# Copyright The Royal Society of Chemistry, 1998 data_Complex_1 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:48:36 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.609(7) _cell_length_b 18.444(7) _cell_length_c 16.099(8) _cell_angle_alpha 90 _cell_angle_beta 104.56(5) _cell_angle_gamma 90 _cell_volume 2761(2) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21.0 _cell_measurement_theta_max 25.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'dardred' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 620.11 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H27 Cl N2 O2 Ru ' _chemical_formula_moiety 'C33 H27 Cl N2 O2 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1264.00 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.921 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.82 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5355 _reflns_number_total 5040 _reflns_number_observed 3454 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.11 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.01195 _diffrn_orient_matrix_UB_12 -0.04362 _diffrn_orient_matrix_UB_13 0.03445 _diffrn_orient_matrix_UB_21 -0.00615 _diffrn_orient_matrix_UB_22 0.03206 _diffrn_orient_matrix_UB_23 0.04905 _diffrn_orient_matrix_UB_31 -0.10667 _diffrn_orient_matrix_UB_32 0.00304 _diffrn_orient_matrix_UB_33 -0.02294 #------------------------------------------------------------------------------ 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 Ru 0 4 -1.259 0.836 'International Tables' Cl 0 4 0.148 0.159 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 132 0.003 0.002 'International Tables' H 0 108 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Ru(1) 0.19417(4) 0.15780(2) 0.35454(2) 0.0370 Uij ? ? Cl(1) 0.1216(1) 0.27412(7) 0.38922(9) 0.0514 Uij ? ? O(1) -0.0070(3) 0.1396(2) 0.3286(2) 0.0445 Uij ? ? O(2) 0.3026(4) 0.2116(2) 0.2901(2) 0.0458 Uij ? ? N(1) 0.2890(5) 0.1364(2) 0.4492(3) 0.0512 Uij ? ? N(2) 0.2230(4) 0.0570(2) 0.2972(2) 0.0407 Uij ? ? C(1) -0.0801(5) 0.0725(2) 0.3257(3) 0.0394 Uij ? ? C(2) -0.1782(5) 0.0786(3) 0.3873(3) 0.0431 Uij ? ? C(3) -0.2607(6) 0.0208(3) 0.4025(4) 0.0618 Uij ? ? C(4) -0.3473(7) 0.0279(4) 0.4588(4) 0.0709 Uij ? ? C(5) -0.3541(7) 0.0916(4) 0.5002(4) 0.0709 Uij ? ? C(6) -0.2741(8) 0.1488(4) 0.4859(5) 0.0834 Uij ? ? C(7) -0.1870(7) 0.1424(3) 0.4298(4) 0.0682 Uij ? ? C(8) -0.1678(5) 0.0598(3) 0.2333(3) 0.0416 Uij ? ? C(9) -0.2028(6) 0.1178(3) 0.1774(4) 0.0582 Uij ? ? C(10) -0.2837(7) 0.1076(4) 0.0941(4) 0.0733 Uij ? ? C(11) -0.3374(7) 0.0400(4) 0.0667(4) 0.0704 Uij ? ? C(12) -0.3074(7) -0.0166(3) 0.1222(4) 0.0719 Uij ? ? C(13) -0.2242(7) -0.0074(3) 0.2045(4) 0.0622 Uij ? ? C(14) 0.0296(5) 0.0121(3) 0.3586(3) 0.0447 Uij ? ? C(15) 0.1347(5) 0.0010(3) 0.3065(3) 0.0434 Uij ? ? C(16) 0.1517(6) -0.0663(3) 0.2723(4) 0.0556 Uij ? ? C(17) 0.2562(7) -0.0770(3) 0.2291(4) 0.0655 Uij ? ? C(18) 0.3446(7) -0.0201(3) 0.2214(4) 0.0621 Uij ? ? C(19) 0.3262(5) 0.0469(3) 0.2552(3) 0.0455 Uij ? ? C(20) 0.4269(6) 0.1082(3) 0.2504(3) 0.0475 Uij ? ? C(21) 0.3556(5) 0.1824(3) 0.2222(3) 0.0450 Uij ? ? C(22) 0.2298(6) 0.1770(3) 0.1416(3) 0.0494 Uij ? ? C(23) 0.1133(6) 0.2226(3) 0.1329(4) 0.0576 Uij ? ? C(24) -0.0002(7) 0.2197(4) 0.0609(5) 0.0777 Uij ? ? C(25) 0.0015(8) 0.1731(5) -0.0037(5) 0.0889 Uij ? ? C(26) 0.1152(9) 0.1269(5) 0.0030(4) 0.0950 Uij ? ? C(27) 0.2300(7) 0.1301(4) 0.0749(4) 0.0759 Uij ? ? C(28) 0.4758(6) 0.2329(3) 0.2112(4) 0.0481 Uij ? ? C(29) 0.4947(6) 0.2517(3) 0.1309(4) 0.0645 Uij ? ? C(30) 0.6144(8) 0.2923(4) 0.1260(5) 0.0793 Uij ? ? C(31) 0.7143(8) 0.3126(4) 0.1963(6) 0.0782 Uij ? ? C(32) 0.6945(7) 0.2964(3) 0.2761(5) 0.0737 Uij ? ? C(33) 0.5766(7) 0.2569(3) 0.2832(4) 0.0606 Uij ? ? H(1) -0.2577 -0.0240 0.3739 0.0741 Uij ? ? H(2) -0.4030 -0.0123 0.4687 0.0849 Uij ? ? H(3) -0.4140 0.0960 0.5387 0.0851 Uij ? ? H(4) -0.2781 0.1934 0.5146 0.1001 Uij ? ? H(5) -0.1320 0.1830 0.4205 0.0817 Uij ? ? H(6) -0.1710 0.1651 0.1964 0.0699 Uij ? ? H(7) -0.3025 0.1475 0.0555 0.0877 Uij ? ? H(8) -0.3945 0.0331 0.0099 0.0845 Uij ? ? H(9) -0.3445 -0.0633 0.1039 0.0863 Uij ? ? H(10) -0.2050 -0.0478 0.2423 0.0746 Uij ? ? H(11) 0.0811 0.0238 0.4155 0.0537 Uij ? ? H(12) -0.0215 -0.0320 0.3591 0.0537 Uij ? ? H(13) 0.0906 -0.1052 0.2788 0.0666 Uij ? ? H(14) 0.2673 -0.1230 0.2049 0.0785 Uij ? ? H(15) 0.4187 -0.0270 0.1926 0.0745 Uij ? ? H(16) 0.4903 0.1140 0.3057 0.0570 Uij ? ? H(17) 0.4805 0.0949 0.2105 0.0570 Uij ? ? H(18) 0.1113 0.2565 0.1770 0.0690 Uij ? ? H(19) -0.0806 0.2507 0.0567 0.0930 Uij ? ? H(20) -0.0761 0.1725 -0.0537 0.1065 Uij ? ? H(21) 0.1154 0.0930 -0.0413 0.1140 Uij ? ? H(22) 0.3105 0.0994 0.0784 0.0910 Uij ? ? H(23) 0.4267 0.2369 0.0800 0.0774 Uij ? ? H(24) 0.6257 0.3061 0.0712 0.0952 Uij ? ? H(25) 0.7978 0.3378 0.1912 0.0937 Uij ? ? H(26) 0.7624 0.3126 0.3263 0.0884 Uij ? ? H(27) 0.5641 0.2460 0.3385 0.0727 Uij ? ? 