# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1285 data_(1) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Oct 2 16:54:04 1998' _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 SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 911.18 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H34 Cl Fe N7 O7 Pb S ' _chemical_formula_moiety 'C28 H34 Cl Fe N7 O7 Pb S ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 20.064(7) _cell_length_b 21.306(8) _cell_length_c 15.751(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6733(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.4 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 1.000 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3584.00 _exptl_absorpt_coefficient_mu 5.629 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.224 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _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 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -7.27 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 -1 3 2 -1 1 2 -3 _diffrn_reflns_number 6544 _reflns_number_total 6544 _reflns_number_observed 3034 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03618 _diffrn_orient_matrix_UB_12 0.00038 _diffrn_orient_matrix_UB_13 -0.04366 _diffrn_orient_matrix_UB_21 -0.03428 _diffrn_orient_matrix_UB_22 0.00022 _diffrn_orient_matrix_UB_23 -0.04609 _diffrn_orient_matrix_UB_31 -0.00013 _diffrn_orient_matrix_UB_32 0.04693 _diffrn_orient_matrix_UB_33 0.00058 #------------------------------------------------------------------------------ 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 C 0 224 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 272 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 56 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 56 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 8 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pb 0 8 -3.394 10.111 ;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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Pb -0.16357(2) 0.37029(2) 0.40704(2) 0.0504(1) Uani d . 1.00 . Fe 0.00479(8) 0.36693(8) 0.36671(9) 0.0464(4) Uani d . 1.00 . Cl -0.2570(3) 0.3837(4) 0.6172(3) 0.118(2) Uani d . 1.00 . S 0.0572(2) 0.3741(2) 0.0696(2) 0.081(1) Uani d . 1.00 . O(1) -0.0562(4) 0.4409(4) 0.3823(4) 0.053(3) Uani d . 1.00 . O(2) -0.0619(4) 0.2971(4) 0.3784(5) 0.053(3) Uani d . 1.00 . O(3) -0.1511(4) 0.3697(4) 0.2564(5) 0.071(3) Uani d . 1.00 . O(4) -0.260(2) 0.414(1) 0.550(1) 0.36(2) Uani d . 1.00 . O(5) -0.243(2) 0.327(1) 0.577(2) 0.40(2) Uani d . 1.00 . O(6) -0.301(1) 0.376(1) 0.672(1) 0.33(1) Uani d . 1.00 . O(7) -0.209(1) 0.400(2) 0.658(2) 0.34(2) Uani d . 1.00 . N(1) 0.0818(5) 0.4257(5) 0.4088(6) 0.052(3) Uani d . 1.00 . N(2) 0.0751(5) 0.3014(5) 0.4111(6) 0.056(3) Uani d . 1.00 . N(3) -0.2063(5) 0.2612(5) 0.3598(7) 0.061(4) Uani d . 1.00 . N(4) -0.2823(5) 0.3764(5) 0.3518(6) 0.065(3) Uani d . 1.00 . N(5) -0.1965(6) 0.4860(5) 0.3698(7) 0.062(4) Uani d . 1.00 . N(6) 0.0216(5) 0.3687(4) 0.2407(6) 0.059(3) Uani d . 1.00 . N(7) -0.1354(6) 0.3858(9) 0.1192(7) 0.097(5) Uani d . 1.00 . C(1) 0.003(1) 0.7010(6) 0.3674(10) 0.100(6) Uani d . 1.00 . C(2) -0.0114(9) 0.6327(6) 0.3740(7) 0.070(4) Uani d . 1.00 . C(3) 0.0361(8) 0.5897(6) 0.3948(7) 0.065(5) Uani d . 1.00 . C(4) 0.0232(7) 0.5245(6) 0.3990(7) 0.056(4) Uani d . 1.00 . C(5) -0.0421(7) 0.5015(6) 0.3818(7) 0.051(4) Uani d . 1.00 . C(6) -0.0926(7) 0.5468(5) 0.3629(7) 0.055(4) Uani d . 1.00 . C(7) -0.0751(7) 0.6096(7) 0.3566(7) 0.064(4) Uani d . 1.00 . C(8) 0.0787(6) 0.4858(7) 0.4151(7) 0.059(4) Uani d . 1.00 . C(9) 0.1462(7) 0.3931(8) 0.4206(8) 0.074(5) Uani d . 1.00 . C(10) 0.1349(7) 0.3274(7) 0.4514(8) 0.067(4) Uani d . 1.00 . C(11) 0.0695(6) 0.2426(6) 0.4017(7) 0.056(4) Uani d . 1.00 . C(12) 0.0111(6) 0.2089(6) 0.3758(6) 0.051(4) Uani d . 1.00 . C(13) 0.0198(7) 0.1444(5) 0.3621(7) 0.054(4) Uani d . 1.00 . C(14) -0.0319(9) 0.1048(6) 0.3397(8) 0.072(5) Uani d . 1.00 . C(15) -0.0226(9) 0.0353(6) 0.3294(9) 0.095(6) Uani d . 1.00 . C(16) -0.0932(8) 0.1321(6) 0.3298(8) 0.073(5) Uani d . 1.00 . C(17) -0.1063(7) 0.1953(5) 0.3451(8) 0.058(4) Uani d . 1.00 . C(18) -0.0523(7) 0.2359(6) 0.3666(7) 0.055(4) Uani d . 1.00 . C(19) -0.1769(7) 0.2122(6) 0.3376(8) 0.062(4) Uani d . 1.00 . C(20) -0.2797(7) 0.2627(8) 0.348(1) 0.089(6) Uani d . 1.00 . C(21) -0.2994(7) 0.3193(7) 0.2988(9) 0.080(5) Uani d . 1.00 . C(22) -0.2940(6) 0.4331(7) 0.3057(8) 0.073(5) Uani d . 1.00 . C(23) -0.2703(9) 0.4885(7) 0.3578(10) 0.090(6) Uani d . 1.00 . C(24) -0.1642(8) 0.5353(6) 0.3540(8) 0.062(4) Uani d . 1.00 . C(25) 0.0358(6) 0.3711(5) 0.1704(7) 0.054(4) Uani d . 1.00 . C(26) -0.1385(9) 0.396(1) 0.202(1) 0.155(9) Uani d . 1.00 . C(27) -0.124(1) 0.437(1) 0.062(1) 0.16(1) Uani d . 1.00 . C(28) -0.139(1) 0.329(1) 0.081(1) 0.16(1) Uani d . 1.00 . H(1) 0.0515 0.7097 0.3807 0.1063 Uiso calc . 1.00 . H(2) -0.0026 0.7179 0.3112 0.1063 Uiso calc . 1.00 . H(3) -0.0209 0.7268 0.4062 0.1063 Uiso calc . 1.00 . H(4) 0.1708 0.3938 0.3662 0.0828 Uiso calc . 1.00 . H(5) 0.1740 0.4170 0.4595 0.0828 Uiso calc . 1.00 . H(6) 0.1306 0.3266 0.5108 0.0800 Uiso calc . 1.00 . H(7) 0.1729 0.3009 0.4361 0.0800 Uiso calc . 1.00 . H(8) -0.0487 0.0110 0.3692 0.0929 Uiso calc . 