# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1155 data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 18 21:32:16 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1585.79 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H72 Cu4 I4 N6 Ni S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 29.22(2) _cell_length_b 11.457(3) _cell_length_c 20.430(5) _cell_angle_alpha 90 _cell_angle_beta 121.87(2) _cell_angle_gamma 90 _cell_volume 5808(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 23.0 _cell_measurement_theta_max 24.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096.00 _exptl_absorpt_coefficient_mu 4.062 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 -2 1 3 -1 3 -6 -2 3 _diffrn_reflns_number 6793 _reflns_number_total 6665 _reflns_number_gt 4529 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.053 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00837 _diffrn_orient_matrix_UB_12 -0.06313 _diffrn_orient_matrix_UB_13 0.02591 _diffrn_orient_matrix_UB_21 -0.00113 _diffrn_orient_matrix_UB_22 -0.05834 _diffrn_orient_matrix_UB_23 -0.03723 _diffrn_orient_matrix_UB_31 0.03940 _diffrn_orient_matrix_UB_32 -0.01514 _diffrn_orient_matrix_UB_33 0.03556 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I -0.13000(2) 0.17862(5) 0.55936(2) 0.0670(1) Uani 1.00 d . . . I(2) I 0.04398(2) 0.22862(4) 0.68497(2) 0.0691(1) Uani 1.00 d . . . Cu(1) Cu -0.03908(3) 0.10054(7) 0.58483(4) 0.0560(2) Uani 1.00 d . . . Cu(2) Cu 0.07228(6) 0.1065(1) 0.80370(5) 0.0712(4) Uani 0.92 d P . . Cu(3) Cu 0.0454(6) 0.154(1) 0.7978(6) 0.061(4) Uiso 0.08 d P . . Ni(1) Ni 0.0000 -0.08918(8) 0.7500 0.0397(2) Uani 1.00 d S . . S(1) S -0.01977(5) -0.0933(1) 0.63092(7) 0.0456(4) Uani 1.00 d . . . S(2) S 0.08641(6) -0.0927(1) 0.79536(7) 0.0497(4) Uani 1.00 d . . . N(1) N 0.0434(2) -0.1036(5) 0.5160(3) 0.059(2) Uani 1.00 d . . . N(2) N 0.1840(2) -0.1185(6) 0.7333(4) 0.082(2) Uani 1.00 d . . . N(3) N 0.3078(2) 0.0099(5) 0.1763(3) 0.069(2) Uani 1.00 d . . . C(1) C 0.0436(2) -0.0990(5) 0.6416(3) 0.044(1) Uani 1.00 d . . . C(2) C 0.0891(2) -0.1009(5) 0.7119(3) 0.047(2) Uani 1.00 d . . . C(3) C 0.0448(2) -0.1011(5) 0.5724(3) 0.050(2) Uani 1.00 d . . . C(4) C 0.1419(2) -0.1086(6) 0.7232(3) 0.056(2) Uani 1.00 d . . . C(5) C 0.3475(5) 0.024(1) 0.1503(7) 0.127(5) Uani 1.00 d . . . C(6) C 0.3750(9) -0.072(2) 0.141(1) 0.23(1) Uani 1.00 d . . . C(7) C 0.4076(9) -0.057(2) 0.112(1) 0.26(1) Uani 1.00 d . . . C(8) C 0.4552(8) -0.062(3) 0.141(1) 0.29(1) Uani 1.00 d . . . C(9) C 0.3323(5) -0.063(1) 0.2509(6) 0.126(4) Uani 1.00 d . . . C(10) C 0.3819(6) -0.032(1) 0.3183(7) 0.152(5) Uani 1.00 d . . . C(11) C 0.3974(7) -0.100(1) 0.3890(7) 0.181(6) Uani 1.00 d . . . C(12) C 0.4385(9) -0.082(2) 0.450(1) 0.25(1) Uani 1.00 d . . . C(13) C 0.2582(5) -0.0497(9) 0.1103(7) 0.120(4) Uani 1.00 d . . . C(14) C 0.2151(5) -0.075(1) 0.1241(7) 0.147(5) Uani 1.00 d . . . C(15) C 0.1709(5) -0.148(1) 0.0617(7) 0.152(5) Uani 1.00 d . . . C(16) C 0.1378(9) -0.195(2) 0.0816(10) 0.25(1) Uani 1.00 d . . . C(17) C 0.2962(3) 0.1288(9) 0.1957(5) 0.092(3) Uani 1.00 d . . . C(18) C 0.2729(3) 0.2166(8) 0.1345(5) 0.087(3) Uani 1.00 d . . . C(19) C 0.2670(4) 0.3330(9) 0.1625(6) 0.109(4) Uani 1.00 d . . . C(20) C 0.2447(5) 0.4241(9) 0.0998(7) 0.136(4) Uani 1.00 d . . . H(1) H 0.3290 0.0642 0.1028 0.1523 Uiso 1.00 calc . . . H(2) H 0.3757 0.0722 0.1884 0.1523 Uiso 1.00 calc . . . H(3) H 0.3939 -0.1123 0.1878 0.2736 Uiso 1.00 calc . . . H(4) H 0.3460 -0.1239 0.1033 0.2736 Uiso 1.00 calc . . . H(5) H 0.3942 -0.1047 0.0693 0.3071 Uiso 1.00 calc . . . H(6) H 0.4027 0.0236 0.0976 0.3071 Uiso 1.00 calc . . . H(7) H 0.4668 -0.1458 0.1583 0.3721 Uiso 1.00 calc . . . H(8) H 0.4667 -0.0462 0.1067 0.3721 Uiso 1.00 calc . . . H(9) H 0.4753 -0.0176 0.1867 0.3721 Uiso 1.00 calc . . . H(10) H 0.3061 -0.0647 0.2652 0.1490 Uiso 1.00 calc . . . H(11) H 0.3368 -0.1402 0.2377 0.1490 Uiso 1.00 calc . . . H(12) H 0.4091 -0.0399 0.3067 0.1834 Uiso 1.00 calc . . . H(13) H 0.3790 0.0464 0.3296 0.1834 Uiso 1.00 calc . . . H(14) H 0.3696 -0.0985 0.3966 0.2057 Uiso 1.00 calc . . . H(15) H 0.4032 -0.1794 0.3768 0.2057 Uiso 1.00 calc . . . H(16) H 0.4423 -0.1353 0.4881 0.3010 Uiso 1.00 calc . . . H(17) H 0.4699 -0.0844 0.4471 0.3010 Uiso 1.00 calc . . . H(18) H 0.4363 -0.0038 0.4670 0.3010 Uiso 1.00 calc . . . H(19) H 0.2438 0.0001 0.0666 0.1427 Uiso 1.00 calc . . . H(20) H 0.2696 -0.1208 0.0996 0.1427 Uiso 1.00 calc . . . H(21) H 0.2307 -0.1168 0.1716 0.1790 Uiso 1.00 calc . . . H(22) H 0.2004 -0.0046 0.1276 0.1790 Uiso 1.00 calc . . . H(23) H 0.1504 -0.1028 0.0170 0.1852 Uiso 1.00 calc . . . H(24) H 0.1869 -0.2123 0.0497 0.1852 Uiso 1.00 calc . . . H(25) H 0.1226 -0.1310 0.0947 0.2968 Uiso 1.00 calc . . . H(26) H 0.1117 -0.2395 0.0429 0.2968 Uiso 1.00 calc . . . H(27) H 0.1594 -0.2401 0.1280 0.2968 Uiso 1.00 calc . . . H(28) H 0.2714 0.1180 0.2124 0.1142 Uiso 1.00 calc . . . H(29) H 0.3289 0.1591 0.2367 0.1142 Uiso 1.00 calc . . . H(30) H 0.2952 0.2251 0.1140 0.1054 Uiso 1.00 calc . . . H(31) H 0.2378 0.1918 0.0947 0.1054 Uiso 1.00 calc . . . H(32) H 0.2439 0.3263 0.1812 0.1304 Uiso 1.00 calc . . . H(33) H 0.3018 0.3583 0.2027 0.1304 Uiso 1.00 calc . . . H(34) H 0.2419 0.4952 0.1192 0.1636 Uiso 1.00 calc . . . H(35) H 0.2682 0.4303 0.0805 0.1636 Uiso 1.00 calc . . . H(36) H 0.2102 0.3982 0.0589 0.1636 Uiso 1.00 calc . . . 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 I(1) 0.0544(2) 0.0967(4) 0.0468(2) 0.0283(2) 0.0247(2) 0.0074(2) I(2) 0.0744(3) 0.0684(3) 0.0534(2) -0.0123(2) 0.0261(2) 0.0036(2) Cu(1) 0.0587(4) 0.0773(5) 0.0413(3) 0.0149(4) 0.0327(3) 0.0043(3) Cu(2) 0.0893(10) 0.0711(8) 0.0473(5) -0.0101(7) 0.0320(5) -0.0068(4) Ni(1) 0.0498(5) 0.0464(5) 0.0301(4) 0.0000 0.0260(4) 0.0000 S(1) 0.0508(7) 0.0610(9) 0.0316(6) 0.0018(6) 0.0262(6) -0.0017(5) S(2) 0.0512(7) 0.0671(9) 0.0342(6) 0.0078(7) 0.0250(6) 0.0064(6) N(1) 0.067(3) 0.079(4) 0.044(2) 0.019(3) 0.037(2) 0.010(2) N(2) 0.056(3) 0.112(5) 0.086(4) 0.008(3) 0.043(3) -0.004(4) N(3) 0.077(4) 0.067(4) 0.065(3) -0.014(3) 0.040(3) 0.008(3) C(1) 0.058(3) 0.051(3) 0.036(2) 0.009(2) 0.033(2) 0.000(2) C(2) 0.060(3) 0.048(3) 0.047(3) 0.009(2) 0.038(3) 0.002(2) C(3) 0.057(3) 0.058(3) 0.044(3) 0.015(3) 0.033(3) 0.005(2) C(4) 0.059(4) 0.066(4) 0.048(3) 0.004(3) 0.033(3) 0.002(3) C(5) 0.138(9) 0.137(9) 0.139(10) 0.046(8) 0.095(8) 0.039(8) C(6) 0.29(2) 0.20(2) 0.33(3) 0.13(2) 0.25(2) 0.10(2) C(7) 0.22(2) 0.38(3) 0.27(2) 0.15(2) 0.19(2) 0.09(2) C(8) 0.16(2) 0.37(3) 0.31(3) -0.02(2) 0.12(2) 0.12(3) C(9) 0.143(9) 0.122(8) 0.083(6) -0.017(7) 0.040(6) 0.030(6) C(10) 0.14(1) 0.16(1) 0.109(9) -0.023(9) 0.035(8) 