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 Ru(1) 0.0377(2) 0.0395(2) 0.0342(2) -0.0010(2) 0.0100(2) -0.0012(2) Cl(1) 0.0570(8) 0.0423(8) 0.0599(8) -0.0050(6) 0.0243(7) -0.0096(6) O(1) 0.036(2) 0.034(2) 0.062(2) -0.002(1) 0.011(2) 0.003(2) O(2) 0.050(2) 0.047(2) 0.047(2) 0.005(2) 0.025(2) 0.005(2) N(1) 0.055(3) 0.054(3) 0.039(2) -0.004(2) 0.001(2) -0.001(2) N(2) 0.039(2) 0.040(2) 0.041(2) 0.008(2) 0.008(2) 0.000(2) C(1) 0.038(3) 0.035(3) 0.046(3) 0.000(2) 0.012(2) 0.003(2) C(2) 0.037(3) 0.045(3) 0.046(3) 0.000(2) 0.007(2) 0.002(2) C(3) 0.060(4) 0.055(4) 0.078(4) 0.002(3) 0.030(3) 0.003(3) C(4) 0.063(4) 0.072(4) 0.087(5) 0.006(3) 0.037(4) 0.029(4) C(5) 0.056(4) 0.106(6) 0.055(4) 0.007(4) 0.023(3) 0.002(4) C(6) 0.079(5) 0.096(6) 0.088(5) -0.022(4) 0.043(4) -0.042(4) C(7) 0.070(4) 0.065(4) 0.078(4) -0.021(3) 0.033(4) -0.022(3) C(8) 0.039(3) 0.042(3) 0.043(3) 0.003(2) 0.010(2) -0.001(2) C(9) 0.064(4) 0.048(3) 0.058(4) -0.002(3) 0.008(3) 0.007(3) C(10) 0.077(5) 0.087(5) 0.049(4) -0.003(4) 0.003(3) 0.018(3) C(11) 0.062(4) 0.090(5) 0.052(4) -0.007(4) 0.001(3) -0.006(4) C(12) 0.078(5) 0.061(4) 0.067(4) -0.012(4) 0.000(4) -0.012(3) C(13) 0.072(4) 0.049(3) 0.057(4) -0.005(3) 0.001(3) 0.001(3) C(14) 0.046(3) 0.039(3) 0.049(3) -0.001(2) 0.012(2) 0.004(2) C(15) 0.040(3) 0.042(3) 0.045(3) 0.007(2) 0.004(2) 0.005(2) C(16) 0.058(4) 0.040(3) 0.066(4) 0.000(3) 0.009(3) -0.009(3) C(17) 0.070(4) 0.052(4) 0.078(4) 0.010(3) 0.024(4) -0.021(3) C(18) 0.066(4) 0.057(4) 0.069(4) 0.014(3) 0.028(3) -0.007(3) C(19) 0.043(3) 0.052(3) 0.042(3) 0.014(2) 0.010(2) 0.002(2) C(20) 0.042(3) 0.057(3) 0.044(3) 0.014(3) 0.012(2) 0.006(3) C(21) 0.043(3) 0.054(3) 0.042(3) 0.011(2) 0.019(2) 0.009(2) C(22) 0.046(3) 0.060(4) 0.045(3) 0.010(3) 0.016(3) 0.012(3) C(23) 0.053(4) 0.062(4) 0.058(4) 0.010(3) 0.016(3) 0.020(3) C(24) 0.054(4) 0.104(6) 0.075(5) 0.027(4) 0.018(4) 0.035(4) C(25) 0.063(5) 0.142(7) 0.057(4) 0.005(5) 0.006(4) 0.020(4) C(26) 0.091(6) 0.135(7) 0.054(4) 0.014(5) 0.009(4) -0.022(4) C(27) 0.067(4) 0.103(5) 0.054(4) 0.028(4) 0.008(3) -0.004(4) C(28) 0.046(3) 0.046(3) 0.057(3) 0.013(3) 0.022(3) 0.008(3) C(29) 0.061(4) 0.079(4) 0.061(4) 0.009(3) 0.029(3) 0.019(3) C(30) 0.084(5) 0.083(5) 0.086(5) 0.010(4) 0.052(4) 0.022(4) C(31) 0.076(5) 0.054(4) 0.121(7) 0.001(4) 0.055(5) 0.001(4) C(32) 0.072(5) 0.053(4) 0.095(5) -0.012(3) 0.021(4) -0.005(4) C(33) 0.065(4) 0.057(4) 0.064(4) -0.003(3) 0.024(3) 0.002(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3454 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0461 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.798 _refine_ls_shift/esd_max 0.0100 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.68 _refine_diff_density_max 1.06 #------------------------------------------------------------------------------ _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 Ru(1) Cl(1) 2.366(1) ? ? yes Ru(1) O(1) 1.902(3) ? ? yes Ru(1) O(2) 1.921(3) ? ? yes Ru(1) N(1) 1.615(4) ? ? yes Ru(1) N(2) 2.125(4) ? ? yes O(1) C(1) 1.418(5) ? ? yes O(2) C(21) 1.422(5) ? ? yes N(2) C(15) 1.368(6) ? ? yes N(2) C(19) 1.346(6) ? ? yes C(1) C(2) 1.534(7) ? ? yes C(1) C(8) 1.533(6) ? ? yes C(1) C(14) 1.534(7) ? ? yes C(2) C(3) 1.386(7) ? ? yes C(2) C(7) 1.375(7) ? ? yes C(3) C(4) 1.382(8) ? ? yes C(4) C(5) 1.360(9) ? ? yes C(5) C(6) 1.359(9) ? ? yes C(6) C(7) 1.381(8) ? ? yes C(8) C(9) 1.383(7) ? ? yes C(8) C(13) 1.385(7) ? ? yes C(9) C(10) 1.384(8) ? ? yes C(10) C(11) 1.379(9) ? ? yes C(11) C(12) 1.357(8) ? ? yes C(12) C(13) 1.375(8) ? ? yes C(14) C(15) 1.480(7) ? ? yes C(15) C(16) 1.384(7) ? ? yes C(16) C(17) 1.373(8) ? ? yes C(17) C(18) 1.375(8) ? ? yes C(18) C(19) 1.381(7) ? ? yes C(19) C(20) 1.502(7) ? ? yes C(20) C(21) 1.547(7) ? ? yes C(21) C(22) 1.538(7) ? ? yes C(21) C(28) 1.529(7) ? ? yes C(22) C(23) 1.378(7) ? ? yes C(22) C(27) 1.379(8) ? ? yes C(23) C(24) 1.378(8) ? ? yes C(24) C(25) 1.353(10) ? ? yes C(25) C(26) 1.368(10) ? ? yes C(26) C(27) 1.385(9) ? ? yes C(28) C(29) 1.394(7) ? ? yes C(28) C(33) 1.383(8) ? ? yes C(29) C(30) 1.391(9) ? ? yes C(30) C(31) 1.340(9) ? ? yes C(31) C(32) 1.377(9) ? ? yes C(32) C(33) 1.375(8) ? ? 