1.00 . H(9) -0.0351 0.0211 0.2732 0.0929 Uiso calc . 1.00 . H(10) 0.0235 0.0222 0.3374 0.0929 Uiso calc . 1.00 . H(11) -0.2947 0.2241 0.3190 0.1033 Uiso calc . 1.00 . H(12) -0.3024 0.2619 0.4026 0.1033 Uiso calc . 1.00 . H(13) -0.3464 0.3178 0.2850 0.0945 Uiso calc . 1.00 . H(14) -0.2752 0.3200 0.2467 0.0945 Uiso calc . 1.00 . H(15) -0.2718 0.4334 0.2524 0.0887 Uiso calc . 1.00 . H(16) -0.3418 0.4396 0.2933 0.0887 Uiso calc . 1.00 . H(17) -0.2912 0.4896 0.4132 0.0984 Uiso calc . 1.00 . H(18) -0.2807 0.5290 0.3315 0.0984 Uiso calc . 1.00 . H(19) -0.1271 0.4457 0.2146 0.1210 Uiso calc . 1.00 . H(20) -0.0773 0.4586 0.0734 0.1456 Uiso calc . 1.00 . H(21) -0.1189 0.4286 0.0009 0.1456 Uiso calc . 1.00 . H(22) -0.1527 0.4737 0.0652 0.1456 Uiso calc . 1.00 . H(23) -0.1787 0.3045 0.0976 0.1760 Uiso calc . 1.00 . H(24) -0.1368 0.3274 0.0207 0.1760 Uiso calc . 1.00 . H(25) -0.1015 0.3011 0.1007 0.1063 Uiso calc . 1.00 . H(26) 0.0811 0.6021 0.4065 0.0832 Uiso calc . 1.00 . H(27) -0.1088 0.6401 0.3422 0.0765 Uiso calc . 1.00 . H(28) 0.1200 0.5065 0.4315 0.0800 Uiso calc . 1.00 . H(29) 0.1100 0.2177 0.4126 0.0655 Uiso calc . 1.00 . H(30) 0.0645 0.1280 0.3680 0.0929 Uiso calc . 1.00 . H(31) -0.1317 0.1056 0.3143 0.0858 Uiso calc . 1.00 . H(32) -0.2056 0.1815 0.3096 0.0984 Uiso calc . 1.00 . H(33) -0.1896 0.5708 0.3310 0.1760 Uiso calc . 1.00 . 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 Pb 0.0497(3) 0.0590(3) 0.0426(2) 0.0030(3) 0.0023(2) 0.0010(2) Fe 0.0467(9) 0.0435(9) 0.0492(8) 0.0043(9) -0.0015(7) -0.0010(7) Cl 0.080(3) 0.204(6) 0.071(2) -0.033(4) 0.003(2) -0.003(3) S 0.097(3) 0.100(3) 0.046(2) 0.012(3) 0.005(2) -0.006(2) O(1) 0.058(5) 0.046(5) 0.054(5) 0.005(4) -0.001(4) -0.006(3) O(2) 0.044(5) 0.050(5) 0.065(5) 0.002(4) 0.008(4) -0.002(4) O(3) 0.064(6) 0.116(7) 0.034(4) -0.001(5) 0.001(4) 0.006(5) O(4) 0.47(4) 0.51(4) 0.10(1) 0.27(4) 0.01(2) 0.08(2) O(5) 0.55(6) 0.18(2) 0.46(4) -0.09(3) 0.35(5) -0.09(3) O(6) 0.19(2) 0.61(5) 0.17(2) -0.17(2) 0.13(2) -0.13(2) O(7) 0.22(3) 0.56(5) 0.26(3) -0.22(3) -0.09(2) 0.05(3) N(1) 0.042(5) 0.067(7) 0.047(5) 0.000(5) -0.002(5) -0.004(5) N(2) 0.045(6) 0.060(7) 0.062(6) 0.009(5) -0.003(5) -0.006(5) N(3) 0.054(7) 0.046(7) 0.081(8) 0.000(5) -0.002(6) 0.006(5) N(4) 0.051(6) 0.075(8) 0.068(6) 0.003(6) -0.001(5) 0.013(6) N(5) 0.061(8) 0.060(7) 0.064(7) 0.020(6) -0.005(6) -0.006(5) N(6) 0.068(7) 0.067(6) 0.043(5) 0.016(6) 0.005(5) -0.005(5) N(7) 0.059(7) 0.19(2) 0.037(6) 0.025(10) 0.000(5) -0.001(9) C(1) 0.15(2) 0.045(9) 0.10(1) -0.02(1) 0.03(1) 0.005(7) C(2) 0.11(1) 0.050(8) 0.046(6) -0.010(9) 0.023(8) 0.003(6) C(3) 0.09(1) 0.062(9) 0.043(7) -0.012(8) -0.006(7) -0.004(6) C(4) 0.064(9) 0.055(8) 0.050(7) -0.015(7) 0.007(6) -0.015(6) C(5) 0.067(9) 0.045(7) 0.043(6) 0.000(7) 0.016(6) -0.004(5) C(6) 0.08(1) 0.043(7) 0.039(7) 0.011(7) 0.004(6) -0.002(5) C(7) 0.08(1) 0.064(9) 0.051(7) 0.011(8) 0.011(7) 0.009(6) C(8) 0.061(9) 0.075(10) 0.041(6) -0.022(7) -0.004(6) -0.006(6) C(9) 0.051(9) 0.09(1) 0.077(9) -0.007(8) -0.011(7) -0.014(8) C(10) 0.061(9) 0.09(1) 0.051(7) 0.006(8) -0.005(7) -0.008(7) C(11) 0.064(8) 0.054(8) 0.048(7) 0.024(7) 0.004(6) 0.004(6) C(12) 0.062(8) 0.050(7) 0.039(6) 0.013(7) 0.002(5) 0.006(5) C(13) 0.067(9) 0.040(7) 0.056(7) 0.020(6) 0.013(6) 0.002(5) C(14) 0.11(1) 0.044(7) 0.057(8) 0.012(9) 0.020(8) 0.013(6) C(15) 0.17(2) 0.035(7) 0.08(1) 0.010(9) 0.03(1) 0.004(6) C(16) 0.11(1) 0.050(7) 0.058(8) -0.015(9) 0.011(8) 0.000(6) C(17) 0.068(9) 0.040(7) 0.066(8) -0.004(7) 0.007(7) 0.007(5) C(18) 0.075(9) 0.046(8) 0.044(7) 0.012(7) 0.006(6) 0.000(5) C(19) 0.064(10) 0.053(8) 0.068(9) -0.010(7) -0.007(7) 0.009(6) C(20) 0.043(9) 0.10(1) 0.12(1) -0.012(9) 0.018(9) -0.02(1) C(21) 0.053(9) 0.09(1) 0.09(1) -0.011(8) -0.018(8) -0.003(9) C(22) 0.046(8) 0.10(1) 0.076(10) 0.015(8) -0.013(7) 0.002(8) C(23) 0.08(1) 0.08(1) 0.11(1) 0.038(10) -0.01(1) 0.007(9) C(24) 0.071(9) 0.061(8) 0.054(7) 0.031(9) -0.016(7) -0.002(6) C(25) 0.043(7) 0.059(7) 0.059(8) 0.012(7) -0.001(5) -0.015(6) C(26) 0.06(1) 0.35(4) 0.06(1) 0.01(2) -0.005(9) -0.04(2) C(27) 0.21(3) 0.14(2) 0.14(2) 0.05(2) -0.08(2) 0.01(1) C(28) 0.15(2) 0.19(3) 0.14(2) -0.03(2) -0.07(2) 0.00(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00160|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00006(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3034 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0570 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_shift/esd_max 0.8720 _refine_ls_shift/esd_mean 0.0560 _refine_diff_density_min -0.89 _refine_diff_density_max 1.57 #------------------------------------------------------------------------------ _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 Pb O(1) 2.656(8) 1_555 1_555 yes Pb O(2) 2.606(8) 1_555 1_555 yes Pb O(3) 2.386(8) 1_555 1_555 yes Pb O(4) 3.10(2) 1_555 1_555 yes Pb N(3) 2.59(1) 1_555 1_555 yes Pb N(4) 2.54(1) 1_555 1_555 yes Pb N(5) 2.62(1) 1_555 1_555 yes Fe O(1) 2.011(8) 1_555 1_555 yes Fe O(2) 2.009(8) 1_555 1_555 yes Fe N(1) 2.095(10) 1_555 1_555 yes Fe N(2) 2.104(10) 1_555 1_555 yes Fe N(6) 2.013(9) 1_555 1_555 yes Cl O(4) 1.24(2) 1_555 1_555 yes Cl O(5) 1.39(2) 1_555 1_555 yes Cl O(6) 1.26(1) 1_555 1_555 yes Cl O(7) 1.20(2) 1_555 1_555 yes S C(25) 1.65(1) 1_555 1_555 yes O(1) C(5) 1.32(1) 1_555 1_555 