0.031(8) C(11) 0.20(2) 0.18(1) 0.079(8) -0.02(1) 0.011(9) 0.034(9) C(12) 0.32(3) 0.24(2) 0.15(2) 0.02(2) 0.10(2) 0.04(2) C(13) 0.133(9) 0.097(7) 0.127(8) -0.037(6) 0.066(7) -0.011(6) C(14) 0.120(9) 0.19(1) 0.125(9) -0.072(9) 0.065(8) -0.033(9) C(15) 0.15(1) 0.15(1) 0.122(9) -0.069(9) 0.042(8) 0.015(8) C(16) 0.32(2) 0.27(2) 0.14(1) -0.16(2) 0.12(2) -0.03(1) C(17) 0.083(5) 0.110(7) 0.081(5) -0.020(5) 0.041(5) -0.001(5) C(18) 0.074(5) 0.100(6) 0.074(5) -0.009(4) 0.030(4) 0.006(5) C(19) 0.114(7) 0.095(7) 0.101(7) 0.013(6) 0.044(6) -0.012(6) C(20) 0.126(9) 0.096(7) 0.125(9) 0.021(7) 0.024(7) 0.007(7) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00360(Fo^2^)^2^]' _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 6650 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_shift/su_max 0.0022 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_min -0.87 _refine_diff_density_max 0.89 #------------------------------------------------------------------------------ _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 I(1) Cu(1) 2.582(2) 1_555 1_555 yes I(1) Cu(2) 2.5241(9) 1_555 2_556 yes I(1) Cu(3) 2.66(1) 1_555 2_556 yes I(2) Cu(1) 2.643(1) 1_555 1_555 yes I(2) Cu(2) 2.531(1) 1_555 1_555 yes I(2) Cu(3) 2.44(1) 1_555 1_555 yes I(2) Cu(3) 2.94(2) 1_555 2_556 yes Cu(1) Cu(3) 2.57(1) 1_555 2_556 yes Cu(1) S(1) 2.362(2) 1_555 1_555 yes Cu(1) N(1) 1.996(4) 1_555 3_556 yes Cu(2) Cu(3) 0.91(2) 1_555 1_555 yes Cu(2) S(2) 2.342(2) 1_555 1_555 yes Cu(3) Cu(3) 2.32(3) 1_555 2_556 yes Ni(1) S(1) 2.184(1) 1_555 1_555 yes Ni(1) S(1) 2.184(1) 1_555 2_556 yes Ni(1) S(2) 2.183(2) 1_555 1_555 yes Ni(1) S(2) 2.183(2) 1_555 2_556 yes S(1) C(1) 1.748(5) 1_555 1_555 yes S(2) C(2) 1.750(5) 1_555 1_555 yes N(1) C(3) 1.134(7) 1_555 1_555 yes N(2) C(4) 1.140(8) 1_555 1_555 yes N(3) C(5) 1.52(1) 1_555 1_555 yes N(3) C(9) 1.55(1) 1_555 1_555 yes N(3) C(13) 1.52(1) 1_555 1_555 yes N(3) C(17) 1.51(1) 1_555 1_555 yes C(1) C(2) 1.345(7) 1_555 1_555 yes C(1) C(3) 1.431(6) 1_555 1_555 yes C(2) C(4) 1.439(8) 1_555 1_555 yes C(5) C(6) 1.43(2) 1_555 1_555 yes C(6) C(7) 1.38(2) 1_555 1_555 yes C(7) C(8) 1.19(2) 1_555 1_555 yes C(9) C(10) 1.42(2) 1_555 1_555 yes C(10) C(11) 1.48(2) 1_555 1_555 yes C(11) C(12) 1.21(2) 1_555 1_555 yes C(13) C(14) 1.46(1) 1_555 1_555 yes C(14) C(15) 1.50(2) 1_555 1_555 yes C(15) C(16) 1.35(2) 1_555 1_555 yes C(17) C(18) 1.46(1) 1_555 1_555 yes C(18) C(19) 1.50(1) 1_555 1_555 yes C(19) C(20) 1.51(1) 1_555 1_555 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 Cu(1) I(1) Cu(2) 69.45(4) 1_555 1_555 2_556 yes Cu(1) I(1) Cu(3) 58.7(3) 1_555 1_555 2_556 yes Cu(2) I(1) Cu(3) 19.9(3) 2_556 1_555 2_556 yes Cu(1) I(2) Cu(2) 97.86(3) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 94.9(3) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 54.5(2) 1_555 1_555 2_556 yes Cu(2) I(2) Cu(3) 20.9(4) 1_555 1_555 1_555 yes Cu(2) I(2) Cu(3) 65.5(2) 1_555 1_555 2_556 yes Cu(3) I(2) Cu(3) 50.0(5) 1_555 1_555 2_556 yes I(1) Cu(1) I(2) 112.97(4) 1_555 1_555 1_555 yes I(1) Cu(1) Cu(3) 62.2(3) 1_555 1_555 2_556 yes I(1) Cu(1) S(1) 114.21(4) 1_555 1_555 1_555 yes I(1) Cu(1) N(1) 106.7(1) 1_555 1_555 3_556 yes I(2) Cu(1) Cu(3) 68.6(4) 1_555 1_555 2_556 yes I(2) Cu(1) S(1) 106.56(4) 1_555 1_555 1_555 yes I(2) Cu(1) N(1) 108.7(2) 1_555 1_555 3_556 yes Cu(3) Cu(1) S(1) 88.3(3) 2_556 1_555 1_555 yes Cu(3) Cu(1) N(1) 163.9(3) 2_556 1_555 3_556 yes S(1) Cu(1) N(1) 107.4(2) 1_555 1_555 3_556 yes I(1) Cu(2) I(2) 124.78(4) 2_556 1_555 1_555 yes I(1) Cu(2) Cu(3) 88.7(7) 2_556 1_555 1_555 yes I(1) Cu(2) S(2) 111.06(6) 2_556 1_555 1_555 yes I(2) Cu(2) Cu(3) 73.9(7) 1_555 1_555 1_555 yes I(2) Cu(2) S(2) 116.74(5) 1_555 1_555 1_555 yes Cu(3) Cu(2) S(2) 138.0(7) 1_555 1_555 1_555 yes I(1) Cu(3) I(2) 122.7(5) 2_556 1_555 1_555 yes I(1) Cu(3) I(2) 101.9(4) 2_556 1_555 2_556 yes I(1) Cu(3) Cu(1) 59.1(2) 2_556 1_555 2_556 yes I(1) Cu(3) Cu(2) 71.3(7) 2_556 1_555 1_555 yes I(1) Cu(3) Cu(3) 155.5(9) 2_556 1_555 2_556 yes I(2) Cu(3) I(2) 115.9(6) 1_555 1_555 2_556 yes I(2) Cu(3) Cu(1) 171.8(8) 1_555 1_555 2_556 yes I(2) Cu(3) Cu(2) 85.2(8) 1_555 1_555 1_555 yes I(2) Cu(3) Cu(3) 76.3(5) 1_555 1_555 2_556 yes I(2) Cu(3) Cu(1) 56.8(3) 2_556 1_555 2_556 yes I(2) Cu(3) Cu(2) 156.9(9) 2_556 1_555 1_555 yes I(2) Cu(3) Cu(3) 53.7(5) 2_556 1_555 2_556 yes Cu(1) Cu(3) Cu(2) 102.7(8) 2_556 1_555 1_555 yes Cu(1) Cu(3) Cu(3) 99.9(8) 2_556 1_555 2_556 yes Cu(2) Cu(3) Cu(3) 129.6(9) 1_555 1_555 2_556 yes S(1) Ni(1) S(1) 177.50(9) 1_555 1_555 2_556 yes S(1) Ni(1) S(2) 92.22(5) 1_555 1_555 1_555 yes S(1) Ni(1) S(2) 87.73(5) 1_555 1_555 2_556 yes S(1) Ni(1) S(2) 87.73(5) 2_556 1_555 1_555 yes S(1) Ni(1) S(2) 92.22(5) 2_556 1_555 2_556 yes S(2) Ni(1) S(2) 177.89(10) 1_555 1_555 2_556 yes Cu(1) S(1) Ni(1) 106.89(6) 1_555 1_555 1_555 yes Cu(1) S(1) C(1) 95.7(2) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 102.8(2) 1_555 1_555 1_555 yes Cu(2) S(2) Ni(1) 78.70(6) 1_555 1_555 1_555 yes Cu(2) S(2) C(2) 102.9(2) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 102.9(2) 1_555 1_555 1_555 yes Cu(1) N(1) C(3) 177.2(5) 3_556 1_555 1_555 yes C(5) N(3) C(9) 111.0(7) 1_555 1_555 1_555 yes C(5) N(3) C(13) 106.5(8) 1_555 1_555 1_555 yes C(5) N(3) C(17) 108.4(6) 1_555 1_555 1_555 yes C(9) N(3) C(13) 111.0(7) 1_555 1_555 1_555 yes C(9) N(3) C(17) 106.5(7) 1_555 1_555 1_555 yes C(13) N(3) C(17) 113.5(7) 1_555 1_555 1_555 yes S(1) C(1) C(2) 121.2(4) 1_555 1_555 1_555 yes S(1) C(1) C(3) 116.9(4) 1_555 1_555 1_555 yes C(2) C(1) C(3) 122.0(5) 1_555 1_555 1_555 yes S(2) C(2) C(1) 120.8(4) 1_555 1_555 1_555 yes S(2) C(2) C(4) 116.3(4) 1_555 1_555 1_555 yes C(1) C(2) C(4) 122.9(4) 1_555 1_555 1_555 yes N(1) C(3) C(1) 177.1(6) 1_555 1_555 1_555 yes N(2) C(4) C(2) 177.6(7) 1_555 1_555 1_555 yes N(3) C(5) C(6) 123(1) 1_555 1_555 1_555 yes N(3) C(5) H(1) 106.3(9) 1_555 1_555 1_555 no N(3) C(5) H(2) 105.4(9) 1_555 1_555 1_555 no C(6) C(5) H(1) 107(1) 1_555 1_555 1_555 no C(6) C(5) H(2) 104(1) 1_555 1_555 1_555 no H(1) C(5) H(2) 109(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 121(1) 1_555 1_555 1_555 yes C(5) C(6) H(3) 108(1) 1_555 1_555 1_555 no C(5) C(6) H(4) 104(1) 1_555 1_555 1_555 no C(7) C(6) H(3) 109(1) 1_555 1_555 1_555 no C(7) C(6) H(4) 103(2) 1_555 1_555 1_555 no H(3) C(6) H(4) 107(1) 1_555 1_555 1_555 no C(6) C(7) C(8) 132(2) 1_555 1_555 1_555 yes C(6) C(7) H(5) 106(2) 1_555 1_555 1_555 no C(6) C(7) H(6) 103(1) 1_555 1_555 1_555 no C(8) C(7) H(5) 103(2) 1_555 1_555 1_555 no C(8) C(7) H(6) 98(3) 1_555 1_555 1_555 no H(5) C(7) H(6) 111(2) 1_555 1_555 1_555 no C(7) C(8) H(7) 107(2) 1_555 1_555 1_555 no C(7) C(8) H(8) 113(2) 1_555 1_555 