . . . yes C17 C16 C21 115.4(9) . . . yes C16 C17 C18 129(1) . . . yes C16 C17 H10 115.3 . . . no C18 C17 H10 115.3 . . . no N1 C18 C17 122.0(9) . . . yes N1 C18 C22 121.5(9) . . . yes C17 C18 C22 116.5(9) . . . yes C7 C19 H11 109.5 . . . no C7 C19 H12 109.5 . . . no C7 C19 H13 109.5 . . . no H11 C19 H12 109.5 . . . no H11 C19 H13 109.5 . . . no H12 C19 H13 109.5 . . . no C9 C20 H14 109.5 . . . no C9 C20 H15 109.5 . . . no C9 C20 H16 109.5 . . . no H14 C20 H15 109.5 . . . no H14 C20 H16 109.5 . . . no H15 C20 H16 109.5 . . . no C16 C21 H17 109.5 . . . no C16 C21 H18 109.5 . . . no C16 C21 H19 109.5 . . . no H17 C21 H18 109.5 . . . no H17 C21 H19 109.5 . . . no H18 C21 H19 109.5 . . . no C18 C22 H20 109.5 . . . no C18 C22 H21 109.5 . . . no C18 C22 H22 109.5 . . . no H20 C22 H21 109.5 . . . no H20 C22 H22 109.5 . . . no H21 C22 H22 109.5 . . . no N5 C23 C24 121.4(9) . . . yes N5 C23 C41 120.0(9) . . . yes C24 C23 C41 118.6(9) . . . yes C23 C24 C25 130.4(8) . . . yes C23 C24 H23 114.8 . . . no C25 C24 H23 114.8 . . . no N6 C25 C24 121.5(9) . . . yes N6 C25 C42 122(1) . . . yes C24 C25 C42 116.6(9) . . . yes N6 C26 C27 125.8(8) . . . yes N6 C26 C31 114.6(8) . . . yes C27 C26 C31 118.9(9) . . . yes C26 C27 C28 121.3(9) . . . yes C26 C27 H24 119.4 . . . no C28 C27 H24 119.4 . . . no C27 C28 C29 119.0(9) . . . yes C27 C28 H25 120.5 . . . no C29 C28 H25 120.5 . . . no C28 C29 C30 121.1(9) . . . yes C28 C29 H26 119.5 . . . no C30 C29 H26 119.5 . . . no C29 C30 C31 120.4(9) . . . yes C29 C30 H27 119.8 . . . no C31 C30 H27 119.8 . . . no N7 C31 C26 113.6(8) . . . yes N7 C31 C30 126.3(8) . . . yes C26 C31 C30 119.3(9) . . . yes N7 C32 C33 121.7(9) . . . yes N7 C32 C43 121.9(9) . . . yes C33 C32 C43 116.4(8) . . . yes C32 C33 C34 130.7(8) . . . yes C32 C33 H28 114.7 . . . no C34 C33 H28 114.7 . . . no N8 C34 C33 121.7(8) . . . yes N8 C34 C44 121.0(9) . . . yes C33 C34 C44 117.3(8) . . . yes N8 C35 C36 127.8(9) . . . yes N8 C35 C40 114.2(9) . . . yes C36 C35 C40 117.8(9) . . . yes C35 C36 C37 122.8(9) . . . yes C35 C36 H29 118.6 . . . no C37 C36 H29 118.6 . . . no C36 C37 C38 120(1) . . . yes C36 C37 H30 120.0 . . . no C38 C37 H30 120.0 . . . no C37 C38 C39 119(1) . . . yes C37 C38 H31 120.4 . . . no C39 C38 H31 120.4 . . . no C38 C39 C40 121.2(9) . . . yes C38 C39 H32 119.4 . . . no C40 C39 H32 119.4 . . . no N5 C40 C35 114.7(9) . . . yes N5 C40 C39 125.3(8) . . . yes C35 C40 C39 119(1) . . . yes C23 C41 H33 109.5 . . . no C23 C41 H34 109.5 . . . no C23 C41 H35 109.5 . . . no H33 C41 H34 109.5 . . . no H33 C41 H35 109.5 . . . no H34 C41 H35 109.5 . . . no C25 C42 H36 109.5 . . . no C25 C42 H37 109.5 . . . no C25 C42 H38 109.5 . . . no H36 C42 H37 109.5 . . . no H36 C42 H38 109.5 . . . no H37 C42 H38 109.5 . . . no C32 C43 H39 109.5 . . . no C32 C43 H40 109.5 . . . no C32 C43 H41 109.5 . . . no H39 C43 H40 109.5 . . . no H39 C43 H41 109.5 . . . no H40 C43 H41 109.5 . . . no C34 C44 H42 109.5 . . . no C34 C44 H43 109.5 . . . no C34 C44 H44 109.5 . . . no H42 C44 H43 109.5 . . . no H42 C44 H44 109.5 . . . no H43 C44 H44 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CU1 C33 3.405(9) . . no CU1 S1 3.501(4) . . no CU1 C32 3.565(9) . . no CU1 C34 3.597(9) . . no CU2 S8 3.339(5) . 4 no CU2 C4 3.56(1) . . no CU2 C3 3.578(9) . . no CU2 C5 3.64(1) . . no S1 C18 3.29(1) . . no S1 N1 3.368(8) . . no S1 C17 3.60(1) . . no S1 C32 3.627(9) . 4_554 no S2 N6 3.627(9) . 4_554 no S3 C9 3.27(1) . . no S3 C20 3.51(1) . . no S3 N3 3.547(8) . . no S3 C8 3.56(1) . . no S5 C23 3.61(1) . 1_545 no S7 C17 3.40(1) . . no S7 C21 3.51(1) . . no S7 C16 3.56(1) . . no S8 N5 3.395(8) . 4_554 no S8 N8 3.481(8) . 4_554 no S8 C23 3.52(1) . 4_554 no N1 N8 3.47(1) . . no N1 C36 3.59(1) . . no N1 C34 3.62(1) . . no N2 C30 3.52(1) . . no N2 N7 3.55(1) . . no N3 C43 3.58(1) . . no N4 C44 3.47(1) . . no N4 C33 3.57(1) . . no N4 C34 3.57(1) . . no N5 C3 3.48(1) . . no N6 C4 3.50(1) . . no N7 C6 3.51(1) . . no N7 C5 3.59(1) . . no N8 C1 3.46(1) . . no N8 C2 3.52(1) . . no C1 C35 3.60(1) . . no C2 C35 3.20(1) . . no C2 C40 3.35(1) . . no C2 C36 3.48(1) . . no C3 C12 3.45(1) . 4_554 no C3 C40 3.52(1) . . no C3 C13 3.53(1) . 4_554 no C4 C26 3.59(1) . . no C4 C12 3.62(1) . 4_554 no C5 C31 3.30(1) . . no C5 C26 3.36(1) . . no C5 C30 3.60(1) . . no C7 C30 3.38(1) . . no C11 C28 3.51(1) . 2_545 no C11 C29 3.62(1) . 2_545 no C13 C37 3.62(1) . 2_645 no C14 C37 3.50(1) . 2_645 no C14 C38 3.57(1) . 2_645 no C15 C33 3.52(1) . . no C16 C44 3.61(1) . . no C18 C36 3.39(1) . . no #------------------------------------------------------------------------------ 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #=END data_Ni(TMTAA)(p4se3) #------------------------------------------------------------------------------ _audit_creation_date '1998-04-02' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 19.0407(8) _cell_length_b 17.3568(8) _cell_length_c 13.5731(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4485.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'chunk' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1163.06 _chemical_formula_analytical ? _chemical_formula_sum 'C44 H44 N8 Ni2 P4 Se3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2328.00 _exptl_absorpt_coefficient_mu 3.461 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Enraf-Nonium CCD' _diffrn_measurement_device_type 'unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 15028 _reflns_number_total 15028 _reflns_number_gt 2521 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 8 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 176 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 176 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 16 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 12 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Se(1) -0.03343(5) 0.2500 0.03289(6) 0.0456(3) 0.500 ST Uani d ? Se(2) 0.00536(4) 0.34838(5) -0.17775(6) 0.0443(3) 0.900 . Uiso d ? Se(3) -0.1036(6) 0.3336(6) -0.1778(8) 0.074(4) 0.100 . Uiso d ? Ni(1) 0.10590(5) 0.2500 0.17265(6) 0.0184(3) 0.500 ST Uani d ? Ni(2) 0.20919(5) 0.2500 0.48239(6) 0.0163(3) 0.500 ST Uani d ? P(1) 0.0488(1) 0.2500 -0.0895(2) 0.0376(7) 0.500 ST Uani d ? P(2) -0.1322(1) 0.2500 -0.0554(2) 0.0480(7) 0.500 ST Uani d ? P(3) -0.1073(1) 0.3120(1) -0.1951(2) 0.0386(7) 0.900 . Uiso d ? P(4) 0.0195(5) 0.3308(5) -0.2020(6) -0.029(2) 0.100 . Uiso d ? N(1) 0.0596(2) 0.3226(2) 0.2504(3) 0.017(1) 1.000 . Uiso d ? N(2) 0.1496(2) 0.3233(2) 0.0922(3) 0.019(1) 1.000 . Uiso d ? N(3) 0.2243(2) 0.3285(2) 0.3921(3) 0.017(1) 1.000 . Uiso d ? N(4) 0.1954(2) 0.3293(2) 0.5730(2) 0.016(1) 1.000 . Uiso d ? C(1) 0.0398(3) 0.2900(3) 0.3418(3) 0.019(1) 1.000 . Uiso d ? C(2) 0.0296(3) 0.3305(3) 0.4293(3) 0.019(1) 1.000 . Uiso d ? C(3) 0.0164(3) 0.2892(3) 0.5171(3) 0.023(1) 1.000 . Uiso d ? C(4) 0.3238(3) 0.2898(3) -0.0287(3) 0.024(1) 1.000 . Uiso d ? C(5) 0.2669(3) 0.3292(3) 0.0079(3) 0.019(1) 1.000 . Uiso d ? C(6) 0.2090(3) 0.2909(2) 0.0447(3) 0.018(1) 1.000 . Uiso d ? C(7) 0.0412(3) 0.3919(3) 0.2188(3) 0.019(1) 1.000 . Uiso d ? C(8) 0.0707(3) 0.4243(3) 0.1339(3) 0.025(1) 1.000 . Uiso d ? C(9) 0.1245(3) 0.3945(3) 0.0770(3) 0.019(1) 1.000 . Uiso d ? C(10) -0.0162(3) 0.4388(3) 0.2679(3) 0.027(1) 1.000 . Uiso d ? C(11) 0.1506(3) 0.4455(3) -0.0049(3) 0.026(1) 1.000 . Uiso d ? C(12) 0.1922(2) 0.3978(3) 0.4234(3) 0.015(1) 1.000 . Uiso d ? C(13) 0.1689(3) 0.4577(3) 0.3640(3) 0.018(1) 1.000 . Uiso d ? C(14) 0.1317(3) 0.5183(3) 0.4036(3) 0.023(1) 1.000 . Uiso d ? C(15) 0.1146(3) 0.5189(3) 0.5035(3) 0.022(1) 1.000 . Uiso d ? C(16) 0.1366(3) 0.4583(3) 0.5630(3) 0.019(1) 1.000 . Uiso d ? C(17) 0.1757(3) 0.3985(3) 0.5257(3) 0.016(1) 1.000 . Uiso d ? C(18) 0.2645(3) 0.3221(3) 0.3125(3) 0.019(1) 1.000 . Uiso d ? C(19) 0.2878(4) 0.2500 0.2789(4) 0.019(2) 0.500 S Uiso d ? C(20) 0.2176(4) 0.2500 0.7134(4) 0.019(2) 0.500 S Uiso d ? C(21) 0.2075(3) 0.3223(3) 0.6700(3) 0.023(1) 1.000 . Uiso d ? C(22) 0.2904(3) 0.3910(3) 0.2557(3) 0.026(1) 1.000 . Uiso d ? C(23) 0.2145(3) 0.3916(3) 0.7365(3) 0.023(1) 1.000 . Uiso d ? H(1) 0.0314 0.3852 0.4299 0.023 1.000 . Uiso c ? H(2) 0.0072 0.3164 0.5764 0.027 1.000 . Uiso c ? H(3) 0.3629 0.3177 -0.0539 0.029 1.000 . Uiso c ? H(4) 0.2674 0.3839 0.0080 0.023 1.000 . Uiso c ? H(5) 0.0516 0.4722 0.1131 0.030 1.000 . Uiso c ? H(6) 0.0022 0.4873 0.2874 0.032 1.000 . Uiso c ? H(7) -0.0537 0.4464 0.2228 0.032 1.000 . Uiso c ? H(8) -0.0330 0.4120 0.3242 0.032 1.000 . Uiso c ? H(9) 0.1878 0.4204 -0.0388 0.032 1.000 . Uiso c ? H(10) 0.1133 0.4557 -0.0495 0.032 1.000 . Uiso c ? H(11) 0.1673 0.4927 0.0219 0.032 1.000 . Uiso c ? H(12) 0.1787 0.4569 0.2954 0.022 1.000 . Uiso c ? H(13) 0.1177 0.5599 0.3627 0.027 1.000 . Uiso c ? H(14) 0.0882 0.5602 0.5306 0.026 1.000 . Uiso c ? H(15) 0.1243 0.4582 0.6309 0.023 1.000 . Uiso c ? H(16) 0.3223 0.2501 0.2284 0.022 0.500 S Uiso d ? H(17) 0.2336 0.2498 0.7797 0.023 0.500 S Uiso d ? H(18) 0.3403 0.3923 0.2574 0.031 1.000 . Uiso c ? H(19) 0.2750 0.3874 0.1892 0.031 1.000 . Uiso c ? H(20) 0.2723 0.4367 0.2845 0.031 1.000 . Uiso c ? H(21) 0.2606 0.3932 0.7632 0.028 1.000 . Uiso c ? H(22) 0.2061 0.4372 0.6996 0.028 1.000 . Uiso c ? H(23) 0.1813 0.3881 0.7885 0.028 1.000 . Uiso c ? 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 Se(1) 0.0521(7) 0.0554(6) 0.0293(5) 0.0000 -0.0103(4) 0.0000 Ni(1) 0.0215(6) 0.0182(5) 0.0157(5) 0.0000 0.0025(4) 0.0000 Ni(2) 0.0228(6) 0.0127(5) 0.0132(4) 0.0000 0.0012(4) 0.0000 P(1) 0.026(2) 0.043(1) 0.044(1) 0.0000 -0.011(1) 0.0000 P(2) 0.039(1) 0.061(2) 0.044(1) 0.0000 0.0002(9) 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; Se(2) and Se(3) represent the disordered Se atoms with populations 0.9 and 0.1 respectively. P(3) and P(4) represent the disordered P atoms with 0.2 populations 0.9 and 0.1 respectively. Ni(1), Ni(2), P(1), P2) and 0.3 Se(1) are on special positions with no disorder. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2521 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_all 0.0605 _refine_ls_wR_factor_ref 0.0605 _refine_ls_goodness_of_fit_all 2.796 _refine_ls_goodness_of_fit_ref 2.796 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.1230 _refine_diff_density_min -1.76 _refine_diff_density_max 1.38 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(1) P(1) 2.282(4) . . yes Se(1) P(2) 2.230(4) . . yes Se(2) Se(3) 2.09(2) . . yes Se(2) P(1) 2.244(3) . . yes Se(2) P(3) 2.248(5) . . yes Se(2) P(4) 0.52(1) . . yes Se(3) P(2) 2.27(2) . . yes Se(3) P(3) 0.45(2) . . yes Se(3) P(3) 2.54(2) . 7 yes Se(3) P(4) 2.37(2) . . yes Ni(1) N(1) 1.864(6) . . yes Ni(1) N(1) 1.864(6) . 7 yes Ni(1) N(2) 1.872(6) . . yes Ni(1) N(2) 1.872(6) . 7 yes Ni(2) N(3) 1.855(6) . . yes Ni(2) N(3) 1.855(6) . 7 yes Ni(2) N(4) 1.864(6) . . yes Ni(2) N(4) 1.864(6) . 7 yes P(1) P(4) 2.15(1) . . yes P(1) P(4) 2.15(1) . 7 yes P(2) P(3) 2.232(5) . . yes P(2) P(3) 2.232(5) . 7 yes P(3) P(3) 2.153(8) . 7 yes P(3) P(4) 2.44(2) . . yes N(1) C(1) 1.415(9) . . yes N(1) C(7) 1.324(9) . . yes N(2) C(6) 1.42(1) . . yes N(2) C(9) 1.342(9) . . yes N(3) C(12) 1.416(9) . . yes N(3) C(18) 1.328(9) . . yes N(4) C(17) 1.413(9) . . yes N(4) C(21) 1.343(9) . . yes C(1) C(1) 1.39(1) . 7 yes C(1) C(2) 1.39(1) . . yes C(2) C(3) 1.41(1) . . yes C(2) H(1) 0.95 . . no C(3) C(3) 1.36(1) . 7 yes C(3) H(2) 0.95 . . no C(4) C(4) 1.38(1) . 7 yes C(4) C(5) 1.37(1) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.38(1) . . yes C(5) H(4) 0.95 . . no C(6) C(6) 1.42(1) . 7 yes C(7) C(8) 1.40(1) . . yes C(7) C(10) 1.52(1) . . yes C(8) C(9) 1.38(1) . . yes C(8) H(5) 0.95 . . no C(9) C(11) 1.51(1) . . yes C(10) H(6) 0.95 . . no C(10) H(7) 0.95 . . no C(10) H(8) 0.95 . . no C(11) H(9) 0.95 . . no C(11) H(10) 0.95 . . no C(11) H(11) 0.95 . . no C(12) C(13) 1.39(1) . . yes C(12) C(17) 1.423(9) . . yes C(13) C(14) 1.38(1) . . yes C(13) H(12) 0.95 . . no C(14) C(15) 1.40(1) . . yes C(14) H(13) 0.95 . . no C(15) C(16) 1.39(1) . . yes C(15) H(14) 0.95 . . no C(16) C(17) 1.38(1) . . yes C(16) H(15) 0.95 . . no C(18) C(19) 1.404(9) . . yes C(18) C(22) 1.51(1) . . yes C(19) H(16) 0.95 . . no C(20) C(21) 1.400(9) . . yes C(20) C(21) 1.400(9) . 7 yes C(20) H(17) 0.95 . . no C(21) C(23) 1.51(1) . . yes C(22) H(18) 0.95 . . no C(22) H(19) 0.95 . . no C(22) H(20) 0.95 . . no C(23) H(21) 0.95 . . no C(23) H(22) 0.95 . . no C(23) H(23) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Se(1) P(2) 100.8(1) . . . yes Se(3) Se(2) P(1) 105.8(5) . . . yes Se(3) Se(2) P(3) 11.1(5) . . . yes Se(3) Se(2) P(4) 116(2) . . . yes P(1) Se(2) P(3) 101.2(1) . . . yes P(1) Se(2) P(4) 73(1) . . . yes P(3) Se(2) P(4) 105(2) . . . yes Se(2) Se(3) P(2) 108.4(8) . . . yes Se(2) Se(3) P(3) 105(3) . . . yes Se(2) Se(3) P(3) 98.6(8) . . 