yes O(2) C(18) 1.33(1) 1_555 1_555 yes O(3) C(26) 1.05(2) 1_555 1_555 yes N(1) C(8) 1.29(2) 1_555 1_555 yes N(1) C(9) 1.48(2) 1_555 1_555 yes N(2) C(10) 1.47(2) 1_555 1_555 yes N(2) C(11) 1.27(2) 1_555 1_555 yes N(3) C(19) 1.25(2) 1_555 1_555 yes N(3) C(20) 1.48(2) 1_555 1_555 yes N(4) C(21) 1.51(2) 1_555 1_555 yes N(4) C(22) 1.43(2) 1_555 1_555 yes N(5) C(23) 1.49(2) 1_555 1_555 yes N(5) C(24) 1.26(2) 1_555 1_555 yes N(6) C(25) 1.14(1) 1_555 1_555 yes N(7) C(26) 1.33(2) 1_555 1_555 yes N(7) C(27) 1.45(3) 1_555 1_555 yes N(7) C(28) 1.35(3) 1_555 1_555 yes C(1) C(2) 1.49(2) 1_555 1_555 yes C(2) C(3) 1.36(2) 1_555 1_555 yes C(2) C(7) 1.40(2) 1_555 1_555 yes C(3) C(4) 1.41(2) 1_555 1_555 yes C(4) C(5) 1.42(2) 1_555 1_555 yes C(4) C(8) 1.41(2) 1_555 1_555 yes C(5) C(6) 1.43(2) 1_555 1_555 yes C(6) C(7) 1.39(2) 1_555 1_555 yes C(6) C(24) 1.46(2) 1_555 1_555 yes C(9) C(10) 1.50(2) 1_555 1_555 yes C(11) C(12) 1.43(2) 1_555 1_555 yes C(12) C(13) 1.40(2) 1_555 1_555 yes C(12) C(18) 1.40(2) 1_555 1_555 yes C(13) C(14) 1.38(2) 1_555 1_555 yes C(14) C(15) 1.50(2) 1_555 1_555 yes C(14) C(16) 1.37(2) 1_555 1_555 yes C(16) C(17) 1.39(2) 1_555 1_555 yes C(17) C(18) 1.43(2) 1_555 1_555 yes C(17) C(19) 1.47(2) 1_555 1_555 yes C(20) C(21) 1.49(2) 1_555 1_555 yes C(22) C(23) 1.52(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 O(1) Pb O(2) 71.3(2) 1_555 1_555 1_555 yes O(1) Pb O(3) 76.8(3) 1_555 1_555 1_555 yes O(1) Pb O(4) 116.1(7) 1_555 1_555 1_555 yes O(1) Pb N(3) 137.3(3) 1_555 1_555 1_555 yes O(1) Pb N(4) 132.9(3) 1_555 1_555 1_555 yes O(1) Pb N(5) 68.8(3) 1_555 1_555 1_555 yes O(2) Pb O(3) 75.1(3) 1_555 1_555 1_555 yes O(2) Pb O(4) 142.2(4) 1_555 1_555 1_555 yes O(2) Pb N(3) 70.9(3) 1_555 1_555 1_555 yes O(2) Pb N(4) 134.9(3) 1_555 1_555 1_555 yes O(2) Pb N(5) 136.2(3) 1_555 1_555 1_555 yes O(3) Pb O(4) 141.9(4) 1_555 1_555 1_555 yes O(3) Pb N(3) 75.2(3) 1_555 1_555 1_555 yes O(3) Pb N(4) 76.0(3) 1_555 1_555 1_555 yes O(3) Pb N(5) 79.0(3) 1_555 1_555 1_555 yes O(4) Pb N(3) 105.8(7) 1_555 1_555 1_555 yes O(4) Pb N(4) 69.6(6) 1_555 1_555 1_555 yes O(4) Pb N(5) 73.9(5) 1_555 1_555 1_555 yes N(3) Pb N(4) 68.7(3) 1_555 1_555 1_555 yes N(3) Pb N(5) 134.3(3) 1_555 1_555 1_555 yes N(4) Pb N(5) 68.8(3) 1_555 1_555 1_555 yes O(1) Fe O(2) 99.4(3) 1_555 1_555 1_555 yes O(1) Fe N(1) 86.7(4) 1_555 1_555 1_555 yes O(1) Fe N(2) 152.6(3) 1_555 1_555 1_555 yes O(1) Fe N(6) 102.0(3) 1_555 1_555 1_555 yes O(2) Fe N(1) 154.7(3) 1_555 1_555 1_555 yes O(2) Fe N(2) 85.7(4) 1_555 1_555 1_555 yes O(2) Fe N(6) 102.5(4) 1_555 1_555 1_555 yes N(1) Fe N(2) 78.3(4) 1_555 1_555 1_555 yes N(1) Fe N(6) 100.2(4) 1_555 1_555 1_555 yes N(2) Fe N(6) 103.2(4) 1_555 1_555 1_555 yes O(4) Cl O(5) 94(1) 1_555 1_555 1_555 yes O(4) Cl O(6) 128(2) 1_555 1_555 1_555 yes O(4) Cl O(7) 109(2) 1_555 1_555 1_555 yes O(5) Cl O(6) 110(1) 1_555 1_555 1_555 yes O(5) Cl O(7) 109(2) 1_555 1_555 1_555 yes O(6) Cl O(7) 103(1) 1_555 1_555 1_555 yes Pb O(1) Fe 93.9(3) 1_555 1_555 1_555 yes Pb O(1) C(5) 136.7(8) 1_555 1_555 1_555 yes Fe O(1) C(5) 129.4(8) 1_555 1_555 1_555 yes Pb O(2) Fe 95.4(3) 1_555 1_555 1_555 yes Pb O(2) C(18) 136.4(8) 1_555 1_555 1_555 yes Fe O(2) C(18) 127.9(8) 1_555 1_555 1_555 yes Pb O(3) C(26) 146(1) 1_555 1_555 1_555 yes Pb O(4) Cl 115(1) 1_555 1_555 1_555 yes Fe N(1) C(8) 125.8(8) 1_555 1_555 1_555 yes Fe N(1) C(9) 113.8(8) 1_555 1_555 1_555 yes C(8) N(1) C(9) 119(1) 1_555 1_555 1_555 yes Fe N(2) C(10) 116.2(8) 1_555 1_555 1_555 yes Fe N(2) C(11) 124.0(8) 1_555 1_555 1_555 yes C(10) N(2) C(11) 119(1) 1_555 1_555 1_555 yes Pb N(3) C(19) 132.5(9) 1_555 1_555 1_555 yes Pb N(3) C(20) 110.2(8) 1_555 1_555 1_555 yes C(19) N(3) C(20) 116(1) 1_555 1_555 1_555 yes Pb N(4) C(21) 111.1(8) 1_555 1_555 1_555 yes Pb N(4) C(22) 111.8(8) 1_555 1_555 1_555 yes C(21) N(4) C(22) 111(1) 1_555 1_555 1_555 yes Pb N(5) C(23) 108.2(9) 1_555 1_555 1_555 yes Pb N(5) C(24) 134.4(9) 1_555 1_555 1_555 yes C(23) N(5) C(24) 117(1) 1_555 1_555 1_555 yes Fe N(6) C(25) 174(1) 1_555 1_555 1_555 yes C(26) N(7) C(27) 120(2) 1_555 1_555 1_555 yes C(26) N(7) C(28) 125(2) 1_555 1_555 1_555 yes C(27) N(7) C(28) 114(1) 1_555 1_555 1_555 yes C(2) C(1) H(1) 111(1) 1_555 1_555 1_555 no C(2) C(1) H(2) 113(1) 1_555 1_555 1_555 no C(2) C(1) H(3) 114(1) 1_555 1_555 1_555 no H(1) C(1) H(2) 104(1) 1_555 1_555 1_555 no H(1) C(1) H(3) 104(1) 1_555 1_555 1_555 no H(2) C(1) H(3) 107(1) 1_555 1_555 1_555 no C(1) C(2) C(3) 122(1) 1_555 1_555 1_555 yes C(1) C(2) C(7) 120(1) 1_555 1_555 1_555 yes C(3) C(2) C(7) 116(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 123(1) 1_555 1_555 1_555 yes C(2) C(3) H(26) 121(1) 1_555 1_555 1_555 no C(4) C(3) H(26) 115(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 119(1) 1_555 1_555 1_555 yes C(3) C(4) C(8) 115(1) 1_555 1_555 1_555 yes C(5) C(4) C(8) 124(1) 1_555 1_555 1_555 yes O(1) C(5) C(4) 122(1) 1_555 1_555 1_555 yes O(1) C(5) C(6) 120(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 117(1) 1_555 1_555 1_555 yes C(5) C(6) C(7) 119(1) 1_555 1_555 1_555 yes C(5) C(6) C(24) 126(1) 1_555 1_555 1_555 yes C(7) C(6) C(24) 113(1) 1_555 1_555 1_555 yes C(2) C(7) C(6) 123(1) 1_555 1_555 1_555 yes C(2) C(7) H(27) 116(1) 1_555 1_555 1_555 no C(6) C(7) H(27) 119(1) 1_555 1_555 1_555 no N(1) C(8) C(4) 127(1) 