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 Cl(1) Ru(1) O(1) 82.4(1) ? ? ? yes Cl(1) Ru(1) O(2) 83.8(1) ? ? ? yes Cl(1) Ru(1) N(1) 97.4(2) ? ? ? yes Cl(1) Ru(1) N(2) 167.0(1) ? ? ? yes O(1) Ru(1) O(2) 129.2(1) ? ? ? yes O(1) Ru(1) N(1) 117.7(2) ? ? ? yes O(1) Ru(1) N(2) 89.2(1) ? ? ? yes O(2) Ru(1) N(1) 112.4(2) ? ? ? yes O(2) Ru(1) N(2) 94.0(1) ? ? ? yes N(1) Ru(1) N(2) 95.3(2) ? ? ? yes Ru(1) O(1) C(1) 129.0(3) ? ? ? yes Ru(1) O(2) C(21) 124.5(3) ? ? ? yes Ru(1) N(2) C(15) 117.4(3) ? ? ? yes Ru(1) N(2) C(19) 122.1(3) ? ? ? yes C(15) N(2) C(19) 120.5(4) ? ? ? yes O(1) C(1) C(2) 107.2(4) ? ? ? yes O(1) C(1) C(8) 108.2(4) ? ? ? yes O(1) C(1) C(14) 109.4(4) ? ? ? yes C(2) C(1) C(8) 111.2(4) ? ? ? yes C(2) C(1) C(14) 108.1(4) ? ? ? yes C(8) C(1) C(14) 112.7(4) ? ? ? yes C(1) C(2) C(3) 122.0(5) ? ? ? yes C(1) C(2) C(7) 120.6(5) ? ? ? yes C(3) C(2) C(7) 117.4(5) ? ? ? yes C(2) C(3) C(4) 120.6(6) ? ? ? yes C(3) C(4) C(5) 120.9(6) ? ? ? yes C(4) C(5) C(6) 119.3(6) ? ? ? yes C(5) C(6) C(7) 120.4(6) ? ? ? yes C(2) C(7) C(6) 121.4(6) ? ? ? yes C(1) C(8) C(9) 119.9(5) ? ? ? yes C(1) C(8) C(13) 122.3(5) ? ? ? yes C(9) C(8) C(13) 117.6(5) ? ? ? yes C(8) C(9) C(10) 120.8(5) ? ? ? yes C(9) C(10) C(11) 120.4(6) ? ? ? yes C(10) C(11) C(12) 119.0(6) ? ? ? yes C(11) C(12) C(13) 121.1(6) ? ? ? yes C(8) C(13) C(12) 121.1(5) ? ? ? yes C(1) C(14) C(15) 114.3(4) ? ? ? yes N(2) C(15) C(14) 119.3(4) ? ? ? yes N(2) C(15) C(16) 119.6(5) ? ? ? yes C(14) C(15) C(16) 120.9(5) ? ? ? yes C(15) C(16) C(17) 120.4(5) ? ? ? yes C(16) C(17) C(18) 118.8(5) ? ? ? yes C(17) C(18) C(19) 120.3(5) ? ? ? yes N(2) C(19) C(18) 120.3(5) ? ? ? yes N(2) C(19) C(20) 119.2(4) ? ? ? yes C(18) C(19) C(20) 120.3(5) ? ? ? yes C(19) C(20) C(21) 115.9(4) ? ? ? yes O(2) C(21) C(20) 109.1(4) ? ? ? yes O(2) C(21) C(22) 108.4(4) ? ? ? yes O(2) C(21) C(28) 106.6(4) ? ? ? yes C(20) C(21) C(22) 112.7(4) ? ? ? yes C(20) C(21) C(28) 106.3(4) ? ? ? yes C(22) C(21) C(28) 113.4(4) ? ? ? yes C(21) C(22) C(23) 119.5(5) ? ? ? yes C(21) C(22) C(27) 122.9(5) ? ? ? yes C(23) C(22) C(27) 117.6(5) ? ? ? yes C(22) C(23) C(24) 120.9(6) ? ? ? yes C(23) C(24) C(25) 120.8(6) ? ? ? yes C(24) C(25) C(26) 119.9(7) ? ? ? yes C(25) C(26) C(27) 119.5(7) ? ? ? yes C(22) C(27) C(26) 121.4(6) ? ? ? yes C(21) C(28) C(29) 122.5(5) ? ? ? yes C(21) C(28) C(33) 119.2(5) ? ? ? yes C(29) C(28) C(33) 118.1(5) ? ? ? yes C(28) C(29) C(30) 119.2(6) ? ? ? yes C(29) C(30) C(31) 121.9(6) ? ? ? yes C(30) C(31) C(32) 119.4(6) ? ? ? yes C(31) C(32) C(33) 120.1(7) ? ? ? yes C(28) C(33) C(32) 121.2(6) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_2b #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:51:37 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 14.107(2) _cell_length_b 10.225(1) _cell_length_c 15.2160(9) _cell_angle_alpha 90 _cell_angle_beta 91.581(7) _cell_angle_gamma 90 _cell_volume 2194.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 48.4 _cell_measurement_theta_max 48.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 659.53 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H18 Cl2 N4 O3 Os ' _chemical_formula_moiety 'C23 H18 Cl2 N4 O3 Os ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1272.00 _exptl_absorpt_coefficient_mu 6.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.427 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.87 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4051 _reflns_number_total 3884 _reflns_number_observed 3223 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.93 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00376 _diffrn_orient_matrix_UB_12 0.00391 _diffrn_orient_matrix_UB_13 -0.06548 _diffrn_orient_matrix_UB_21 -0.07074 _diffrn_orient_matrix_UB_22 -0.00426 _diffrn_orient_matrix_UB_23 -0.00541 _diffrn_orient_matrix_UB_31 -0.00323 _diffrn_orient_matrix_UB_32 0.09762 _diffrn_orient_matrix_UB_33 0.00239 #------------------------------------------------------------------------------ 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 Os 0 4 -1.216 7.603 'International Tables' Cl 0 8 0.148 0.159 'International Tables' O 0 12 0.011 0.006 'International Tables' N 0 16 0.006 0.003 'International Tables' C 0 92 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Os(1) 0.06302(1) 0.18172(2) 0.006768(9) 0.0305 Uij ? ? Cl(1) -0.17455(9) 0.4477(1) 0.35191(7) 0.0523 Uij ? ? Cl(2) -0.25019(8) 0.6107(1) 0.18735(8) 0.0494 Uij ? ? O(1) 0.0969(2) -0.0089(3) 0.0154(2) 0.0360 Uij ? ? O(2) 0.0632(2) 0.1264(3) 0.2766(2) 0.0379 Uij ? ? O(3) -0.1227(2) 0.4457(3) -0.0976(2) 0.0435 Uij ? ? N(1) 0.1634(3) 0.2587(4) 0.0065(2) 0.0417 Uij ? ? N(2) 0.0275(2) 0.1828(3) 0.1334(2) 0.0311 Uij ? ? N(3) -0.0380(3) 0.3135(3) 0.0000(2) 0.0306 Uij ? ? N(4) 0.0352(2) 0.1801(3) -0.1287(2) 0.0295 Uij ? ? C(1) 0.1562(3) -0.0399(4) 0.0848(2) 0.0300 Uij ? ? C(2) 0.2238(3) -0.1364(4) 0.0702(3) 0.0356 Uij ? ? C(3) 0.2867(3) -0.1756(4) 0.1366(3) 0.0414 Uij ? ? C(4) 0.2831(3) -0.1173(5) 0.2185(3) 0.0433 Uij ? ? C(5) 