7 yes Se(2) Se(3) P(4) 11.5(3) . . . yes P(2) Se(3) P(3) 79(3) . . . yes P(2) Se(3) P(3) 54.9(5) . . 7 yes P(2) Se(3) P(4) 109.0(8) . . . yes P(3) Se(3) P(3) 28(2) . . 7 yes P(3) Se(3) P(4) 94(3) . . . yes P(3) Se(3) P(4) 89.6(8) 7 . . yes N(1) Ni(1) N(1) 85.0(4) . . 7 yes N(1) Ni(1) N(2) 94.6(3) . . . yes N(1) Ni(1) N(2) 178.1(3) . . 7 yes N(1) Ni(1) N(2) 178.1(3) 7 . . yes N(1) Ni(1) N(2) 94.6(3) 7 . 7 yes N(2) Ni(1) N(2) 85.6(4) . . 7 yes N(3) Ni(2) N(3) 94.5(4) . . 7 yes N(3) Ni(2) N(4) 85.2(3) . . . yes N(3) Ni(2) N(4) 179.2(3) . . 7 yes N(3) Ni(2) N(4) 179.2(3) 7 . . yes N(3) Ni(2) N(4) 85.2(3) 7 . 7 yes N(4) Ni(2) N(4) 95.2(4) . . 7 yes Se(1) P(1) Se(2) 97.8(1) . . . yes Se(1) P(1) Se(2) 97.8(1) . . 7 yes Se(1) P(1) P(4) 109.9(4) . . . yes Se(1) P(1) P(4) 109.9(4) . . 7 yes Se(2) P(1) Se(2) 99.1(2) . . 7 yes Se(2) P(1) P(4) 13.5(4) . . . yes Se(2) P(1) P(4) 91.2(4) . . 7 yes Se(2) P(1) P(4) 91.2(4) 7 . . yes Se(2) P(1) P(4) 13.5(4) 7 . 7 yes P(4) P(1) P(4) 81.6(7) . . 7 yes Se(1) P(2) Se(3) 101.0(5) . . . yes Se(1) P(2) Se(3) 101.0(5) . . 7 yes Se(1) P(2) P(3) 106.1(2) . . . yes Se(1) P(2) P(3) 106.1(2) . . 7 yes Se(3) P(2) Se(3) 79(1) . . 7 yes Se(3) P(2) P(3) 11.4(5) . . . yes Se(3) P(2) P(3) 68.6(5) . . 7 yes Se(3) P(2) P(3) 68.6(5) 7 . . yes Se(3) P(2) P(3) 11.4(5) 7 . 7 yes P(3) P(2) P(3) 57.7(2) . . 7 yes Se(2) P(3) Se(3) 64(3) . . . yes Se(2) P(3) Se(3) 104.1(6) . . 7 yes Se(2) P(3) P(2) 104.4(2) . . . yes Se(2) P(3) P(3) 106.3(1) . . 7 yes Se(2) P(3) P(4) 12.0(3) . . . yes Se(3) P(3) Se(3) 141(3) . . 7 yes Se(3) P(3) P(2) 89(3) . . . yes Se(3) P(3) P(3) 147(3) . . 7 yes Se(3) P(3) P(4) 76(3) . . . yes Se(3) P(3) P(2) 56.4(5) 7 . . yes Se(3) P(3) P(3) 5.5(5) 7 . 7 yes Se(3) P(3) P(4) 96.3(6) 7 . . yes P(2) P(3) P(3) 61.2(1) . . 7 yes P(2) P(3) P(4) 107.9(3) . . . yes P(3) P(3) P(4) 97.7(3) 7 . . yes Se(2) P(4) Se(3) 53(2) . . . yes Se(2) P(4) P(1) 94(1) . . . yes Se(2) P(4) P(3) 63(2) . . . yes Se(3) P(4) P(1) 99.9(7) . . . yes Se(3) P(4) P(3) 10.5(5) . . . yes P(1) P(4) P(3) 98.2(5) . . . yes Ni(1) N(1) C(1) 110.6(5) . . . yes Ni(1) N(1) C(7) 123.8(5) . . . yes C(1) N(1) C(7) 125.2(6) . . . yes Ni(1) N(2) C(6) 110.5(5) . . . yes Ni(1) N(2) C(9) 123.9(6) . . . yes C(6) N(2) C(9) 125.4(6) . . . yes Ni(2) N(3) C(12) 111.0(5) . . . yes Ni(2) N(3) C(18) 124.5(5) . . . yes C(12) N(3) C(18) 124.3(6) . . . yes Ni(2) N(4) C(17) 111.4(4) . . . yes Ni(2) N(4) C(21) 123.8(5) . . . yes C(17) N(4) C(21) 124.6(6) . . . yes N(1) C(1) C(1) 113.6(4) . . 7 yes N(1) C(1) C(2) 125.6(7) . . . yes C(1) C(1) C(2) 120.3(4) 7 . . yes C(1) C(2) C(3) 119.1(7) . . . yes C(1) C(2) H(1) 120.4 . . . no C(3) C(2) H(1) 120.4 . . . no C(2) C(3) C(3) 120.5(4) . . 7 yes C(2) C(3) H(2) 119.6 . . . no C(3) C(3) H(2) 119.9 7 . . no C(4) C(4) C(5) 119.8(5) 7 . . yes C(4) C(4) H(3) 120.6 7 . . no C(5) C(4) H(3) 119.6 . . . no C(4) C(5) C(6) 121.4(7) . . . yes C(4) C(5) H(4) 119.3 . . . no C(6) C(5) H(4) 119.3 . . . no N(2) C(6) C(5) 127.7(7) . . . yes N(2) C(6) C(6) 113.3(4) . . 7 yes C(5) C(6) C(6) 118.8(4) . . 7 yes N(1) C(7) C(8) 121.7(7) . . . yes N(1) C(7) C(10) 122.4(7) . . . yes C(8) C(7) C(10) 115.8(7) . . . yes C(7) C(8) C(9) 127.3(8) . . . yes C(7) C(8) H(5) 116.3 . . . no C(9) C(8) H(5) 116.3 . . . no N(2) C(9) C(8) 121.4(7) . . . yes N(2) C(9) C(11) 122.6(7) . . . yes C(8) C(9) C(11) 115.9(7) . . . yes C(7) C(10) H(6) 109.5 . . . no C(7) C(10) H(7) 109.5 . . . no C(7) C(10) H(8) 109.5 . . . no H(6) C(10) H(7) 109.5 . . . no H(6) C(10) H(8) 109.5 . . . no H(7) C(10) H(8) 109.5 . . . no C(9) C(11) H(9) 109.5 . . . no C(9) C(11) H(10) 109.5 . . . no C(9) C(11) H(11) 109.5 . . . no H(9) C(11) H(10) 109.5 . . . no H(9) C(11) H(11) 109.5 . . . no H(10) C(11) H(11) 109.5 . . . no N(3) C(12) C(13) 126.9(6) . . . yes N(3) C(12) C(17) 113.3(6) . . . yes C(13) C(12) C(17) 119.3(7) . . . yes C(12) C(13) C(14) 120.6(7) . . . yes C(12) C(13) H(12) 119.7 . . . no C(14) C(13) H(12) 119.7 . . . no C(13) C(14) C(15) 120.4(7) . . . yes C(13) C(14) H(13) 119.8 . . . no C(15) C(14) H(13) 119.8 . . . no C(14) C(15) C(16) 119.2(7) . . . yes C(14) C(15) H(14) 120.4 . . . no C(16) C(15) H(14) 120.4 . . . no C(15) C(16) C(17) 121.3(7) . . . yes C(15) C(16) H(15) 119.3 . . . no C(17) C(16) H(15) 119.3 . . . no N(4) C(17) C(12) 112.2(6) . . . yes N(4) C(17) C(16) 128.1(7) . . . yes C(12) C(17) C(16) 119.1(7) . . . yes N(3) C(18) C(19) 121.4(7) . . . yes N(3) C(18) C(22) 122.7(7) . . . yes C(19) C(18) C(22) 115.9(7) . . . yes C(18) C(19) C(18) 126(1) . . 7 yes C(18) C(19) H(16) 117.0 . . . no C(18) C(19) H(16) 117.0 7 . . no C(21) C(20) C(21) 128(1) . . 7 yes C(21) C(20) H(17) 116.2 . . . no C(21) C(20) H(17) 116.2 7 . . no N(4) C(21) C(20) 121.1(7) . . . yes N(4) C(21) C(23) 122.0(7) . . . yes C(20) C(21) C(23) 116.8(7) . . . yes C(18) C(22) H(18) 109.5 . . . no C(18) C(22) H(19) 109.5 . . . no C(18) C(22) H(20) 109.5 . . . no H(18) C(22) H(19) 109.5 . . . no H(18) C(22) H(20) 109.5 . . . no H(19) C(22) H(20) 109.5 . . . no C(21) C(23) H(21) 109.5 . . . no C(21) C(23) H(22) 109.5 . . . no C(21) C(23) H(23) 109.5 . . . no H(21) C(23) H(22) 109.5 . . . no H(21) C(23) H(23) 109.5 . . . no H(22) C(23) H(23) 109.5 . . . no #------------------------------------------------------------------------------ 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #=END data_Nitmtaa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'tmtaa dimer' _chemical_formula_moiety 'C22 H22 Ni N4 ' _chemical_formula_sum 'C22 H22 N4 Ni' _chemical_formula_weight 401.15 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9493(8) _cell_length_b 14.9208(8) _cell_length_c 15.6235(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.070(3) _cell_angle_gamma 90.00 _cell_volume 3717.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour 'green/purple dichroic' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Enraf-Nonius CCD _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 27347 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_sigmaI/netI 0.2645 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 29.96 _reflns_number_total 10312 _reflns_number_gt 4286 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] 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 10312 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2505 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _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 N1 N 0.1196(3) 0.7474(3) 0.0346(3) 0.0286(11) Uani 1 d . . . Ni1 Ni 0.13356(4) 0.62775(5) 0.00136(4) 0.0273(2) Uani 1 d . . . C1 C 0.0850(4) 0.7999(5) -0.0329(4) 0.0364(16) Uani 1 d . . . Ni2 Ni 0.44324(4) 0.15824(5) 0.08037(4) 0.0262(2) Uani 1 d . . . N2 N 0.2084(3) 0.5998(3) 0.0913(3) 0.0272(11) Uani 1 d . . . C2 C 0.0467(3) 0.7482(5) -0.0974(4) 0.0356(16) Uani 1 d . . . N3 N 0.1466(3) 0.5072(3) -0.0311(3) 0.0309(12) Uani 1 d . . . C3 C 0.0125(4) 0.7910(6) -0.1694(4) 0.051(2) Uani 1 d . . . H3 H -0.0130 0.7568 -0.2141 0.061 Uiso 1 calc R . . N4 N 0.0538(3) 0.6549(4) -0.0844(3) 0.0335(12) Uani 1 d . . . C4 C 0.0160(5) 0.8841(6) -0.1754(5) 0.065(3) Uani 1 d . . . H4 H -0.0097 0.9133 -0.2231 0.078 Uiso 1 calc R . . N5 N 0.3341(3) 0.1343(3) 0.1172(3) 0.0332(12) Uani 1 d . . . C5 C 0.0559(4) 0.9343(6) -0.1137(5) 0.058(2) Uani 1 d . . . H5 H 0.0591 0.9976 -0.1195 0.069 Uiso 1 calc R . . N6 N 0.4834(3) 0.1955(3) 0.1866(3) 0.0248(11) Uani 1 d . . . C6 C 0.0919(4) 0.8924(5) -0.0420(5) 0.0492(19) Uani 1 d . . . H6 H 0.1209 0.9268 0.0003 0.059 Uiso 1 calc R . . N7 N 0.5531(3) 0.1765(3) 0.0441(3) 0.0241(11) Uani 1 d . . . C7 C 0.1298(4) 0.7773(4) 0.1149(4) 0.0336(15) Uani 1 d . . . N8 N 0.4047(3) 0.1201(3) -0.0262(3) 0.0296(11) Uani 1 d . . . C8 C 0.0963(4) 0.8659(4) 0.1445(4) 0.0488(18) Uani 1 d . . . H8A H 0.0702 0.8974 0.0959 0.073 Uiso 1 calc R . . H8B H 0.1425 0.9021 0.1682 0.073 Uiso 1 calc R . . H8C H 0.0546 0.8559 0.1887 0.073 Uiso 1 calc R . . C9 C 0.1688(4) 0.7247(4) 0.1768(4) 0.0338(15) Uani 1 d . . . H9 H 0.1681 0.7474 0.2336 0.041 Uiso 1 calc R . . C10 C 0.2090(4) 0.6424(4) 0.1662(4) 0.0303(14) Uani 1 d . . . C11 C 0.2482(4) 0.6005(5) 0.2470(4) 0.0427(17) Uani 1 d . . . H11A H 0.2746 0.5433 0.2324 0.064 Uiso 1 calc R . . H11B H 0.2045 0.5901 0.2891 0.064 Uiso 1 calc R . . H11C H 0.2906 0.6412 0.2713 0.064 Uiso 1 calc R . . C12 C 0.2558(4) 0.5225(4) 0.0729(4) 0.0316(14) Uani 1 d . . . C13 C 0.3330(4) 0.4994(5) 0.1090(4) 0.0404(16) Uani 1 d . . . H13 H 0.3576 0.5360 0.1524 0.048 Uiso 1 calc R . . C14 C 0.3744(4) 0.4223(5) 0.0815(5) 0.0481(18) Uani 1 d . . . H14 H 0.4267 0.4061 0.1072 0.058 Uiso 1 calc R . . C15 C 0.3399(4) 0.3694(5) 0.0173(4) 0.0453(18) Uani 1 d . . . H15 H 0.3679 0.3165 -0.0001 0.054 Uiso 1 calc R . . C16 C 0.2655(4) 0.3935(4) -0.0211(4) 0.0420(17) Uani 1 d . . . H16 H 0.2432 0.3576 -0.0663 0.050 Uiso 1 calc R . . C17 C 0.2215(4) 0.4696(4) 0.0048(4) 0.0332(15) Uani 1 d . . . C18 C 0.0889(4) 0.4600(4) -0.0728(4) 0.0371(16) Uani 1 d . . . C19 C 0.0888(4) 0.3594(5) -0.0780(4) 0.0500(19) Uani 1 d . . . H19A H 0.1398 0.3359 -0.0501 0.075 Uiso 1 calc R . . H19B H 0.0872 0.3409 -0.1382 0.075 Uiso 1 calc R . . H19C H 0.0395 0.3358 -0.0491 0.075 Uiso 1 calc R . . C20 C 0.0191(4) 0.5018(5) -0.1105(3) 0.0404(17) Uani 1 d . . . H20 H -0.0227 0.4630 -0.1337 0.048 Uiso 1 calc R . . C21 C 0.0032(4) 0.5921(5) -0.1183(3) 0.0386(17) Uani 1 d . . . C22 C -0.0788(4) 0.6166(6) -0.1642(4) 0.058(2) Uani 1 d . . . H22A H -0.0844 0.6820 -0.1665 0.088 Uiso 1 calc R . . H22B H -0.1259 0.5911 -0.1330 0.088 Uiso 1 calc R . . H22C H -0.0787 0.5924 -0.2225 0.088 Uiso 1 calc R . . C23 C 0.2775(4) 0.1331(4) 0.0480(4) 0.0389(16) Uani 1 d . . . C24 C 0.3151(4) 0.1276(4) -0.0317(4) 0.0374(15) Uani 1 d . . . C25 C 0.2685(5) 0.1364(5) -0.1058(5) 0.0525(19) Uani 1 d . . . H25 H 0.2949 0.1367 -0.1599 0.063 Uiso 1 calc R . . C26 C 0.1820(5) 0.1448(5) -0.1004(6) 0.067(2) Uani 1 d . . . H26 H 0.1489 0.1497 -0.1514 0.080 Uiso 1 calc R . . C27 C 0.1440(5) 0.1461(6) -0.0236(6) 0.072(3) Uani 1 d . . . H27 H 0.0846 0.1482 -0.0214 0.086 Uiso 1 calc R . . C28 C 0.1901(4) 0.1446(5) 0.0501(5) 0.058(2) Uani 1 d . . . H28 H 0.1632 0.1512 0.1035 0.069 Uiso 1 calc R . . C29 C 0.3166(4) 0.1154(4) 0.1997(4) 0.0416(18) Uani 1 d . . . C30 C 0.2329(4) 0.0765(5) 0.2246(5) 0.058(2) Uani 1 d . . . H30A H 0.1964 0.0717 0.1737 0.087 Uiso 1 calc R . . H30B H 0.2067 0.1156 0.2668 0.087 Uiso 1 calc R . . H30C H 0.2415 0.0168 0.2495 0.087 Uiso 1 calc R . . C31 C 0.3751(4) 0.1263(4) 0.2643(4) 0.0401(16) Uani 1 d . . . H31 H 0.3610 0.1013 0.3181 0.048 Uiso 1 calc R . . C32 C 0.4520(4) 0.1689(4) 0.2613(4) 0.0318(15) Uani 1 d . . . C33 C 0.4989(4) 0.1792(4) 0.3460(4) 0.0423(17) Uani 1 d . . . H33A H 0.5522 0.2100 0.3367 0.063 Uiso 1 calc R . . H33B H 0.5099 0.1198 0.3706 0.063 Uiso 1 calc R . . H33C H 0.4650 0.2143 0.3854 0.063 Uiso 1 calc R . . C34 C 0.5567(3) 0.2482(4) 0.1785(3) 0.0242(13) Uani 1 d . . . C35 C 0.5864(4) 0.3121(4) 0.2362(4) 0.0361(15) Uani 1 d . . . H35 H 0.5588 0.3209 0.2889 0.043 Uiso 1 calc R . . C36 C 0.6559(4) 0.3630(5) 0.2170(4) 0.0449(18) Uani 1 d . . . H36 H 0.6768 0.4060 0.2568 0.054 Uiso 1 calc R . . C37 C 0.6946(4) 0.3509(5) 0.1398(4) 0.0435(17) Uani 1 d . . . H37 H 0.7433 0.3849 0.1275 0.052 Uiso 1 calc R . . C38 C 0.6640(4) 0.2899(4) 0.0793(4) 0.0372(16) Uani 1 d . . . H38 H 0.6899 0.2846 0.0253 0.045 Uiso 1 calc R . . C39 C 0.5951(3) 0.2369(4) 0.0988(3) 0.0262(13) Uani 1 d . . . C40 C 0.5875(4) 0.1282(4) -0.0173(3) 0.0263(13) Uani 1 d . . . C41 C 0.6818(4) 0.1225(5) -0.0279(4) 0.0387(16) Uani 1 d . . . H41A H 0.7099 0.1594 0.0160 0.058 Uiso 1 calc R . . H41B H 0.6965 0.1445 -0.0848 0.058 Uiso 1 calc R . . H41C H 0.7000 0.0601 -0.0216 0.058 Uiso 1 calc R . . C42 C 0.5396(4) 0.0795(4) -0.0749(3) 0.0300(14) Uani 1 d . . . H42 H 0.5690 0.0419 -0.1132 0.036 Uiso 1 calc R . . C43 C 0.4530(4) 0.0794(4) -0.0828(3) 0.0295(14) Uani 1 d . . . C44 C 0.4166(4) 0.0268(4) -0.1582(4) 0.0441(17) Uani 1 d . . . H44A H 0.3553 0.0309 -0.1582 0.066 Uiso 1 calc R . . H44B H 0.4335 -0.0362 -0.1532 0.066 Uiso 1 calc R . . H44C H 0.4376 0.0517 -0.2117 0.066 Uiso 1 calc R . . 