1_555 no C(7) C(8) H(9) 114(3) 1_555 1_555 1_555 no H(7) C(8) H(8) 104(2) 1_555 1_555 1_555 no H(7) C(8) H(9) 103(2) 1_555 1_555 1_555 no H(8) C(8) H(9) 110(2) 1_555 1_555 1_555 no N(3) C(9) C(10) 121.7(9) 1_555 1_555 1_555 yes N(3) C(9) H(10) 106.3(10) 1_555 1_555 1_555 no N(3) C(9) H(11) 106.5(9) 1_555 1_555 1_555 no C(10) C(9) H(10) 106(1) 1_555 1_555 1_555 no C(10) C(9) H(11) 106(1) 1_555 1_555 1_555 no H(10) C(9) H(11) 109(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 116(1) 1_555 1_555 1_555 yes C(9) C(10) H(12) 107(1) 1_555 1_555 1_555 no C(9) C(10) H(13) 107(1) 1_555 1_555 1_555 no C(11) C(10) H(12) 109(1) 1_555 1_555 1_555 no C(11) C(10) H(13) 106(1) 1_555 1_555 1_555 no H(12) C(10) H(13) 110(1) 1_555 1_555 1_555 no C(10) C(11) C(12) 123(1) 1_555 1_555 1_555 yes C(10) C(11) H(14) 108(1) 1_555 1_555 1_555 no C(10) C(11) H(15) 103(1) 1_555 1_555 1_555 no C(12) C(11) H(14) 108(1) 1_555 1_555 1_555 no C(12) C(11) H(15) 101(1) 1_555 1_555 1_555 no H(14) C(11) H(15) 110(1) 1_555 1_555 1_555 no C(11) C(12) H(16) 111(2) 1_555 1_555 1_555 no C(11) C(12) H(17) 113(2) 1_555 1_555 1_555 no C(11) C(12) H(18) 107(2) 1_555 1_555 1_555 no H(16) C(12) H(17) 109(2) 1_555 1_555 1_555 no H(16) C(12) H(18) 107(2) 1_555 1_555 1_555 no H(17) C(12) H(18) 107(2) 1_555 1_555 1_555 no N(3) C(13) C(14) 115.8(9) 1_555 1_555 1_555 yes N(3) C(13) H(19) 107.7(8) 1_555 1_555 1_555 no N(3) C(13) H(20) 107(1) 1_555 1_555 1_555 no C(14) C(13) H(19) 107(1) 1_555 1_555 1_555 no C(14) C(13) H(20) 108(1) 1_555 1_555 1_555 no H(19) C(13) H(20) 109(1) 1_555 1_555 1_555 no C(13) C(14) C(15) 113(1) 1_555 1_555 1_555 yes C(13) C(14) H(21) 107(1) 1_555 1_555 1_555 no C(13) C(14) H(22) 108(1) 1_555 1_555 1_555 no C(15) C(14) H(21) 108(1) 1_555 1_555 1_555 no C(15) C(14) H(22) 108(1) 1_555 1_555 1_555 no H(21) C(14) H(22) 110(1) 1_555 1_555 1_555 no C(14) C(15) C(16) 113(1) 1_555 1_555 1_555 yes C(14) C(15) H(23) 109(1) 1_555 1_555 1_555 no C(14) C(15) H(24) 108(1) 1_555 1_555 1_555 no C(16) C(15) H(23) 108(1) 1_555 1_555 1_555 no C(16) C(15) H(24) 106(1) 1_555 1_555 1_555 no H(23) C(15) H(24) 108(1) 1_555 1_555 1_555 no C(15) C(16) H(25) 106(1) 1_555 1_555 1_555 no C(15) C(16) H(26) 111(1) 1_555 1_555 1_555 no C(15) C(16) H(27) 108(2) 1_555 1_555 1_555 no H(25) C(16) H(26) 111(2) 1_555 1_555 1_555 no H(25) C(16) H(27) 106(1) 1_555 1_555 1_555 no H(26) C(16) H(27) 111(1) 1_555 1_555 1_555 no N(3) C(17) C(18) 117.7(7) 1_555 1_555 1_555 yes N(3) C(17) H(28) 107.1(8) 1_555 1_555 1_555 no N(3) C(17) H(29) 107.8(8) 1_555 1_555 1_555 no C(18) C(17) H(28) 107.1(8) 1_555 1_555 1_555 no C(18) C(17) H(29) 107.6(8) 1_555 1_555 1_555 no H(28) C(17) H(29) 109.4(9) 1_555 1_555 1_555 no C(17) C(18) C(19) 112.5(8) 1_555 1_555 1_555 yes C(17) C(18) H(30) 109.2(8) 1_555 1_555 1_555 no C(17) C(18) H(31) 109.3(8) 1_555 1_555 1_555 no C(19) C(18) H(30) 108.7(8) 1_555 1_555 1_555 no C(19) C(18) H(31) 107.7(8) 1_555 1_555 1_555 no H(30) C(18) H(31) 109.4(8) 1_555 1_555 1_555 no C(18) C(19) C(20) 112.3(9) 1_555 1_555 1_555 yes C(18) C(19) H(32) 109.6(10) 1_555 1_555 1_555 no C(18) C(19) H(33) 108.4(9) 1_555 1_555 1_555 no C(20) C(19) H(32) 108.6(10) 1_555 1_555 1_555 no C(20) C(19) H(33) 107(1) 1_555 1_555 1_555 no H(32) C(19) H(33) 110(1) 1_555 1_555 1_555 no C(19) C(20) H(34) 109(1) 1_555 1_555 1_555 no C(19) C(20) H(35) 108.5(10) 1_555 1_555 1_555 no C(19) C(20) H(36) 108(1) 1_555 1_555 1_555 no H(34) C(20) H(35) 110(1) 1_555 1_555 1_555 no H(34) C(20) H(36) 111(1) 1_555 1_555 1_555 no H(35) C(20) H(36) 108(1) 1_555 1_555 1_555 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 I(1) Cu(1) 2.582(2) 1_555 1_555 ? I(1) Cu(2) 2.5241(9) 1_555 2_556 ? I(1) Cu(3) 2.66(1) 1_555 2_556 ? I(2) Cu(1) 2.643(1) 1_555 1_555 ? I(2) Cu(2) 2.531(1) 1_555 1_555 ? I(2) Cu(3) 2.94(2) 1_555 2_556 ? Cu(1) Cu(3) 2.57(1) 1_555 2_556 ? N(2) C(14) 3.59(2) 1_555 4_555 ? C(12) C(12) 3.59(5) 1_555 3_656 ? I(1) Cu(2) 2.5241(9) 1_555 2_556 ? I(1) Cu(1) 2.582(2) 1_555 1_555 ? I(1) Cu(3) 2.66(1) 1_555 2_556 ? I(2) Cu(2) 2.531(1) 1_555 1_555 ? I(2) Cu(1) 2.643(1) 1_555 1_555 ? I(2) Cu(3) 2.94(2) 1_555 2_556 ? Cu(1) Cu(3) 2.57(1) 1_555 2_556 ? Cu(1) Cu(2) 2.909(1) 1_555 2_556 ? Cu(2) Cu(3) 2.98(1) 1_555 2_556 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #===END data_(TBA)2[Pd(mnt)2(CuI)4] #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 18 21:30:52 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1633.49 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H72 Cu4 I4 N6 Pd S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 29.260(5) _cell_length_b 11.458(7) _cell_length_c 20.714(4) _cell_angle_alpha 90 _cell_angle_beta 122.57(1) _cell_angle_gamma 90 _cell_volume 5852(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.5 _cell_measurement_theta_max 19.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168.00 _exptl_absorpt_coefficient_mu 4.017 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.62 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 3 2 2 2 2 -6 0 4 _diffrn_reflns_number 6855 _reflns_number_total 6727 _reflns_number_gt 3933 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01673 _diffrn_orient_matrix_UB_12 0.07103 _diffrn_orient_matrix_UB_13 0.00703 _diffrn_orient_matrix_UB_21 -0.03271 _diffrn_orient_matrix_UB_22 -0.01025 _diffrn_orient_matrix_UB_23 -0.05285 _diffrn_orient_matrix_UB_31 -0.01718 _diffrn_orient_matrix_UB_32 -0.04966 _diffrn_orient_matrix_UB_33 0.02096 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.86945(2) 0.17252(6) 0.55987(3) 0.0719(2) Uani 1.00 d . . . I(2) I 1.04447(2) 0.22334(5) 0.68539(3) 0.0746(2) Uani 1.00 d . . . Pd(1) Pd 1.0000 -0.09502(6) 0.7500 0.0439(2) Uani 1.00 d S . . Cu(1) Cu 0.96047(4) 0.09754(9) 0.58332(5) 0.0611(3) Uani 1.00 d . . . Cu(2) Cu 1.07665(6) 0.1016(1) 0.80373(6) 0.0747(4) Uani 0.90 d P . . Cu(3) Cu 1.0444(5) 0.154(1) 0.8012(6) 0.069(4) Uiso 0.10 d P . . S(1) S 0.97958(7) -0.0974(2) 0.62614(9) 0.0504(5) Uani 1.00 d . . . S(2) S 1.09129(7) -0.0977(2) 0.79536(9) 0.0551(5) Uani 1.00 d . . . N(1) N 1.0442(3) -0.1040(6) 0.5161(3) 0.064(2) Uani 1.00 d . . . N(2) N 1.1844(3) -0.1205(8) 0.7291(5) 0.093(3) Uani 1.00 d . . . N(3) N 0.3098(3) 0.0104(7) 0.1780(4) 0.081(3) Uani 1.00 d . . . C(1) C 1.0443(3) -0.1021(6) 0.6408(4) 0.051(2) Uani 1.00 d . . . C(2) C 1.0908(3) -0.1049(6) 0.7104(4) 0.050(2) Uani 1.00 d . . . C(3) C 1.0455(3) -0.1031(6) 0.5723(4) 0.053(2) Uani 1.00 d . . . C(4) C 1.1429(3) -0.1110(7) 0.7199(4) 0.061(2) Uani 1.00 d . . . C(5) C 0.2602(6) -0.051(1) 0.1141(8) 0.140(5) Uani 1.00 d . . . C(6) C 0.2197(6) -0.079(2) 0.1259(8) 0.168(7) Uani 1.00 d . . . C(7) C 