0.2161(3) -0.0233(4) 0.2338(3) 0.0364 Uij ? ? C(6) 0.1505(3) 0.0161(4) 0.1690(2) 0.0298 Uij ? ? C(7) 0.0775(3) 0.1122(4) 0.1983(3) 0.0311 Uij ? ? C(8) -0.0374(3) 0.2828(4) 0.1547(2) 0.0291 Uij ? ? C(9) -0.0699(3) 0.3142(4) 0.2373(3) 0.0361 Uij ? ? C(10) -0.1364(3) 0.4129(4) 0.2468(2) 0.0361 Uij ? ? C(11) -0.1707(3) 0.4831(4) 0.1750(3) 0.0329 Uij ? ? C(12) -0.1398(3) 0.4536(4) 0.0915(2) 0.0332 Uij ? ? C(13) -0.0742(3) 0.3545(4) 0.0815(2) 0.0288 Uij ? ? C(14) -0.0678(3) 0.3569(4) -0.0817(3) 0.0325 Uij ? ? C(15) -0.0247(3) 0.2770(4) -0.1543(2) 0.0294 Uij ? ? C(16) -0.0466(3) 0.3012(4) -0.2407(3) 0.0346 Uij ? ? C(17) -0.0069(3) 0.2241(4) -0.3066(3) 0.0341 Uij ? ? C(18) 0.0547(3) 0.1262(4) -0.2782(3) 0.0373 Uij ? ? C(19) 0.0744(3) 0.1052(4) -0.1901(3) 0.0323 Uij ? ? C(20) -0.0324(3) 0.2432(5) -0.4039(3) 0.0443 Uij ? ? C(21) -0.0796(5) 0.3751(7) -0.4207(3) 0.0875 Uij ? ? C(22) -0.0986(5) 0.1343(7) -0.4333(3) 0.0805 Uij ? ? C(23) 0.0573(4) 0.2379(7) -0.4573(3) 0.0761 Uij ? ? H(1) 0.2268 -0.1759 0.0138 0.0427 Uij ? ? H(2) 0.3320 -0.2421 0.1260 0.0497 Uij ? ? H(3) 0.3269 -0.1422 0.2640 0.0520 Uij ? ? H(4) 0.2144 0.0161 0.2903 0.0437 Uij ? ? H(5) -0.0465 0.2681 0.2876 0.0434 Uij ? ? H(6) -0.1635 0.5008 0.0418 0.0398 Uij ? ? H(7) -0.0888 0.3703 -0.2563 0.0416 Uij ? ? H(8) 0.0841 0.0724 -0.3204 0.0447 Uij ? ? H(9) 0.1163 0.0367 -0.1727 0.0388 Uij ? ? H(10) -0.0374 0.4431 -0.4030 0.1049 Uij ? ? H(11) -0.0950 0.3838 -0.4816 0.1049 Uij ? ? H(12) -0.1359 0.3807 -0.3880 0.1049 Uij ? ? H(13) -0.1545 0.1371 -0.3999 0.0966 Uij ? ? H(14) -0.1150 0.1450 -0.4939 0.0966 Uij ? ? H(15) -0.0680 0.0524 -0.4246 0.0966 Uij ? ? H(16) 0.0878 0.1561 -0.4482 0.0912 Uij ? ? H(17) 0.0411 0.2481 -0.5180 0.0912 Uij ? ? H(18) 0.0989 0.3064 -0.4391 0.0912 Uij ? ? 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 Os(1) 0.0319(1) 0.0345(1) 0.0249(1) 0.00833(6) -0.00391(7) 0.00458(6) Cl(1) 0.0534(7) 0.0707(8) 0.0327(5) 0.0108(6) 0.0026(5) -0.0080(5) Cl(2) 0.0533(7) 0.0418(6) 0.0535(7) 0.0157(5) 0.0099(5) 0.0006(5) O(1) 0.034(2) 0.041(2) 0.033(1) 0.010(1) -0.013(1) -0.003(1) O(2) 0.047(2) 0.042(2) 0.024(1) 0.005(1) -0.011(1) -0.001(1) O(3) 0.055(2) 0.041(2) 0.034(2) 0.020(2) -0.008(1) 0.004(1) N(1) 0.042(2) 0.047(2) 0.036(2) 0.005(2) -0.006(2) 0.006(2) N(2) 0.033(2) 0.037(2) 0.023(2) 0.005(1) -0.006(1) 0.004(1) N(3) 0.033(2) 0.033(2) 0.026(2) 0.002(1) -0.005(1) 0.003(1) N(4) 0.024(2) 0.033(2) 0.031(2) -0.001(1) -0.004(1) 0.002(1) C(1) 0.026(2) 0.029(2) 0.034(2) 0.002(2) -0.010(2) 0.006(2) C(2) 0.032(2) 0.040(2) 0.035(2) 0.006(2) -0.003(2) 0.003(2) C(3) 0.034(2) 0.041(3) 0.049(3) 0.009(2) -0.002(2) 0.010(2) C(4) 0.035(2) 0.051(3) 0.043(2) 0.005(2) -0.016(2) 0.011(2) C(5) 0.036(2) 0.038(2) 0.034(2) 0.002(2) -0.008(2) 0.003(2) C(6) 0.033(2) 0.027(2) 0.030(2) -0.005(2) -0.005(2) 0.006(2) C(7) 0.029(2) 0.029(2) 0.035(2) -0.006(2) -0.011(2) 0.007(2) C(8) 0.028(2) 0.032(2) 0.028(2) 0.001(2) -0.006(2) 0.001(2) C(9) 0.036(2) 0.041(3) 0.031(2) 0.003(2) -0.006(2) 0.006(2) C(10) 0.037(2) 0.041(2) 0.030(2) -0.004(2) 0.002(2) -0.004(2) C(11) 0.031(2) 0.027(2) 0.041(2) 0.003(2) 0.001(2) 0.002(2) C(12) 0.035(2) 0.032(2) 0.032(2) 0.001(2) -0.003(2) 0.004(2) C(13) 0.030(2) 0.032(2) 0.025(2) -0.001(2) -0.002(2) 0.001(2) C(14) 0.039(2) 0.030(2) 0.029(2) 0.003(2) -0.003(2) 0.003(2) C(15) 0.028(2) 0.030(2) 0.030(2) 0.001(2) -0.002(2) 0.004(2) C(16) 0.034(2) 0.037(2) 0.033(2) 0.005(2) -0.004(2) 0.006(2) C(17) 0.031(2) 0.039(2) 0.032(2) -0.002(2) -0.002(2) 0.002(2) C(18) 0.035(2) 0.043(2) 0.034(2) -0.001(2) 0.001(2) -0.005(2) C(19) 0.027(2) 0.033(2) 0.036(2) 0.002(2) -0.002(2) -0.003(2) C(20) 0.050(3) 0.057(3) 0.026(2) 0.007(2) 0.002(2) 0.002(2) C(21) 0.130(6) 0.101(5) 0.031(3) 0.042(5) -0.005(3) 0.007(3) C(22) 0.091(5) 0.110(5) 0.040(3) -0.026(4) -0.025(3) 0.007(3) C(23) 0.076(4) 0.110(5) 0.043(3) 0.002(4) 0.018(3) 0.004(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3223 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0197 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0280 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.390 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.08 _refine_diff_density_max 0.61 #------------------------------------------------------------------------------ _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 Os(1) O(1) 2.010(3) ? ? yes Os(1) N(1) 1.621(4) ? ? yes Os(1) N(2) 2.004(3) ? ? yes Os(1) N(3) 1.962(3) ? ? yes Os(1) N(4) 2.088(3) ? ? yes Cl(1) C(10) 1.738(4) ? ? yes Cl(2) C(11) 1.734(4) ? ? yes O(1) C(1) 1.366(4) ? ? yes O(2) C(7) 1.222(4) ? ? yes O(3) C(14) 1.213(5) ? ? yes N(2) C(7) 1.398(5) ? ? yes N(2) C(8) 1.416(5) ? ? yes N(3) C(13) 1.417(5) ? ? yes