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 N1 0.015(2) 0.032(3) 0.039(3) 0.011(2) 0.001(2) -0.002(2) Ni1 0.0215(4) 0.0350(5) 0.0252(4) 0.0032(3) 0.0013(3) -0.0029(3) C1 0.017(3) 0.049(4) 0.044(4) 0.020(3) 0.006(3) 0.003(3) Ni2 0.0221(4) 0.0250(4) 0.0316(4) -0.0035(3) 0.0054(3) 0.0015(3) N2 0.023(3) 0.028(3) 0.031(3) 0.006(2) 0.000(2) -0.004(2) C2 0.015(3) 0.057(5) 0.034(3) 0.018(3) 0.005(3) 0.007(3) N3 0.026(3) 0.040(3) 0.027(2) -0.002(2) 0.009(2) -0.009(2) C3 0.033(4) 0.080(6) 0.040(4) 0.019(4) 0.004(3) 0.010(4) N4 0.025(3) 0.056(4) 0.020(2) 0.005(2) 0.004(2) -0.002(3) C4 0.034(4) 0.092(7) 0.068(5) 0.055(5) 0.015(4) 0.021(4) N5 0.023(3) 0.022(3) 0.054(3) -0.014(2) 0.007(2) -0.001(2) C5 0.033(4) 0.062(5) 0.079(5) 0.039(5) 0.012(4) 0.011(4) N6 0.023(3) 0.025(3) 0.027(2) 0.001(2) 0.008(2) 0.000(2) C6 0.031(4) 0.049(5) 0.067(5) 0.021(4) 0.011(4) 0.002(3) N7 0.023(3) 0.028(3) 0.022(2) 0.002(2) 0.003(2) 0.000(2) C7 0.022(3) 0.034(4) 0.045(4) -0.001(3) 0.007(3) -0.003(3) N8 0.022(3) 0.026(3) 0.041(3) -0.007(2) -0.003(2) 0.006(2) C8 0.046(4) 0.039(4) 0.061(4) -0.007(3) 0.000(4) -0.001(3) C9 0.030(4) 0.035(4) 0.037(3) -0.008(3) 0.007(3) -0.009(3) C10 0.024(3) 0.036(4) 0.031(3) -0.001(3) -0.001(2) -0.004(3) C11 0.037(4) 0.061(5) 0.030(3) -0.001(3) -0.006(3) 0.001(3) C12 0.029(4) 0.031(4) 0.035(3) 0.008(3) 0.007(3) 0.002(3) C13 0.033(4) 0.045(4) 0.044(4) 0.006(3) -0.002(3) 0.001(3) C14 0.034(4) 0.045(5) 0.065(5) 0.016(4) 0.006(3) 0.008(4) C15 0.044(4) 0.037(4) 0.055(4) 0.010(4) 0.018(4) 0.015(4) C16 0.045(4) 0.041(4) 0.040(4) -0.003(3) 0.018(3) -0.003(3) C17 0.027(3) 0.037(4) 0.036(3) 0.006(3) 0.010(3) 0.000(3) C18 0.045(4) 0.038(4) 0.028(3) -0.003(3) 0.016(3) -0.011(3) C19 0.047(4) 0.060(5) 0.043(4) -0.012(3) 0.017(3) -0.010(4) C20 0.037(4) 0.064(5) 0.020(3) -0.005(3) 0.011(3) -0.015(4) C21 0.031(4) 0.073(5) 0.012(3) 0.004(3) 0.002(3) -0.007(4) C22 0.046(5) 0.100(7) 0.029(3) 0.015(4) -0.003(3) -0.011(4) C23 0.027(4) 0.035(4) 0.055(4) -0.014(3) 0.003(3) 0.000(3) C24 0.028(4) 0.030(4) 0.053(4) -0.013(3) -0.014(3) -0.002(3) C25 0.046(5) 0.045(5) 0.066(5) -0.020(4) -0.012(4) 0.006(4) C26 0.042(5) 0.074(6) 0.084(6) -0.023(5) -0.035(4) 0.006(4) C27 0.039(5) 0.081(7) 0.096(7) -0.034(5) -0.004(5) 0.011(4) C28 0.034(4) 0.052(5) 0.086(6) -0.030(4) 0.001(4) -0.001(4) C29 0.039(4) 0.031(4) 0.056(4) -0.010(3) 0.031(4) -0.002(3) C30 0.047(5) 0.057(5) 0.072(5) -0.019(4) 0.026(4) -0.023(4) C31 0.044(4) 0.041(4) 0.036(3) -0.008(3) 0.018(3) -0.005(3) C32 0.039(4) 0.022(3) 0.035(3) -0.002(3) 0.014(3) 0.001(3) C33 0.051(4) 0.042(4) 0.034(3) 0.006(3) 0.013(3) -0.001(3) C34 0.019(3) 0.027(3) 0.026(3) 0.002(2) 0.001(2) 0.000(2) C35 0.033(4) 0.047(4) 0.028(3) 0.002(3) 0.008(3) -0.008(3) C36 0.046(4) 0.054(5) 0.035(3) -0.007(3) 0.008(3) -0.014(3) C37 0.032(4) 0.056(5) 0.042(4) 0.003(3) 0.002(3) -0.022(3) C38 0.031(4) 0.051(4) 0.030(3) -0.001(3) 0.005(3) -0.002(3) C39 0.023(3) 0.030(3) 0.027(3) 0.001(3) 0.002(2) 0.002(3) C40 0.030(3) 0.028(3) 0.021(3) 0.007(3) 0.008(2) 0.005(3) C41 0.030(4) 0.051(4) 0.035(3) -0.009(3) 0.013(3) 0.006(3) C42 0.043(4) 0.022(3) 0.025(3) 0.001(3) 0.007(3) 0.002(3) C43 0.044(4) 0.022(3) 0.023(3) -0.005(2) 0.000(3) -0.003(3) C44 0.059(5) 0.031(4) 0.042(4) -0.010(3) -0.007(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 C7 1.338(7) . ? N1 C1 1.418(7) . ? N1 Ni1 1.873(5) . ? Ni1 N2 1.873(5) . ? Ni1 N4 1.875(5) . ? Ni1 N3 1.881(5) . ? C1 C6 1.393(9) . ? C1 C2 1.401(9) . ? Ni2 N6 1.853(4) . ? Ni2 N8 1.853(5) . ? Ni2 N7 1.871(4) . ? Ni2 N5 1.877(5) . ? N2 C10 1.331(7) . ? N2 C12 1.412(7) . ? C2 C3 1.395(8) . ? C2 N4 1.410(8) . ? N3 C18 1.321(7) . ? N3 C17 1.426(7) . ? C3 C4 1.395(11) . ? N4 C21 1.338(8) . ? C4 C5 1.368(11) . ? N5 C29 1.353(8) . ? N5 C23 1.396(8) . ? C5 C6 1.397(10) . ? N6 C32 1.338(7) . ? N6 C34 1.417(7) . ? N7 C40 1.327(7) . ? N7 C39 1.404(7) . ? C7 C9 1.384(8) . ? C7 C8 1.501(8) . ? N8 C43 1.330(7) . ? N8 C24 1.435(8) . ? C9 C10 1.397(8) . ? C10 C11 1.533(8) . ? C12 C13 1.388(8) . ? C12 C17 1.425(8) . ? C13 C14 1.399(9) . ? C14 C15 1.382(10) . ? C15 C16 1.368(9) . ? C16 C17 1.400(8) . ? C18 C20 1.397(9) . ? C18 C19 1.503(9) . ? C20 C21 1.377(9) . ? C21 C22 1.525(9) . ? C23 C24 1.395(8) . ? C23 C28 1.406(9) . ? C24 C25 1.370(9) . ? C25 C26 1.390(10) . ? C26 C27 1.354(11) . ? C27 C28 1.354(10) . ? C29 C31 1.372(9) . ? C29 C30 1.513(8) . ? C31 C32 1.383(9) . ? C32 C33 1.515(8) . ? C34 C35 1.389(8) . ? C34 C39 1.409(7) . ? C35 C36 1.381(8) . ? C36 C37 1.377(8) . ? C37 C38 1.394(8) . ? C38 C39 1.392(8) . ? C40 C42 1.377(8) . ? C40 C41 1.520(8) . ? C42 C43 1.384(8) . ? C43 C44 1.521(8) . ? 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 C7 N1 C1 123.5(5) . . ? C7 N1 Ni1 124.4(4) . . ? C1 N1 Ni1 111.5(4) . . ? N2 Ni1 N1 94.6(2) . . ? N2 Ni1 N4 176.83(18) . . ? N1 Ni1 N4 84.9(2) . . ? N2 Ni1 N3 85.3(2) . . ? N1 Ni1 N3 179.31(18) . . ? N4 Ni1 N3 95.2(2) . . ? C6 C1 C2 120.5(6) . . ? C6 C1 N1 126.4(6) . . ? C2 C1 N1 112.9(6) . . ? N6 Ni2 N8 179.12(19) . . ? N6 Ni2 N7 85.30(18) . . ? N8 Ni2 N7 93.97(19) . . ? N6 Ni2 N5 95.1(2) . . ? N8 Ni2 N5 85.6(2) . . ? N7 Ni2 N5 177.4(2) . . ? C10 N2 C12 125.0(5) . . ? C10 N2 Ni1 123.2(4) . . ? C12 N2 Ni1 111.4(4) . . ? C3 C2 C1 119.1(7) . . ? C3 C2 N4 126.6(7) . . ? C1 C2 N4 114.0(5) . . ? C18 N3 C17 123.7(6) . . ? C18 N3 Ni1 124.3(4) . . ? C17 N3 Ni1 111.4(4) . . ? C4 C3 C2 119.7(7) . . ? C21 N4 C2 126.0(6) . . ? C21 N4 Ni1 121.8(5) . . ? C2 N4 Ni1 111.6(4) . . ? C5 C4 C3 121.1(7) . . ? C29 N5 C23 126.3(5) . . ? C29 N5 Ni2 122.7(4) . . ? C23 N5 Ni2 110.8(4) . . ? C4 C5 C6 120.0(8) . . ? C32 N6 C34 124.4(5) . . ? C32 N6 Ni2 124.3(4) . . ? C34 N6 Ni2 111.0(3) . . ? C1 C6 C5 119.5(7) . . ? C40 N7 C39 126.1(5) . . ? C40 N7 Ni2 122.8(4) . . ? C39 N7 Ni2 110.4(3) . . ? N1 C7 C9 120.7(5) . . ? N1 C7 C8 123.0(6) . . ? C9 C7 C8 116.2(5) . . ? C43 N8 C24 125.7(5) . . ? C43 N8 Ni2 123.4(4) . . ? C24 N8 Ni2 110.1(4) . . ? C7 C9 C10 128.1(5) . . ? N2 C10 C9 121.9(5) . . ? N2 C10 C11 121.7(5) . . ? C9 C10 C11 116.2(5) . . ? C13 C12 N2 126.5(6) . . ? C13 C12 C17 119.4(6) . . ? N2 C12 C17 113.9(5) . . ? C12 C13 C14 120.0(6) . . ? C15 C14 C13 120.5(7) . . ? C16 C15 C14 120.0(6) . . ? C15 C16 C17 121.4(6) . . ? C16 C17 C12 118.5(6) . . ? C16 C17 N3 128.8(6) . . ? C12 C17 N3 112.6(5) . . ? N3 C18 C20 120.7(6) . . ? N3 C18 C19 124.0(6) . . ? C20 C18 C19 115.1(6) . . ? C21 C20 C18 128.2(6) . . ? N4 C21 C20 122.8(6) . . ? N4 C21 C22 121.6(7) . . ? C20 C21 C22 115.5(6) . . ? C24 C23 N5 114.2(5) . . ? C24 C23 C28 118.1(6) . . ? N5 C23 C28 127.5(6) . . ? C25 C24 C23 121.0(6) . . ? C25 C24 N8 125.6(6) . . ? C23 C24 N8 113.3(5) . . ? C24 C25 C26 118.7(7) . . ? C27 C26 C25 121.1(8) . . ? C28 C27 C26 120.6(8) . . ? C27 C28 C23 120.3(7) . . ? N5 C29 C31 121.8(5) . . ? N5 C29 C30 121.6(7) . . ? C31 C29 C30 116.6(6) . . ? C29 C31 C32 128.4(6) . . ? N6 C32 C31 120.8(6) . . ? N6 C32 C33 123.0(5) . . ? C31 C32 C33 116.1(5) . . ? C35 C34 C39 120.5(5) . . ? C35 C34 N6 126.5(4) . . ? C39 C34 N6 112.7(5) . . ? C36 C35 C34 120.1(5) . . ? C37 C36 C35 119.6(6) . . ? C36 C37 C38 121.4(6) . . ? C39 C38 C37 119.4(5) . . ? C38 C39 N7 127.0(5) . . ? C38 C39 C34 118.9(5) . . ? N7 C39 C34 113.8(5) . . ? N7 C40 C42 121.8(5) . . ? N7 C40 C41 122.2(5) . . ? C42 C40 C41 116.0(5) . . ? C40 C42 C43 126.8(5) . . ? N8 C43 C42 122.0(5) . . ? N8 C43 C44 122.2(5) . . ? C42 C43 C44 115.8(5) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.628 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.156 #=END data_(toluene)Nitmtaa _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H30 N4 Ni' _chemical_formula_weight 493.28 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4126(5) _cell_length_b 13.3634(7) _cell_length_c 17.5322(9) _cell_angle_alpha 92.5950(10) _cell_angle_beta 90.5910(10) _cell_angle_gamma 101.8630(10) _cell_volume 2384.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'cube' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method ? _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Simens SMART CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14446 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.22 _reflns_number_total 10009 _reflns_number_observed 7378 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+17.0177P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10009 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_obs 0.0900 _refine_ls_wR_factor_all 0.2292 _refine_ls_wR_factor_obs 0.2204 _refine_ls_goodness_of_fit_all 1.229 _refine_ls_goodness_of_fit_obs 1.388 _refine_ls_restrained_S_all 1.229 _refine_ls_restrained_S_obs 1.388 _refine_ls_shift/esd_max 0.027 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1A Ni 0.65028(8) 0.50328(6) 0.36905(5) 0.0234(2) Uani 1 d . . N1A N 0.5179(5) 0.3867(4) 0.3816(3) 0.0237(11) Uiso 1 d . . N2A N 0.5387(5) 0.5966(4) 0.3770(3) 0.0232(11) Uani 1 d . . N3A N 0.7828(5) 0.6190(4) 0.3589(3) 0.0246(12) Uani 1 d . . N4A N 0.7625(5) 0.4107(4) 0.3635(3) 0.0240(11) Uiso 1 d . . C1A C 0.3162(7) 0.2932(5) 0.4446(4) 0.033(2) Uani 1 d . . H1A1 H 0.2557(7) 0.2632(5) 0.4041(4) 0.039 Uiso 1 calc R . H1A2 H 0.2682(7) 0.3104(5) 0.4880(4) 0.039 Uiso 1 calc R . H1A3 H 0.3684(7) 0.2452(5) 0.4585(4) 0.039 Uiso 1 calc R . C2A C 0.4050(6) 0.3895(5) 0.4177(4) 0.0255(14) Uani 1 d . . C3A C 0.3661(6) 0.4805(5) 0.4345(4) 0.0269(14) Uani 1 d . . H3A H 0.2901(6) 0.4754(5) 0.4627(4) 0.032 Uiso 1 calc R . C4A C 0.4251(6) 0.5792(5) 0.4149(4) 0.0261(14) Uani 1 d . . C5A C 0.3576(7) 0.6649(5) 0.4398(4) 0.033(2) Uani 1 d . . H5A1 H 0.2982(7) 0.6427(5) 0.4800(4) 0.039 Uiso 1 calc R . H5A2 H 0.3097(7) 0.6829(5) 0.3972(4) 0.039 Uiso 1 calc R . H5A3 H 0.4222(7) 0.7234(5) 0.4579(4) 0.039 Uiso 1 calc R . C6A C 0.5963(6) 0.6910(5) 0.3471(4) 0.0254(14) Uani 1 d . . C7A C 0.5318(7) 0.7645(5) 0.3195(4) 0.0290(15) Uani 1 d . . H7A H 0.4414(7) 0.7558(5) 0.3244(4) 0.035 Uiso 1 calc R . C8A C 0.6006(7) 0.8504(5) 0.2850(4) 0.034(2) Uani 1 d . . H8A H 0.5572(7) 0.9009(5) 0.2704(4) 0.041 Uiso 1 calc R . C9A C 0.7336(8) 0.8610(5) 0.2721(4) 0.035(2) Uani 1 d . . H9A H 0.7786(8) 0.9164(5) 0.2463(4) 0.042 Uiso 1 calc R . C10A C 0.7996(7) 0.7879(5) 0.2983(4) 0.032(2) Uani 1 d . . H10A H 0.8893(7) 0.7957(5) 0.2905(4) 0.038 Uiso 1 calc R . C11A C 0.7336(7) 0.7035(5) 0.3358(4) 0.0265(14) Uani 1 d . . C12A C 0.9101(6) 0.6237(5) 0.3803(4) 0.0262(14) Uani 1 d . . C13A C 1.0077(7) 0.7252(5) 0.3906(4) 0.034(2) Uani 1 d . . H13A H 1.0509(7) 0.7414(5) 0.3433(4) 0.040 Uiso 1 calc R . H13B H 1.0717(7) 0.7201(5) 0.4293(4) 0.040 Uiso 1 calc R . H13C H 0.9621(7) 0.7782(5) 0.4058(4) 0.040 Uiso 1 calc R . C14A C 0.9565(6) 0.5364(5) 0.3966(4) 0.0269(14) Uani 1 d . . H14A H 1.0419(6) 0.5471(5) 0.4161(4) 0.032 Uiso 1 calc R . C15A C 0.8897(6) 0.4343(5) 0.3872(4) 0.0269(14) Uani 1 d . . C16A C 0.9647(7) 0.3542(6) 0.4083(4) 0.036(2) Uani 1 d . . H16A H 1.0333(7) 0.3837(6) 0.4446(4) 0.043 Uiso 1 calc R . H16B H 1.0024(7) 0.3293(6) 0.3634(4) 0.043 Uiso 1 calc R . H16C H 0.9062(7) 0.2985(6) 0.4305(4) 0.043 Uiso 1 calc R . C17A C 0.6933(6) 0.3093(5) 0.3447(4) 0.0262(14) Uani 1 d . . C18A C 0.7463(7) 0.2319(6) 0.3104(4) 0.033(2) Uani 1 d . . H18A H 0.8360(7) 0.2424(6) 0.3018(4) 0.039 Uiso 1 calc R . C19A C 0.6652(8) 0.1388(6) 0.2890(5) 0.040(2) Uani 1 d . . H19A H 0.7004(8) 0.0862(6) 0.2667(5) 0.048 Uiso 1 calc R . C20A C 0.5322(8) 0.1244(6) 0.3008(4) 0.038(2) Uani 1 d . . H20A H 0.4783(8) 0.0616(6) 0.2870(4) 0.046 Uiso 1 calc R . C21A C 0.4779(7) 0.2018(5) 0.3329(4) 0.0310(15) Uani 1 d . . H21A H 0.3877(7) 0.1907(5) 0.3399(4) 0.037 Uiso 1 calc R . C22A C 0.5560(6) 0.2961(5) 0.3550(4) 0.0255(14) Uani 1 d . . Ni1B Ni 0.15952(8) 0.01540(6) 0.13061(5) 0.0241(2) Uani 1 d . . N1B N 0.0279(6) -0.1031(4) 0.1172(3) 0.0258(12) Uani 1 d . . N2B N 0.0466(5) 0.1073(4) 0.1255(3) 0.0239(11) Uani 1 d . . N3B N 0.2925(5) 0.1335(4) 0.1422(3) 0.0239(11) Uani 1 d . . N4B N 0.2736(5) -0.0761(4) 0.1337(3) 0.0244(12) Uani 1 d . . C1B C -0.1786(7) -0.2034(6) 0.0521(4) 0.035(2) Uani 1 d . . H1B1 H -0.2253(7) -0.1915(6) 0.0070(4) 0.042 Uiso 1 calc R . H1B2 H -0.2402(7) -0.2274(6) 0.0909(4) 0.042 Uiso 1 calc R . H1B3 H -0.1275(7) -0.2540(6) 0.0402(4) 0.042 Uiso 1 calc R . C2B C -0.0886(6) -0.1046(5) 0.0806(4) 0.0262(14) Uani 1 d . . C3B C -0.1290(6) -0.0146(5) 0.0660(4) 0.0269(14) Uani 1 d . . H3B H -0.2065(6) -0.0225(5) 0.0374(4) 0.032 Uiso 1 calc R . C4B C -0.0701(6) 0.0857(5) 0.0880(4) 0.0250(14) Uani 1 d . . C5B C -0.1416(7) 0.1671(6) 0.0647(4) 0.035(2) Uani 1 d . . H5B1 H -0.1999(7) 0.1796(6) 0.1044(4) 0.042 Uiso 1 calc R . H5B2 H -0.1914(7) 0.1444(6) 0.0185(4) 0.042 Uiso 1 calc R . H5B3 H -0.0792(7) 0.2291(6) 0.0563(4) 0.042 Uiso 1 calc R . C6B C 0.1059(6) 0.2047(5) 0.1573(4) 0.0254(14) Uani 1 d . . C7B C 0.0418(7) 0.2801(5) 0.1857(4) 0.032(2) Uani 1 d . . H7B H -0.0490(7) 0.2702(5) 0.1805(4) 0.038 Uiso 1 calc R . C8B C 0.1124(8) 0.3699(5) 0.2214(4) 0.036(2) Uani 1 d . . H8B H 0.0690(8) 0.4209(5) 0.2381(4) 0.043 Uiso 1 calc R . C9B C 0.2479(8) 0.3840(5) 0.2326(4) 0.036(2) Uani 1 d . . H9B H 0.2944(8) 0.4433(5) 0.2579(4) 0.044 Uiso 1 calc R . C10B C 0.3128(7) 0.3091(5) 0.2057(4) 0.033(2) Uani 1 d . . H10B H 0.4031(7) 0.3185(5) 0.2131(4) 0.039 Uiso 1 calc R . C11B C 0.2443(7) 0.2200(5) 0.1678(4) 0.0272(14) Uani 1 d . . C12B C 0.4188(6) 0.1372(5) 0.1200(4) 0.0274(14) Uani 1 d . . C13B C 0.5149(7) 0.2361(5) 0.1124(4) 0.035(2) Uani 1 d . . H13D H 0.5755(7) 0.2279(5) 0.0728(4) 0.042 Uiso 1 calc R . H13E H 0.5623(7) 0.2554(5) 0.1599(4) 0.042 Uiso 1 calc R . H13F H 0.4687(7) 0.2885(5) 0.0997(4) 0.042 Uiso 1 calc R . C14B C 0.4636(6) 0.0485(5) 0.1021(4) 0.0274(14) Uani 1 d . . H14B H 0.5475(6) 0.0575(5) 0.0822(4) 0.033 Uiso 1 calc R . C15B C 0.3984(6) -0.0531(5) 0.1102(4) 0.0237(13) Uani 1 d . . C16B C 0.4732(7) -0.1349(6) 0.0888(4) 0.034(2) Uani 1 d . . H16D H 0.5254(7) -0.1461(6) 0.1318(4) 0.040 Uiso 1 calc R . H16E H 0.5294(7) -0.1135(6) 0.0469(4) 0.040 Uiso 1 calc R . H16F H 0.4126(7) -0.1973(6) 0.0740(4) 0.040 Uiso 1 calc R . C17B C 0.2068(6) -0.1750(5) 0.1514(4) 0.0280(14) Uani 1 d . . C18B C 0.2611(7) -0.2498(6) 0.1839(4) 0.034(2) Uani 1 d . . H18B H 0.3513(7) -0.2378(6) 0.1928(4) 0.041 Uiso 1 calc R . C19B C 0.1841(8) -0.3417(6) 0.2033(5) 0.040(2) Uani 1 d . . H19B H 0.2225(8) -0.3918(6) 0.2238(5) 0.048 Uiso 1 calc R . C20B C 0.0489(8) -0.3588(6) 0.1920(5) 0.038(2) Uani 1 d . . H20B H -0.0039(8) -0.4202(6) 0.2053(5) 0.045 Uiso 1 calc R . C21B C -0.0070(7) -0.2832(5) 0.1606(4) 0.032(2) Uani 1 d . . H21B H -0.0974(7) -0.2958(5) 0.1526(4) 0.038 Uiso 1 calc R . C22B C 0.0679(6) -0.1898(5) 0.1407(4) 0.0273(14) Uani 1 d . . C1C C 0.5433(13) 0.5875(14) 0.1482(11) 0.111(7) Uani 1 d . . H1C1 H 0.4779(156) 0.5739(127) 0.1337(95) 0.133 Uiso 1 d . . H1C2 H 0.6264(149) 0.5133(109) 0.1930(80) 0.133 Uiso 1 d . . H1C3 H 0.5913(140) 0.6616(111) 0.1761(81) 0.133 Uiso 1 d . . C2C C 0.6411(9) 0.5408(6) 0.1037(5) 0.051(2) Uani 1 d . . C3C C 0.7188(15) 0.4815(7) 0.1416(9) 0.089(5) Uani 1 d . . H3C H 0.7435(128) 0.4409(98) 0.1806(74) 0.107 Uiso 1 d . . C4C C 0.8103(13) 0.4401(9) 0.0960(12) 0.093(5) Uani 1 d . . H4C H 0.8477(128) 0.3888(100) 0.1214(72) 0.111 Uiso 1 d . . C5C C 0.8214(15) 0.4537(13) 0.0180(15) 0.120(7) Uani 1 d . . H5C H 0.8988(151) 0.4065(112) -0.0169(82) 0.144 Uiso 1 d . . C6C C 0.7505(14) 0.5100(11) -0.0139(11) 0.098(5) Uani 1 d . . H6C H 0.8011(139) 0.5141(103) -0.0661(78) 0.118 Uiso 1 d . . C7C C 0.6615(10) 0.5514(7) 0.0282(6) 0.056(2) Uani 1 d . . H7C H 0.6202(100) 0.5922(76) 0.0069(57) 0.067 Uiso 1 d . . C1D C 0.0407(13) 0.0730(11) 0.3444(9) 0.117(6) Uani 1 d . . H1D3 H 0.0079(13) 0.0254(11) 0.3026(9) 0.140 Uiso 1 calc R . H1D2 H 0.0849(13) 0.1367(11) 0.3249(9) 0.140 Uiso 1 calc R . H1D1 H -0.0310(13) 0.0844(11) 0.3753(9) 0.140 Uiso 1 calc R . C2D C 0.1341(10) 0.0306(7) 0.3915(6) 0.060(3) Uani 1 d . . C3D C 0.2075(16) -0.0297(9) 0.3551(9) 0.105(6) Uani 1 d . . H3D H 0.1972(16) -0.0460(9) 0.3029(9) 0.126 Uiso 1 calc R . C4D C 0.2982(19) -0.0658(10) 0.3992(15) 0.129(9) Uani 1 d . . H4D H 0.3505(19) -0.1062(10) 0.3756(15) 0.155 Uiso 1 calc R . C5D C 0.3142(17) -0.0423(16) 0.4822(18) 0.165(12) Uani 1 d . . H5D H 0.3722(17) -0.0689(16) 0.5122(18) 0.199 Uiso 1 calc R . C6D C 0.2425(16) 0.0174(13) 0.5100(10) 0.110(6) Uani 1 d . . H6D H 0.2533(16) 0.0387(13) 0.5614(10) 0.133 Uiso 1 calc R . C7D C 0.1506(10) 0.0510(7) 0.4670(6) 0.058(3) Uani 1 d . . H7D H 0.0971(10) 0.0898(7) 0.4913(6) 0.069 Uiso 1 calc R . 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 Ni1A 0.0166(4) 0.0235(4) 0.0314(5) 0.0015(3) -0.0008(3) 0.0070(3) N2A 0.020(3) 0.021(3) 0.030(3) 0.002(2) -0.002(2) 0.008(2) N3A 0.026(3) 0.016(3) 0.029(3) 0.006(2) -0.001(2) -0.002(2) C1A 0.022(3) 0.034(4) 0.040(4) 0.003(3) 0.003(3) 0.001(3) C2A 0.016(3) 0.027(3) 0.032(4) 0.007(3) -0.006(3) -0.001(3) C3A 0.009(3) 0.035(4) 0.036(4) 0.002(3) 0.000(2) 0.004(3) C4A 0.016(3) 0.036(4) 0.028(3) -0.007(3) -0.008(2) 0.011(3) C5A 0.025(4) 0.035(4) 0.042(4) -0.001(3) 0.000(3) 0.017(3) C6A 0.023(3) 0.025(3) 0.031(3) 0.000(3) -0.001(3) 0.010(3) C7A 0.026(3) 0.028(4) 0.035(4) 0.005(3) -0.003(3) 0.010(3) C8A 0.035(4) 0.028(4) 0.044(4) 0.004(3) -0.003(3) 0.017(3) C9A 0.042(4) 0.020(3) 0.042(4) 0.007(3) 0.000(3) 0.006(3) C10A 0.030(4) 0.025(3) 0.040(4) 0.005(3) 0.001(3) 0.004(3) C11A 0.026(3) 0.023(3) 0.032(4) 0.003(3) 0.003(3) 0.009(3) C12A 0.017(3) 0.029(4) 0.032(4) 0.003(3) 0.001(3) 0.003(3) C13A 0.022(3) 0.032(4) 0.043(4) -0.002(3) 0.001(3) -0.001(3) C14A 0.013(3) 0.036(4) 0.032(4) 0.000(3) -0.001(3) 0.004(3) C15A 0.017(3) 0.038(4) 0.027(3) 0.004(3) 0.001(3) 0.010(3) C16A 0.026(4) 0.054(5) 0.032(4) 0.004(3) -0.003(3) 0.017(3) C17A 0.023(3) 0.023(3) 0.034(4) 0.003(3) 0.002(3) 0.006(3) C18A 0.026(4) 0.038(4) 0.038(4) 0.006(3) 0.005(3) 0.012(3) C19A 0.045(5) 0.027(4) 0.051(5) 0.001(3) 0.004(4) 0.012(3) C20A 0.044(5) 0.025(4) 0.046(5) 0.001(3) -0.001(4) 0.006(3) C21A 0.026(4) 0.029(4) 0.038(4) 0.002(3) -0.001(3) 0.006(3) C22A 0.025(3) 0.025(3) 0.028(3) 0.002(3) -0.004(3) 0.008(3) Ni1B 0.0183(4) 0.0232(4) 0.0322(5) 0.0005(3) -0.0035(3) 0.0080(3) N1B 0.033(3) 0.014(3) 0.029(3) -0.003(2) 0.002(2) 0.001(2) N2B 0.018(3) 0.024(3) 0.030(3) 0.000(2) 0.001(2) 0.007(2) N3B 0.025(3) 0.017(3) 0.030(3) 0.004(2) 0.001(2) 0.004(2) N4B 0.019(3) 0.025(3) 0.030(3) 0.001(2) -0.007(2) 0.006(2) C1B 0.020(3) 0.041(4) 0.043(4) -0.002(3) -0.004(3) 0.001(3) C2B 0.017(3) 0.030(4) 0.032(4) 0.002(3) 0.005(3) 0.004(3) C3B 0.014(3) 0.034(4) 0.034(4) -0.001(3) -0.001(3) 0.008(3) C4B 0.024(3) 0.029(3) 0.027(3) 0.003(3) -0.001(3) 0.016(3) C5B 0.028(4) 0.034(4) 0.049(4) 0.006(3) -0.004(3) 0.017(3) C6B 0.025(3) 0.024(3) 0.030(3) 0.003(3) 0.000(3) 0.010(3) C7B 0.031(4) 0.033(4) 0.035(4) 0.001(3) 0.001(3) 0.017(3) C8B 0.042(4) 0.024(4) 0.045(4) 0.001(3) 0.001(3) 0.017(3) C9B 0.050(5) 0.021(3) 0.039(4) -0.002(3) -0.009(3) 0.011(3) C10B 0.032(4) 0.030(4) 0.037(4) 0.001(3) -0.006(3) 0.009(3) C11B 0.027(3) 0.023(3) 0.035(4) -0.001(3) -0.006(3) 0.013(3) C12B 0.021(3) 0.033(4) 0.028(3) 0.006(3) -0.006(3) 0.003(3) C13B 0.026(4) 0.033(4) 0.046(4) 0.007(3) -0.004(3) 0.003(3) C14B 0.017(3) 0.035(4) 0.031(4) 0.001(3) -0.003(3) 0.008(3) C15B 0.019(3) 0.028(3) 0.026(3) 0.002(3) -0.007(2) 0.010(3) C16B 0.030(4) 0.038(4) 0.037(4) 0.004(3) -0.001(3) 0.017(3) C17B 0.023(3) 0.027(4) 0.034(4) -0.001(3) -0.004(3) 0.007(3) C18B 0.028(4) 0.035(4) 0.041(4) 0.001(3) -0.007(3) 0.011(3) C19B 0.046(5) 0.030(4) 0.048(5) 0.006(3) -0.010(4) 0.018(3) C20B 0.042(4) 0.023(4) 0.047(5) 0.007(3) -0.003(3) 0.004(3) C21B 0.028(4) 0.027(4) 0.040(4) 0.001(3) -0.003(3) 0.007(3) C22B 0.021(3) 0.031(4) 0.031(4) 0.001(3) -0.001(3) 0.008(3) C1C 0.059(8) 0.112(12) 0.138(14) -0.067(11) 0.018(9) -0.022(8) C2C 0.057(6) 0.032(4) 0.057(6) 0.006(4) -0.015(4) -0.008(4) C3C 0.111(11) 0.020(4) 0.126(11) 0.016(6) -0.068(9) -0.007(6) C4C 0.072(8) 0.040(6) 0.168(16) -0.007(8) -0.063(10) 0.021(6) C5C 0.060(9) 0.092(12) 0.200(21) -0.052(13) -0.015(12) 0.008(8) C6C 0.062(8) 0.078(9) 0.140(13) -0.033(9) 0.019(8) -0.009(7) C7C 0.056(6) 0.041(5) 0.066(7) 0.004(4) -0.015(5) 0.002(4) C1D 0.083(9) 0.103(11) 0.144(13) 0.063(10) -0.030(9) -0.040(8) C2D 0.064(6) 0.040(5) 0.066(6) 0.015(5) 0.016(5) -0.014(5) C3D 0.125(13) 0.048(7) 0.120(12) -0.026(7) 0.082(10) -0.030(8) C4D 0.114(14) 0.040(7) 0.241(24) 0.028(11) 0.108(17) 0.023(8) C5D 0.064(10) 0.106(15) 0.335(36) 0.111(20) 0.041(17) 0.016(10) C6D 0.089(11) 0.109(12) 0.113(12) 0.056(10) -0.025(9) -0.036(9) C7D 0.060(6) 0.045(5) 0.059(6) -0.007(4) 0.019(5) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1A N3A 1.865(5) . ? Ni1A N4A 1.869(5) . ? Ni1A N2A 1.873(5) . ? Ni1A N1A 1.879(5) . ? N1A C2A 1.347(8) . ? N1A C22A 1.410(8) . ? N2A C4A 1.346(8) . ? N2A C6A 1.408(8) . ? N3A C12A 1.362(8) . ? N3A C11A 1.407(8) . ? N4A C15A 1.353(8) . ? N4A C17A 1.420(8) . ? C1A C2A 1.519(9) . ? C2A C3A 1.381(9) . ? C3A C4A 1.394(10) . ? C4A C5A 1.512(9) . ? C6A C7A 1.399(9) . ? C6A C11A 1.422(9) . ? C7A C8A 1.390(10) . ? C8A C9A 1.385(10) . ? C9A C10A 1.396(9) . ? C10A C11A 1.390(9) . ? C12A C14A 1.391(9) . ? C12A C13A 1.521(9) . ? C14A C15A 1.400(9) . ? C15A C16A 1.506(9) . ? C17A C18A 1.386(9) . ? C17A C22A 1.418(9) . ? C18A C19A 1.386(10) . ? C19A C20A 1.377(11) . ? C20A C21A 1.379(10) . ? C21A C22A 1.388(9) . ? Ni1B N2B 1.871(5) . ? Ni1B N4B 1.874(5) . ? Ni1B N1B 1.873(5) . ? Ni1B N3B 1.875(5) . ? N1B C2B 1.364(8) . ? N1B C22B 1.386(8) . ? N2B C4B 1.347(8) . ? N2B C6B 1.408(8) . ? N3B C12B 1.367(8) . ? N3B C11B 1.410(8) . ? N4B C15B 1.345(8) . ? N4B C17B 1.411(9) . ? C1B C2B 1.514(9) . ? C2B C3B 1.386(9) . ? C3B C4B 1.390(9) . ? C4B C5B 1.507(8) . ? C6B C7B 1.395(9) . ? C6B C11B 1.422(9) . ? C7B C8B 1.391(10) . ? C8B C9B 1.395(11) . ? C9B C10B 1.387(10) . ? C10B C11B 1.392(9) . ? C12B C14B 1.385(9) . ? C12B C13B 1.497(9) . ? C14B C15B 1.402(9) . ? C15B C16B 1.504(9) . ? C17B C18B 1.386(9) . ? C17B C22B 1.428(9) . ? C18B C19B 1.380(10) . ? C19B C20B 1.390(11) . ? C20B C21B 1.396(9) . ? C21B C22B 1.390(10) . ? C1C C2C 1.51(2) . ? C2C C7C 1.351(14) . ? C2C C3C 1.423(14) . ? C3C C4C 1.43(2) . ? C4C C5C 1.39(2) . ? C5C C6C 1.30(2) . ? C6C C7C 1.38(2) . ? C1D C2D 1.48(2) . ? C2D C7D 1.342(13) . ? C2D C3D 1.36(2) . ? C3D C4D 1.39(2) . ? C4D C5D 1.47(3) . ? C5D C6D 1.28(2) . ? C6D C7D 1.37(2) . ? 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 N3A Ni1A N4A 95.0(2) . . ? N3A Ni1A N2A 84.9(2) . . ? N4A Ni1A N2A 178.6(2) . . ? N3A Ni1A N1A 178.7(2) . . ? N4A Ni1A N1A 84.7(2) . . ? N2A Ni1A N1A 95.3(2) . . ? C2A N1A C22A 124.4(6) . . ? C2A N1A Ni1A 123.3(4) . . ? C22A N1A Ni1A 112.0(4) . . ? C4A N2A C6A 124.4(5) . . ? C4A N2A Ni1A 123.7(5) . . ? C6A N2A Ni1A 111.5(4) . . ? C12A N3A C11A 124.0(5) . . ? C12A N3A Ni1A 123.2(4) . . ? C11A N3A Ni1A 112.3(4) . . ? C15A N4A C17A 123.7(6) . . ? C15A N4A Ni1A 123.6(5) . . ? C17A N4A Ni1A 111.9(4) . . ? N1A C2A C3A 121.7(6) . . ? N1A C2A C1A 121.9(6) . . ? C3A C2A C1A 116.4(6) . . ? C2A C3A C4A 128.9(6) . . ? N2A C4A C3A 120.9(6) . . ? N2A C4A C5A 122.0(6) . . ? C3A C4A C5A 117.1(6) . . ? C7A C6A N2A 127.3(6) . . ? C7A C6A C11A 118.4(6) . . ? N2A C6A C11A 113.7(5) . . ? C8A C7A C6A 121.1(6) . . ? C9A C8A C7A 120.3(6) . . ? C8A C9A C10A 119.4(7) . . ? C11A C10A C9A 121.1(7) . . ? C10A C11A N3A 127.8(6) . . ? C10A C11A C6A 119.5(6) . . ? N3A C11A C6A 112.3(6) . . ? N3A C12A C14A 121.8(6) . . ? N3A C12A C13A 121.7(6) . . ? C14A C12A C13A 116.5(6) . . ? C12A C14A C15A 127.6(6) . . ? N4A C15A C14A 120.9(6) . . ? N4A C15A C16A 122.6(6) . . ? C14A C15A C16A 116.5(6) . . ? C18A C17A C22A 120.8(6) . . ? C18A C17A N4A 125.7(6) . . ? C22A C17A N4A 113.1(6) . . ? C17A C18A C19A 119.7(7) . . ? C20A C19A C18A 119.8(7) . . ? C19A C20A C21A 121.0(7) . . ? C20A C21A C22A 120.8(7) . . ? C21A C22A N1A 129.0(6) . . ? C21A C22A C17A 117.8(6) . . ? N1A C22A C17A 113.0(6) . . ? N2B Ni1B N4B 178.8(2) . . ? N2B Ni1B N1B 95.7(2) . . ? N4B Ni1B N1B 84.6(2) . . ? N2B Ni1B N3B 84.7(2) . . ? N4B Ni1B N3B 95.0(2) . . ? N1B Ni1B N3B 178.9(2) . . ? C2B N1B C22B 124.1(6) . . ? C2B N1B Ni1B 122.8(4) . . ? C22B N1B Ni1B 112.7(4) . . ? C4B N2B C6B 124.5(5) . . ? C4B N2B Ni1B 123.6(4) . . ? C6B N2B Ni1B 111.4(4) . . ? C12B N3B C11B 123.9(6) . . ? C12B N3B Ni1B 123.4(4) . . ? C11B N3B Ni1B 112.4(4) . . ? C15B N4B C17B 124.6(5) . . ? C15B N4B Ni1B 123.2(4) . . ? C17B N4B Ni1B 111.5(4) . . ? N1B C2B C3B 121.2(6) . . ? N1B C2B C1B 122.2(6) . . ? C3B C2B C1B 116.7(6) . . ? C2B C3B C4B 129.2(6) . . ? N2B C4B C3B 120.9(6) . . ? N2B C4B C5B 122.9(6) . . ? C3B C4B C5B 116.1(6) . . ? C7B C6B N2B 126.7(6) . . ? C7B C6B C11B 118.7(6) . . ? N2B C6B C11B 114.2(5) . . ? C8B C7B C6B 120.6(7) . . ? C7B C8B C9B 120.5(6) . . ? C10B C9B C8B 119.6(7) . . ? C9B C10B C11B 120.8(7) . . ? C10B C11B N3B 128.1(6) . . ? C10B C11B C6B 119.8(6) . . ? N3B C11B C6B 111.8(6) . . ? N3B C12B C14B 121.1(6) . . ? N3B C12B C13B 122.4(6) . . ? C14B C12B C13B 116.5(6) . . ? C12B C14B C15B 128.1(6) . . ? N4B C15B C14B 121.4(6) . . ? N4B C15B C16B 121.8(6) . . ? C14B C15B C16B 116.7(6) . . ? C18B C17B N4B 126.5(6) . . ? C18B C17B C22B 120.2(6) . . ? N4B C17B C22B 112.9(6) . . ? C19B C18B C17B 121.3(7) . . ? C18B C19B C20B 119.5(7) . . ? C19B C20B C21B 119.5(7) . . ? C22B C21B C20B 122.3(7) . . ? N1B C22B C21B 129.6(6) . . ? N1B C22B C17B 113.1(6) . . ? C21B C22B C17B 117.0(6) . . ? C7C C2C C3C 116.4(12) . . ? C7C C2C C1C 124.1(12) . . ? C3C C2C C1C 119.6(13) . . ? C4C C3C C2C 116.6(13) . . ? C5C C4C C3C 122.5(12) . . ? C6C C5C C4C 118.7(17) . . ? C5C C6C C7C 120.4(18) . . ? C2C C7C C6C 125.4(12) . . ? C7D C2D C3D 119.5(13) . . ? C7D C2D C1D 122.9(12) . . ? C3D C2D C1D 117.6(14) . . ? C2D C3D C4D 117.1(15) . . ? C3D C4D C5D 122.3(15) . . ? C6D C5D C4D 115.2(20) . . ? C5D C6D C7D 122.5(20) . . ? C2D C7D C6D 123.2(13) . . ? _refine_diff_density_max 1.263 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.111 #=END data_Zntmtaa _audit_creation_date 97-09-22 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical Zn2_C22_H22_N4 _chemical_formula_moiety ? _chemical_formula_structural [Zn(C22H22N4)]2 _chemical_formula_sum C44_H44_Zn2_N8 _chemical_formula_weight 815.67 _chemical_melting_point ? _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 14.107(6) _cell_length_b 16.371(8) _cell_length_c 16.670(7) _cell_angle_alpha 90.00000 _cell_angle_beta 99.94(3) _cell_angle_gamma 90.00000 _cell_volume 3792(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 20.4 _cell_measurement_theta_max 21.0 _cell_special_details ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description ? _exptl_crystal_preparation ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1696 _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_coefficient_mu 1.31 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.78 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _diffrn_measurement_device CAD4 _diffrn_measurement_method 2theta/theta _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 8 10 -11 -8 10 11 -8 -10 11 8 -10 -11 8 9 8 8 -9 8 -8 -9 -8 -8 9 -8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 7212 _diffrn_reflns_av_R_equivalents .037 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_reduction_process equatorial_monochr_Lp loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 176 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 0 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 176 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Zn ? 