1_555 1_555 1_555 yes N(1) C(8) H(28) 115(1) 1_555 1_555 1_555 no C(4) C(8) H(28) 117(1) 1_555 1_555 1_555 no N(1) C(9) C(10) 110(1) 1_555 1_555 1_555 yes N(1) C(9) H(4) 108(1) 1_555 1_555 1_555 no N(1) C(9) H(5) 109(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 111(1) 1_555 1_555 1_555 no C(10) C(9) H(5) 111(1) 1_555 1_555 1_555 no H(4) C(9) H(5) 104(1) 1_555 1_555 1_555 no N(2) C(10) C(9) 109(1) 1_555 1_555 1_555 yes N(2) C(10) H(6) 110(1) 1_555 1_555 1_555 no N(2) C(10) H(7) 108(1) 1_555 1_555 1_555 no C(9) C(10) H(6) 110(1) 1_555 1_555 1_555 no C(9) C(10) H(7) 109(1) 1_555 1_555 1_555 no H(6) C(10) H(7) 107(1) 1_555 1_555 1_555 no N(2) C(11) C(12) 126(1) 1_555 1_555 1_555 yes N(2) C(11) H(29) 116(1) 1_555 1_555 1_555 no C(12) C(11) H(29) 116(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 115(1) 1_555 1_555 1_555 yes C(11) C(12) C(18) 124(1) 1_555 1_555 1_555 yes C(13) C(12) C(18) 120(1) 1_555 1_555 1_555 yes C(12) C(13) C(14) 122(1) 1_555 1_555 1_555 yes C(12) C(13) H(30) 117(1) 1_555 1_555 1_555 no C(14) C(13) H(30) 119(1) 1_555 1_555 1_555 no C(13) C(14) C(15) 122(1) 1_555 1_555 1_555 yes C(13) C(14) C(16) 116(1) 1_555 1_555 1_555 yes C(15) C(14) C(16) 121(1) 1_555 1_555 1_555 yes C(14) C(15) H(8) 113(1) 1_555 1_555 1_555 no C(14) C(15) H(9) 112(1) 1_555 1_555 1_555 no C(14) C(15) H(10) 112(1) 1_555 1_555 1_555 no H(8) C(15) H(9) 106(1) 1_555 1_555 1_555 no H(8) C(15) H(10) 106(1) 1_555 1_555 1_555 no H(9) C(15) H(10) 105(1) 1_555 1_555 1_555 no C(14) C(16) C(17) 124(1) 1_555 1_555 1_555 yes C(14) C(16) H(31) 119(1) 1_555 1_555 1_555 no C(17) C(16) H(31) 116(1) 1_555 1_555 1_555 no C(16) C(17) C(18) 118(1) 1_555 1_555 1_555 yes C(16) C(17) C(19) 113(1) 1_555 1_555 1_555 yes C(18) C(17) C(19) 127(1) 1_555 1_555 1_555 yes O(2) C(18) C(12) 121(1) 1_555 1_555 1_555 yes O(2) C(18) C(17) 121(1) 1_555 1_555 1_555 yes C(12) C(18) C(17) 117(1) 1_555 1_555 1_555 yes N(3) C(19) C(17) 129(1) 1_555 1_555 1_555 yes N(3) C(19) H(32) 114(1) 1_555 1_555 1_555 no C(17) C(19) H(32) 116(1) 1_555 1_555 1_555 no N(3) C(20) C(21) 110(1) 1_555 1_555 1_555 yes N(3) C(20) H(11) 109(1) 1_555 1_555 1_555 no N(3) C(20) H(12) 111(1) 1_555 1_555 1_555 no C(21) C(20) H(11) 110(1) 1_555 1_555 1_555 no C(21) C(20) H(12) 110(1) 1_555 1_555 1_555 no H(11) C(20) H(12) 104(1) 1_555 1_555 1_555 no N(4) C(21) C(20) 107(1) 1_555 1_555 1_555 yes N(4) C(21) H(13) 111(1) 1_555 1_555 1_555 no N(4) C(21) H(14) 110(1) 1_555 1_555 1_555 no C(20) C(21) H(13) 110(1) 1_555 1_555 1_555 no C(20) C(21) H(14) 109(1) 1_555 1_555 1_555 no H(13) C(21) H(14) 107(1) 1_555 1_555 1_555 no N(4) C(22) C(23) 109(1) 1_555 1_555 1_555 yes N(4) C(22) H(15) 112(1) 1_555 1_555 1_555 no N(4) C(22) H(16) 112(1) 1_555 1_555 1_555 no C(23) C(22) H(15) 109(1) 1_555 1_555 1_555 no C(23) C(22) H(16) 107(1) 1_555 1_555 1_555 no H(15) C(22) H(16) 106(1) 1_555 1_555 1_555 no N(5) C(23) C(22) 110(1) 1_555 1_555 1_555 yes N(5) C(23) H(17) 108(1) 1_555 1_555 1_555 no N(5) C(23) H(18) 107(1) 1_555 1_555 1_555 no C(22) C(23) H(17) 111(1) 1_555 1_555 1_555 no C(22) C(23) H(18) 112(1) 1_555 1_555 1_555 no H(17) C(23) H(18) 105(1) 1_555 1_555 1_555 no N(5) C(24) C(6) 128(1) 1_555 1_555 1_555 yes N(5) C(24) H(33) 116(1) 1_555 1_555 1_555 no C(6) C(24) H(33) 114(1) 1_555 1_555 1_555 no S C(25) N(6) 179(1) 1_555 1_555 1_555 yes O(3) C(26) N(7) 137(2) 1_555 1_555 1_555 yes O(3) C(26) H(19) 114(1) 1_555 1_555 1_555 no N(7) C(26) H(19) 108(2) 1_555 1_555 1_555 no N(7) C(27) H(20) 111(1) 1_555 1_555 1_555 no N(7) C(27) H(21) 118(2) 1_555 1_555 1_555 no N(7) C(27) H(22) 118(2) 1_555 1_555 1_555 no H(20) C(27) H(21) 99(2) 1_555 1_555 1_555 no H(20) C(27) H(22) 100(2) 1_555 1_555 1_555 no H(21) C(27) H(22) 105(1) 1_555 1_555 1_555 no N(7) C(28) H(23) 114(2) 1_555 1_555 1_555 no N(7) C(28) H(24) 118(2) 1_555 1_555 1_555 no N(7) C(28) H(25) 110(1) 1_555 1_555 1_555 no H(23) C(28) H(24) 106(2) 1_555 1_555 1_555 no H(23) C(28) H(25) 101(2) 1_555 1_555 1_555 no H(24) C(28) H(25) 103(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 Pb O(1) 2.656(8) 1_555 1_555 ? Pb O(2) 2.606(8) 1_555 1_555 ? Pb O(4) 3.10(2) 1_555 1_555 ? Pb N(3) 2.59(1) 1_555 1_555 ? Pb N(4) 2.54(1) 1_555 1_555 ? Pb N(5) 2.62(1) 1_555 1_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_(2) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Oct 9 14:09:25 1998' _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 SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 848.51 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H41 Cl2 Fe N8 O11 S ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.892(3) _cell_length_b 24.786(7) _cell_length_c 15.500(4) _cell_angle_alpha 90 _cell_angle_beta 95.38(2) _cell_angle_gamma 90 _cell_volume 3783(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.8 #------------------------------------------------------------------------------ _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 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.500 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1764.00 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.931 _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 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.56 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -4 