0.1743(6) -0.156(1) 0.0623(9) 0.169(7) Uani 1.00 d . . . C(8) C 0.138(1) -0.191(2) 0.082(1) 0.27(1) Uani 1.00 d . . . C(9) C 0.3359(6) -0.061(1) 0.2533(9) 0.153(6) Uani 1.00 d . . . C(10) C 0.3847(7) -0.028(2) 0.3194(9) 0.190(7) Uani 1.00 d . . . C(11) C 0.4000(9) -0.095(2) 0.3878(8) 0.220(8) Uani 1.00 d . . . C(12) C 0.436(1) -0.075(2) 0.450(1) 0.28(1) Uani 1.00 d . . . C(13) C 0.3489(6) 0.026(1) 0.1511(9) 0.148(7) Uani 1.00 d . . . C(14) C 0.3773(9) -0.065(2) 0.142(1) 0.22(1) Uani 1.00 d . . . C(15) C 0.409(1) -0.046(3) 0.112(2) 0.31(2) Uani 1.00 d . . . C(16) C 0.456(1) -0.060(3) 0.140(2) 0.31(2) Uani 1.00 d . . . C(17) C 0.2975(5) 0.128(1) 0.1960(7) 0.104(4) Uani 1.00 d . . . C(18) C 0.2732(4) 0.2151(10) 0.1355(6) 0.093(4) Uani 1.00 d . . . C(19) C 0.2673(5) 0.331(1) 0.1620(7) 0.126(5) Uani 1.00 d . . . C(20) C 0.2438(6) 0.424(1) 0.1012(8) 0.142(5) Uani 1.00 d . . . H(1) H 0.2446 -0.0005 0.0687 0.1736 Uiso 1.00 calc . . . H(2) H 0.2720 -0.1207 0.1009 0.1736 Uiso 1.00 calc . . . H(3) H 0.2351 -0.1204 0.1728 0.2170 Uiso 1.00 calc . . . H(4) H 0.2026 -0.0103 0.1280 0.2170 Uiso 1.00 calc . . . H(5) H 0.1550 -0.1154 0.0165 0.1963 Uiso 1.00 calc . . . H(6) H 0.1904 -0.2248 0.0562 0.1963 Uiso 1.00 calc . . . H(7) H 0.1240 -0.1251 0.0901 0.3052 Uiso 1.00 calc . . . H(8) H 0.1128 -0.2397 0.0440 0.3052 Uiso 1.00 calc . . . H(9) H 0.1594 -0.2346 0.1297 0.3052 Uiso 1.00 calc . . . H(10) H 0.3108 -0.0614 0.2685 0.1794 Uiso 1.00 calc . . . H(11) H 0.3408 -0.1382 0.2410 0.1794 Uiso 1.00 calc . . . H(12) H 0.4123 -0.0421 0.3068 0.2318 Uiso 1.00 calc . . . H(13) H 0.3832 0.0485 0.3282 0.2318 Uiso 1.00 calc . . . H(14) H 0.3689 -0.1071 0.3853 0.2879 Uiso 1.00 calc . . . H(15) H 0.4141 -0.1677 0.3798 0.2879 Uiso 1.00 calc . . . H(16) H 0.4326 -0.1350 0.4789 0.3395 Uiso 1.00 calc . . . H(17) H 0.4660 -0.0640 0.4545 0.3395 Uiso 1.00 calc . . . H(18) H 0.4208 -0.0032 0.4599 0.3395 Uiso 1.00 calc . . . H(19) H 0.3288 0.0647 0.1038 0.1796 Uiso 1.00 calc . . . H(20) H 0.3763 0.0775 0.1885 0.1796 Uiso 1.00 calc . . . H(21) H 0.4009 -0.0962 0.1917 0.2656 Uiso 1.00 calc . . . H(22) H 0.3500 -0.1213 0.1111 0.2656 Uiso 1.00 calc . . . H(23) H 0.3936 -0.1184 0.0744 0.3458 Uiso 1.00 calc . . . H(24) H 0.3973 0.0157 0.0861 0.3458 Uiso 1.00 calc . . . H(25) H 0.4693 -0.1349 0.1631 0.4112 Uiso 1.00 calc . . . H(26) H 0.4626 -0.0528 0.0990 0.4112 Uiso 1.00 calc . . . H(27) H 0.4730 -0.0007 0.1750 0.4112 Uiso 1.00 calc . . . H(28) H 0.2736 0.1147 0.2133 0.1320 Uiso 1.00 calc . . . H(29) H 0.3309 0.1576 0.2373 0.1320 Uiso 1.00 calc . . . H(30) H 0.2949 0.2226 0.1138 0.1145 Uiso 1.00 calc . . . H(31) H 0.2378 0.1896 0.0961 0.1145 Uiso 1.00 calc . . . H(32) H 0.2460 0.3257 0.1817 0.1493 Uiso 1.00 calc . . . H(33) H 0.3031 0.3586 0.1996 0.1493 Uiso 1.00 calc . . . H(34) H 0.2421 0.4939 0.1229 0.1682 Uiso 1.00 calc . . . H(35) H 0.2653 0.4316 0.0801 0.1682 Uiso 1.00 calc . . . H(36) H 0.2082 0.3989 0.0623 0.1682 Uiso 1.00 calc . . . 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 I(1) 0.0625(3) 0.1026(5) 0.0493(3) 0.0300(3) 0.0293(2) 0.0092(3) I(2) 0.0812(4) 0.0730(4) 0.0574(3) -0.0140(3) 0.0292(3) 0.0035(3) Pd(1) 0.0572(4) 0.0499(4) 0.0345(3) 0.0000 0.0313(3) 0.0000 Cu(1) 0.0666(6) 0.0816(7) 0.0456(5) 0.0154(5) 0.0370(4) 0.0049(5) Cu(2) 0.088(1) 0.0752(9) 0.0512(7) -0.0111(7) 0.0306(6) -0.0069(6) S(1) 0.0584(10) 0.066(1) 0.0347(8) 0.0008(9) 0.0301(8) -0.0027(8) S(2) 0.060(1) 0.072(1) 0.0393(8) 0.0112(9) 0.0305(8) 0.0088(8) N(1) 0.073(4) 0.084(5) 0.047(3) 0.021(4) 0.041(3) 0.007(3) N(2) 0.070(5) 0.135(7) 0.094(6) 0.020(5) 0.057(4) 0.002(5) N(3) 0.089(5) 0.071(5) 0.081(5) -0.016(4) 0.044(4) 0.012(4) C(1) 0.072(5) 0.055(4) 0.048(4) 0.014(4) 0.046(4) 0.007(3) C(2) 0.056(4) 0.058(4) 0.048(4) 0.007(3) 0.037(3) 0.005(3) C(3) 0.066(4) 0.056(4) 0.049(4) 0.015(4) 0.038(4) 0.013(3) C(4) 0.068(5) 0.067(5) 0.061(5) 0.005(4) 0.043(4) 0.002(4) C(5) 0.15(1) 0.100(9) 0.13(1) -0.045(9) 0.052(10) 0.005(8) C(6) 0.14(1) 0.25(2) 0.12(1) -0.08(1) 0.074(10) -0.02(1) C(7) 0.13(1) 0.17(2) 0.15(1) -0.08(1) 0.04(1) -0.01(1) C(8) 0.28(3) 0.36(3) 0.14(2) -0.16(2) 0.10(2) 0.02(2) C(9) 0.15(1) 0.16(1) 0.13(1) -0.01(1) 0.055(10) 0.06(1) C(10) 0.15(1) 0.19(2) 0.12(1) -0.03(1) 0.00(1) 0.06(1) C(11) 0.24(2) 0.20(2) 0.066(9) -0.03(2) -0.02(1) 0.01(1) C(12) 0.41(4) 0.25(3) 0.16(2) 0.03(3) 0.15(2) 0.03(2) C(13) 0.17(1) 0.17(1) 0.14(1) 0.05(1) 0.11(1) 0.03(1) C(14) 0.25(2) 0.22(2) 0.27(2) 0.13(2) 0.19(2) 0.10(2) C(15) 0.31(3) 0.42(4) 0.35(4) 0.21(3) 0.29(3) 0.17(3) C(16) 0.24(3) 0.32(4) 0.42(4) 0.02(3) 0.22(3) 0.14(3) C(17) 0.100(8) 0.110(9) 0.102(8) -0.021(7) 0.054(7) 0.000(7) C(18) 0.086(7) 0.088(7) 0.093(7) -0.006(6) 0.040(6) 0.008(6) C(19) 0.123(10) 0.12(1) 0.108(10) 0.023(8) 0.048(8) 0.006(8) C(20) 0.14(1) 0.12(1) 0.12(1) 0.010(9) 0.040(9) 0.002(9) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00360(Fo^2^)^2^]' _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 6725 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_shift/su_max 0.0023 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_min -0.81 _refine_diff_density_max 0.95 #------------------------------------------------------------------------------ _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 I(1) Cu(1) 2.583(1) 1_555 1_555 yes I(1) Cu(2) 2.516(1) 1_555 2_756 yes I(1) Cu(3) 2.62(1) 1_555 2_756 yes I(2) Cu(1) 2.645(1) 1_555 1_555 yes I(2) Cu(2) 2.521(1) 1_555 1_555 yes I(2) Cu(3) 2.53(1) 1_555 1_555 yes I(2) Cu(3) 2.87(1) 1_555 2_756 yes Pd(1) S(1) 2.300(2) 1_555 1_555 yes Pd(1) S(1) 2.300(2) 1_555 2_756 yes Pd(1) S(2) 2.306(2) 1_555 1_555 yes Pd(1) S(2) 2.306(2) 1_555 2_756 yes Cu(1) Cu(3) 2.56(1) 1_555 2_756 yes Cu(1) S(1) 2.357(2) 1_555 1_555 yes Cu(1) N(1) 1.991(6) 1_555 3_756 yes Cu(2) Cu(3) 1.10(1) 1_555 1_555 yes Cu(2) S(2) 2.347(2) 1_555 1_555 yes Cu(3) Cu(3) 2.30(2) 1_555 2_756 yes S(1) C(1) 1.749(7) 1_555 1_555 yes S(2) C(2) 1.755(6) 1_555 1_555 yes N(1) C(3) 1.145(8) 1_555 1_555 yes N(2) C(4) 1.129(9) 1_555 1_555 yes N(3) C(5) 1.51(1) 1_555 1_555 yes N(3) C(9) 1.55(1) 1_555 1_555 yes N(3) C(13) 1.53(2) 1_555 1_555 yes N(3) C(17) 1.49(1) 1_555 1_555 yes C(1) C(2) 1.349(9) 1_555 1_555 yes C(1) C(3) 1.437(8) 1_555 1_555 yes C(2) C(4) 1.429(10) 1_555 1_555 yes C(5) C(6) 1.37(2) 1_555 1_555 yes C(6) C(7) 1.55(2) 1_555 1_555 yes C(7) C(8) 1.39(2) 1_555 1_555 yes C(9) C(10) 1.40(2) 1_555 1_555 yes C(10) C(11) 1.45(2) 1_555 1_555 yes C(11) C(12) 1.17(3) 1_555 1_555 yes C(13) C(14) 1.40(2) 1_555 1_555 yes C(14) C(15) 1.39(3) 1_555 1_555 yes C(15) C(16) 1.17(3) 1_555 1_555 yes C(17) C(18) 1.46(1) 1_555 1_555 yes C(18) C(19) 1.48(2) 1_555 1_555 yes C(19) C(20) 