0 8 .222 1.431 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 32 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Zn1 .29378(4) .51782(3) .37684(3) .0408(3) Uani ? ? C10 .3211(3) .4255(3) .2124(3) .040(3) Uani ? ? C11 .3823(3) .4935(3) .2331(3) .038(2) Uani ? ? C111 .4642(5) .4986(4) .1855(4) .058(4) Uani ? ? N11 .3724(3) .5454(2) .2916(2) .036(2) Uani ? ? C12 .4284(3) .6152(3) .3151(3) .037(3) Uani ? ? C13 .4647(4) .6670(3) .2608(3) .046(3) Uani ? ? C14 .5144(4) .7378(3) .2885(4) .052(3) Uani ? ? C15 .5248(4) .7578(3) .3690(4) .053(3) Uani ? ? C16 .4843(4) .7101(3) .4222(3) .043(3) Uani ? ? C17 .4375(3) .6380(3) .3984(3) .037(3) Uani ? ? N18 .3886(3) .5878(2) .4465(2) .037(2) Uani ? ? C18 .4131(4) .5743(3) .5264(3) .041(3) Uani ? ? C181 .5032(5) .6102(4) .5760(4) .052(4) Uani ? ? C10' .3612(4) .5224(3) .5695(3) .046(3) Uani ? ? C11' .2490(4) .3907(3) .2515(3) .040(3) Uani ? ? C111' .2137(5) .3079(4) .2217(4) .052(4) Uani ? ? N11' .2205(3) .4272(2) .3142(2) .039(2) Uani ? ? C12' .1425(3) .4041(3) .3523(3) .041(3) Uani ? ? C13' .0582(4) .3700(3) .3119(3) .049(3) Uani ? ? C14' -.0200(5) .3598(4) .3507(4) .063(4) Uani ? ? C15' -.0146(5) .3868(4) .4293(4) .064(4) Uani ? ? C16' .0682(4) .4212(3) .4718(4) .053(3) Uani ? ? C17' .1492(3) .4298(3) .4340(3) .040(3) Uani ? ? N18' .2325(3) .4740(2) .4667(2) .042(2) Uani ? ? C18' .2779(4) .4742(3) .5428(3) .045(3) Uani ? ? C181' .2491(7) .4171(5) .6060(5) .073(5) Uani ? ? Zn2 .19971(4) .51006(3) .10726(3) .0433(3) Uani ? ? C20 -.0073(4) .4251(3) .0858(4) .053(3) Uani ? ? C21 .0541(4) .3887(3) .0390(3) .045(3) Uani ? ? C211 .0091(6) .3248(4) -.0210(5) .066(5) Uani ? ? N21 .1455(3) .4113(2) .0443(2) .041(2) Uani ? ? C22 .2147(4) .3796(3) .0006(3) .043(3) Uani ? ? C23 .2214(5) .2990(3) -.0235(4) .056(4) Uani ? ? C24 .2948(5) .2726(4) -.0624(4) .062(4) Uani ? ? C25 .3648(5) .3263(4) -.0750(4) .062(4) Uani ? ? C26 .3627(4) .4058(4) -.0484(3) .052(3) Uani ? ? C27 .2880(4) .4344(3) -.0121(3) .042(3) Uani ? ? N28 .2835(3) .5138(2) .0206(2) .041(2) Uani ? ? C28 .3098(3) .5827(3) -.0099(3) .044(3) Uani ? ? C281 .3418(6) .5869(5) -.0912(5) .066(4) Uani ? ? C20' .3031(4) .6583(3) .0284(3) .047(3) Uani ? ? C21' .0046(4) .4898(3) .1420(3) .050(3) Uani ? ? N21' .0885(3) .5259(2) .1652(2) .045(2) Uani ? ? C211' -.0861(5) .5163(6) .1705(5) .067(5) Uani ? ? C22' .1088(3) .5886(3) .2223(3) .045(3) Uani ? ? C23' .0720(5) .5967(4) .2941(4) .061(4) Uani ? ? C24' .1020(5) .6564(4) .3503(4) .070(4) Uani ? ? C25' .1722(5) .7101(4) .3381(4) .069(4) Uani ? ? C26' .2137(4) .7027(4) .2693(4) .056(4) Uani ? ? C27' .1835(3) .6444(3) .2099(3) .042(3) Uani ? ? C28' .2640(3) .6817(3) .0962(3) .044(3) Uani ? ? C281' .2606(6) .7726(4) .1097(5) .067(4) Uani ? ? N28' .2267(3) .6275(2) .1418(2) .042(2) Uani ? ? H10 .339(3) .393(2) .177(2) .023(11) Uiso ? ? H111a .478(4) .443(4) .167(3) .074(18) Uiso ? ? H111b .448(4) .537(3) .141(4) .08(2) Uiso ? ? H111c .518(4) .523(3) .217(3) .050(15) Uiso ? ? H13 .441(3) .655(2) .202(2) .025(11) Uiso ? ? H14 .528(4) .771(3) .249(3) .069(18) Uiso ? ? H15 .555(3) .803(3) .385(3) .036(13) Uiso ? ? H16 .484(3) .729(2) .477(2) .021(10) Uiso ? ? H181a .518(4) .575(4) .621(4) .08(2) Uiso ? ? H181b .556(4) .612(3) .553(3) .056(18) Uiso ? ? H181c .486(3) .664(3) .591(2) .035(13) Uiso ? ? H10' .389(3) .513(2) .631(3) .034(11) Uiso ? ? H111'a .162(4) .315(3) .177(3) .059(17) Uiso ? ? H111'b .260(4) .280(4) .206(4) .08(2) Uiso ? ? H111'c .192(4) .275(3) .265(3) .061(16) Uiso ? ? H13' .051(3) .358(3) .256(3) .041(14) Uiso ? ? H14' -.078(4) .342(3) .321(3) .050(15) Uiso ? ? H15' -.062(4) .384(3) .455(3) .062(17) Uiso ? ? H16' .078(3) .438(3) .528(3) .043(14) Uiso ? ? H181'a .196(5) .447(4) .626(4) .11(3) Uiso ? ? H181'b .209(5) .372(4) .579(4) .12(3) Uiso ? ? H181'c .292(4) .412(4) .646(4) .07(2) Uiso ? ? H20 -.070(4) .408(3) .072(3) .055(16) Uiso ? ? H211a -.056(5) .329(4) -.029(4) .09(2) Uiso ? ? H211b .030(5) .266(4) .012(4) .12(2) Uiso ? ? H211c .024(5) .325(4) -.069(4) .09(3) Uiso ? ? H23 .180(4) .267(3) -.013(3) .052(17) Uiso ? ? H24 .298(4) .217(3) -.077(3) .057(16) Uiso ? ? H25 .409(4) .313(4) -.102(4) .09(2) Uiso ? ? H26 .407(3) .438(3) -.047(3) .038(15) Uiso ? ? H281a .319(5) .639(5) -.118(4) .12(3) Uiso ? ? H281b .307(4) .550(3) -.132(3) .058(17) Uiso ? ? H281c .403(5) .574(4) -.084(4) .09(2) Uiso ? ? H20' .318(3) .695(2) .001(2) .027(12) Uiso ? ? H211'a -.129(5) .513(4) .138(4) .08(3) Uiso ? ? H211'b -.085(3) .568(3) .183(3) .038(16) Uiso ? ? H211'c -.092(4) .498(3) .229(4) .075(18) Uiso ? ? H23' .031(3) .555(3) .304(2) .031(12) Uiso ? ? H24' .076(5) .662(4) .394(4) .09(2) Uiso ? ? H25' .192(4) .753(3) .375(3) .061(17) Uiso ? ? H26' .258(3) .735(3) .264(3) .040(15) Uiso ? ? H281'a .315(5) .785(4) .155(4) .09(2) Uiso ? ? H281'b .215(4) .786(3) .132(3) .049(17) Uiso ? ? H281'c .261(4) .804(3) .061(3) .069(19) Uiso ? ? 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 Zn1 .0433(4) .0416(3) .0400(3) -.0041(3) .0141(3) .0010(3) C10 .038(3) .049(3) .034(3) .005(2) .006(2) -.006(2) C11 .031(2) .046(3) .038(3) .003(2) .007(2) .003(2) C111 .050(4) .064(4) .067(4) -.013(3) .027(3) -.019(4) N11 .038(2) .038(2) .033(2) -.0019(18) .0093(17) .0000(17) C12 .029(3) .040(3) .043(3) .002(2) .007(2) .004(2) C13 .040(3) .054(3) .045(3) -.003(3) .008(2) .007(3) C14 .049(3) .050(3) .058(4) -.005(3) .014(3) .012(3) C15 .055(4) .036(3) .069(4) -.014(3) .014(3) -.000(3) C16 .049(3) .039(3) .042(3) .000(2) .009(3) -.004(2) C17 .035(3) .033(3) .045(3) .003(2) .010(2) .005(2) N18 .038(2) .033(2) .040(2) .0040(18) .0127(18) .0003(17) C18 .051(3) .033(3) .038(3) .010(2) .005(2) -.003(2) C181 .056(4) .048(4) .050(4) .001(3) .001(3) .001(3) C10' .065(4) .039(3) .034(3) .008(3) .009(2) .005(2) C11' .041(3) .041(3) .037(3) .005(2) .003(2) .003(2) C111' .066(4) .044(3) .048(4) -.003(3) .010(3) -.002(3) N11' .035(2) .042(2) .040(2) -.0050(18) .0075(18) .0028(18) C12' .041(3) .037(3) .046(3) .000(2) .008(2) .009(2) C13' .048(4) .052(3) .047(4) -.011(3) .006(3) .003(3) C14' .052(4) .067(4) .072(4) -.016(3) .013(3) .016(3) C15' .049(4) .068(4) .084(5) -.005(3) .034(4) .014(3) C16' .059(4) .050(3) .057(4) .001(3) .028(3) .005(3) C17' .044(3) .032(3) .049(3) -.002(2) .019(2) .005(2) N18' .051(3) .038(2) .040(2) -.000(2) .019(2) .0040(18) C18' .065(4) .036(3) .039(3) .006(3) .022(3) .006(2) C181' .097(6) .073(5) .049(4) -.024(5) .009(4) .015(4) Zn2 .0419(4) .0409(3) .0505(4) -.0073(3) .0172(3) -.0024(3) C20 .040(3) .053(4) .063(4) -.009(3) .003(3) .025(3) C21 .042(3) .040(3) .048(3) -.006(2) -.003(2) .015(2) C211 .058(5) .059(4) .072(6) -.017(3) -.011(4) .001(4) N21 .041(3) .038(2) .044(2) -.005(2) .004(2) .0030(18) C22 .045(3) .039(3) .042(3) -.002(2) -.000(2) .001(2) C23 .057(4) .044(4) .062(4) -.006(3) -.004(3) .001(3) C24 .079(5) .048(4) .055(4) .009(4) -.002(3) -.005(3) C25 .082(5) .060(4) .048(4) .018(4) .023(3) -.005(3) C26 .057(4) .050(4) .051(3) .002(3) .016(3) .002(3) C27 .053(3) .042(3) .031(3) .003(2) .004(2) .002(2) N28 .042(2) .041(2) .041(2) -.003(2) .0134(18) .0041(19) C28 .033(3) .049(3) .055(3) .002(2) .015(2) .005(3) C281 .079(5) .061(4) .065(5) .009(4) .036(4) .009(4) C20' .044(3) .039(3) .061(4) -.006(3) .019(3) .011(3) C21' .036(3) .053(3) .062(3) .001(3) .015(2) .027(3) N21' .041(3) .042(2) .054(3) -.000(2) .015(2) .006(2) C211' .046(4) .089(6) .067(5) .006(4) .012(3) .019(4) C22' .039(3) .047(3) .052(3) .017(2) .017(3) .011(3) C23' .067(4) .057(4) .065(4) .006(3) .028(3) .009(3) C24' .080(5) .084(5) .054(4) .013(4) .029(4) -.003(4) C25' .070(5) .081(5) .056(4) .008(4) .009(3) -.017(4) C26' .044(4) .057(4) .069(4) .002(3) .013(3) -.008(3) C27' .036(3) .041(3) .050(3) .013(2) .009(2) .001(2) C28' .033(3) .040(3) .059(3) .002(2) .011(2) .005(2) C281' .076(5) .038(3) .097(6) .006(3) .045(5) .001(4) N28' .036(2) .041(2) .051(3) .0022(18) .012(2) -.000(2) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1279(422) _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 4047 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .082 _refine_ls_R_factor_obs .041 _refine_ls_wR_factor_all .064 _refine_ls_wR_factor_obs .049 _refine_ls_goodness_of_fit_all 1.234 _refine_ls_goodness_of_fit_obs 1.268 _refine_ls_shift/esd_max .042 _refine_ls_shift/esd_mean .001 _refine_diff_density_min -.42 _refine_diff_density_max .539 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N11 1.999(4) . . ? Zn1 N18 1.979(4) . . ? Zn1 N11' 1.997(4) . . ? Zn1 N18' 1.989(4) . . ? C10 C11 1.415(7) . . ? C10 C11' 1.418(7) . . ? C10 Zn2 2.625(5) . . ? C10 H10 .87(4) . . ? C11 C111 1.512(9) . . ? C11 N11 1.319(6) . . ? C111 H111a .99(6) . . ? C111 H111b .98(6) . . ? C111 H111c .94(5) . . ? N11 C12 1.406(6) . . ? C12 C13 1.400(7) . . ? C12 C17 1.422(7) . . ? C13 C14 1.392(7) . . ? C13 H13 1.00(4) . . ? C14 C15 1.365(9) . . ? C14 H14 .90(6) . . ? C15 C16 1.377(8) . . ? C15 H15 .87(4) . . ? C16 C17 1.378(7) . . ? C16 H16 .96(4) . . ? C17 N18 1.409(6) . . ? N18 C18 1.335(6) . . ? C18 C181 1.511(8) . . ? C18 C10' 1.397(7) . . ? C181 H181a .94(6) . . ? C181 H181b .90(6) . . ? C181 H181c .96(5) . . ? C10' C18' 1.422(7) . . ? C10' H10' 1.04(4) . . ? C11' C111' 1.499(8) . . ? C11' N11' 1.326(6) . . ? C111' H111'a .96(5) . . ? C111' H111'b .88(6) . . ? C111' H111'c 1.00(5) . . ? N11' C12' 1.413(7) . . ? C12' C13' 1.380(7) . . ? C12' C17' 1.414(7) . . ? C13' C14' 1.382(9) . . ? C13' H13' .94(5) . . ? C14' C15' 1.371(10) . . ? C14' H14' .93(5) . . ? C15' C16' 1.379(8) . . ? C15' H15' .86(6) . . ? C16' C17' 1.404(8) . . ? C16' H16' .96(5) . . ? C17' N18' 1.407(6) . . ? N18' C18' 1.318(6) . . ? C18' C181' 1.516(10) . . ? C181' H181'a 1.00(7) . . ? C181' H181'b .99(7) . . ? C181' H181'c .82(6) . . ? Zn2 N21 2.006(4) . . ? Zn2 N28 2.018(4) . . ? Zn2 N21' 1.996(4) . . ? Zn2 N28' 2.024(4) . . ? C20 C21 1.396(8) . . ? C20 C21' 1.404(8) . . ? C20 H20 .92(5) . . ? C21 C211 1.509(9) . . ? C21 N21 1.330(7) . . ? C211 H211a .90(7) . . ? C211 H211b 1.13(7) . . ? C211 H211c .86(7) . . ? N21 C22 1.414(7) . . ? C22 C23 1.387(7) . . ? C22 C27 1.412(7) . . ? C23 C24 1.383(10) . . ? C23 H23 .83(5) . . ? C24 C25 1.365(10) . . ? C24 H24 .95(5) . . ? C25 C26 1.377(9) . . ? C25 H25 .85(7) . . ? C26 C27 1.385(8) . . ? C26 H26 .82(5) . . ? C27 N28 1.415(6) . . ? N28 C28 1.317(6) . . ? C28 C281 1.502(10) . . ? C28 C20' 1.403(7) . . ? C281 H281a .99(7) . . ? C281 H281b .98(5) . . ? C281 H281c .88(7) . . ? C20' C28' 1.394(8) . . ? C20' H20' .81(4) . . ? C21' N21' 1.320(6) . . ? C21' C211' 1.503(10) . . ? N21' C22' 1.395(6) . . ? C211' H211'a .74(6) . . ? C211' H211'b .87(5) . . ? C211' H211'c 1.04(6) . . ? C22' C23' 1.392(9) . . ? C22' C27' 1.436(7) . . ? C23' C24' 1.370(9) . . ? C23' H23' .94(4) . . ? C24' C25' 1.366(11) . . ? C24' H24' .87(7) . . ? C25' C26' 1.381(10) . . ? C25' H25' .95(5) . . ? C26' C27' 1.387(8) . . ? C26' H26' .83(5) . . ? C27' N28' 1.406(7) . . ? C28' C281' 1.508(8) . . ? C28' N28' 1.335(7) . . ? C281' H281'a 1.00(6) . . ? C281' H281'b .83(6) . . ? C281' H281'c .96(6) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Zn1 C10 3.211(5) . . ? Zn1 C11 2.915(5) . . ? Zn1 C12 2.808(5) . . ? Zn1 C17 2.803(5) . . ? Zn1 C18 2.908(5) . . ? Zn1 C181 3.526(7) . 