1 1 -1 2 1 -1 3 _diffrn_reflns_number 7257 _reflns_number_total 6837 _reflns_number_observed 5075 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03809 _diffrn_orient_matrix_UB_12 -0.01490 _diffrn_orient_matrix_UB_13 0.05346 _diffrn_orient_matrix_UB_21 -0.04228 _diffrn_orient_matrix_UB_22 -0.03085 _diffrn_orient_matrix_UB_23 -0.03490 _diffrn_orient_matrix_UB_31 0.08503 _diffrn_orient_matrix_UB_32 -0.02202 _diffrn_orient_matrix_UB_33 0.01274 #------------------------------------------------------------------------------ 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 C 0 120 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 164 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Fe 0 4 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 44 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.125 0.123 ;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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Fe(1) 0.15123(6) 0.34945(2) 0.62304(4) 0.0416(2) Uani d . 1.00 . Cl(1) 0.3275(2) 0.42609(6) 0.17390(8) 0.0704(4) Uani d . 1.00 . Cl(2) 0.8166(2) 0.19819(8) 0.2926(1) 0.0922(6) Uani d . 1.00 . S(1) -0.0646(2) 0.51852(6) 0.6556(2) 0.0998(6) Uani d . 1.00 . O(1) 0.3367(3) 0.3774(1) 0.6325(2) 0.0487(8) Uani d . 1.00 . O(2) 0.1670(3) 0.3456(1) 0.7481(2) 0.0470(8) Uani d . 1.00 . O(3) 0.9521(8) 0.3894(3) 0.0299(4) 0.140(3) Uani d . 1.00 . O(4) 0.2480(7) 0.4632(2) 0.1214(4) 0.131(2) Uani d . 1.00 . O(5) 0.2463(6) 0.3956(2) 0.2266(3) 0.103(2) Uani d . 1.00 . O(6) 0.4292(7) 0.4536(3) 0.2263(3) 0.144(2) Uani d . 1.00 . O(7) 0.3897(7) 0.3909(3) 0.1206(4) 0.141(3) Uani d . 1.00 . O(8) 0.764(1) 0.2074(5) 0.2083(5) 0.224(5) Uani d . 1.00 . O(9) 0.7143(10) 0.2097(5) 0.3389(7) 0.248(6) Uani d . 1.00 . O(10) 0.9322(8) 0.2216(5) 0.3212(9) 0.279(6) Uani d . 1.00 . O(11) 0.8403(9) 0.1429(4) 0.279(1) 0.293(7) Uani d . 1.00 . N(1) 0.1651(4) 0.3554(2) 0.4845(2) 0.052(1) Uani d . 1.00 . N(2) -0.0396(4) 0.3104(2) 0.5660(3) 0.057(1) Uani d . 1.00 . N(3) 0.1965(4) 0.2664(1) 0.6318(3) 0.051(1) Uani d . 1.00 . N(4) 0.0924(5) 0.3988(2) 0.8907(3) 0.069(1) Uani d . 1.00 . N(5) 0.2988(5) 0.4365(2) 0.8669(3) 0.061(1) Uani d . 1.00 . N(6) 0.5082(4) 0.4112(2) 0.7617(2) 0.054(1) Uani d . 1.00 . N(7) 0.0474(4) 0.4195(2) 0.6249(3) 0.059(1) Uani d . 1.00 . N(8) 0.8142(5) 0.3716(2) 0.1319(3) 0.070(1) Uani d . 1.00 . C(1) 0.7003(6) 0.4650(3) 0.4069(4) 0.076(2) Uani d . 1.00 . C(2) 0.6026(5) 0.4422(2) 0.4669(3) 0.056(1) Uani d . 1.00 . C(3) 0.4784(5) 0.4211(2) 0.4341(3) 0.054(1) Uani d . 1.00 . C(4) 0.3855(4) 0.3989(2) 0.4882(3) 0.046(1) Uani d . 1.00 . C(5) 0.4189(4) 0.3982(2) 0.5782(3) 0.041(1) Uani d . 1.00 . C(6) 0.5445(4) 0.4205(2) 0.6118(3) 0.050(1) Uani d . 1.00 . C(7) 0.6340(5) 0.4416(2) 0.5544(3) 0.055(1) Uani d . 1.00 . C(8) 0.2596(5) 0.3774(2) 0.4464(3) 0.049(1) Uani d . 1.00 . C(9) 0.0444(6) 0.3364(2) 0.4294(3) 0.065(2) Uani d . 1.00 . C(10) -0.0768(6) 0.3368(2) 0.4824(4) 0.068(2) Uani d . 1.00 . C(11) -0.0238(5) 0.2510(2) 0.5599(4) 0.063(2) Uani d . 1.00 . C(12) 0.1241(6) 0.2355(2) 0.5607(3) 0.063(2) Uani d . 1.00 . C(13) 0.2592(5) 0.2417(2) 0.6958(3) 0.055(1) Uani d . 1.00 . C(14) 0.3068(4) 0.2672(2) 0.7771(3) 0.050(1) Uani d . 1.00 . C(15) 0.3951(5) 0.2386(2) 0.8368(4) 0.060(1) Uani d . 1.00 . C(16) 0.4362(5) 0.2586(2) 0.9187(4) 0.062(2) Uani d . 1.00 . C(17) 0.5362(6) 0.2282(2) 0.9806(4) 0.082(2) Uani d . 1.00 . C(18) 0.3799(5) 0.3079(2) 0.9419(3) 0.054(1) Uani d . 1.00 . C(19) 0.2926(5) 0.3372(2) 0.8848(3) 0.049(1) Uani d . 1.00 . C(20) 0.2539(4) 0.3174(2) 0.8007(3) 0.045(1) Uani d . 1.00 . C(21) 0.2436(5) 0.3911(2) 0.9127(3) 0.055(1) Uani d . 1.00 . C(22) 0.0693(10) 0.4572(3) 0.8717(5) 0.113(3) Uani d . 1.00 . C(23) 0.2056(10) 0.4817(3) 0.8804(4) 0.095(2) Uani d . 1.00 . C(24) 0.4394(7) 0.4504(2) 0.8964(3) 0.076(2) Uani d . 1.00 . C(25) 0.5429(6) 0.4160(2) 0.8552(3) 0.068(2) Uani d . 1.00 . C(26) 0.5846(5) 0.4249(2) 0.7026(3) 0.054(1) Uani d . 1.00 . C(27) 0.0024(5) 0.4610(2) 0.6358(3) 0.055(1) Uani d . 1.00 . C(28) 0.9284(10) 0.3891(4) 0.1067(8) 0.125(4) Uani d . 1.00 . C(29) 0.811(2) 0.3723(5) 0.2222(7) 0.222(7) Uani d . 1.00 . C(30) 0.711(1) 0.3566(6) 0.076(1) 0.217(6) Uani d . 1.00 . H(1) 0.7343 0.4920 0.4169 0.1065 Uiso calc . 1.00 . H(2) 0.6581 0.4790 0.3571 0.1065 Uiso calc . 1.00 . H(3) 0.7439 0.4463 0.3742 0.1065 Uiso calc . 1.00 . H(4) 0.4470 0.4251 0.3734 0.1065 Uiso calc . 1.00 . H(5) 0.2571 0.3825 0.3826 0.1065 Uiso calc . 1.00 . H(6) 0.0235 0.3588 0.3768 0.1065 Uiso calc . 1.00 . H(7) 0.0616 0.2975 0.4017 0.1065 Uiso calc . 1.00 . H(8) -0.1101 0.3757 0.4958 0.1065 Uiso calc . 1.00 . H(9) -0.1624 0.3240 0.4462 0.1065 Uiso calc . 1.00 . H(10) -0.1096 0.3178 0.6038 0.0681 Uiso calc . 1.00 . H(11) -0.0581 0.2350 0.6188 0.1065 Uiso calc . 1.00 . H(12) -0.0774 0.2369 0.5076 0.1065 Uiso calc . 1.00 . H(13) 0.1565 0.2412 0.5082 0.1065 Uiso calc . 1.00 . H(14) 0.1318 0.1978 0.5653 0.1065 Uiso calc . 1.00 . H(15) 0.2882 0.1997 0.7027 0.1065 Uiso calc . 1.00 . H(16) 0.4360 0.2022 0.8179 0.1065 Uiso calc . 1.00 . H(17) 0.5824 0.1997 0.9545 0.1065 Uiso calc . 1.00 . H(18) 0.6348 0.2427 0.9992 0.1065 Uiso calc . 1.00 . H(19) 0.5008 0.2220 1.0388 0.1065 Uiso calc . 1.00 . H(20) 0.4048 0.3259 1.0018 0.1065 Uiso calc . 1.00 . H(21) 0.2622 0.3978 0.9779 0.1065 Uiso calc . 