1.50(2) 1_555 1_555 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 Cu(1) I(1) Cu(2) 73.86(4) 1_555 1_555 2_756 yes Cu(1) I(1) Cu(3) 58.8(2) 1_555 1_555 2_756 yes Cu(2) I(1) Cu(3) 24.6(3) 2_756 1_555 2_756 yes Cu(1) I(2) Cu(2) 100.11(4) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 96.5(2) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 55.0(2) 1_555 1_555 2_756 yes Cu(2) I(2) Cu(3) 25.2(3) 1_555 1_555 1_555 yes Cu(2) I(2) Cu(3) 68.7(2) 1_555 1_555 2_756 yes Cu(3) I(2) Cu(3) 50.0(4) 1_555 1_555 2_756 yes S(1) Pd(1) S(1) 178.6(1) 1_555 1_555 2_756 yes S(1) Pd(1) S(2) 90.15(6) 1_555 1_555 1_555 yes S(1) Pd(1) S(2) 89.83(6) 1_555 1_555 2_756 yes S(1) Pd(1) S(2) 89.83(6) 2_756 1_555 1_555 yes S(1) Pd(1) S(2) 90.15(6) 2_756 1_555 2_756 yes S(2) Pd(1) S(2) 178.5(1) 1_555 1_555 2_756 yes I(1) Cu(1) I(2) 112.92(4) 1_555 1_555 1_555 yes I(1) Cu(1) Cu(3) 61.3(2) 1_555 1_555 2_756 yes I(1) Cu(1) S(1) 113.43(6) 1_555 1_555 1_555 yes I(1) Cu(1) N(1) 107.7(2) 1_555 1_555 3_756 yes I(2) Cu(1) Cu(3) 67.0(3) 1_555 1_555 2_756 yes I(2) Cu(1) S(1) 106.60(5) 1_555 1_555 1_555 yes I(2) Cu(1) N(1) 108.9(2) 1_555 1_555 3_756 yes Cu(3) Cu(1) S(1) 90.6(3) 2_756 1_555 1_555 yes Cu(3) Cu(1) N(1) 162.1(3) 2_756 1_555 3_756 yes S(1) Cu(1) N(1) 107.1(2) 1_555 1_555 3_756 yes I(1) Cu(2) I(2) 126.40(5) 2_756 1_555 1_555 yes I(1) Cu(2) Cu(3) 83.0(5) 2_756 1_555 1_555 yes I(1) Cu(2) S(2) 111.59(7) 2_756 1_555 1_555 yes I(2) Cu(2) Cu(3) 77.8(5) 1_555 1_555 1_555 yes I(2) Cu(2) S(2) 117.00(6) 1_555 1_555 1_555 yes Cu(3) Cu(2) S(2) 135.9(5) 1_555 1_555 1_555 yes I(1) Cu(3) I(2) 121.7(4) 2_756 1_555 1_555 yes I(1) Cu(3) I(2) 105.0(4) 2_756 1_555 2_756 yes I(1) Cu(3) Cu(1) 59.9(2) 2_756 1_555 2_756 yes I(1) Cu(3) Cu(2) 72.4(5) 2_756 1_555 1_555 yes I(1) Cu(3) Cu(3) 162.2(8) 2_756 1_555 2_756 yes I(2) Cu(3) I(2) 118.0(4) 1_555 1_555 2_756 yes I(2) Cu(3) Cu(1) 175.7(6) 1_555 1_555 2_756 yes I(2) Cu(3) Cu(2) 77.1(6) 1_555 1_555 1_555 yes I(2) Cu(3) Cu(3) 72.7(5) 1_555 1_555 2_756 yes I(2) Cu(3) Cu(1) 58.0(3) 2_756 1_555 2_756 yes I(2) Cu(3) Cu(2) 161.3(7) 2_756 1_555 1_555 yes I(2) Cu(3) Cu(3) 57.2(5) 2_756 1_555 2_756 yes Cu(1) Cu(3) Cu(2) 107.1(7) 2_756 1_555 1_555 yes Cu(1) Cu(3) Cu(3) 105.0(7) 2_756 1_555 2_756 yes Cu(2) Cu(3) Cu(3) 123.9(8) 1_555 1_555 2_756 yes Pd(1) S(1) Cu(1) 105.96(7) 1_555 1_555 1_555 yes Pd(1) S(1) C(1) 101.5(2) 1_555 1_555 1_555 yes Cu(1) S(1) C(1) 96.3(2) 1_555 1_555 1_555 yes Pd(1) S(2) Cu(2) 78.45(7) 1_555 1_555 1_555 yes Pd(1) S(2) C(2) 102.1(2) 1_555 1_555 1_555 yes Cu(2) S(2) C(2) 102.5(2) 1_555 1_555 1_555 yes Cu(1) N(1) C(3) 176.8(6) 3_756 1_555 1_555 yes C(5) N(3) C(9) 111.0(9) 1_555 1_555 1_555 yes C(5) N(3) C(13) 106(1) 1_555 1_555 1_555 yes C(5) N(3) C(17) 113.0(9) 1_555 1_555 1_555 yes C(9) N(3) C(13) 111.6(9) 1_555 1_555 1_555 yes C(9) N(3) C(17) 106.1(10) 1_555 1_555 1_555 yes C(13) N(3) C(17) 108.5(9) 1_555 1_555 1_555 yes S(1) C(1) C(2) 124.2(5) 1_555 1_555 1_555 yes S(1) C(1) C(3) 115.3(5) 1_555 1_555 1_555 yes C(2) C(1) C(3) 120.5(6) 1_555 1_555 1_555 yes S(2) C(2) C(1) 121.9(5) 1_555 1_555 1_555 yes S(2) C(2) C(4) 115.6(5) 1_555 1_555 1_555 yes C(1) C(2) C(4) 122.4(6) 1_555 1_555 1_555 yes N(1) C(3) C(1) 177.3(8) 1_555 1_555 1_555 yes N(2) C(4) C(2) 176.8(9) 1_555 1_555 1_555 yes N(3) C(5) C(6) 117(1) 1_555 1_555 1_555 yes N(3) C(5) H(1) 107.3(10) 1_555 1_555 1_555 no N(3) C(5) H(2) 108(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 107(1) 1_555 1_555 1_555 no C(6) C(5) H(2) 109(1) 1_555 1_555 1_555 no H(1) C(5) H(2) 105(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 114(1) 1_555 1_555 1_555 yes C(5) C(6) H(3) 108(1) 1_555 1_555 1_555 no C(5) C(6) H(4) 109(1) 1_555 1_555 1_555 no C(7) C(6) H(3) 107(1) 1_555 1_555 1_555 no C(7) C(6) H(4) 106(1) 1_555 1_555 1_555 no H(3) C(6) H(4) 109(1) 1_555 1_555 1_555 no C(6) C(7) C(8) 110(1) 1_555 1_555 1_555 yes C(6) C(7) H(5) 110(1) 1_555 1_555 1_555 no C(6) C(7) H(6) 108(1) 1_555 1_555 1_555 no C(8) C(7) H(5) 107(1) 1_555 1_555 1_555 no C(8) C(7) H(6) 107(1) 1_555 1_555 1_555 no H(5) C(7) H(6) 110(1) 1_555 1_555 1_555 no C(7) C(8) H(7) 107(1) 1_555 1_555 1_555 no C(7) C(8) H(8) 108(2) 1_555 1_555 1_555 no C(7) C(8) H(9) 105(2) 1_555 1_555 1_555 no H(7) C(8) H(8) 114(2) 1_555 1_555 1_555 no H(7) C(8) H(9) 110(2) 1_555 1_555 1_555 no H(8) C(8) H(9) 110(2) 1_555 1_555 1_555 no N(3) C(9) C(10) 122(1) 1_555 1_555 1_555 yes N(3) C(9) H(10) 106(1) 1_555 1_555 1_555 no N(3) C(9) H(11) 106(1) 1_555 1_555 1_555 no C(10) C(9) H(10) 104(1) 1_555 1_555 1_555 no C(10) C(9) H(11) 106(1) 1_555 1_555 1_555 no H(10) C(9) H(11) 109(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 115(1) 1_555 1_555 1_555 yes C(9) C(10) H(12) 104(1) 1_555 1_555 1_555 no C(9) C(10) H(13) 108(1) 1_555 1_555 1_555 no C(11) C(10) H(12) 108(1) 1_555 1_555 1_555 no C(11) C(10) H(13) 109(1) 1_555 1_555 1_555 no H(12) C(10) H(13) 110(1) 1_555 1_555 1_555 no C(10) C(11) C(12) 127(2) 1_555 1_555 1_555 yes C(10) C(11) H(14) 104(1) 1_555 1_555 1_555 no C(10) C(11) H(15) 102(1) 1_555 1_555 1_555 no C(12) C(11) H(14) 111(2) 1_555 1_555 1_555 no C(12) C(11) H(15) 98(2) 1_555 1_555 1_555 no H(14) C(11) H(15) 111(2) 1_555 1_555 1_555 no C(11) C(12) H(16) 102(3) 1_555 1_555 1_555 no C(11) C(12) H(17) 113(2) 1_555 1_555 1_555 no C(11) C(12) H(18) 98(2) 1_555 1_555 1_555 no H(16) C(12) H(17) 119(3) 1_555 1_555 1_555 no H(16) C(12) H(18) 105(2) 1_555 1_555 1_555 no H(17) C(12) H(18) 113(2) 1_555 1_555 1_555 no N(3) C(13) C(14) 125(1) 1_555 1_555 1_555 yes N(3) C(13) H(19) 105(1) 1_555 1_555 1_555 no N(3) C(13) H(20) 103(1) 1_555 1_555 1_555 no C(14) C(13) H(19) 107(1) 1_555 1_555 1_555 no C(14) C(13) H(20) 105(1) 1_555 1_555 1_555 no H(19) C(13) H(20) 108(1) 1_555 1_555 1_555 no C(13) C(14) C(15) 122(2) 1_555 1_555 1_555 yes C(13) C(14) H(21) 105(1) 1_555 1_555 1_555 no C(13) C(14) H(22) 104(1) 1_555 1_555 1_555 no C(15) C(14) H(21) 105(2) 1_555 1_555 1_555 no C(15) C(14) H(22) 108(2) 1_555 1_555 1_555 no H(21) C(14) H(22) 109(2) 1_555 1_555 1_555 no C(14) C(15) C(16) 130(3) 1_555 1_555 1_555 yes C(14) C(15) H(23) 95(2) 1_555 1_555 1_555 no C(14) C(15) H(24) 105(1) 1_555 1_555 1_555 no C(16) C(15) H(23) 100(3) 1_555 1_555 1_555 no C(16) C(15) H(24) 113(4) 1_555 1_555 1_555 no H(23) C(15) H(24) 108(3) 1_555 1_555 1_555 no C(15) C(16) H(25) 115(3) 1_555 1_555 1_555 no C(15) C(16) H(26) 107(3) 1_555 1_555 1_555 no C(15) C(16) H(27) 106(4) 1_555 1_555 1_555 no H(25) C(16) H(26) 107(3) 1_555 1_555 1_555 no H(25) C(16) H(27) 110(3) 1_555 1_555 1_555 no H(26) C(16) H(27) 109(2) 1_555 1_555 1_555 no N(3) C(17) C(18) 118.6(10) 1_555 1_555 1_555 yes