N(3) C(14) 1.375(5) ? ? yes N(4) C(15) 1.352(5) ? ? yes N(4) C(19) 1.339(5) ? ? yes C(1) C(2) 1.395(5) ? ? yes C(1) C(6) 1.408(5) ? ? yes C(2) C(3) 1.386(6) ? ? yes C(3) C(4) 1.383(6) ? ? yes C(4) C(5) 1.372(6) ? ? yes C(5) C(6) 1.393(5) ? ? yes C(6) C(7) 1.500(5) ? ? yes C(8) C(9) 1.388(6) ? ? yes C(8) C(13) 1.420(5) ? ? yes C(9) C(10) 1.388(6) ? ? yes C(10) C(11) 1.384(6) ? ? yes C(11) C(12) 1.387(5) ? ? yes C(12) C(13) 1.384(5) ? ? yes C(14) C(15) 1.514(5) ? ? yes C(15) C(16) 1.365(6) ? ? yes C(16) C(17) 1.403(6) ? ? yes C(17) C(18) 1.387(6) ? ? yes C(17) C(20) 1.527(5) ? ? yes C(18) C(19) 1.378(6) ? ? yes C(20) C(21) 1.522(8) ? ? yes C(20) C(22) 1.513(8) ? ? yes C(20) C(23) 1.524(7) ? ? 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) Os(1) N(1) 105.4(2) ? ? ? yes O(1) Os(1) N(2) 90.4(1) ? ? ? yes O(1) Os(1) N(3) 147.2(1) ? ? ? yes O(1) Os(1) N(4) 95.4(1) ? ? ? yes N(1) Os(1) N(2) 104.0(2) ? ? ? yes N(1) Os(1) N(3) 107.4(2) ? ? ? yes N(1) Os(1) N(4) 98.2(1) ? ? ? yes N(2) Os(1) N(3) 81.2(1) ? ? ? yes N(2) Os(1) N(4) 154.7(1) ? ? ? yes N(3) Os(1) N(4) 80.6(1) ? ? ? yes Os(1) O(1) C(1) 114.5(2) ? ? ? yes Os(1) N(2) C(7) 122.8(3) ? ? ? yes Os(1) N(2) C(8) 113.8(2) ? ? ? yes C(7) N(2) C(8) 121.9(3) ? ? ? yes Os(1) N(3) C(13) 115.8(2) ? ? ? yes Os(1) N(3) C(14) 118.2(3) ? ? ? yes C(13) N(3) C(14) 125.9(3) ? ? ? yes Os(1) N(4) C(15) 112.2(2) ? ? ? yes Os(1) N(4) C(19) 128.6(3) ? ? ? yes C(15) N(4) C(19) 119.0(3) ? ? ? yes O(1) C(1) C(2) 116.6(3) ? ? ? yes O(1) C(1) C(6) 124.1(3) ? ? ? yes C(2) C(1) C(6) 119.3(3) ? ? ? yes C(1) C(2) C(3) 121.0(4) ? ? ? yes C(2) C(3) C(4) 119.6(4) ? ? ? yes C(3) C(4) C(5) 119.8(4) ? ? ? yes C(4) C(5) C(6) 122.0(4) ? ? ? yes C(1) C(6) C(5) 118.3(4) ? ? ? yes C(1) C(6) C(7) 126.3(3) ? ? ? yes C(5) C(6) C(7) 115.3(3) ? ? ? yes O(2) C(7) N(2) 122.3(4) ? ? ? yes O(2) C(7) C(6) 120.0(3) ? ? ? yes N(2) C(7) C(6) 117.7(3) ? ? ? yes N(2) C(8) C(9) 127.3(3) ? ? ? yes N(2) C(8) C(13) 114.7(3) ? ? ? yes C(9) C(8) C(13) 118.0(3) ? ? ? yes C(8) C(9) C(10) 120.2(4) ? ? ? yes Cl(1) C(10) C(9) 118.2(3) ? ? ? yes Cl(1) C(10) C(11) 120.7(3) ? ? ? yes C(9) C(10) C(11) 121.1(4) ? ? ? yes Cl(2) C(11) C(10) 121.2(3) ? ? ? yes Cl(2) C(11) C(12) 118.9(3) ? ? ? yes C(10) C(11) C(12) 119.9(4) ? ? ? yes C(11) C(12) C(13) 119.3(4) ? ? ? yes N(3) C(13) C(8) 113.6(3) ? ? ? yes N(3) C(13) C(12) 124.9(3) ? ? ? yes C(8) C(13) C(12) 121.5(3) ? ? ? yes O(3) C(14) N(3) 126.8(4) ? ? ? yes O(3) C(14) C(15) 121.8(4) ? ? ? yes N(3) C(14) C(15) 111.4(3) ? ? ? yes N(4) C(15) C(14) 116.5(3) ? ? ? yes N(4) C(15) C(16) 122.2(4) ? ? ? yes C(14) C(15) C(16) 121.3(4) ? ? ? yes C(15) C(16) C(17) 120.1(4) ? ? ? yes C(16) C(17) C(18) 116.2(4) ? ? ? yes C(16) C(17) C(20) 122.2(4) ? ? ? yes C(18) C(17) C(20) 121.6(4) ? ? ? yes C(17) C(18) C(19) 121.5(4) ? ? ? yes N(4) C(19) C(18) 120.9(4) ? ? ? yes C(17) C(20) C(21) 111.5(4) ? ? ? yes C(17) C(20) C(22) 108.6(4) ? ? ? yes C(17) C(20) C(23) 109.6(4) ? ? ? yes C(21) C(20) C(22) 109.8(5) ? ? ? yes C(21) C(20) C(23) 107.9(5) ? ? ? yes C(22) C(20) C(23) 109.3(5) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_3a #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:57:21 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 15.346(3) _cell_length_b 19.721(3) _cell_length_c 22.744(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6883(1) _cell_formula_units_Z 8 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _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 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 701.87 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 N4 O4 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2944.00 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 7052 _reflns_number_total 7052 _reflns_number_observed 3902 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.65 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 8 -1.259 0.836 'International Tables' O 0 32 0.011 0.006 'International Tables' N 0 32 0.006 0.003 'International Tables' C 0 288 0.003 0.002 'International Tables' H 0 384 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Ru(1) 0.20827(2) 0.09940(2) 0.00427(1) 0.0508 Uij ? ? O(1) 0.1516(2) 0.0126(1) 0.0208(1) 0.0614 Uij ? ? O(2) 0.2288(2) 0.0492(1) -0.0687(1) 0.0631 Uij ? ? O(3) 0.2335(3) 0.0789(2) 0.1855(2) 0.0963 Uij ? ? O(4) 0.4524(2) 0.1650(2) -0.0490(2) 0.0908 Uij ? ? N(1) 0.1346(2) 0.1545(2) -0.0082(1) 0.0636 Uij ? ? N(2) 0.2397(2) 0.1098(2) 0.0894(1) 0.0554 Uij ? ? N(3) 0.3216(2) 0.1477(2) -0.0041(2) 0.0555 Uij ? ? N(4) 0.6813(3) 0.1439(2) 0.0885(2) 0.0677 Uij ? ? C(1) 0.1064(3) 0.0020(2) 0.0707(2) 0.0550 Uij ? ? C(2) 0.0350(3) -0.0407(2) 0.0659(2) 