1.00 . H(22) 0.0368 0.3879 0.9352 0.1065 Uiso calc . 1.00 . H(23) 0.0583 0.3803 0.8379 0.1065 Uiso calc . 1.00 . H(24) 0.0110 0.4726 0.9122 0.1859 Uiso calc . 1.00 . H(25) 0.0262 0.4618 0.8142 0.1176 Uiso calc . 1.00 . H(26) 0.2367 0.4916 0.9362 0.1065 Uiso calc . 1.00 . H(27) 0.2225 0.5093 0.8413 0.1065 Uiso calc . 1.00 . H(28) 0.4706 0.4411 0.9687 0.1065 Uiso calc . 1.00 . H(29) 0.4570 0.4882 0.8763 0.1065 Uiso calc . 1.00 . H(30) 0.6346 0.4331 0.8617 0.1065 Uiso calc . 1.00 . H(31) 0.5448 0.3769 0.8794 0.1065 Uiso calc . 1.00 . H(32) 0.4205 0.3948 0.7378 0.1065 Uiso calc . 1.00 . H(33) 0.6778 0.4452 0.7270 0.1065 Uiso calc . 1.00 . H(34) 0.7200 0.4558 0.5775 0.2293 Uiso calc . 1.00 . H(35) 0.9950 0.4019 0.1465 0.1859 Uiso calc . 1.00 . H(36) 0.8090 0.4076 0.2422 0.2036 Uiso calc . 1.00 . H(37) 0.8676 0.3489 0.2491 0.2036 Uiso calc . 1.00 . H(38) 0.7113 0.3579 0.2309 0.2036 Uiso calc . 1.00 . H(39) 0.6348 0.3430 0.1111 0.1859 Uiso calc . 1.00 . H(40) 0.7342 0.3255 0.0427 0.1859 Uiso calc . 1.00 . H(41) 0.6753 0.3842 0.0412 0.1859 Uiso calc . 1.00 . 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 Fe(1) 0.0462(4) 0.0350(4) 0.0451(4) -0.0049(2) 0.0114(3) -0.0032(2) Cl(1) 0.094(1) 0.0666(8) 0.0529(7) -0.0109(7) 0.0175(6) -0.0035(6) Cl(2) 0.083(1) 0.101(1) 0.097(1) 0.0010(9) 0.0355(9) -0.0153(10) S(1) 0.0702(10) 0.0520(8) 0.173(2) 0.0133(7) -0.009(1) -0.027(1) O(1) 0.047(2) 0.055(2) 0.044(2) -0.013(1) 0.008(1) 0.000(1) O(2) 0.057(2) 0.041(2) 0.046(2) 0.005(1) 0.018(1) 0.001(1) O(3) 0.196(7) 0.134(5) 0.105(4) 0.014(4) 0.086(4) 0.005(4) O(4) 0.142(5) 0.113(4) 0.136(5) 0.022(4) 0.002(4) 0.054(4) O(5) 0.139(4) 0.080(3) 0.096(3) -0.013(3) 0.046(3) 0.010(3) O(6) 0.205(6) 0.142(5) 0.079(3) -0.099(5) -0.022(4) 0.015(3) O(7) 0.145(5) 0.192(7) 0.090(4) 0.041(5) 0.036(3) -0.032(4) O(8) 0.29(1) 0.29(1) 0.095(5) 0.107(10) 0.045(6) 0.053(6) O(9) 0.178(8) 0.36(2) 0.223(9) -0.005(9) 0.131(7) -0.098(9) O(10) 0.111(5) 0.27(1) 0.47(2) -0.062(6) 0.065(8) -0.27(1) O(11) 0.140(7) 0.143(8) 0.59(2) -0.013(6) 0.03(1) -0.15(1) N(1) 0.058(2) 0.048(2) 0.048(2) -0.007(2) 0.003(2) -0.005(2) N(2) 0.052(2) 0.053(2) 0.068(3) -0.011(2) 0.016(2) -0.010(2) N(3) 0.054(2) 0.038(2) 0.064(2) -0.006(2) 0.021(2) -0.012(2) N(4) 0.071(3) 0.072(3) 0.065(3) 0.019(2) 0.017(2) -0.013(2) N(5) 0.094(3) 0.039(2) 0.052(2) 0.001(2) 0.022(2) -0.001(2) N(6) 0.055(2) 0.058(2) 0.050(2) -0.014(2) 0.004(2) -0.004(2) N(7) 0.066(3) 0.043(2) 0.067(3) 0.004(2) 0.008(2) 0.002(2) N(8) 0.071(3) 0.069(3) 0.070(3) 0.008(2) 0.003(2) -0.009(2) C(1) 0.071(3) 0.081(4) 0.083(4) -0.007(3) 0.040(3) 0.012(3) C(2) 0.056(3) 0.048(3) 0.067(3) 0.001(2) 0.024(2) 0.005(2) C(3) 0.059(3) 0.049(3) 0.057(3) 0.005(2) 0.021(2) 0.006(2) C(4) 0.052(2) 0.040(2) 0.047(2) 0.000(2) 0.014(2) 0.001(2) C(5) 0.044(2) 0.035(2) 0.044(2) -0.001(2) 0.013(2) -0.001(2) C(6) 0.046(2) 0.046(2) 0.059(3) 0.001(2) 0.011(2) -0.002(2) C(7) 0.044(2) 0.051(3) 0.073(3) -0.004(2) 0.015(2) 0.002(2) C(8) 0.061(3) 0.046(2) 0.041(2) 0.002(2) 0.010(2) 0.001(2) C(9) 0.067(3) 0.072(3) 0.053(3) -0.021(3) -0.006(2) 0.001(2) C(10) 0.060(3) 0.073(4) 0.068(3) -0.011(3) -0.009(3) 0.001(3) C(11) 0.061(3) 0.047(3) 0.082(3) -0.020(2) 0.011(3) -0.015(2) C(12) 0.080(4) 0.043(2) 0.067(3) -0.006(2) 0.019(3) -0.016(2) C(13) 0.057(3) 0.037(2) 0.075(3) 0.003(2) 0.022(2) -0.002(2) C(14) 0.050(2) 0.034(2) 0.067(3) -0.003(2) 0.015(2) -0.002(2) C(15) 0.055(3) 0.040(2) 0.085(4) 0.001(2) 0.011(3) 0.011(2) C(16) 0.055(3) 0.051(3) 0.079(3) -0.006(2) 0.004(2) 0.015(2) C(17) 0.077(4) 0.060(3) 0.105(5) 0.005(3) -0.016(3) 0.016(3) C(18) 0.052(3) 0.048(2) 0.063(3) -0.010(2) 0.008(2) 0.010(2) C(19) 0.053(3) 0.043(2) 0.053(3) -0.004(2) 0.017(2) 0.004(2) C(20) 0.044(2) 0.037(2) 0.056(3) -0.003(2) 0.016(2) 0.007(2) C(21) 0.072(3) 0.052(3) 0.042(2) 0.005(2) 0.013(2) -0.002(2) C(22) 0.134(7) 0.102(6) 0.109(6) 0.065(5) 0.044(5) 0.036(4) C(23) 0.148(7) 0.055(3) 0.087(4) 0.032(4) 0.040(4) 0.006(3) C(24) 0.116(5) 0.063(3) 0.051(3) -0.030(3) 0.015(3) -0.011(2) C(25) 0.078(4) 0.073(3) 0.051(3) -0.027(3) -0.002(2) 0.003(2) C(26) 0.051(3) 0.049(3) 0.060(3) -0.005(2) 0.001(2) 0.000(2) C(27) 0.043(2) 0.048(3) 0.074(3) -0.005(2) 0.002(2) -0.001(2) C(28) 0.101(6) 0.093(6) 0.18(1) 0.016(5) 0.027(6) -0.014(6) C(29) 0.43(3) 0.140(10) 0.087(7) -0.04(1) -0.04(1) 0.015(6) C(30) 0.147(9) 0.17(1) 0.31(2) 0.048(8) -0.11(1) -0.12(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00203|Fo|^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 5075 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0619 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1043 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.950 _refine_ls_shift/esd_max 2.7374 _refine_ls_shift/esd_mean 0.0061 _refine_diff_density_min -0.55 _refine_diff_density_max 0.93 #------------------------------------------------------------------------------ _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 Fe(1) O(1) 1.954(3) 1_555 1_555 yes Fe(1) O(2) 1.932(3) 1_555 1_555 yes Fe(1) N(1) 2.170(4) 1_555 1_555 yes Fe(1) N(2) 2.229(4) 1_555 1_555 yes Fe(1) N(3) 2.109(4) 1_555 1_555 yes Fe(1) N(7) 2.019(4) 1_555 1_555 yes Cl(1) O(4) 1.416(5) 1_555 1_555 yes Cl(1) O(5) 1.417(5) 1_555 1_555 yes Cl(1) O(6) 1.409(5) 1_555 1_555 yes Cl(1) O(7) 