N(3) C(17) H(28) 106.1(10) 1_555 1_555 1_555 no N(3) C(17) H(29) 106(1) 1_555 1_555 1_555 no C(18) C(17) H(28) 108(1) 1_555 1_555 1_555 no C(18) C(17) H(29) 108(1) 1_555 1_555 1_555 no H(28) C(17) H(29) 108(1) 1_555 1_555 1_555 no C(17) C(18) C(19) 113(1) 1_555 1_555 1_555 yes C(17) C(18) H(30) 108.9(10) 1_555 1_555 1_555 no C(17) C(18) H(31) 109.1(10) 1_555 1_555 1_555 no C(19) C(18) H(30) 109(1) 1_555 1_555 1_555 no C(19) C(18) H(31) 107(1) 1_555 1_555 1_555 no H(30) C(18) H(31) 108(1) 1_555 1_555 1_555 no C(18) C(19) C(20) 114(1) 1_555 1_555 1_555 yes C(18) C(19) H(32) 110(1) 1_555 1_555 1_555 no C(18) C(19) H(33) 107(1) 1_555 1_555 1_555 no C(20) C(19) H(32) 107(1) 1_555 1_555 1_555 no C(20) C(19) H(33) 104(1) 1_555 1_555 1_555 no H(32) C(19) H(33) 111(1) 1_555 1_555 1_555 no C(19) C(20) H(34) 108(1) 1_555 1_555 1_555 no C(19) C(20) H(35) 109(1) 1_555 1_555 1_555 no C(19) C(20) H(36) 107(1) 1_555 1_555 1_555 no H(34) C(20) H(35) 111(1) 1_555 1_555 1_555 no H(34) C(20) H(36) 110(1) 1_555 1_555 1_555 no H(35) C(20) H(36) 109(1) 1_555 1_555 1_555 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 I(1) Cu(1) 2.583(1) 1_555 1_555 ? I(1) Cu(2) 2.516(1) 1_555 2_756 ? I(1) Cu(3) 2.62(1) 1_555 2_756 ? I(2) Cu(1) 2.645(1) 1_555 1_555 ? I(2) Cu(2) 2.521(1) 1_555 1_555 ? I(2) Cu(3) 2.53(1) 1_555 1_555 ? I(2) Cu(3) 2.87(1) 1_555 2_756 ? Cu(1) Cu(3) 2.56(1) 1_555 2_756 ? I(1) Cu(2) 2.516(1) 1_555 2_756 ? I(1) Cu(1) 2.583(1) 1_555 1_555 ? I(2) Cu(2) 2.521(1) 1_555 1_555 ? I(2) Cu(1) 2.645(1) 1_555 1_555 ? Pd(1) Cu(2) 2.942(1) 1_555 1_555 ? Pd(1) Cu(2) 2.942(1) 1_555 2_756 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #===END data_(TBA)[PtCu2I2(mnt)] #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 18 22:01:51 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1722.18 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H72 Cu4 I4 N6 Pt S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 29.179(3) _cell_length_b 11.462(4) _cell_length_c 20.735(2) _cell_angle_alpha 90 _cell_angle_beta 122.602(6) _cell_angle_gamma 90 _cell_volume 5841(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.6 _cell_measurement_theta_max 20.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296.00 _exptl_absorpt_coefficient_mu 6.098 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.60 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -6 -1 -1 -4 3 -1 -5 _diffrn_reflns_number 6835 _reflns_number_total 6706 _reflns_number_gt 4201 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.099 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00323 _diffrn_orient_matrix_UB_12 -0.08603 _diffrn_orient_matrix_UB_13 -0.00461 _diffrn_orient_matrix_UB_21 -0.03683 _diffrn_orient_matrix_UB_22 -0.01160 _diffrn_orient_matrix_UB_23 -0.00846 _diffrn_orient_matrix_UB_31 -0.01698 _diffrn_orient_matrix_UB_32 0.00877 _diffrn_orient_matrix_UB_33 -0.05643 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt 1.0000 -0.09388(4) 0.2500 0.0458(1) Uani 1.00 d S . . I(1) I 1.13136(2) 0.17052(7) 0.43897(3) 0.0741(2) Uani 1.00 d . . . I(2) I 0.95691(3) 0.22417(6) 0.31517(3) 0.0733(2) Uani 1.00 d . . . Cu(1) Cu 1.04084(4) 0.0981(1) 0.41890(6) 0.0635(3) Uani 1.00 d . . . Cu(2) Cu 0.9308(1) 0.1044(2) 0.19697(9) 0.0851(7) Uani 0.78 d P . . Cu(3) Cu 0.9573(3) 0.1515(7) 0.2020(3) 0.059(2) Uiso 0.22 d P . . S(1) S 1.02022(8) -0.0968(2) 0.37345(10) 0.0524(5) Uani 1.00 d . . . S(2) S 0.90865(8) -0.0985(2) 0.2044(1) 0.0564(6) Uani 1.00 d . . . N(1) N 0.9552(3) -0.1028(7) 0.4825(4) 0.066(2) Uani 1.00 d . . . N(2) N 0.8155(4) -0.1218(9) 0.2712(5) 0.094(3) Uani 1.00 d . . . N(3) N 1.1908(3) -0.4879(8) 0.8221(5) 0.081(3) Uani 1.00 d . . . C(1) C 0.9557(3) -0.1014(7) 0.3592(4) 0.053(2) Uani 1.00 d . . . C(2) C 0.9094(3) -0.1052(7) 0.2889(4) 0.055(2) Uani 1.00 d . . . C(3) C 0.9541(3) -0.1033(8) 0.4269(4) 0.055(2) Uani 1.00 d . . . C(4) C 0.8572(4) -0.1112(8) 0.2798(5) 0.061(3) Uani 1.00 d . . . C(5) C 1.1528(8) -0.475(2) 0.852(1) 0.158(8) Uani 1.00 d . . . C(6) C 1.125(1) -0.564(2) 0.861(1) 0.20(1) Uani 1.00 d . . . C(7) C 1.089(1) -0.542(3) 0.887(2) 0.26(2) Uani 1.00 d . . . C(8) C 1.044(1) -0.561(4) 0.863(2) 0.28(2) Uani 1.00 d . . . C(9) C 1.1645(7) -0.563(2) 0.7490(9) 0.147(7) Uani 1.00 d . . . C(10) C 1.1145(8) -0.529(2) 0.680(1) 0.177(8) Uani 1.00 d . . . C(11) C 1.098(1) -0.600(2) 0.609(1) 0.29(1) Uani 1.00 d . . . C(12) C 1.064(2) -0.583(3) 0.549(2) 0.31(2) Uani 1.00 d . . . C(13) C 1.2016(5) -0.371(1) 0.8037(7) 0.105(5) Uani 1.00 d . . . C(14) C 1.2274(5) -0.283(1) 0.8638(7) 0.106(5) Uani 1.00 d . . . C(15) C 1.2319(7) -0.166(2) 0.8372(9) 0.145(7) Uani 1.00 d . . . C(16) C 1.2559(7) -0.078(2) 0.8963(10) 0.153(7) Uani 1.00 d . . . C(17) C 1.2410(7) -0.544(1) 0.884(1) 0.164(7) Uani 1.00 d . . . C(18) C 1.2809(7) -0.584(2) 0.8734(9) 0.182(9) Uani 1.00 d . . . C(19) C 1.3277(7) -0.658(2) 0.936(1) 0.171(8) Uani 1.00 d . . . C(20) C 1.364(1) -0.693(2) 0.921(1) 0.24(1) Uani 1.00 d . . . H(1) H 1.1754 -0.4434 0.9023 0.1914 Uiso 1.00 calc . . . H(2) H 1.1261 -0.4212 0.8198 0.1914 Uiso 1.00 calc . . . H(3) H 1.1022 -0.5963 0.8119 0.2300 Uiso 1.00 calc . . . H(4) H 1.1517 -0.6190 0.8941 0.2300 Uiso 1.00 calc . . . H(5) H 1.1056 -0.6071 0.9303 0.3031 Uiso 1.00 calc . . . H(6) H 1.0993 -0.4750 0.9110 0.3031 Uiso 1.00 calc . . . H(7) H 1.0366 -0.5455 0.8999 0.4046 Uiso 1.00 calc . . . H(8) H 1.0272 -0.5028 0.8226 0.4046 Uiso 1.00 calc . . . H(9) H 1.0335 -0.6350 0.8416 0.4046 Uiso 1.00 calc . . . H(10) H 1.1916 -0.5686 0.7356 0.1754 Uiso 1.00 calc . . . H(11) H 1.1597 -0.6384 0.7633 0.1754 Uiso 1.00 calc . . . H(12) H 1.0873 -0.5335 0.6921 0.2159 Uiso 1.00 calc . . . H(13) H 1.1187 -0.4527 0.6689 0.2159 Uiso 1.00 calc . . . H(14) H 1.1284 -0.6231 0.6123 0.3301 Uiso 1.00 calc . . . H(15) H 1.0815 -0.6725 0.6186 0.3301 Uiso 1.00 calc . . . H(16) H 1.0795 -0.5181 0.5359 0.4010 Uiso 1.00 calc . . . H(17) H 1.0636 -0.6489 0.5194 0.4010 Uiso 1.00 calc . . . H(18) H 1.0325 -0.5667 0.5424 0.4010 Uiso 1.00 calc . . . H(19) H 1.2246 -0.3817 0.7843 0.1263 Uiso 1.00 calc . . . H(20) H 1.1677 -0.3398 0.7637 0.1263 Uiso 1.00 calc . . . H(21) H 1.2063 -0.2763 0.8861 0.1263 Uiso 1.00 calc . . . H(22) H 1.2628 -0.3096 0.9012 0.1263 Uiso 1.00 calc . . . H(23) H 1.2533 -0.1744 0.8159 0.1697 Uiso 1.00 calc . . . H(24) H 1.1962 -0.1421 0.7989 0.1697 Uiso 1.00 calc . . . H(25) H 1.2919 -0.1009 0.9350 0.1865 Uiso 1.00 calc . . . H(26) H 1.2571 -0.0063 0.8745 0.1865 Uiso 1.00 calc . . . H(27) H 1.2348 -0.0692 0.9184 0.1865 Uiso 1.00 calc . . . H(28) H 1.2580 -0.4874 0.9247 0.1949 Uiso 1.00 calc . . . H(29) H 1.2289 -0.6074 0.9016 0.1949 Uiso 1.00 calc . . . H(30) H 1.2627 -0.6353 0.8292 0.2314 Uiso 1.00 calc . . . H(31) H 1.2964 -0.5220 0.8640 0.2314 Uiso 1.00 calc . . . H(32) H 1.3468 -0.6107 0.9805 0.2093 Uiso 1.00 calc . . . H(33) H 1.3126 -0.7236 0.9469 0.2093 Uiso 1.00 calc . . . H(34) H 1.3902 -0.7413 0.9626 0.2762 Uiso 1.00 calc . . . H(35) H 1.3444 -0.7470 0.8765 0.2762 Uiso 1.00 calc . . . H(36) H 1.3787 -0.6342 0.9101 0.2762 Uiso 1.00 calc . . . 