0.0625 Uij ? ? C(3) -0.0139(3) -0.0558(2) 0.1150(2) 0.0703 Uij ? ? C(4) 0.0078(3) -0.0296(3) 0.1691(2) 0.0769 Uij ? ? C(5) 0.0786(4) 0.0127(2) 0.1732(2) 0.0704 Uij ? ? C(6) 0.1289(3) 0.0297(2) 0.1247(2) 0.0543 Uij ? ? C(7) 0.2044(3) 0.0739(2) 0.1359(2) 0.0635 Uij ? ? C(8) 0.3022(3) 0.1608(2) 0.0986(2) 0.0601 Uij ? ? C(9) 0.3202(3) 0.1931(2) 0.1521(2) 0.0752 Uij ? ? C(10) 0.3779(4) 0.2456(3) 0.1541(3) 0.0896 Uij ? ? C(11) 0.4179(4) 0.2674(2) 0.1043(3) 0.0895 Uij ? ? C(12) 0.4042(3) 0.2361(2) 0.0505(2) 0.0733 Uij ? ? C(13) 0.3459(3) 0.1822(2) 0.0483(2) 0.0592 Uij ? ? C(14) 0.3774(4) 0.1455(2) -0.0516(2) 0.0658 Uij ? ? C(15) 0.3429(3) 0.1189(2) -0.1084(2) 0.0618 Uij ? ? C(16) 0.3882(3) 0.1374(2) -0.1600(2) 0.0789 Uij ? ? C(17) 0.3634(4) 0.1142(3) -0.2139(2) 0.0900 Uij ? ? C(18) 0.2933(4) 0.0709(3) -0.2199(2) 0.0829 Uij ? ? C(19) 0.2481(3) 0.0518(2) -0.1706(2) 0.0689 Uij ? ? C(20) 0.2722(3) 0.0746(2) -0.1145(2) 0.0604 Uij ? ? C(21) 0.6728(3) 0.1704(2) 0.0257(2) 0.0756 Uij ? ? C(22) 0.6984(4) 0.1218(3) -0.0224(3) 0.0914 Uij ? ? C(23) 0.6864(4) 0.1563(3) -0.0809(3) 0.0946 Uij ? ? C(24) 0.7181(5) 0.1149(3) -0.1302(3) 0.1221 Uij ? ? C(25) 0.6234(4) 0.0824(2) 0.0986(2) 0.0763 Uij ? ? C(26) 0.5274(4) 0.0921(3) 0.0857(3) 0.0920 Uij ? ? C(27) 0.4758(4) 0.0278(3) 0.1019(3) 0.1006 Uij ? ? C(28) 0.4666(5) 0.0197(4) 0.1668(4) 0.1487 Uij ? ? C(29) 0.6546(3) 0.2022(2) 0.1293(3) 0.0830 Uij ? ? C(30) 0.6553(4) 0.1877(3) 0.1945(3) 0.1095 Uij ? ? C(31) 0.6473(10) 0.2466(6) 0.2345(5) 0.2302 Uij ? ? C(32) 0.5977(8) 0.2932(5) 0.2305(5) 0.2079 Uij ? ? C(33) 0.7733(3) 0.1207(2) 0.1018(2) 0.0714 Uij ? ? C(34) 0.8448(4) 0.1736(3) 0.0946(3) 0.0954 Uij ? ? C(35) 0.9329(4) 0.1447(3) 0.1129(3) 0.1090 Uij ? ? C(36) 1.0069(9) 0.1887(6) 0.1158(6) 0.111(4) Uij ? ? C(37) 0.9310(9) 0.1542(7) 0.1776(7) 0.134(5) Uij ? ? H(1) 0.0199 -0.0595 0.0288 0.0749 Uij ? ? H(2) -0.0631 -0.0847 0.1114 0.0843 Uij ? ? H(3) -0.0254 -0.0405 0.2030 0.0922 Uij ? ? H(4) 0.0936 0.0310 0.2105 0.0840 Uij ? ? H(5) 0.2923 0.1784 0.1871 0.0898 Uij ? ? H(6) 0.3901 0.2670 0.1906 0.1075 Uij ? ? H(7) 0.4562 0.3051 0.1063 0.1070 Uij ? ? H(8) 0.4337 0.2511 0.0162 0.0877 Uij ? ? H(9) 0.4370 0.1667 -0.1571 0.0945 Uij ? ? H(10) 0.3948 0.1279 -0.2478 0.1079 Uij ? ? H(11) 0.2764 0.0546 -0.2576 0.0993 Uij ? ? H(12) 0.1995 0.0224 -0.1745 0.0824 Uij ? ? H(13) 0.6136 0.1827 0.0197 0.0906 Uij ? ? H(14) 0.7086 0.2095 0.0223 0.0906 Uij ? ? H(15) 0.7577 0.1091 -0.0177 0.1093 Uij ? ? H(16) 0.6626 0.0826 -0.0206 0.1093 Uij ? ? H(17) 0.6261 0.1651 -0.0865 0.1139 Uij ? ? H(18) 0.7175 0.1979 -0.0805 0.1139 Uij ? ? H(19) 0.6869 0.0732 -0.1313 0.1464 Uij ? ? H(20) 0.7094 0.1386 -0.1661 0.1464 Uij ? ? H(21) 0.7785 0.1059 -0.1251 0.1464 Uij ? ? H(22) 0.6443 0.0468 0.0743 0.0913 Uij ? ? H(23) 0.6290 0.0696 0.1388 0.0913 Uij ? ? H(24) 0.5061 0.1292 0.1081 0.1103 Uij ? ? H(25) 0.5201 0.1013 0.0450 0.1103 Uij ? ? H(26) 0.4195 0.0307 0.0849 0.1203 Uij ? ? H(27) 0.5055 -0.0106 0.0865 0.1203 Uij ? ? H(28) 0.4365 0.0576 0.1825 0.1793 Uij ? ? H(29) 0.4351 -0.0206 0.1750 0.1793 Uij ? ? H(30) 0.5229 0.0168 0.1842 0.1793 Uij ? ? H(31) 0.6933 0.2389 0.1223 0.0996 Uij ? ? H(32) 0.5970 0.2153 0.1189 0.0996 Uij ? ? H(33) 0.6084 0.1577 0.2025 0.1314 Uij ? ? H(34) 0.7090 0.1658 0.2033 0.1314 Uij ? ? H(35) 0.6343 0.2270 0.2719 0.2754 Uij ? ? H(36) 0.7033 0.2662 0.2354 0.2754 Uij ? ? H(37) 0.6064 0.3232 0.2624 0.2452 Uij ? ? H(38) 0.6089 0.3165 0.1944 0.2452 Uij ? ? H(39) 0.5397 0.2770 0.2305 0.2452 Uij ? ? H(40) 0.7746 0.1054 0.1414 0.0853 Uij ? ? H(41) 0.7864 0.0840 0.0762 0.0853 Uij ? ? H(42) 0.8474 0.1872 0.0546 0.1142 Uij ? ? H(43) 0.8316 0.2117 0.1185 0.1142 Uij ? ? H(44) 1.0500 0.1682 0.1395 0.1398 Uij ? ? H(45) 1.0284 0.1956 0.0773 0.1398 Uij ? ? H(46) 0.9893 0.2306 0.1324 0.1398 Uij ? ? H(47) 0.9844 0.1386 0.1938 0.1398 Uij ? ? H(48) 0.9239 0.2010 0.1861 0.1398 Uij ? ? H(49) 0.8840 0.1293 0.1936 0.1398 Uij ? ? 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 Ru(1) 0.0559(3) 0.0460(2) 0.0506(2) 0.0005(2) -0.0025(2) 0.0004(1) O(1) 0.077(2) 0.053(2) 0.054(2) -0.008(1) 0.007(2) -0.004(1) O(2) 0.079(2) 0.059(2) 0.052(2) -0.008(2) 0.005(2) -0.001(1) O(3) 0.113(3) 0.125(3) 0.051(2) -0.032(2) -0.017(2) 0.008(2) O(4) 0.059(3) 0.113(3) 0.101(3) -0.017(2) 0.009(2) 0.007(2) N(1) 0.061(3) 0.057(2) 0.072(3) 0.003(2) -0.008(2) 0.002(2) N(2) 0.056(2) 0.057(2) 0.054(2) -0.001(2) -0.006(2) -0.005(2) N(3) 0.057(2) 0.049(2) 0.060(2) 0.002(2) 0.000(2) 0.004(2) N(4) 0.069(3) 0.053(2) 0.081(3) 0.009(2) 0.001(2) 0.012(2) C(1) 0.059(3) 0.050(2) 0.055(3) 0.006(2) 0.000(2) 0.010(2) C(2) 0.070(3) 0.054(3) 0.063(3) -0.002(2) 0.000(3) 0.009(2) C(3) 0.067(4) 0.065(3) 