3_666 ? Zn1 C10' 3.188(5) . . ? Zn1 C11' 2.940(5) . . ? Zn1 C12' 2.808(5) . . ? Zn1 C17' 2.795(5) . . ? Zn1 C18' 2.903(5) . . ? Zn1 Zn2 4.462(2) . . ? Zn1 C22' 3.532(5) . . ? Zn1 C23' 3.446(6) . . ? Zn1 C24' 3.501(7) . . ? Zn1 C25' 3.590(7) . . ? Zn1 C26' 3.599(6) . . ? Zn1 C27' 3.601(5) . . ? Zn1 H181a 3.05(6) . 3_666 ? Zn1 H181b 3.08(5) . 3_666 ? C10 C111 2.454(9) . . ? C10 N11 2.406(6) . . ? C10 C111' 2.472(8) . . ? C10 N11' 2.392(7) . . ? C10 H111a 2.47(6) . . ? C10 H111'b 2.54(6) . . ? C11 C12 2.440(6) . . ? C11 C11' 2.581(7) . . ? C11 Zn2 3.040(4) . . ? C11 H10 1.94(4) . . ? C11 H111a 2.06(6) . . ? C11 H111b 2.06(6) . . ? C11 H111c 2.04(5) . . ? C111 N11 2.487(8) . . ? C111 C12 2.991(9) . . ? C111 Zn2 3.739(7) . . ? C111 H10 2.46(4) . . ? C111 H13 2.60(4) . . ? N11 C13 2.480(7) . . ? N11 C17 2.397(6) . . ? N11 N18 2.647(5) . . ? N11 N11' 2.959(5) . . ? N11 Zn2 3.623(4) . . ? N11 H111c 2.60(5) . . ? N11 H13 2.61(4) . . ? C12 C14 2.426(7) . . ? C12 C15 2.772(7) . . ? C12 C16 2.395(7) . . ? C12 N18 2.397(6) . . ? C12 H111c 2.69(5) . . ? C12 H13 2.02(4) . . ? C13 C15 2.378(8) . . ? C13 C16 2.748(8) . . ? C13 C17 2.436(8) . . ? C13 H111c 2.61(5) . . ? C13 H14 1.95(5) . . ? C14 C16 2.383(8) . . ? C14 C17 2.809(8) . . ? C14 H13 2.12(4) . . ? C14 H15 1.93(4) . . ? C15 C17 2.412(7) . . ? C15 H14 2.02(5) . . ? C15 H16 2.03(4) . . ? C16 N18 2.488(6) . . ? C16 H15 1.97(5) . . ? C17 C18 2.453(7) . . ? C17 C181 2.982(8) . . ? C17 H16 2.01(4) . . ? N18 C181 2.491(7) . . ? N18 C10' 2.402(6) . . ? N18 N18' 2.948(6) . . ? N18 H16 2.68(4) . . ? C18 C18' 2.564(7) . . ? C18 H181a 1.97(5) . . ? C18 H181b 2.07(5) . . ? C18 H181c 2.00(4) . . ? C18 H10' 2.09(4) . . ? C181 C10' 2.452(9) . . ? C181 H16 2.54(4) . . ? C181 H10' 2.54(4) . . ? C10' N18' 2.405(6) . . ? C10' C181' 2.485(11) . . ? C10' H181a 2.40(6) . . ? C10' H181'c 2.50(6) . . ? C11' C12' 2.450(7) . . ? C11' Zn2 3.083(5) . . ? C11' H10 1.92(4) . . ? C11' H111'a 2.02(5) . . ? C11' H111'b 1.99(6) . . ? C11' H111'c 2.09(5) . . ? C111' N11' 2.480(7) . . ? C111' C12' 2.996(9) . . ? C111' Zn2 3.809(6) . . ? C111' H10 2.46(4) . . ? C111' H13' 2.60(5) . . ? N11' C13' 2.469(7) . . ? N11' C17' 2.387(7) . . ? N11' N18' 2.634(5) . . ? N11' Zn2 3.671(4) . . ? N11' H111'c 2.64(5) . . ? N11' H13' 2.67(4) . . ? C12' C14' 2.401(8) . . ? C12' C15' 2.762(9) . . ? C12' C16' 2.423(8) . . ? C12' N18' 2.393(6) . . ? C12' H13' 2.02(4) . . ? C13' C15' 2.378(10) . . ? C13' C16' 2.776(8) . . ? C13' C17' 2.419(7) . . ? C13' H111'c 2.66(5) . . ? C13' H14' 2.01(5) . . ? C14' C16' 2.401(8) . . ? C14' C17' 2.792(8) . . ? C14' H13' 2.01(5) . . ? C14' H15' 1.97(6) . . ? C15' C17' 2.404(8) . . ? C15' H14' 2.01(4) . . ? C15' H16' 2.09(4) . . ? C16' N18' 2.488(7) . . ? C16' H15' 1.91(6) . . ? C16' H181'b 2.55(7) . . ? C17' C18' 2.444(6) . . ? C17' C181' 2.976(9) . . ? C17' H16' 2.00(5) . . ? C17' H181'b 2.59(7) . . ? N18' C181' 2.475(9) . . ? N18' H16' 2.63(5) . . ? N18' H181'b 2.56(7) . . ? C18' H10' 2.06(4) . . ? C18' H181'a 2.01(7) . . ? C18' H181'b 2.07(8) . . ? C18' H181'c 1.98(6) . . ? C181' H10' 2.50(4) . . ? C181' H16' 2.56(4) . . ? Zn2 C20 3.198(6) . . ? Zn2 C21 2.942(5) . . ? Zn2 C22 2.810(5) . . ? Zn2 C27 2.810(5) . . ? Zn2 C28 2.947(5) . . ? Zn2 C20' 3.226(6) . . ? Zn2 C21' 2.928(6) . . ? Zn2 C22' 2.797(5) . . ? Zn2 C27' 2.821(5) . . ? Zn2 C28' 2.967(5) . . ? Zn2 H10 2.84(4) . . ? Zn2 H111b 3.48(6) . . ? Zn2 H111'a 3.48(5) . . ? Zn2 H20 3.49(5) . 3_565 ? Zn2 H211a 3.45(6) . 3_565 ? C20 C211 2.463(10) . . ? C20 N21 2.385(8) . . ? C20 N21' 2.383(7) . . ? C20 C211' 2.449(11) . . ? C20 H211a 2.48(6) . . ? C20 H211'a 2.51(7) . . ? C21 C22 2.464(8) . . ? C21 C21' 2.567(8) . . ? C21 H20 1.95(5) . . ? C21 H211a 2.01(6) . . ? C21 H211b 2.08(7) . . ? C21 H211c 2.06(6) . . ? C211 N21 2.483(8) . . ? C211 C22 2.998(10) . . ? C211 H20 2.48(5) . . ? C211 H23 2.57(5) . . ? N21 C23 2.495(7) . . ? N21 C27 2.391(7) . . ? N21 N28 2.650(6) . . ? N21 N21' 2.964(6) . . ? N21 H111'a 2.69(5) . . ? N21 H23 2.63(5) . . ? C22 C24 2.421(8) . . ? C22 C25 2.785(9) . . ? C22 C26 2.408(8) . . ? C22 N28 2.401(6) . . ? C22 H23 1.91(5) . . ? C23 C25 2.373(10) . . ? C23 C26 2.737(9) . . ? C23 C27 2.402(8) . . ? C23 H24 2.03(5) . . ? C24 C26 2.377(9) . . ? C24 C27 2.786(8) . . ? C24 H23 1.94(6) . . ? C24 H25 1.96(7) . . ? C25 C27 2.409(8) . . ? C25 H24 2.02(5) . . ? C25 H26 1.96(5) . . ? C26 N28 2.479(7) . . ? C26 H25 1.93(6) . . ? C27 C28 2.447(7) . . ? C27 C281 2.983(9) . . ? C27 H26 1.88(5) . . ? N28 C281 2.473(9) . . ? N28 C20' 2.383(7) . . ? N28 N28' 2.957(6) . . ? N28 H26 2.56(5) . . ? N28 H281b 2.70(5) . . ? C28 C28' 2.562(7) . . ? C28 H281a 2.04(7) . . ? C28 H281b 2.11(5) . . ? C28 H281c 1.96(7) . . ? C28 H20' 1.85(4) . . ? C281 C20' 2.452(10) . . ? C281 H26 2.66(5) . . ? C281 H20' 2.40(4) . . ? C20' C281' 2.446(10) . . ? C20' N28' 2.387(7) . . ? C20' H281a 2.50(7) . . ? C20' H281'c 2.54(6) . . ? C21' C22' 2.426(7) . . ? C21' H20 1.95(5) . . ? C21' H211'a 1.92(7) . . ? C21' H211'b 2.00(5) . . ? C21' H211'c 2.16(6) . . ? N21' C211' 2.485(9) . . ? N21' C23' 2.489(8) . . ? N21' C27' 2.403(6) . . ? N21' N28' 2.642(6) . . ? N21' H211'b 2.61(5) . . ? N21' H23' 2.63(4) . . ? C211' C22' 2.980(9) . . ? C211' H20 2.45(5) . . ? C211' H23' 2.61(4) . . ? C22' C24' 2.423(9) . . ? C22' C25' 2.810(8) . . ? C22' C26' 2.427(8) . . ? C22' N28' 2.396(7) . . ? C22' H23' 1.98(5) . . ? C23' C25' 2.373(9) . . ? C23' C26' 2.732(9) . . ? C23' C27' 2.412(9) . . ? C23' H211'b 2.67(4) . . ? C23' H24' 1.96(6) . . ? C24' C26' 2.370(10) . . ? C24' C27' 2.787(9) . . ? C24' H23' 2.03(4) . . ? C24' H25' 2.03(5) . . ? C25' C27' 2.422(8) . . ? C25' H24' 1.94(7) . . ? C25' H26' 1.92(5) . . ? C26' N28' 2.489(8) . . ? C26' H25' 2.02(5) . . ? C26' H281'b 2.66(5) . . ? C27' C28' 2.450(8) . . ? C27' H26' 1.94(5) . . ? C28' H20' 1.89(4) . . ? C28' H281'a 2.02(6) . . ? C28' H281'b 1.98(5) . . ? C28' H281'c 2.09(5) . . ? C281' N28' 2.500(8) . . ? C281' H20' 2.47(4) . . ? C281' H26' 2.65(5) . . ? N28' H26' 2.66(5) . . ? N28' H281'b 2.61(5) . . ? H10 H111a 2.16(7) . . ? H10 H111'b 2.26(7) . . ? H111a H111b 1.64(8) . . ? H111a H111c 1.61(7) . . ? H111a H281c 2.37(9) . 3_665 ? H111b H111c 1.49(7) . . ? H111b H13 2.20(7) . . ? H13 H14 2.33(6) . . ? H14 H15 2.29(7) . . ? H15 H16 2.31(6) . . ? H16 H181c 2.18(6) . . ? H181a H181b 1.47(8) . . ? H181a H181c 1.58(7) . . ? H181a H10' 2.12(7) . . ? H181b H181c 1.53(7) . . ? H10' H181'c 2.19(7) . . ? H111'a H111'b 1.49(8) . . ? H111'a H111'c 1.61(7) . . ? H111'a H13' 2.34(8) . . ? H111'b H111'c 1.50(9) . . ? H111'c H13' 2.40(7) . . ? H13' H14' 2.29(7) . . ? H14' H15' 2.31(7) . . ? H14' H281'b 2.39(8) . 2_545 ? H15' H16' 2.31(7) . . ? H16' H181'a 2.13(7) . . ? H16' H181'b 2.18(8) . . ? H181'a H181'b 1.49(10) . . ? H181'a H181'c 1.46(9) . . ? H181'b H181'c 1.62(9) . . ? H20 H211a 2.17(8) . . ? H20 H211'a 2.27(9) . . ? H211a H211b 1.65(9) . . ? H211a H211c 1.40(10) . . ? H211b H211c 1.66(9) . . ? H211b H23 2.23(9) . . ? H23 H24 2.28(8) . . ? H24 H25 2.31(8) . . ? H25 H26 2.25(8) . . ? H26 H281c 2.31(8) . . ? H281a H281b 1.49(9) . . ? H281a H281c 1.62(9) . . ? H281a H20' 2.18(8) . . ? H281b H281c 1.51(8) . . ? H20' H281'c 2.26(7) . . ? H211'a H211'b 1.26(8) . . ? H211'a H211'c 1.53(9) . . ? H211'b H211'c 1.40(7) . . ? H211'b H23' 2.38(6) . . ? H211'c H23' 2.17(7) . . ? H23' H24' 2.31(7) . . ? H24' H25' 2.28(8) . . ? H25' H26' 2.24(7) . . ? H26' H281'a 2.26(8) . . ? H26' H281'b 2.33(7) . . ? H281'a H281'b 1.39(8) . . ? H281'a H281'c 1.66(8) . . ? H281'b H281'c 1.48(8) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Zn1 N18 83.40(16) . . . ? N11 Zn1 N11' 95.54(16) . . . ? N11 Zn1 N18' 169.67(15) . . . ? N18 Zn1 N11' 166.84(15) . . . ? N18 Zn1 N18' 95.96(16) . . . ? N11' Zn1 N18' 82.72(16) . . . ? C11 C10 C11' 131.4(5) . . . ? C11 C10 Zn2 92.7(3) . . . ? C11 C10 H10 115(3) . . . ? C11' C10 Zn2 94.7(3) . . . ? C11' C10 H10 112(3) . . . ? Zn2 C10 H10 96(2) . . . ? C10 C11 C111 113.9(5) . . . ? C10 C11 N11 123.3(4) . . . ? C111 C11 N11 122.8(4) . . . ? C11 C111 H111a 109(3) . . . ? C11 C111 H111b 110(4) . . . ? C11 C111 H111c 110(3) . . . ? H111a C111 H111b 113(5) . . . ? H111a C111 H111c 113(4) . . . ? H111b C111 H111c 102(4) . . . ? Zn1 N11 C11 121.5(3) . . . ? Zn1 N11 C12 109.9(3) . . . ? C11 N11 C12 127.1(4) . . . ? N11 C12 C13 124.3(4) . . . ? N11 C12 C17 115.9(4) . . . ? C13 C12 C17 119.4(4) . . . ? C12 C13 C14 120.7(5) . . . ? C12 C13 H13 114(2) . . . ? C14 C13 H13 124(2) . . . ? C13 C14 C15 119.2(6) . . . ? C13 C14 H14 115(3) . . . ? C15 C14 H14 125(3) . . . ? C14 C15 C16 120.7(5) . . . ? C14 C15 H15 118(3) . . . ? C16 C15 H15 121(3) . . . ? C15 C16 C17 122.2(5) . . . ? C15 C16 H16 120(2) . . . ? C17 C16 H16 118(2) . . . ? C12 C17 C16 117.6(4) . . . ? C12 C17 N18 115.7(4) . . . ? C16 C17 N18 126.4(4) . . . ? Zn1 N18 C17 110.5(3) . . . ? Zn1 N18 C18 121.5(3) . . . ? C17 N18 C18 126.7(4) . . . ? N18 C18 C181 122.0(5) . . . ? N18 C18 C10' 123.0(4) . . . ? C181 C18 C10' 114.9(4) . . . ? C18 C181 H181a 105(3) . . . ? C18 C181 H181b 117(3) . . . ? C18 C181 H181c 106(2) . . . ? H181a C181 H181b 106(5) . . . ? H181a C181 H181c 112(5) . . . ? H181b C181 H181c 111(4) . . . ? C18 C10' C18' 130.9(4) . . . ? C18 C10' H10' 117(2) . . . ? C18' C10' H10' 112(2) . . . ? C10 C11' C111' 115.9(5) . . . ? C10 C11' N11' 121.3(4) . . . ? C111' C11' N11' 122.6(5) . . . ? C11' C111' H111'a 109(3) . . . ? C11' C111' H111'b 111(4) . . . ? C11' C111' H111'c 112(3) . . . ? H111'a C111' H111'b 109(5) . . . ? H111'a C111' H111'c 110(4) . . . ? H111'b C111' H111'c 106(5) . . . ? Zn1 N11' C11' 123.2(3) . . . ? Zn1 N11' C12' 109.7(3) . . . ? C11' N11' C12' 126.8(4) . . . ? N11' C12' C13' 124.2(5) . . . ? N11' C12' C17' 115.2(4) . . . ? C13' C12' C17' 119.9(5) . . . ? C12' C13' C14' 120.7(5) . . . ? C12' C13' H13' 120(3) . . . ? C14' C13' H13' 119(3) . . . ? C13' C14' C15' 119.5(6) . . . ? C13' C14' H14' 119(3) . . . ? C15' C14' H14' 121(3) . . . ? C14' C15' C16' 121.7(7) . . . ? C14' C15' H15' 123(3) . . . ? C16' C15' H15' 115(3) . . . ? C15' C16' C17' 119.6(6) . . . ? C15' C16' H16' 126(3) . . . ? C17' C16' H16' 115(3) . . . ? C12' C17' C16' 118.6(4) . . . ? C12' C17' N18' 116.0(4) . . . ? C16' C17' N18' 124.5(5) . . . ? Zn1 N18' C17' 109.6(3) . . . ? Zn1 N18' C18' 121.4(4) . . . ? C17' N18' C18' 127.5(4) . . . ? C10' C18' N18' 122.7(5) . . . ? C10' C18' C181' 115.5(5) . . . ? N18' C18' C181' 121.6(5) . . . ? C18' C181' H181'a 104(4) . . . ? C18' C181' H181'b 110(4) . . . ? C18' C181' H181'c 112(4) . . . ? H181'a C181' H181'b 96(6) . . . ? H181'a C181' H181'c 105(6) . . . ? H181'b C181' H181'c 126(6) . . . ? C10 Zn2 N21 94.05(15) . . . ? C10 Zn2 N28 95.66(16) . . . ? C10 Zn2 N21' 102.82(16) . . . ? C10 Zn2 N28' 103.99(15) . . . ? N21 Zn2 N28 82.37(16) . . . ? N21 Zn2 N21' 95.57(17) . . . ? N21 Zn2 N28' 161.88(15) . . . ? N28 Zn2 N21' 161.51(15) . . . ? N28 Zn2 N28' 94.06(16) . . . ? N21' Zn2 N28' 82.18(16) . . . ? C21 C20 C21' 132.9(5) . . . ? C21 C20 H20 114(3) . . . ? C21' C20 H20 113(3) . . . ? C20 C21 C211 115.9(5) . . . ? C20 C21 N21 122.1(4) . . . ? C211 C21 N21 121.9(5) . . . ? C21 C211 H211a 110(4) . . . ? C21 C211 H211b 103(3) . . . ? C21 C211 H211c 118(4) . . . ? H211a C211 H211b 108(5) . . . ? H211a C211 H211c 105(6) . . . ? H211b C211 H211c 112(6) . . . ? Zn2 N21 C21 122.5(3) . . . ? Zn2 N21 C22 109.3(3) . . . ? C21 N21 C22 127.7(4) . . . ? N21 C22 C23 125.9(5) . . . ? N21 C22 C27 115.6(4) . . . ? C23 C22 C27 118.2(5) . . . ? C22 C23 C24 121.8(6) . . . ? C22 C23 H23 117(4) . . . ? C24 C23 H23 121(4) . . . ? C23 C24 C25 119.4(6) . . . ? C23 C24 H24 120(3) . . . ? C25 C24 H24 121(3) . . . ? C24 C25 C26 120.2(7) . . . ? C24 C25 H25 122(4) . . . ? C26 C25 H25 118(4) . . . ? C25 C26 C27 121.4(6) . . . ? C25 C26 H26 124(3) . . . ? C27 C26 H26 114(3) . . . ? C22 C27 C26 118.9(5) . . . ? C22 C27 N28 116.3(5) . . . ? C26 C27 N28 124.6(5) . . . ? Zn2 N28 C27 108.6(3) . . . ? Zn2 N28 C28 122.8(3) . . . ? C27 N28 C28 127.1(4) . . . ? N28 C28 C281 122.5(5) . . . ? N28 C28 C20' 122.3(5) . . . ? C281 C28 C20' 115.1(5) . . . ? C28 C281 H281a 109(4) . . . ? C28 C281 H281b 114(3) . . . ? C28 C281 H281c 108(4) . . . ? H281a C281 H281b 98(5) . . . ? H281a C281 H281c 120(6) . . . ? H281b C281 H281c 108(5) . . . ? C28 C20' C28' 132.7(5) . . . ? C28 C20' H20' 110(3) . . . ? C28' C20' H20' 116(3) . . . ? C20 C21' N21' 122.0(5) . . . ? C20 C21' C211' 114.7(5) . . . ? N21' C21' C211' 123.2(5) . . . ? Zn2 N21' C21' 122.7(4) . . . ? Zn2 N21' C22' 109.9(3) . . . ? C21' N21' C22' 126.6(5) . . . ? C21' C211' H211'a 113(6) . . . ? C21' C211' H211'b 112(3) . . . ? C21' C211' H211'c 115(3) . . . ? H211'a C211' H211'b 103(6) . . . ? H211'a C211' H211'c 118(6) . . . ? H211'b C211' H211'c 93(4) . . . ? N21' C22' C23' 126.5(5) . . . ? N21' C22' C27' 116.1(5) . . . ? C23' C22' C27' 117.0(5) . . . ? C22' C23' C24' 122.7(6) . . . ? C22' C23' H23' 115(3) . . . ? C24' C23' H23' 122(3) . . . ? C23' C24' C25' 120.3(7) . . . ? C23' C24' H24' 121(4) . . . ? C25' C24' H24' 119(4) . . . ? C24' C25' C26' 119.3(6) . . . ? C24' C25' H25' 121(3) . . . ? C26' C25' H25' 119(3) . . . ? C25' C26' C27' 122.1(6) . . . ? C25' C26' H26' 118(3) . . . ? C27' C26' H26' 120(3) . . . ? C22' C27' C26' 118.6(5) . . . ? C22' C27' N28' 114.9(4) . . . ? C26' C27' N28' 126.1(5) . . . ? C20' C28' C281' 114.8(5) . . . ? C20' C28' N28' 122.0(5) . . . ? C281' C28' N28' 123.0(6) . . . ? C28' C281' H281'a 106(4) . . . ? C28' C281' H281'b 113(4) . . . ? C28' C281' H281'c 113(3) . . . ? H281'a C281' H281'b 99(5) . . . ? H281'a C281' H281'c 115(5) . . . ? H281'b C281' H281'c 111(5) . . . ? Zn2 N28' C27' 109.3(3) . . . ? Zn2 N28' C28' 122.8(3) . . . ? C27' N28' C28' 126.7(4) . . . ? 