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 Pt(1) 0.0591(3) 0.0537(3) 0.0334(2) 0.0000 0.0307(2) 0.0000 I(1) 0.0612(4) 0.1094(5) 0.0485(3) -0.0283(4) 0.0274(3) -0.0054(3) I(2) 0.0804(4) 0.0781(4) 0.0551(3) 0.0141(3) 0.0322(3) -0.0032(3) Cu(1) 0.0702(6) 0.0864(8) 0.0461(5) -0.0171(6) 0.0392(5) -0.0064(5) Cu(2) 0.112(2) 0.079(1) 0.0483(9) 0.020(2) 0.0328(10) 0.0046(8) S(1) 0.063(1) 0.067(1) 0.0338(8) -0.003(1) 0.0307(8) 0.0013(9) S(2) 0.061(1) 0.077(1) 0.0363(9) -0.012(1) 0.0297(9) -0.0072(10) N(1) 0.078(5) 0.084(5) 0.049(4) -0.024(4) 0.044(4) -0.011(4) N(2) 0.078(6) 0.125(8) 0.095(6) -0.007(6) 0.057(5) 0.011(6) N(3) 0.082(6) 0.080(6) 0.072(5) 0.018(5) 0.035(4) -0.012(5) C(1) 0.066(5) 0.058(5) 0.043(4) -0.008(4) 0.036(4) -0.001(4) C(2) 0.067(5) 0.064(5) 0.045(4) -0.015(4) 0.038(4) -0.009(4) C(3) 0.063(5) 0.071(5) 0.041(4) -0.019(4) 0.035(4) -0.008(4) C(4) 0.069(6) 0.071(6) 0.052(4) -0.011(5) 0.039(4) -0.006(4) C(5) 0.19(2) 0.18(2) 0.16(1) -0.04(1) 0.13(1) -0.04(1) C(6) 0.24(2) 0.21(2) 0.24(2) -0.10(2) 0.18(2) -0.09(2) C(7) 0.29(4) 0.33(4) 0.33(4) -0.13(3) 0.27(4) -0.10(3) C(8) 0.18(3) 0.36(5) 0.28(3) 0.03(3) 0.10(3) -0.09(3) C(9) 0.15(1) 0.17(2) 0.10(1) 0.00(1) 0.05(1) -0.05(1) C(10) 0.15(1) 0.17(2) 0.14(1) 0.03(1) 0.03(1) -0.04(1) C(11) 0.37(4) 0.16(2) 0.09(1) 0.03(2) -0.04(2) -0.01(1) C(12) 0.45(6) 0.25(3) 0.20(3) 0.06(3) 0.16(3) 0.07(3) C(13) 0.114(10) 0.11(1) 0.096(9) 0.023(8) 0.059(8) 0.012(8) C(14) 0.093(9) 0.12(1) 0.090(8) -0.002(8) 0.038(7) -0.019(8) C(15) 0.16(1) 0.13(1) 0.12(1) -0.05(1) 0.06(1) 0.00(1) C(16) 0.15(1) 0.13(1) 0.13(1) -0.02(1) 0.04(1) 0.01(1) C(17) 0.13(1) 0.11(1) 0.17(2) 0.03(1) 0.03(1) 0.00(1) C(18) 0.13(1) 0.33(3) 0.11(1) 0.09(2) 0.08(1) 0.02(1) C(19) 0.11(1) 0.20(2) 0.14(1) 0.07(1) 0.03(1) -0.01(1) C(20) 0.24(3) 0.31(3) 0.14(2) 0.12(2) 0.09(2) 0.00(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on 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 calculated 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. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00360(Fo^2^)^2^]' _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 6706 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_shift/su_max 0.0060 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_min -0.81 _refine_diff_density_max 0.87 #------------------------------------------------------------------------------ _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 Pt(1) Cu(2) 2.838(2) 1_555 1_555 yes Pt(1) Cu(2) 2.838(2) 1_555 2_755 yes Pt(1) S(1) 2.296(2) 1_555 1_555 yes Pt(1) S(1) 2.296(2) 1_555 2_755 yes Pt(1) S(2) 2.299(2) 1_555 1_555 yes Pt(1) S(2) 2.299(2) 1_555 2_755 yes I(1) Cu(1) 2.580(1) 1_555 1_555 yes I(1) Cu(2) 2.510(2) 1_555 2_755 yes I(1) Cu(3) 2.672(6) 1_555 2_755 yes I(2) Cu(1) 2.652(1) 1_555 1_555 yes I(2) Cu(2) 2.542(2) 1_555 1_555 yes I(2) Cu(3) 2.496(5) 1_555 1_555 yes I(2) Cu(3) 2.836(8) 1_555 2_755 yes Cu(1) Cu(3) 2.609(6) 1_555 2_755 yes Cu(1) S(1) 2.372(3) 1_555 1_555 yes Cu(1) N(1) 1.985(6) 1_555 3_756 yes Cu(2) Cu(3) 0.903(6) 1_555 1_555 yes Cu(2) S(2) 2.441(4) 1_555 1_555 yes Cu(3) Cu(3) 2.19(1) 1_555 2_755 yes S(1) C(1) 1.743(8) 1_555 1_555 yes S(2) C(2) 1.743(7) 1_555 1_555 yes N(1) C(3) 1.137(9) 1_555 1_555 yes N(2) C(4) 1.14(1) 1_555 1_555 yes N(3) C(5) 1.55(2) 1_555 1_555 yes N(3) C(9) 1.54(2) 1_555 1_555 yes N(3) C(13) 1.47(2) 1_555 1_555 yes N(3) C(17) 1.48(2) 1_555 1_555 yes C(1) C(2) 1.35(1) 1_555 1_555 yes C(1) C(3) 1.428(9) 1_555 1_555 yes C(2) C(4) 1.43(1) 1_555 1_555 yes C(5) C(6) 1.38(2) 1_555 1_555 yes C(6) C(7) 1.43(3) 1_555 1_555 yes C(7) C(8) 1.14(3) 1_555 1_555 yes C(9) C(10) 1.43(2) 1_555 1_555 yes C(10) C(11) 1.51(3) 1_555 1_555 yes C(11) C(12) 1.12(3) 1_555 1_555 yes C(13) C(14) 1.46(2) 1_555 1_555 yes C(14) C(15) 1.48(2) 1_555 1_555 yes C(15) C(16) 1.45(2) 1_555 1_555 yes C(17) C(18) 1.38(2) 1_555 1_555 yes C(18) C(19) 1.54(2) 1_555 1_555 yes C(19) C(20) 1.31(3) 1_555 1_555 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 Cu(2) Pt(1) Cu(2) 73.6(2) 1_555 1_555 2_755 yes Cu(2) Pt(1) S(1) 98.36(7) 1_555 1_555 1_555 yes Cu(2) Pt(1) S(1) 82.98(6) 1_555 1_555 2_755 yes Cu(2) Pt(1) S(2) 55.5(1) 1_555 1_555 1_555 yes Cu(2) Pt(1) S(2) 127.1(1) 1_555 1_555 2_755 yes Cu(2) Pt(1) S(1) 82.98(6) 2_755 1_555 1_555 yes Cu(2) Pt(1) S(1) 98.36(7) 2_755 1_555 2_755 yes Cu(2) Pt(1) S(2) 127.1(1) 2_755 1_555 1_555 yes Cu(2) Pt(1) S(2) 55.5(1) 2_755 1_555 2_755 yes S(1) Pt(1) S(1) 178.3(1) 1_555 1_555 2_755 yes S(1) Pt(1) S(2) 90.16(7) 1_555 1_555 1_555 yes S(1) Pt(1) S(2) 89.80(7) 1_555 1_555 2_755 yes S(1) Pt(1) S(2) 89.80(7) 2_755 1_555 1_555 yes S(1) Pt(1) S(2) 90.16(7) 2_755 1_555 2_755 yes S(2) Pt(1) S(2) 177.4(1) 1_555 1_555 2_755 yes Cu(1) I(1) Cu(2) 70.35(7) 1_555 1_555 2_755 yes Cu(1) I(1) Cu(3) 59.5(1) 1_555 1_555 2_755 yes Cu(2) I(1) Cu(3) 19.7(1) 2_755 1_555 2_755 yes Cu(1) I(2) Cu(2) 98.82(5) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 96.3(1) 1_555 1_555 1_555 yes Cu(1) I(2) Cu(3) 56.7(1) 1_555 1_555 2_755 yes Cu(2) I(2) Cu(3) 20.6(1) 1_555 1_555 1_555 yes Cu(2) I(2) Cu(3) 63.0(1) 1_555 1_555 2_755 yes Cu(3) I(2) Cu(3) 48.1(2) 1_555 1_555 2_755 yes I(1) Cu(1) I(2) 111.92(5) 1_555 1_555 1_555 yes I(1) Cu(1) Cu(3) 62.0(1) 1_555 1_555 2_755 yes I(1) Cu(1) S(1) 112.67(7) 1_555 1_555 1_555 yes I(1) Cu(1) N(1) 109.8(2) 1_555 1_555 3_756 yes I(2) Cu(1) Cu(3) 65.2(2) 1_555 1_555 2_755 yes I(2) Cu(1) S(1) 105.37(6) 1_555 1_555 1_555 yes I(2) Cu(1) N(1) 109.7(2) 1_555 1_555 3_756 yes Cu(3) Cu(1) S(1) 88.4(2) 2_755 1_555 1_555 yes Cu(3) Cu(1) N(1) 164.4(3) 2_755 1_555 3_756 yes S(1) Cu(1) N(1) 107.2(2) 1_555 1_555 3_756 yes Pt(1) Cu(2) I(1) 127.58(6) 1_555 1_555 2_755 yes Pt(1) Cu(2) I(2) 106.15(6) 1_555 1_555 1_555 yes Pt(1) Cu(2) Cu(3) 92.8(4) 1_555 1_555 1_555 yes Pt(1) Cu(2) S(2) 50.96(6) 1_555 1_555 1_555 yes I(1) Cu(2) I(2) 125.39(8) 2_755 1_555 1_555 yes I(1) Cu(2) Cu(3) 90.3(4) 2_755 1_555 1_555 yes I(1) Cu(2) S(2) 107.6(1) 2_755 1_555 1_555 yes I(2) Cu(2) Cu(3) 76.8(4) 1_555 1_555 1_555 yes I(2) Cu(2) S(2) 113.9(1) 1_555 1_555 1_555 yes Cu(3) Cu(2) S(2) 143.4(4) 1_555 1_555 1_555 yes I(1) Cu(3) I(2) 120.6(2) 2_755 1_555 1_555 yes I(1) Cu(3) I(2) 103.8(2) 2_755 1_555 2_755 yes I(1) Cu(3) Cu(1) 58.5(1) 2_755 