0.079(4) -0.007(2) -0.003(3) 0.018(3) C(4) 0.075(4) 0.089(3) 0.067(4) 0.001(3) 0.008(3) 0.018(3) C(5) 0.075(4) 0.083(3) 0.053(3) 0.005(3) -0.003(3) 0.009(2) C(6) 0.053(3) 0.063(3) 0.047(3) 0.003(2) -0.002(2) 0.008(2) C(7) 0.067(4) 0.075(3) 0.049(3) 0.002(3) 0.001(3) 0.000(2) C(8) 0.063(3) 0.053(3) 0.064(3) 0.003(2) -0.006(3) -0.006(2) C(9) 0.081(4) 0.072(3) 0.073(3) -0.002(3) -0.011(3) -0.017(2) C(10) 0.099(5) 0.084(4) 0.086(4) -0.006(3) -0.022(4) -0.026(3) C(11) 0.083(4) 0.057(3) 0.128(6) -0.005(3) -0.035(4) -0.011(3) C(12) 0.067(4) 0.055(3) 0.098(4) -0.002(2) -0.025(3) 0.009(3) C(13) 0.057(3) 0.049(2) 0.072(3) 0.004(2) -0.015(3) -0.003(2) C(14) 0.069(4) 0.058(3) 0.071(3) 0.007(3) 0.004(3) 0.013(2) C(15) 0.066(4) 0.057(3) 0.063(3) 0.011(2) 0.013(3) 0.012(2) C(16) 0.083(4) 0.071(3) 0.083(4) 0.007(3) 0.021(3) 0.010(3) C(17) 0.118(5) 0.088(4) 0.064(4) 0.012(4) 0.023(3) 0.020(3) C(18) 0.108(5) 0.081(3) 0.059(3) 0.020(3) 0.007(3) 0.008(3) C(19) 0.083(4) 0.068(3) 0.055(3) 0.013(3) 0.000(3) 0.003(2) C(20) 0.072(4) 0.054(2) 0.055(3) 0.011(2) 0.006(3) 0.007(2) C(21) 0.091(4) 0.062(3) 0.074(3) 0.016(3) -0.002(3) 0.018(3) C(22) 0.109(5) 0.084(4) 0.081(4) 0.018(3) -0.001(4) 0.003(3) C(23) 0.097(5) 0.108(5) 0.079(4) 0.001(4) 0.009(3) 0.006(3) C(24) 0.146(7) 0.131(5) 0.088(5) -0.001(5) 0.003(4) -0.011(4) C(25) 0.078(4) 0.060(3) 0.092(4) 0.003(3) 0.000(3) 0.021(2) C(26) 0.072(4) 0.086(4) 0.118(5) 0.011(3) -0.014(3) 0.023(3) C(27) 0.071(4) 0.096(4) 0.134(6) -0.006(3) -0.016(4) 0.019(4) C(28) 0.117(6) 0.172(7) 0.157(8) -0.022(5) -0.008(6) 0.071(6) C(29) 0.081(4) 0.068(3) 0.100(4) 0.016(3) 0.007(3) -0.001(3) C(30) 0.130(6) 0.112(5) 0.086(4) 0.012(4) 0.000(4) -0.009(4) C(31) 0.31(2) 0.24(1) 0.140(8) 0.15(1) 0.014(9) -0.046(8) C(32) 0.19(1) 0.163(9) 0.27(1) 0.002(7) -0.041(9) -0.063(9) C(33) 0.071(4) 0.059(3) 0.084(4) 0.006(2) -0.008(3) 0.009(2) C(34) 0.087(5) 0.080(4) 0.119(5) -0.009(3) 0.008(4) 0.012(3) C(35) 0.063(4) 0.108(4) 0.156(7) 0.001(3) -0.022(4) 0.009(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3902 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0423 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0561 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.143 _refine_ls_shift/esd_max 0.1620 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.48 _refine_diff_density_max 0.40 #------------------------------------------------------------------------------ _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 Ru(1) O(1) 1.956(3) ? ? yes Ru(1) O(2) 1.957(3) ? ? yes Ru(1) N(1) 1.594(4) ? ? yes Ru(1) N(2) 2.006(3) ? ? yes Ru(1) N(3) 1.992(4) ? ? yes O(1) C(1) 1.346(5) ? ? yes O(2) C(20) 1.335(5) ? ? yes O(3) C(7) 1.217(5) ? ? yes O(4) C(14) 1.215(5) ? ? yes N(2) C(7) 1.383(6) ? ? yes N(2) C(8) 1.404(5) ? ? yes N(3) C(13) 1.424(5) ? ? yes N(3) C(14) 1.379(5) ? ? yes N(4) C(21) 1.525(6) ? ? yes N(4) C(25) 1.521(6) ? ? yes N(4) C(29) 1.535(6) ? ? yes N(4) C(33) 1.515(6) ? ? yes C(1) C(2) 1.386(6) ? ? yes C(1) C(6) 1.389(6) ? ? yes C(2) C(3) 1.378(6) ? ? yes C(3) C(4) 1.377(7) ? ? yes C(4) C(5) 1.372(6) ? ? yes C(5) C(6) 1.387(6) ? ? yes C(6) C(7) 1.473(6) ? ? yes C(8) C(9) 1.403(6) ? ? yes C(8) C(13) 1.391(6) ? ? yes C(9) C(10) 1.362(7) ? ? yes C(10) C(11) 1.358(8) ? ? yes C(11) C(12) 1.386(7) ? ? yes C(12) C(13) 1.390(6) ? ? yes C(14) C(15) 1.493(6) ? ? yes C(15) C(16) 1.412(6) ? ? yes C(15) C(20) 1.398(7) ? ? yes C(16) C(17) 1.361(7) ? ? yes C(17) C(18) 1.381(8) ? ? yes C(18) C(19) 1.370(7) ? ? yes C(19) C(20) 1.403(6) ? ? yes C(21) C(22) 1.507(7) ? ? yes C(22) C(23) 1.505(8) ? ? yes C(23) C(24) 1.471(8) ? ? yes C(25) C(26) 1.515(7) ? ? yes C(26) C(27) 1.540(7) ? ? yes C(27) C(28) 1.490(9) ? ? yes C(29) C(30) 1.510(8) ? ? yes C(30) C(31) 1.48(1) ? ? yes C(31) C(32) 1.20(1) ? ? yes C(33) C(34) 1.521(7) ? ? yes C(34) C(35) 1.525(7) ? ? yes C(35) C(36) 1.43(1) ? ? yes C(35) C(37) 1.49(2) ? ? 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) Ru(1) O(2) 78.0(1) ? ? ? yes O(1) Ru(1) N(1) 108.4(2) ? ? ? yes O(1) Ru(1) N(2) 90.6(1) ? ? ? yes O(1) Ru(1) N(3) 145.6(1) ? ? ? yes O(2) Ru(1) N(1) 108.0(1) ? ? ? yes O(2) Ru(1) N(2) 146.2(1) ? ? ? yes O(2) Ru(1) N(3) 91.1(1) ? ? ? yes N(1) Ru(1) N(2) 105.8(2) ? ? ? yes N(1) Ru(1) N(3) 106.0(2) ? ? ? yes N(2) Ru(1) N(3) 80.4(1) ? ? ? yes Ru(1) O(1) C(1) 121.8(2) ? ? ? yes Ru(1) O(2) C(20) 123.5(3) ? ? ? yes Ru(1) N(2) C(7) 126.3(3) ? ? ? yes Ru(1) N(2) C(8) 112.4(3) ? ? ? yes C(7) N(2) C(8) 121.3(4) ? ? ? yes Ru(1) N(3) C(13) 112.1(3) ? ? ? yes Ru(1) N(3) C(14) 127.0(3) ? ? ? yes C(13) N(3) C(14) 120.6(4) ? ? ? yes C(21) N(4) C(25) 111.5(4) ? ? ? yes C(21) N(4) C(29) 106.7(3) ? ? ? yes C(21) N(4) C(33) 111.7(4) ? ? ? yes