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 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_total 6662 _reflns_number_observed 4048 _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .841 _reflns_d_resolution_low 13.895 _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=END data_c60cutmtaa #------------------------------------------------------------------------------ _audit_creation_date '1999-06-23' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 14.5538(6) _cell_length_b 17.5225(8) _cell_length_c 18.3011(7) _cell_angle_alpha 90 _cell_angle_beta 107.8447(9) _cell_angle_gamma 90 _cell_volume 4442.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123K _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'cube' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1126.65 _chemical_formula_analytical ? _chemical_formula_sum 'C82 H22 Cu N4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2284.00 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Enraf-Nonius CCD' _diffrn_measurement_device_type 'Enraf-Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 11332 _reflns_number_total 11332 _reflns_number_gt 2698 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.260 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 4 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 328 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 88 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.2216(1) 0.0601(1) 0.2007(1) 0.0297(6) 1.000 . Uiso d ? N(1) 0.2926(9) 0.1473(7) 0.1840(8) 0.027(4) 1.000 . Uiso d ? N(2) 0.2834(9) 0.0539(7) 0.3102(7) 0.022(3) 1.000 . Uiso d ? N(3) 0.1627(8) 0.0638(8) 0.0919(7) 0.025(3) 1.000 . Uiso d ? N(4) 0.1544(8) -0.0297(6) 0.2152(8) 0.022(4) 1.000 . Uiso d ? C(1) 0.242(1) 0.1820(8) 0.1129(9) 0.020(4) 1.000 . Uiso d ? C(2) 0.250(1) 0.2605(9) 0.097(1) 0.027(5) 1.000 . Uiso d ? C(3) 0.183(1) 0.2909(9) 0.032(1) 0.036(5) 1.000 . Uiso d ? C(4) 0.113(1) 0.2467(8) -0.0175(9) 0.022(4) 1.000 . Uiso d ? C(5) 0.108(1) 0.1698(9) -0.003(1) 0.024(5) 1.000 . Uiso d ? C(6) 0.171(1) 0.1373(9) 0.063(1) 0.026(5) 1.000 . Uiso d ? C(7) 0.229(1) 0.0112(9) 0.344(1) 0.032(5) 1.000 . Uiso d ? C(8) 0.232(1) 0.0126(9) 0.423(1) 0.038(5) 1.000 . Uiso d ? C(9) 0.168(1) -0.0258(9) 0.447(1) 0.037(5) 1.000 . Uiso d ? C(10) 0.093(1) -0.069(1) 0.398(1) 0.052(6) 1.000 . Uiso d ? C(11) 0.089(1) -0.073(1) 0.320(1) 0.048(6) 1.000 . Uiso d ? C(12) 0.157(1) -0.0350(9) 0.293(1) 0.037(5) 1.000 . Uiso d ? C(13) 0.384(1) 0.1605(9) 0.229(1) 0.031(5) 1.000 . Uiso d ? C(14) 0.418(1) 0.1304(9) 0.303(1) 0.029(5) 1.000 . Uiso d ? C(15) 0.371(1) 0.0838(9) 0.341(1) 0.033(5) 1.000 . Uiso d ? C(16) 0.450(1) 0.2005(9) 0.193(1) 0.033(5) 1.000 . Uiso d ? C(17) 0.430(1) 0.066(1) 0.424(1) 0.046(5) 1.000 . Uiso d ? C(18) 0.138(1) -0.0002(8) 0.051(1) 0.019(4) 1.000 . Uiso d ? C(19) 0.122(1) -0.0680(9) 0.0850(9) 0.024(4) 1.000 . Uiso d ? C(20) 0.125(1) -0.0826(9) 0.161(1) 0.027(5) 1.000 . Uiso d ? C(21) 0.131(1) -0.0044(9) -0.032(1) 0.029(5) 1.000 . Uiso d ? C(22) 0.100(1) -0.1632(9) 0.180(1) 0.031(5) 1.000 . Uiso d ? C(23) 0.058(1) 0.148(1) 0.249(1) 0.046(6) 1.000 . Uiso d ? C(24) 0.124(1) 0.211(1) 0.257(1) 0.055(6) 1.000 . Uiso d ? C(25) 0.109(1) 0.267(1) 0.204(1) 0.060(6) 1.000 . Uiso d ? C(26) 0.023(2) 0.266(1) 0.139(1) 0.063(6) 1.000 . Uiso d ? C(27) -0.044(1) 0.205(1) 0.132(1) 0.066(7) 1.000 . Uiso d ? C(28) -0.029(1) 0.145(1) 0.189(1) 0.047(5) 1.000 . Uiso d ? C(29) -0.120(1) 0.125(1) 0.198(1) 0.047(6) 1.000 . Uiso d ? C(30) -0.116(1) 0.105(1) 0.273(1) 0.050(6) 1.000 . Uiso d ? C(31) -0.029(1) 0.108(1) 0.337(1) 0.056(6) 1.000 . Uiso d ? C(32) 0.055(1) 0.128(1) 0.322(1) 0.052(6) 1.000 . Uiso d ? C(33) 0.121(1) 0.178(1) 0.382(1) 0.061(6) 1.000 . Uiso d ? C(34) 0.097(1) 0.205(1) 0.444(1) 0.060(6) 1.000 . Uiso d ? C(35) 0.116(1) 0.286(1) 0.469(1) 0.063(6) 1.000 . Uiso d ? C(36) 0.158(1) 0.331(1) 0.427(1) 0.064(6) 1.000 . Uiso d ? C(37) 0.183(1) 0.302(1) 0.359(1) 0.051(6) 1.000 . Uiso d ? C(38) 0.162(1) 0.224(1) 0.340(1) 0.063(6) 1.000 . Uiso d ? C(39) 0.162(1) 0.365(1) 0.304(1) 0.071(7) 1.000 . Uiso d ? C(40) 0.128(1) 0.429(1) 0.334(1) 0.057(6) 1.000 . Uiso d ? C(41) 0.056(2) 0.474(1) 0.285(1) 0.065(7) 1.000 . Uiso d ? C(42) 0.018(1) 0.456(1) 0.206(1) 0.057(6) 1.000 . Uiso d ? C(43) 0.053(2) 0.392(1) 0.176(1) 0.069(7) 1.000 . Uiso d ? C(44) 0.129(1) 0.345(1) 0.228(1) 0.058(6) 1.000 . Uiso d ? C(45) -0.013(2) 0.342(1) 0.122(1) 0.069(7) 1.000 . Uiso d ? C(46) -0.113(2) 0.358(1) 0.099(1) 0.077(7) 1.000 . Uiso d ? C(47) -0.150(2) 0.426(1) 0.130(1) 0.077(7) 1.000 . Uiso d ? C(48) -0.084(2) 0.469(1) 0.182(1) 0.081(8) 1.000 . Uiso d ? C(49) -0.112(2) 0.499(1) 0.249(1) 0.064(7) 1.000 . Uiso d ? C(50) -0.196(2) 0.479(1) 0.262(1) 0.078(7) 1.000 . Uiso d ? C(51) -0.262(1) 0.428(1) 0.205(1) 0.065(6) 1.000 . Uiso d ? C(52) -0.243(2) 0.402(1) 0.141(1) 0.068(7) 1.000 . Uiso d ? C(53) -0.258(1) 0.320(1) 0.117(1) 0.067(7) 1.000 . Uiso d ? C(54) -0.302(1) 0.275(1) 0.155(1) 0.070(7) 1.000 . Uiso d ? C(55) -0.326(1) 0.303(1) 0.225(1) 0.051(6) 1.000 . Uiso d ? C(56) -0.306(1) 0.380(1) 0.247(1) 0.055(6) 1.000 . Uiso d ? C(57) -0.267(1) 0.396(1) 0.331(1) 0.054(6) 1.000 . Uiso d ? C(58) -0.251(1) 0.341(1) 0.381(1) 0.057(6) 1.000 . Uiso d ? C(59) -0.269(2) 0.259(1) 0.360(1) 0.064(7) 1.000 . Uiso d ? C(60) -0.305(2) 0.247(1) 0.283(2) 0.077(7) 1.000 . Uiso d ? C(61) -0.271(1) 0.178(1) 0.252(1) 0.065(7) 1.000 . Uiso d ? C(62) -0.197(1) 0.133(1) 0.298(1) 0.050(6) 1.000 . Uiso d ? C(63) -0.157(1) 0.149(1) 0.378(1) 0.058(6) 1.000 . Uiso d ? C(64) -0.191(2) 0.213(1) 0.408(1) 0.079(8) 1.000 . Uiso d ? C(65) -0.131(2) 0.263(1) 0.462(1) 0.072(7) 1.000 . Uiso d ? C(66) -0.034(2) 0.248(1) 0.486(1) 0.084(8) 1.000 . Uiso d ? C(67) 0.008(2) 0.184(1) 0.456(1) 0.073(7) 1.000 . Uiso d ? C(68) -0.054(2) 0.135(1) 0.403(1) 0.070(7) 1.000 . Uiso d ? C(69) 0.033(2) 0.310(1) 0.493(1) 0.077(7) 1.000 . Uiso d ? C(70) 0.002(2) 0.384(1) 0.478(1) 0.065(7) 1.000 . Uiso d ? C(71) -0.101(2) 0.400(1) 0.455(1) 0.064(7) 1.000 . Uiso d ? C(72) -0.165(1) 0.341(1) 0.446(1) 0.057(6) 1.000 . Uiso d ? C(73) -0.194(1) 0.174(1) 0.147(1) 0.062(6) 1.000 . Uiso d ? C(74) -0.267(1) 0.197(1) 0.178(1) 0.062(7) 1.000 . Uiso d ? C(75) -0.146(2) 0.222(1) 0.107(1) 0.075(7) 1.000 . Uiso d ? C(76) -0.174(2) 0.300(1) 0.093(1) 0.076(7) 1.000 . Uiso d ? C(77) -0.022(1) 0.501(1) 0.314(1) 0.052(6) 1.000 . Uiso d ? C(78) -0.024(1) 0.483(1) 0.386(1) 0.059(6) 1.000 . Uiso d ? C(79) 0.050(1) 0.434(1) 0.437(1) 0.065(6) 1.000 . Uiso d ? C(80) 0.124(1) 0.411(1) 0.411(1) 0.070(7) 1.000 . Uiso d ? C(81) -0.200(1) 0.460(1) 0.336(1) 0.055(6) 1.000 . Uiso d ? C(82) -0.115(1) 0.459(1) 0.400(1) 0.049(6) 1.000 . Uiso d ? H(1) 0.2990 0.2915 0.1298 0.033 1.000 . Uiso c ? H(2) 0.1862 0.3437 0.0215 0.043 1.000 . Uiso c ? H(3) 0.0682 0.2691 -0.0614 0.026 1.000 . Uiso c ? H(4) 0.0609 0.1389 -0.0377 0.029 1.000 . Uiso c ? H(5) 0.2813 0.0412 0.4593 0.046 1.000 . Uiso c ? H(6) 0.1724 -0.0237 0.5000 0.045 1.000 . Uiso c ? H(7) 0.0468 -0.0943 0.4162 0.063 1.000 . Uiso c ? H(8) 0.0392 -0.1026 0.2853 0.058 1.000 . Uiso c ? H(9) 0.4819 0.1441 0.3318 0.035 1.000 . Uiso c ? H(10) 0.5118 0.2065 0.2295 0.039 1.000 . Uiso c ? H(11) 0.4562 0.1711 0.1507 0.039 1.000 . Uiso c ? H(12) 0.4245 0.2493 0.1746 0.039 1.000 . Uiso c ? H(13) 0.3936 0.0330 0.4458 0.055 1.000 . Uiso c ? H(14) 0.4882 0.0409 0.4241 0.055 1.000 . Uiso c ? H(15) 0.4445 0.1116 0.4523 0.055 1.000 . Uiso c ? H(16) 0.1069 -0.1108 0.0516 0.029 1.000 . Uiso c ? H(17) 0.0677 -0.0206 -0.0603 0.035 1.000 . Uiso c ? H(18) 0.1431 0.0445 -0.0490 0.035 1.000 . Uiso c ? H(19) 0.1769 -0.0399 -0.0384 0.035 1.000 . Uiso c ? H(20) 0.0363 -0.1755 0.1488 0.037 1.000 . Uiso c ? H(21) 0.1442 -0.1984 0.1694 0.037 1.000 . Uiso c ? H(22) 0.1037 -0.1659 0.2323 0.037 1.000 . Uiso c ? 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 #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2698 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.1116 _refine_ls_wR_factor_all 0.1037 _refine_ls_wR_factor_ref 0.1037 _refine_ls_goodness_of_fit_all 3.977 _refine_ls_goodness_of_fit_ref 3.977 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0006 _refine_diff_density_min -0.88 _refine_diff_density_max 0.78 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 1.923(6) . . yes Cu(1) N(2) 1.932(6) . . yes Cu(1) N(3) 1.911(6) . . yes Cu(1) N(4) 1.917(6) . . yes N(1) C(1) 1.401(8) . . yes N(1) C(13) 1.325(8) . . yes N(2) C(7) 1.401(9) . . yes N(2) C(15) 1.334(9) . . yes N(3) C(6) 1.398(8) . . yes N(3) C(18) 1.323(8) . . yes N(4) C(12) 1.406(9) . . yes N(4) C(20) 1.320(8) . . yes C(1) C(2) 1.409(9) . . yes C(1) C(6) 1.399(9) . . yes C(2) C(3) 1.383(9) . . yes C(2) H(1) 0.95 . . no C(3) C(4) 1.397(9) . . yes C(3) H(2) 0.95 . . no C(4) C(5) 1.392(9) . . yes C(4) H(3) 0.95 . . no C(5) C(6) 1.401(9) . . yes C(5) H(4) 0.95 . . no C(7) C(8) 1.40(1) . . yes C(7) C(12) 1.41(1) . . yes C(8) C(9) 1.38(1) . . yes C(8) H(5) 0.95 . . no C(9) C(10) 1.41(1) . . yes C(9) H(6) 0.95 . . no C(10) C(11) 1.38(1) . . yes C(10) H(7) 0.95 . . no C(11) C(12) 1.43(1) . . yes C(11) H(8) 0.95 . . no C(13) C(14) 1.40(1) . . yes C(13) C(16) 1.52(1) . . yes C(14) C(15) 1.40(1) . . yes C(14) H(9) 0.95 . . no C(15) C(17) 1.50(1) . . yes C(16) H(10) 0.95 . . no C(16) H(11) 0.95 . . no C(16) H(12) 0.95 . . no C(17) H(13) 0.95 . . no C(17) H(14) 0.95 . . no C(17) H(15) 0.95 . . no C(18) C(19) 1.407(9) . . yes C(18) C(21) 1.494(9) . . yes C(19) C(20) 1.405(9) . . yes C(19) H(16) 0.95 . . no C(20) C(22) 1.539(9) . . yes C(21) H(17) 0.95 . . no C(21) H(18) 0.95 . . no C(21) H(19) 0.95 . . no C(22) H(20) 0.95 . . no C(22) H(21) 0.95 . . no C(22) H(22) 0.95 . . no C(23) C(24) 1.44(1) . . yes C(23) C(28) 1.37(1) . . yes C(23) C(32) 1.39(1) . . yes C(24) C(25) 1.33(1) . . yes C(24) C(38) 1.48(1) . . yes C(25) C(26) 1.40(1) . . yes C(25) C(44) 1.45(2) . . yes C(26) C(27) 1.43(1) . . yes C(26) C(45) 1.44(2) . . yes C(27) C(28) 1.44(1) . . yes C(27) C(75) 1.41(1) . . yes C(28) C(29) 1.45(1) . . yes C(29) C(30) 1.36(1) . . yes C(29) C(73) 1.44(1) . . yes C(30) C(31) 1.46(1) . . yes C(30) C(62) 1.42(1) . . yes C(31) C(32) 1.38(1) . . yes C(31) C(68) 1.46(1) . . yes C(32) C(33) 1.46(1) . . yes C(33) C(34) 1.35(1) . . yes C(33) C(38) 1.40(1) . . yes C(34) C(35) 1.46(2) . . yes C(34) C(67) 1.47(2) . . yes C(35) C(36) 1.39(2) . . yes C(35) C(69) 1.45(2) . . yes C(36) C(37) 1.43(1) . . yes C(36) C(80) 1.46(1) . . yes C(37) C(38) 1.36(1) . . yes C(37) C(39) 1.46(2) . . yes C(39) C(40) 1.44(2) . . yes C(39) C(44) 1.36(1) . . yes C(40) C(41) 1.39(1) . . yes C(40) C(80) 1.46(1) . . yes C(41) C(42) 1.44(2) . . yes C(41) C(77) 1.43(2) . . yes C(42) C(43) 1.37(2) . . yes C(42) C(48) 1.44(2) . . yes C(43) C(44) 1.45(2) . . yes C(43) C(45) 1.45(2) . . yes C(45) C(46) 1.38(1) . . yes C(46) C(47) 1.44(2) . . yes C(46) C(76) 1.42(1) . . yes C(47) C(48) 1.39(2) . . yes C(47) C(52) 1.47(2) . . yes C(48) C(49) 1.45(2) . . yes C(49) C(50) 1.37(1) . . yes C(49) C(77) 1.46(2) . . yes C(50) C(51) 1.45(2) . . yes C(50) C(81) 1.43(1) . . yes C(51) C(52) 1.36(1) . . yes C(51) C(56) 1.44(1) . . yes C(52) C(53) 1.46(1) . . yes C(53) C(54) 1.37(1) . . yes C(53) C(76) 1.46(1) . . yes C(54) C(55) 1.46(2) . . yes C(54) C(74) 1.46(1) . . yes C(55) C(56) 1.37(1) . . yes C(55) C(60) 1.44(2) . . yes