1_555 2_755 yes I(1) Cu(3) Cu(2) 70.0(4) 2_755 1_555 1_555 yes I(1) Cu(3) Cu(3) 161.6(5) 2_755 1_555 2_755 yes I(2) Cu(3) I(2) 118.2(3) 1_555 1_555 2_755 yes I(2) Cu(3) Cu(1) 174.0(4) 1_555 1_555 2_755 yes I(2) Cu(3) Cu(2) 82.6(4) 1_555 1_555 1_555 yes I(2) Cu(3) Cu(3) 74.1(3) 1_555 1_555 2_755 yes I(2) Cu(3) Cu(1) 58.1(1) 2_755 1_555 2_755 yes I(2) Cu(3) Cu(2) 157.0(5) 2_755 1_555 1_555 yes I(2) Cu(3) Cu(3) 57.8(3) 2_755 1_555 2_755 yes Cu(1) Cu(3) Cu(2) 102.0(5) 2_755 1_555 1_555 yes Cu(1) Cu(3) Cu(3) 105.7(4) 2_755 1_555 2_755 yes Cu(2) Cu(3) Cu(3) 126.0(5) 1_555 1_555 2_755 yes Pt(1) S(1) Cu(1) 106.68(8) 1_555 1_555 1_555 yes Pt(1) S(1) C(1) 101.9(2) 1_555 1_555 1_555 yes Cu(1) S(1) C(1) 96.6(3) 1_555 1_555 1_555 yes Pt(1) S(2) Cu(2) 73.50(9) 1_555 1_555 1_555 yes Pt(1) S(2) C(2) 101.8(3) 1_555 1_555 1_555 yes Cu(2) S(2) C(2) 104.2(3) 1_555 1_555 1_555 yes Cu(1) N(1) C(3) 178.0(7) 3_756 1_555 1_555 yes C(5) N(3) C(9) 111(1) 1_555 1_555 1_555 yes C(5) N(3) C(13) 108(1) 1_555 1_555 1_555 yes C(5) N(3) C(17) 106(1) 1_555 1_555 1_555 yes C(9) N(3) C(13) 108(1) 1_555 1_555 1_555 yes C(9) N(3) C(17) 110(1) 1_555 1_555 1_555 yes C(13) N(3) C(17) 111(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 122.9(6) 1_555 1_555 1_555 yes S(1) C(1) C(3) 115.9(6) 1_555 1_555 1_555 yes C(2) C(1) C(3) 121.1(7) 1_555 1_555 1_555 yes S(2) C(2) C(1) 123.1(6) 1_555 1_555 1_555 yes S(2) C(2) C(4) 115.7(6) 1_555 1_555 1_555 yes C(1) C(2) C(4) 121.1(7) 1_555 1_555 1_555 yes N(1) C(3) C(1) 177.0(9) 1_555 1_555 1_555 yes N(2) C(4) C(2) 176(1) 1_555 1_555 1_555 yes N(3) C(5) C(6) 125(1) 1_555 1_555 1_555 yes N(3) C(5) H(1) 104(1) 1_555 1_555 1_555 no N(3) C(5) H(2) 105(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 104(1) 1_555 1_555 1_555 no C(6) C(5) H(2) 105(2) 1_555 1_555 1_555 no H(1) C(5) H(2) 111(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 121(2) 1_555 1_555 1_555 yes C(5) C(6) H(3) 105(2) 1_555 1_555 1_555 no C(5) C(6) H(4) 105(2) 1_555 1_555 1_555 no C(7) C(6) H(3) 104(2) 1_555 1_555 1_555 no C(7) C(6) H(4) 109(2) 1_555 1_555 1_555 no H(3) C(6) H(4) 110(2) 1_555 1_555 1_555 no C(6) C(7) C(8) 134(3) 1_555 1_555 1_555 yes C(6) C(7) H(5) 96(2) 1_555 1_555 1_555 no C(6) C(7) H(6) 106(1) 1_555 1_555 1_555 no C(8) C(7) H(5) 97(3) 1_555 1_555 1_555 no C(8) C(7) H(6) 111(4) 1_555 1_555 1_555 no H(5) C(7) H(6) 106(3) 1_555 1_555 1_555 no C(7) C(8) H(7) 109(3) 1_555 1_555 1_555 no C(7) C(8) H(8) 100(4) 1_555 1_555 1_555 no C(7) C(8) H(9) 112(3) 1_555 1_555 1_555 no H(7) C(8) H(8) 110(3) 1_555 1_555 1_555 no H(7) C(8) H(9) 113(4) 1_555 1_555 1_555 no H(8) C(8) H(9) 108(3) 1_555 1_555 1_555 no N(3) C(9) C(10) 121(1) 1_555 1_555 1_555 yes N(3) C(9) H(10) 105(1) 1_555 1_555 1_555 no N(3) C(9) H(11) 106(1) 1_555 1_555 1_555 no C(10) C(9) H(10) 106(1) 1_555 1_555 1_555 no C(10) C(9) H(11) 107(1) 1_555 1_555 1_555 no H(10) C(9) H(11) 107(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 116(1) 1_555 1_555 1_555 yes C(9) C(10) H(12) 106(1) 1_555 1_555 1_555 no C(9) C(10) H(13) 107(1) 1_555 1_555 1_555 no C(11) C(10) H(12) 110(2) 1_555 1_555 1_555 no C(11) C(10) H(13) 105(2) 1_555 1_555 1_555 no H(12) C(10) H(13) 111(1) 1_555 1_555 1_555 no C(10) C(11) C(12) 128(3) 1_555 1_555 1_555 yes C(10) C(11) H(14) 107(2) 1_555 1_555 1_555 no C(10) C(11) H(15) 100(2) 1_555 1_555 1_555 no C(12) C(11) H(14) 111(4) 1_555 1_555 1_555 no C(12) C(11) H(15) 97(3) 1_555 1_555 1_555 no H(14) C(11) H(15) 106(2) 1_555 1_555 1_555 no C(11) C(12) H(16) 100(4) 1_555 1_555 1_555 no C(11) C(12) H(17) 105(3) 1_555 1_555 1_555 no C(11) C(12) H(18) 115(4) 1_555 1_555 1_555 no H(16) C(12) H(17) 105(3) 1_555 1_555 1_555 no H(16) C(12) H(18) 113(3) 1_555 1_555 1_555 no H(17) C(12) H(18) 114(4) 1_555 1_555 1_555 no N(3) C(13) C(14) 119(1) 1_555 1_555 1_555 yes N(3) C(13) H(19) 107(1) 1_555 1_555 1_555 no N(3) C(13) H(20) 107(1) 1_555 1_555 1_555 no C(14) C(13) H(19) 106(1) 1_555 1_555 1_555 no C(14) C(13) H(20) 106(1) 1_555 1_555 1_555 no H(19) C(13) H(20) 108(1) 1_555 1_555 1_555 no C(13) C(14) C(15) 114(1) 1_555 1_555 1_555 yes C(13) C(14) H(21) 107(1) 1_555 1_555 1_555 no C(13) C(14) H(22) 107(1) 1_555 1_555 1_555 no C(15) C(14) H(21) 108(1) 1_555 1_555 1_555 no C(15) C(14) H(22) 108(1) 1_555 1_555 1_555 no H(21) C(14) H(22) 109(1) 1_555 1_555 1_555 no C(14) C(15) C(16) 114(1) 1_555 1_555 1_555 yes C(14) C(15) H(23) 107(1) 1_555 1_555 1_555 no C(14) C(15) H(24) 107(1) 1_555 1_555 1_555 no C(16) C(15) H(23) 108(1) 1_555 1_555 1_555 no C(16) C(15) H(24) 108(1) 1_555 1_555 1_555 no H(23) C(15) H(24) 109(1) 1_555 1_555 1_555 no C(15) C(16) H(25) 109(1) 1_555 1_555 1_555 no C(15) C(16) H(26) 109(1) 1_555 1_555 1_555 no C(15) C(16) H(27) 109(1) 1_555 1_555 1_555 no H(25) C(16) H(26) 109(1) 1_555 1_555 1_555 no H(25) C(16) H(27) 109(1) 1_555 1_555 1_555 no H(26) C(16) H(27) 109(1) 1_555 1_555 1_555 no N(3) C(17) C(18) 121(1) 1_555 1_555 1_555 yes N(3) C(17) H(28) 105(1) 1_555 1_555 1_555 no N(3) C(17) H(29) 105(1) 1_555 1_555 1_555 no C(18) C(17) H(28) 106(1) 1_555 1_555 1_555 no C(18) C(17) H(29) 109(1) 1_555 1_555 1_555 no H(28) C(17) H(29) 107(2) 1_555 1_555 1_555 no C(17) C(18) C(19) 119(1) 1_555 1_555 1_555 yes C(17) C(18) H(30) 105(1) 1_555 1_555 1_555 no C(17) C(18) H(31) 109(2) 1_555 1_555 1_555 no C(19) C(18) H(30) 104(1) 1_555 1_555 1_555 no C(19) C(18) H(31) 107(1) 1_555 1_555 1_555 no H(30) C(18) H(31) 110(1) 1_555 1_555 1_555 no C(18) C(19) C(20) 115(2) 1_555 1_555 1_555 yes C(18) C(19) H(32) 106(1) 1_555 1_555 1_555 no C(18) C(19) H(33) 108(1) 1_555 1_555 1_555 no C(20) C(19) H(32) 106(2) 1_555 1_555 1_555 no C(20) C(19) H(33) 110(2) 1_555 1_555 1_555 no H(32) C(19) H(33) 108(2) 1_555 1_555 1_555 no C(19) C(20) H(34) 108(2) 1_555 1_555 1_555 no C(19) C(20) H(35) 106(2) 1_555 1_555 1_555 no C(19) C(20) H(36) 113(2) 1_555 1_555 1_555 no H(34) C(20) H(35) 104(2) 1_555 1_555 1_555 no H(34) C(20) H(36) 113(2) 1_555 1_555 1_555 no H(35) C(20) H(36) 110(2) 1_555 1_555 1_555 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 Pt(1) Cu(2) 2.838(2) 1_555 1_555 ? Pt(1) Cu(2) 2.838(2) 1_555 2_755 ? I(1) Cu(1) 2.580(1) 1_555 1_555 ? I(1) Cu(2) 2.510(2) 1_555 2_755 ? I(1) Cu(3) 2.672(6) 1_555 2_755 ? I(2) Cu(1) 2.652(1) 1_555 1_555 ? I(2) Cu(2) 2.542(2) 1_555 1_555 ? I(2) Cu(3) 2.836(8) 1_555 2_755 ? Cu(1) Cu(3) 2.609(6) 1_555 2_755 ? Pt(1) Cu(2) 2.838(2) 1_555 1_555 ? Pt(1) Cu(2) 2.838(2) 1_555 2_755 ? I(1) Cu(2) 2.510(2) 1_555 2_755 ? I(1) Cu(1) 2.580(1) 1_555 1_555 ? I(2) Cu(2) 2.542(2) 1_555 1_555 ? I(2) Cu(1) 2.652(1) 1_555 1_555 ? Cu(1) Cu(2) 2.933(3) 1_555 2_755 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;