1.385(6) 1_555 1_555 yes Cl(2) O(8) 1.380(8) 1_555 1_555 yes Cl(2) O(9) 1.325(7) 1_555 1_555 yes Cl(2) O(10) 1.322(7) 1_555 1_555 yes Cl(2) O(11) 1.408(9) 1_555 1_555 yes S(1) C(27) 1.615(5) 1_555 1_555 yes O(1) C(5) 1.327(5) 1_555 1_555 yes O(2) C(20) 1.328(5) 1_555 1_555 yes O(3) C(28) 1.23(1) 1_555 1_555 yes N(1) C(8) 1.274(6) 1_555 1_555 yes N(1) C(9) 1.478(6) 1_555 1_555 yes N(2) C(10) 1.468(7) 1_555 1_555 yes N(2) C(11) 1.486(6) 1_555 1_555 yes N(3) C(12) 1.472(6) 1_555 1_555 yes N(3) C(13) 1.276(6) 1_555 1_555 yes N(4) C(21) 1.514(7) 1_555 1_555 yes N(4) C(22) 1.492(9) 1_555 1_555 yes N(5) C(21) 1.463(6) 1_555 1_555 yes N(5) C(23) 1.478(7) 1_555 1_555 yes N(5) C(24) 1.464(8) 1_555 1_555 yes N(6) C(25) 1.463(6) 1_555 1_555 yes N(6) C(26) 1.286(6) 1_555 1_555 yes N(7) C(27) 1.139(6) 1_555 1_555 yes N(8) C(28) 1.30(1) 1_555 1_555 yes N(8) C(29) 1.40(1) 1_555 1_555 yes N(8) C(30) 1.33(1) 1_555 1_555 yes C(1) C(2) 1.513(6) 1_555 1_555 yes C(2) C(3) 1.387(7) 1_555 1_555 yes C(2) C(7) 1.363(7) 1_555 1_555 yes C(3) C(4) 1.413(6) 1_555 1_555 yes C(4) C(5) 1.404(6) 1_555 1_555 yes C(4) C(8) 1.450(6) 1_555 1_555 yes C(5) C(6) 1.414(6) 1_555 1_555 yes C(6) C(7) 1.413(6) 1_555 1_555 yes C(6) C(26) 1.431(7) 1_555 1_555 yes C(9) C(10) 1.515(8) 1_555 1_555 yes C(11) C(12) 1.512(8) 1_555 1_555 yes C(13) C(14) 1.449(7) 1_555 1_555 yes C(14) C(15) 1.405(7) 1_555 1_555 yes C(14) C(20) 1.409(6) 1_555 1_555 yes C(15) C(16) 1.388(8) 1_555 1_555 yes C(16) C(17) 1.512(8) 1_555 1_555 yes C(16) C(18) 1.405(7) 1_555 1_555 yes C(18) C(19) 1.383(7) 1_555 1_555 yes C(19) C(20) 1.413(6) 1_555 1_555 yes C(19) C(21) 1.498(6) 1_555 1_555 yes C(22) C(23) 1.47(1) 1_555 1_555 yes C(24) C(25) 1.518(9) 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 O(1) Fe(1) O(2) 87.4(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(1) 84.5(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(2) 159.8(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(3) 98.6(1) 1_555 1_555 1_555 yes O(1) Fe(1) N(7) 99.7(2) 1_555 1_555 1_555 yes O(2) Fe(1) N(1) 171.7(1) 1_555 1_555 1_555 yes O(2) Fe(1) N(2) 111.2(1) 1_555 1_555 1_555 yes O(2) Fe(1) N(3) 83.7(1) 1_555 1_555 1_555 yes O(2) Fe(1) N(7) 91.2(1) 1_555 1_555 1_555 yes N(1) Fe(1) N(2) 76.5(1) 1_555 1_555 1_555 yes N(1) Fe(1) N(3) 95.6(1) 1_555 1_555 1_555 yes N(1) Fe(1) N(7) 92.0(2) 1_555 1_555 1_555 yes N(2) Fe(1) N(3) 76.6(2) 1_555 1_555 1_555 yes N(2) Fe(1) N(7) 88.0(2) 1_555 1_555 1_555 yes N(3) Fe(1) N(7) 160.7(2) 1_555 1_555 1_555 yes O(4) Cl(1) O(5) 111.3(4) 1_555 1_555 1_555 yes O(4) Cl(1) O(6) 110.2(4) 1_555 1_555 1_555 yes O(4) Cl(1) O(7) 108.6(4) 1_555 1_555 1_555 yes O(5) Cl(1) O(6) 109.8(3) 1_555 1_555 1_555 yes O(5) Cl(1) O(7) 108.4(4) 1_555 1_555 1_555 yes O(6) Cl(1) O(7) 108.4(5) 1_555 1_555 1_555 yes O(8) Cl(2) O(9) 103.7(7) 1_555 1_555 1_555 yes O(8) Cl(2) O(10) 118.9(9) 1_555 1_555 1_555 yes O(8) Cl(2) O(11) 94.3(7) 1_555 1_555 1_555 yes O(9) Cl(2) O(10) 113.8(6) 1_555 1_555 1_555 yes O(9) Cl(2) O(11) 115.8(8) 1_555 1_555 1_555 yes O(10) Cl(2) O(11) 109.0(6) 1_555 1_555 1_555 yes Fe(1) O(1) C(5) 135.8(3) 1_555 1_555 1_555 yes Fe(1) O(2) C(20) 129.0(3) 1_555 1_555 1_555 yes Fe(1) N(1) C(8) 127.2(3) 1_555 1_555 1_555 yes Fe(1) N(1) C(9) 115.3(3) 1_555 1_555 1_555 yes C(8) N(1) C(9) 117.2(4) 1_555 1_555 1_555 yes Fe(1) N(2) C(10) 106.8(3) 1_555 1_555 1_555 yes Fe(1) N(2) C(11) 111.4(3) 1_555 1_555 1_555 yes Fe(1) N(2) H(10) 107.8(3) 1_555 1_555 1_555 no C(10) N(2) C(11) 113.8(4) 1_555 1_555 1_555 yes C(10) N(2) H(10) 108.5(4) 1_555 1_555 1_555 no C(11) N(2) H(10) 108.2(4) 1_555 1_555 1_555 no Fe(1) N(3) C(12) 112.0(3) 1_555 1_555 1_555 yes Fe(1) N(3) C(13) 127.1(3) 1_555 1_555 1_555 yes C(12) N(3) C(13) 120.0(4) 1_555 1_555 1_555 yes C(21) N(4) C(22) 107.2(5) 1_555 1_555 1_555 yes C(21) N(4) H(22) 115.1(4) 1_555 1_555 1_555 no C(21) N(4) H(23) 112.9(4) 1_555 1_555 1_555 no C(22) N(4) H(22) 109.1(5) 1_555 1_555 1_555 no C(22) N(4) H(23) 104.8(5) 1_555 1_555 1_555 no H(22) N(4) H(23) 107.2(5) 1_555 1_555 1_555 no C(21) N(5) C(23) 104.4(4) 1_555 1_555 1_555 yes C(21) N(5) C(24) 114.6(4) 1_555 1_555 1_555 yes C(23) N(5) C(24) 111.4(5) 1_555 1_555 1_555 yes C(25) N(6) C(26) 125.8(4) 1_555 1_555 1_555 yes C(25) N(6) H(32) 121.1(4) 1_555 1_555 1_555 no C(26) N(6) H(32) 113.1(4) 1_555 1_555 1_555 no Fe(1) N(7) C(27) 169.9(4) 1_555 1_555 1_555 yes C(28) N(8) C(29) 113.4(9) 1_555 1_555 1_555 yes C(28) N(8) C(30) 121(1) 1_555 1_555 1_555 yes C(29) N(8) C(30) 124(1) 1_555 1_555 1_555 yes C(2) C(1) H(1) 120.0(6) 1_555 1_555 1_555 no C(2) C(1) H(2) 113.3(5) 1_555 1_555 1_555 no C(2) C(1) H(3) 124.2(6) 1_555 1_555 1_555 no H(1) C(1) H(2) 89.8(6) 1_555 1_555 1_555 no H(1) C(1) H(3) 111.7(6) 1_555 1_555 1_555 no H(2) C(1) H(3) 85.3(5) 1_555 1_555 1_555 no C(1) C(2) C(3) 120.6(5) 1_555 1_555 1_555 yes C(1) C(2) C(7) 121.1(5) 1_555 1_555 1_555 yes C(3) C(2) C(7) 118.2(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 122.2(4) 1_555 1_555 1_555 yes C(2) C(3) H(4) 120.7(4) 1_555 1_555 1_555 no C(4) C(3) H(4) 116.7(5) 1_555 1_555 1_555 no C(3) C(4) C(5) 119.3(4) 1_555 1_555 1_555 yes C(3) C(4) C(8) 117.2(4) 1_555 1_555 1_555 yes C(5) C(4) C(8) 123.5(4) 1_555 1_555 1_555 yes O(1) C(5) C(4) 122.3(4) 1_555 1_555 1_555 yes O(1) C(5) C(6) 119.2(4) 1_555 