C(56) C(57) 1.47(2) . . yes C(57) C(58) 1.35(2) . . yes C(57) C(81) 1.45(2) . . yes C(58) C(59) 1.47(2) . . yes C(58) C(72) 1.41(2) . . yes C(59) C(60) 1.38(2) . . yes C(59) C(64) 1.44(2) . . yes C(60) C(61) 1.44(2) . . yes C(61) C(62) 1.41(1) . . yes C(61) C(74) 1.45(2) . . yes C(62) C(63) 1.43(2) . . yes C(63) C(64) 1.36(2) . . yes C(63) C(68) 1.47(2) . . yes C(64) C(65) 1.47(2) . . yes C(65) C(66) 1.38(2) . . yes C(65) C(72) 1.41(2) . . yes C(66) C(67) 1.43(2) . . yes C(66) C(69) 1.44(2) . . yes C(67) C(68) 1.34(2) . . yes C(69) C(70) 1.37(1) . . yes C(70) C(71) 1.43(1) . . yes C(70) C(79) 1.48(1) . . yes C(71) C(72) 1.41(1) . . yes C(71) C(82) 1.41(1) . . yes C(73) C(74) 1.38(1) . . yes C(73) C(75) 1.45(1) . . yes C(75) C(76) 1.40(1) . . yes C(77) C(78) 1.36(1) . . yes C(78) C(79) 1.45(1) . . yes C(78) C(82) 1.46(1) . . yes C(79) C(80) 1.36(1) . . yes C(81) C(82) 1.37(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 96.0(3) . . . yes N(1) Cu(1) N(3) 83.9(3) . . . yes N(1) Cu(1) N(4) 178.3(3) . . . yes N(2) Cu(1) N(3) 178.4(3) . . . yes N(2) Cu(1) N(4) 85.1(3) . . . yes N(3) Cu(1) N(4) 95.0(3) . . . yes Cu(1) N(1) C(1) 110.4(5) . . . yes Cu(1) N(1) C(13) 120.1(6) . . . yes C(1) N(1) C(13) 128.3(7) . . . yes Cu(1) N(2) C(7) 110.1(6) . . . yes Cu(1) N(2) C(15) 121.6(6) . . . yes C(7) N(2) C(15) 128.0(7) . . . yes Cu(1) N(3) C(6) 110.5(5) . . . yes Cu(1) N(3) C(18) 121.9(6) . . . yes C(6) N(3) C(18) 125.8(7) . . . yes Cu(1) N(4) C(12) 109.1(5) . . . yes Cu(1) N(4) C(20) 120.6(5) . . . yes C(12) N(4) C(20) 129.0(7) . . . yes N(1) C(1) C(2) 124.4(7) . . . yes N(1) C(1) C(6) 114.3(7) . . . yes C(2) C(1) C(6) 120.7(8) . . . yes C(1) C(2) C(3) 118.9(7) . . . yes C(1) C(2) H(1) 120.5 . . . no C(3) C(2) H(1) 120.6 . . . no C(2) C(3) C(4) 121.3(7) . . . yes C(2) C(3) H(2) 119.2 . . . no C(4) C(3) H(2) 119.5 . . . no C(3) C(4) C(5) 119.4(7) . . . yes C(3) C(4) H(3) 120.3 . . . no C(5) C(4) H(3) 120.3 . . . no C(4) C(5) C(6) 120.6(7) . . . yes C(4) C(5) H(4) 119.8 . . . no C(6) C(5) H(4) 119.6 . . . no N(3) C(6) C(1) 114.9(7) . . . yes N(3) C(6) C(5) 125.1(7) . . . yes C(1) C(6) C(5) 119.1(7) . . . yes N(2) C(7) C(8) 126.7(9) . . . yes N(2) C(7) C(12) 114.1(8) . . . yes C(8) C(7) C(12) 118.8(8) . . . yes C(7) C(8) C(9) 121.6(9) . . . yes C(7) C(8) H(5) 119.0 . . . no C(9) C(8) H(5) 119.4 . . . no C(8) C(9) C(10) 120.2(9) . . . yes C(8) C(9) H(6) 120.1 . . . no C(10) C(9) H(6) 119.7 . . . no C(9) C(10) C(11) 119.4(8) . . . yes C(9) C(10) H(7) 120.6 . . . no C(11) C(10) H(7) 120.1 . . . no C(10) C(11) C(12) 120.8(8) . . . yes C(10) C(11) H(8) 119.5 . . . no C(12) C(11) H(8) 119.7 . . . no N(4) C(12) C(7) 116.2(8) . . . yes N(4) C(12) C(11) 124.0(9) . . . yes C(7) C(12) C(11) 119.2(8) . . . yes N(1) C(13) C(14) 122.0(8) . . . yes N(1) C(13) C(16) 119.0(8) . . . yes C(14) C(13) C(16) 118.8(8) . . . yes C(13) C(14) C(15) 130.1(8) . . . yes C(13) C(14) H(9) 114.8 . . . no C(15) C(14) H(9) 115.2 . . . no N(2) C(15) C(14) 121.9(8) . . . yes N(2) C(15) C(17) 122.0(8) . . . yes C(14) C(15) C(17) 116.0(8) . . . yes C(13) C(16) H(10) 109.4 . . . no C(13) C(16) H(11) 109.6 . . . no C(13) C(16) H(12) 109.5 . . . no H(10) C(16) H(11) 109.4 . . . no H(10) C(16) H(12) 109.4 . . . no H(11) C(16) H(12) 109.6 . . . no C(15) C(17) H(13) 109.4 . . . no C(15) C(17) H(14) 109.4 . . . no C(15) C(17) H(15) 109.6 . . . no H(13) C(17) H(14) 109.3 . . . no H(13) C(17) H(15) 109.5 . . . no H(14) C(17) H(15) 109.6 . . . no N(3) C(18) C(19) 120.3(8) . . . yes N(3) C(18) C(21) 123.9(7) . . . yes C(19) C(18) C(21) 115.7(7) . . . yes C(18) C(19) C(20) 128.9(7) . . . yes C(18) C(19) H(16) 115.6 . . . no C(20) C(19) H(16) 115.5 . . . no N(4) C(20) C(19) 123.0(7) . . . yes N(4) C(20) C(22) 121.5(7) . . . yes C(19) C(20) C(22) 115.4(8) . . . yes C(18) C(21) H(17) 109.6 . . . no C(18) C(21) H(18) 109.7 . . . no C(18) C(21) H(19) 109.6 . . . no H(17) C(21) H(18) 109.3 . . . no H(17) C(21) H(19) 109.2 . . . no H(18) C(21) H(19) 109.3 . . . no C(20) C(22) H(20) 109.3 . . . no C(20) C(22) H(21) 109.4 . . . no C(20) C(22) H(22) 109.5 . . . no H(20) C(22) H(21) 109.4 . . . no H(20) C(22) H(22) 109.6 . . . no H(21) C(22) H(22) 109.7 . . . no C(24) C(23) C(28) 119(1) . . . yes C(24) C(23) C(32) 110(1) . . . yes C(28) C(23) C(32) 119(1) . . . yes C(23) C(24) C(25) 122(1) . . . yes C(23) C(24) C(38) 105(1) . . . yes C(25) C(24) C(38) 121(1) . . . yes C(24) C(25) C(26) 121(2) . . . yes C(24) C(25) C(44) 120(2) . . . yes C(26) C(25) C(44) 108(1) . . . yes C(25) C(26) C(27) 119(1) . . . yes C(25) C(26) C(45) 109(2) . . . yes C(27) C(26) C(45) 121(2) . . . yes C(26) C(27) C(28) 119(1) . . . yes C(26) C(27) C(75) 119(1) . . . yes C(28) C(27) C(75) 110(1) . . . yes C(23) C(28) C(27) 119(1) . . . yes C(23) C(28) C(29) 122(1) . . . yes C(27) C(28) C(29) 107(1) . . . yes C(28) C(29) C(30) 118(1) . . . yes C(28) C(29) C(73) 108(1) . . . yes C(30) C(29) C(73) 123(1) . . . yes C(29) C(30) C(31) 121(1) . . . yes C(29) C(30) C(62) 120(2) . . . yes C(31) C(30) C(62) 107(2) . . . yes C(30) C(31) C(32) 118(1) . . . yes C(30) C(31) C(68) 109(2) . . . yes C(32) C(31) C(68) 121(2) . . . yes C(23) C(32) C(31) 123(2) . . . yes C(23) C(32) C(33) 109(1) . . . yes C(31) C(32) C(33) 117(2) . . . yes C(32) C(33) C(34) 120(2) . . . yes C(32) C(33) C(38) 107(1) . . . yes C(34) C(33) C(38) 120(2) . . . yes C(33) C(34) C(35) 121(1) . . . yes C(33) C(34) C(67) 122(2) . . . yes C(35) C(34) C(67) 104(2) . . . yes C(34) C(35) C(36) 118(1) . . . yes C(34) C(35) C(69) 111(2) . . . yes C(36) C(35) C(69) 120(2) . . . yes C(35) C(36) C(37) 119(1) . . . yes C(35) C(36) C(80) 119(2) . . . yes C(37) C(36) C(80) 109(2) . . . yes C(36) C(37) C(38) 121(1) . . . yes C(36) C(37) C(39) 108(1) . . . yes C(38) C(37) C(39) 120(2) . . . yes C(24) C(38) C(33) 109(1) . . . yes C(24) C(38) C(37) 119(1) . . . yes C(33) C(38) C(37) 121(2) . . . yes C(37) C(39) C(40) 108(2) . . . yes C(37) C(39) C(44) 120(2) . . . yes C(40) C(39) C(44) 121(2) . . . yes C(39) C(40) C(41) 120(2) . . . yes C(39) C(40) C(80) 109(2) . . . yes C(41) C(40) C(80) 118(1) . . . yes C(40) C(41) C(42) 119(2) . . . yes C(40) C(41) C(77) 121(2) . . . yes C(42) C(41) C(77) 109(2) . . . yes C(41) C(42) C(43) 119(2) . . . yes C(41) C(42) C(48) 107(2) . . . yes C(43) C(42) C(48) 121(2) . . . yes C(42) C(43) C(44) 122(2) . . . yes C(42) C(43) C(45) 121(2) . . . yes C(44) C(43) C(45) 106(2) . . . yes C(25) C(44) C(39) 121(2) . . . yes C(25) C(44) C(43) 108(2) . . . yes C(39) C(44) C(43) 118(2) . . . yes C(26) C(45) C(43) 109(2) . . . yes C(26) C(45) C(46) 119(2) . . . yes C(43) C(45) C(46) 118(2) . . . yes C(45) C(46) C(47) 121(2) . . . yes C(45) C(46) C(76) 121(2) . . . yes C(47) C(46) C(76) 108(2) . . . yes C(46) C(47) C(48) 120(2) . . . yes C(46) C(47) C(52) 109(2) . . . yes C(48) C(47) C(52) 117(2) . . . yes C(42) C(48) C(47) 119(2) . . . yes C(42) C(48) C(49) 109(2) . . . yes C(47) C(48) C(49) 121(2) . . . yes C(48) C(49) C(50) 121(2) . . . yes C(48) C(49) C(77) 106(2) . . . yes C(50) C(49) C(77) 121(2) . . . yes C(49) C(50) C(51) 119(2) . . . yes C(49) C(50) C(81) 119(2) . . . yes C(51) C(50) C(81) 110(2) . . . yes C(50) C(51) C(52) 120(2) . . . yes C(50) C(51) C(56) 106(2) . . . yes C(52) C(51) C(56) 123(2) . . . yes C(47) C(52) C(51) 122(2) . . . yes C(47) C(52) C(53) 106(2) . . . yes C(51) C(52) C(53) 120(2) . . . yes C(52) C(53) C(54) 119(2) . . . yes C(52) C(53) C(76) 108(2) . . . yes C(54) C(53) C(76) 120(2) . . . yes C(53) C(54) C(55) 119(1) . . . yes C(53) C(54) C(74) 122(1) . . . yes C(55) C(54) C(74) 107(2) . . . yes C(54) C(55) C(56) 122(2) . . . yes C(54) C(55) C(60) 107(1) . . . yes C(56) C(55) C(60) 119(2) . . . yes C(51) C(56) C(55) 117(2) . . . yes C(51) C(56) C(57) 109(1) . . . yes C(55) C(56) C(57) 121(2) . . . yes C(56) C(57) C(58) 119(2) . . . yes C(56) C(57) C(81) 107(2) . . . yes C(58) C(57) C(81) 120(2) . . . yes C(57) C(58) C(59) 120(2) . . . yes C(57) C(58) C(72) 122(2) . . . yes C(59) C(58) C(72) 107(2) . . . yes C(58) C(59) C(60) 120(2) . . . yes C(58) C(59) C(64) 107(2) . . . yes C(60) C(59) C(64) 121(2) . . . yes C(55) C(60) C(59) 121(2) . . . yes C(55) C(60) C(61) 111(2) . . . yes C(59) C(60) C(61) 117(2) . . . yes C(60) C(61) C(62) 122(2) . . . yes C(60) C(61) C(74) 106(2) . . . yes C(62) C(61) C(74) 119(1) . . . yes C(30) C(62) C(61) 120(2) . . . yes C(30) C(62) C(63) 110(2) . . . yes C(61) C(62) C(63) 119(2) . . . yes C(62) C(63) C(64) 120(2) . . . yes C(62) C(63) C(68) 108(2) . . . yes C(64) C(63) C(68) 120(2) . . . yes C(59) C(64) C(63) 121(2) . . . yes C(59) C(64) C(65) 108(2) . . . yes C(63) C(64) C(65) 119(2) . . . yes C(64) C(65) C(66) 119(2) . . . yes C(64) C(65) C(72) 107(2) . . . yes C(66) C(65) C(72) 123(2) . . . yes C(65) C(66) C(67) 121(2) . . . yes C(65) C(66) C(69) 118(2) . . . yes C(67) C(66) C(69) 108(2) . . . yes C(34) C(67) C(66) 110(2) . . . yes C(34) C(67) C(68) 117(2) . . . yes C(66) C(67) C(68) 121(2) . . . yes C(31) C(68) C(63) 106(2) . . . yes C(31) C(68) C(67) 122(2) . . . yes C(63) C(68) C(67) 120(2) . . . yes C(35) C(69) C(66) 107(2) . . . yes C(35) C(69) C(70) 122(2) . . . yes C(66) C(69) C(70) 120(2) . . . yes C(69) C(70) C(71) 121(1) . . . yes C(69) C(70) C(79) 118(1) . . . yes C(71) C(70) C(79) 108(1) . . . yes C(70) C(71) C(72) 119(1) . . . yes C(70) C(71) C(82) 108(1) . . . yes C(72) C(71) C(82) 122(1) . . . yes C(58) C(72) C(65) 111(2) . . . yes C(58) C(72) C(71) 117(2) . . . yes C(65) C(72) C(71) 119(2) . . . yes C(29) C(73) C(74) 118(1) . . . yes C(29) C(73) C(75) 108(1) . . . yes C(74) C(73) C(75) 122(1) . . . yes C(54) C(74) C(61) 109(1) . . . yes C(54) C(74) C(73) 118(2) . . . yes C(61) C(74) C(73) 121(1) . . . yes C(27) C(75) C(73) 108(1) . . . yes C(27) C(75) C(76) 121(1) . . . yes C(73) C(75) C(76) 119(1) . . . yes C(46) C(76) C(53) 109(1) . . . yes C(46) C(76) C(75) 120(1) . . . yes C(53) C(76) C(75) 119(2) . . . yes C(41) C(77) C(49) 108(2) . . . yes C(41) C(77) C(78) 120(2) . . . yes C(49) C(77) C(78) 119(2) . . . yes C(77) C(78) C(79) 121(1) . . . yes C(77) C(78) C(82) 121(1) . . . yes C(79) C(78) C(82) 107(1) . . . yes C(70) C(79) C(78) 107(1) . . . yes C(70) C(79) C(80) 122(1) . . . yes C(78) C(79) C(80) 119(1) . . . yes C(36) C(80) C(40) 107(1) . . . yes C(36) C(80) C(79) 120(2) . . . yes C(40) C(80) C(79) 122(1) . . . yes C(50) C(81) C(57) 108(2) . . . yes C(50) C(81) C(82) 122(2) . . . yes C(57) C(81) C(82) 119(2) . . . yes C(71) C(82) C(78) 110(1) . . . yes C(71) C(82) C(81) 119(1) . . . yes C(78) C(82) C(81) 119(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) C(23) 3.198(9) . . no Cu(1) C(24) 3.30(1) . . no Cu(1) C(40) 3.37(1) . 2_545 no Cu(1) C(41) 3.54(1) . 2_545 no N(1) C(24) 3.29(1) . . no N(1) C(25) 3.51(1) . . no N(2) C(42) 3.48(1) . 2_545 no N(2) C(24) 3.54(1) . . no N(2) C(23) 3.55(1) . . no N(4) C(39) 3.39(1) . 2_545 no N(4) C(23) 3.54(1) . . no C(1) C(25) 3.27(1) . . no C(1) C(24) 3.55(2) . . no C(2) C(25) 3.24(1) . . no C(2) C(65) 3.51(1) . 4_554 no C(3) C(64) 3.31(1) . 4_554 no C(3) C(65) 3.50(2) . 4_554 no C(3) C(26) 3.55(1) . . no C(3) C(59) 3.59(2) . 4_554 no C(4) C(59) 3.28(1) . 4_554 no C(4) C(58) 3.47(2) . 4_554 no C(4) C(26) 3.54(1) . . no C(4) C(64) 3.58(2) . 4_554 no C(5) C(58) 3.42(1) . 4_554 no C(7) C(32) 3.22(1) . . no C(7) C(33) 3.48(1) . . no C(7) C(23) 3.53(1) . . no C(8) C(33) 3.29(1) . . no C(8) C(32) 3.36(1) . . no C(11) C(32) 3.58(1) . . no C(12) C(32) 3.35(1) . . no C(12) C(23) 3.51(1) . . no C(13) C(41) 3.44(1) . 2_545 no C(13) C(22) 3.52(1) . 2 no C(14) C(42) 3.24(1) . 2_545 no C(14) C(41) 3.29(1) . 2_545 no C(15) C(42) 3.09(1) . 2_545 no C(15) C(41) 3.49(2) . 2_545 no C(15) C(43) 3.59(2) . 2_545 no C(16) C(60) 3.50(1) . 1_655 no C(16) C(22) 3.58(1) . 2 no C(17) C(42) 3.33(1) . 2_545 no C(17) C(43) 3.59(2) . 2_545 no C(19) C(39) 3.41(2) . 2_545 no C(19) C(40) 3.49(1) . 2_545 no C(19) C(37) 3.56(1) . 2_545 no C(20) C(39) 3.12(1) . 2_545 no C(20) C(40) 3.57(1) . 2_545 no C(22) C(39) 3.41(1) . 2_545 no C(22) C(37) 3.53(1) . 2_545 no C(30) C(50) 3.42(2) . 2_445 no C(34) C(53) 3.32(2) . 4 no C(34) C(76) 3.59(2) . 4 no C(35) C(53) 3.39(2) . 4 no C(35) C(54) 3.49(2) . 4 no C(35) C(76) 3.50(2) . 4 no C(49) C(62) 3.57(2) . 2_455 no C(49) C(61) 3.59(2) . 2_455 no C(50) C(62) 3.18(1) . 2_455 no C(50) C(61) 3.55(2) . 2_455 no C(54) C(69) 3.57(2) . 4_454 no C(70) C(78) 3.38(1) . 3_566 no C(71) C(79) 3.50(1) . 3_566 no C(79) C(82) 3.44(1) . 3_566 no #------------------------------------------------------------------------------ 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_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #=END