1_555 1_555 yes C(4) C(5) C(6) 118.5(4) 1_555 1_555 1_555 yes C(5) C(6) C(7) 119.7(4) 1_555 1_555 1_555 yes C(5) C(6) C(26) 123.0(4) 1_555 1_555 1_555 yes C(7) C(6) C(26) 117.3(4) 1_555 1_555 1_555 yes C(2) C(7) C(6) 122.1(4) 1_555 1_555 1_555 yes C(2) C(7) H(34) 118.7(5) 1_555 1_555 1_555 no C(6) C(7) H(34) 119.2(5) 1_555 1_555 1_555 no N(1) C(8) C(4) 125.9(4) 1_555 1_555 1_555 yes N(1) C(8) H(5) 124.3(5) 1_555 1_555 1_555 no C(4) C(8) H(5) 109.7(4) 1_555 1_555 1_555 no N(1) C(9) C(10) 108.8(4) 1_555 1_555 1_555 yes N(1) C(9) H(6) 113.0(4) 1_555 1_555 1_555 no N(1) C(9) H(7) 111.5(5) 1_555 1_555 1_555 no C(10) C(9) H(6) 109.1(5) 1_555 1_555 1_555 no C(10) C(9) H(7) 112.7(5) 1_555 1_555 1_555 no H(6) C(9) H(7) 101.6(5) 1_555 1_555 1_555 no N(2) C(10) C(9) 109.3(4) 1_555 1_555 1_555 yes N(2) C(10) H(8) 107.0(5) 1_555 1_555 1_555 no N(2) C(10) H(9) 118.2(5) 1_555 1_555 1_555 no C(9) C(10) H(8) 113.2(5) 1_555 1_555 1_555 no C(9) C(10) H(9) 111.0(5) 1_555 1_555 1_555 no H(8) C(10) H(9) 97.8(5) 1_555 1_555 1_555 no N(2) C(11) C(12) 111.1(4) 1_555 1_555 1_555 yes N(2) C(11) H(11) 105.4(4) 1_555 1_555 1_555 no N(2) C(11) H(12) 110.5(5) 1_555 1_555 1_555 no C(12) C(11) H(11) 106.3(5) 1_555 1_555 1_555 no C(12) C(11) H(12) 111.2(5) 1_555 1_555 1_555 no H(11) C(11) H(12) 112.1(4) 1_555 1_555 1_555 no N(3) C(12) C(11) 106.1(4) 1_555 1_555 1_555 yes N(3) C(12) H(13) 113.5(5) 1_555 1_555 1_555 no N(3) C(12) H(14) 115.5(5) 1_555 1_555 1_555 no C(11) C(12) H(13) 111.9(5) 1_555 1_555 1_555 no C(11) C(12) H(14) 109.0(5) 1_555 1_555 1_555 no H(13) C(12) H(14) 101.0(4) 1_555 1_555 1_555 no N(3) C(13) C(14) 124.2(4) 1_555 1_555 1_555 yes N(3) C(13) H(15) 130.0(5) 1_555 1_555 1_555 no C(14) C(13) H(15) 105.9(4) 1_555 1_555 1_555 no C(13) C(14) C(15) 118.9(4) 1_555 1_555 1_555 yes C(13) C(14) C(20) 120.9(4) 1_555 1_555 1_555 yes C(15) C(14) C(20) 119.8(4) 1_555 1_555 1_555 yes C(14) C(15) C(16) 122.2(5) 1_555 1_555 1_555 yes C(14) C(15) H(16) 119.2(5) 1_555 1_555 1_555 no C(16) C(15) H(16) 118.6(5) 1_555 1_555 1_555 no C(15) C(16) C(17) 121.4(5) 1_555 1_555 1_555 yes C(15) C(16) C(18) 117.1(5) 1_555 1_555 1_555 yes C(17) C(16) C(18) 121.5(5) 1_555 1_555 1_555 yes C(16) C(17) H(17) 114.3(6) 1_555 1_555 1_555 no C(16) C(17) H(18) 122.6(5) 1_555 1_555 1_555 no C(16) C(17) H(19) 112.4(6) 1_555 1_555 1_555 no H(17) C(17) H(18) 84.2(5) 1_555 1_555 1_555 no H(17) C(17) H(19) 119.1(6) 1_555 1_555 1_555 no H(18) C(17) H(19) 101.4(6) 1_555 1_555 1_555 no C(16) C(18) C(19) 122.2(5) 1_555 1_555 1_555 yes C(16) C(18) H(20) 122.4(5) 1_555 1_555 1_555 no C(19) C(18) H(20) 115.4(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.4(4) 1_555 1_555 1_555 yes C(18) C(19) C(21) 118.9(4) 1_555 1_555 1_555 yes C(20) C(19) C(21) 120.6(4) 1_555 1_555 1_555 yes O(2) C(20) C(14) 122.6(4) 1_555 1_555 1_555 yes O(2) C(20) C(19) 119.1(4) 1_555 1_555 1_555 yes C(14) C(20) C(19) 118.2(4) 1_555 1_555 1_555 yes N(4) C(21) N(5) 101.6(4) 1_555 1_555 1_555 yes N(4) C(21) C(19) 112.7(4) 1_555 1_555 1_555 yes N(4) C(21) H(21) 106.4(4) 1_555 1_555 1_555 no N(5) C(21) C(19) 113.6(4) 1_555 1_555 1_555 yes N(5) C(21) H(21) 108.2(4) 1_555 1_555 1_555 no C(19) C(21) H(21) 113.4(4) 1_555 1_555 1_555 no N(4) C(22) C(23) 105.1(6) 1_555 1_555 1_555 yes N(4) C(22) H(24) 110.1(7) 1_555 1_555 1_555 no N(4) C(22) H(25) 110.2(8) 1_555 1_555 1_555 no C(23) C(22) H(24) 111.9(9) 1_555 1_555 1_555 no C(23) C(22) H(25) 111.1(8) 1_555 1_555 1_555 no H(24) C(22) H(25) 108.4(7) 1_555 1_555 1_555 no N(5) C(23) C(22) 104.7(6) 1_555 1_555 1_555 yes N(5) C(23) H(26) 100.2(6) 1_555 1_555 1_555 no N(5) C(23) H(27) 108.0(6) 1_555 1_555 1_555 no C(22) C(23) H(26) 114.7(7) 1_555 1_555 1_555 no C(22) C(23) H(27) 117.2(8) 1_555 1_555 1_555 no H(26) C(23) H(27) 110.3(8) 1_555 1_555 1_555 no N(5) C(24) C(25) 113.3(4) 1_555 1_555 1_555 yes N(5) C(24) H(28) 114.5(5) 1_555 1_555 1_555 no N(5) C(24) H(29) 107.9(6) 1_555 1_555 1_555 no C(25) C(24) H(28) 99.6(5) 1_555 1_555 1_555 no C(25) C(24) H(29) 104.4(5) 1_555 1_555 1_555 no H(28) C(24) H(29) 116.5(5) 1_555 1_555 1_555 no N(6) C(25) C(24) 110.9(5) 1_555 1_555 1_555 yes N(6) C(25) H(30) 105.1(4) 1_555 1_555 1_555 no N(6) C(25) H(31) 106.1(4) 1_555 1_555 1_555 no C(24) C(25) H(30) 111.1(5) 1_555 1_555 1_555 no C(24) C(25) H(31) 111.3(5) 1_555 1_555 1_555 no H(30) C(25) H(31) 112.1(6) 1_555 1_555 1_555 no N(6) C(26) C(6) 123.6(4) 1_555 1_555 1_555 yes N(6) C(26) H(33) 114.3(4) 1_555 1_555 1_555 no C(6) C(26) H(33) 121.7(4) 1_555 1_555 1_555 no S(1) C(27) N(7) 177.0(5) 1_555 1_555 1_555 yes O(3) C(28) N(8) 122.6(10) 1_555 1_555 1_555 yes O(3) C(28) H(35) 117(1) 1_555 1_555 1_555 no N(8) C(28) H(35) 120(1) 1_555 1_555 1_555 no N(8) C(29) H(36) 110.5(10) 1_555 1_555 1_555 no N(8) C(29) H(37) 112(1) 1_555 1_555 1_555 no N(8) C(29) H(38) 103.4(10) 1_555 1_555 1_555 no H(36) C(29) H(37) 119(1) 1_555 1_555 1_555 no H(36) C(29) H(38) 102(1) 1_555 1_555 1_555 no H(37) C(29) H(38) 105(1) 1_555 1_555 1_555 no N(8) C(30) H(39) 107(1) 1_555 1_555 1_555 no N(8) C(30) H(40) 111.4(10) 1_555 1_555 1_555 no N(8) C(30) H(41) 113(1) 1_555 1_555 1_555 no H(39) C(30) H(40) 104(1) 1_555 1_555 1_555 no H(39) C(30) H(41) 106(1) 1_555 1_555 1_555 no H(40) C(30) H(41) 112(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;