C(25) N(4) C(29) 110.5(4) ? ? ? yes C(25) N(4) C(33) 105.9(3) ? ? ? yes C(29) N(4) C(33) 110.7(4) ? ? ? yes O(1) C(1) C(2) 115.8(4) ? ? ? yes O(1) C(1) C(6) 123.8(4) ? ? ? yes C(2) C(1) C(6) 120.4(4) ? ? ? yes C(1) C(2) C(3) 119.9(4) ? ? ? yes C(2) C(3) C(4) 120.7(4) ? ? ? yes C(3) C(4) C(5) 118.7(5) ? ? ? yes C(4) C(5) C(6) 122.2(5) ? ? ? yes C(1) C(6) C(5) 118.0(4) ? ? ? yes C(1) C(6) C(7) 125.6(4) ? ? ? yes C(5) C(6) C(7) 116.4(4) ? ? ? yes O(3) C(7) N(2) 121.7(5) ? ? ? yes O(3) C(7) C(6) 119.7(4) ? ? ? yes N(2) C(7) C(6) 118.6(4) ? ? ? yes N(2) C(8) C(9) 126.1(4) ? ? ? yes N(2) C(8) C(13) 115.2(4) ? ? ? yes C(9) C(8) C(13) 118.6(4) ? ? ? yes C(8) C(9) C(10) 120.2(5) ? ? ? yes C(9) C(10) C(11) 120.4(5) ? ? ? yes C(10) C(11) C(12) 121.8(5) ? ? ? yes C(11) C(12) C(13) 118.0(5) ? ? ? yes N(3) C(13) C(8) 114.6(4) ? ? ? yes N(3) C(13) C(12) 124.3(4) ? ? ? yes C(8) C(13) C(12) 121.0(4) ? ? ? yes O(4) C(14) N(3) 122.8(5) ? ? ? yes O(4) C(14) C(15) 119.3(5) ? ? ? yes N(3) C(14) C(15) 117.9(5) ? ? ? yes C(14) C(15) C(16) 117.0(5) ? ? ? yes C(14) C(15) C(20) 125.5(4) ? ? ? yes C(16) C(15) C(20) 117.4(5) ? ? ? yes C(15) C(16) C(17) 121.5(5) ? ? ? yes C(16) C(17) C(18) 121.0(5) ? ? ? yes C(17) C(18) C(19) 118.8(5) ? ? ? yes C(18) C(19) C(20) 121.5(5) ? ? ? yes O(2) C(20) C(15) 122.9(4) ? ? ? yes O(2) C(20) C(19) 117.3(4) ? ? ? yes C(15) C(20) C(19) 119.7(4) ? ? ? yes N(4) C(21) C(22) 116.1(4) ? ? ? yes C(21) C(22) C(23) 108.9(5) ? ? ? yes C(22) C(23) C(24) 112.5(5) ? ? ? yes N(4) C(25) C(26) 116.0(4) ? ? ? yes C(25) C(26) C(27) 110.5(4) ? ? ? yes C(26) C(27) C(28) 112.0(6) ? ? ? yes N(4) C(29) C(30) 116.7(4) ? ? ? yes C(29) C(30) C(31) 116.9(6) ? ? ? yes C(30) C(31) C(32) 127(1) ? ? ? yes N(4) C(33) C(34) 116.3(4) ? ? ? yes C(33) C(34) C(35) 110.7(5) ? ? ? yes C(34) C(35) C(36) 119.3(7) ? ? ? yes C(34) C(35) C(37) 101.9(8) ? ? ? yes C(36) C(35) C(37) 83.9(8) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_3b #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:53:53 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 19.816(2) _cell_length_b 22.746(4) _cell_length_c 15.430(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6955(1) _cell_formula_units_Z 8 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 29.1 _cell_measurement_theta_max 32.3 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _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 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 791.00 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 N4 O4 Os ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3200.00 _exptl_absorpt_coefficient_mu 3.708 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.388 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -1.18 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 6753 _reflns_number_total 6753 _reflns_number_observed 3047 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01339 _diffrn_orient_matrix_UB_12 -0.00056 _diffrn_orient_matrix_UB_13 -0.06248 _diffrn_orient_matrix_UB_21 -0.00168 _diffrn_orient_matrix_UB_22 0.04393 _diffrn_orient_matrix_UB_23 -0.00144 _diffrn_orient_matrix_UB_31 0.04863 _diffrn_orient_matrix_UB_32 0.00167 _diffrn_orient_matrix_UB_33 0.01715 #------------------------------------------------------------------------------ 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 Os 0 8 -1.216 7.603 'International Tables' O 0 32 0.011 0.006 'International Tables' N 0 32 0.006 0.003 'International Tables' C 0 288 0.003 0.002 'International Tables' H 0 384 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Os(1) 0.39959(1) 0.00301(1) 0.29244(2) 0.0506 Uij ? ? O(1) 0.4863(3) 0.0203(2) 0.3493(3) 0.0619 Uij ? ? O(2) 0.4516(3) -0.0697(2) 0.2712(3) 0.0605 Uij ? ? O(3) 0.4173(4) 0.1849(3) 0.2678(4) 0.0975 Uij ? ? O(4) 0.3368(3) -0.0506(3) 0.0478(4) 0.0878 Uij ? ? N(1) 0.3439(3) -0.0117(3) 0.3659(4) 0.0665 Uij ? ? N(2) 0.3878(3) 0.0881(3) 0.2603(4) 0.0568 Uij ? ? N(3) 0.3523(3) -0.0058(3) 0.1779(4) 0.0558 Uij ? ? N(4) 0.6454(3) -0.0891(3) 0.1820(4) 0.0659 Uij ? ? C(1) 0.4962(4) 0.0704(4) 0.3939(5) 0.0553 Uij ? ? C(2) 0.5396(4) 0.0662(4) 0.4654(6) 0.0651 Uij ? ? C(3) 0.5543(5) 0.1162(4) 0.5153(5) 0.0702 Uij ? ? C(4) 0.5269(5) 0.1686(4) 0.4929(6) 0.0826 Uij ? ? C(5) 0.4832(5) 0.1739(4) 0.4223(6) 0.0685 Uij ? ? C(6) 0.4674(4) 0.1239(3) 0.3729(5) 0.0563 Uij ? ? C(7) 0.4223(5) 0.1349(4) 0.2972(6) 0.0665 Uij ? ? C(8) 0.3366(4) 0.0972(4) 0.1966(5) 0.0627 Uij ? ? C(9) 0.3046(5) 0.1499(4) 0.1801(6) 0.0749 Uij ? ? C(10) 0.2527(5) 0.1519(5) 0.1225(7) 0.0870 Uij ? ? C(11) 0.2318(5) 0.1021(6) 0.0801(7) 0.0885 Uij ? ? C(12) 0.2649(5) 0.0482(4) 0.0945(5) 0.0724 Uij ? ? C(13) 0.3170(4) 0.0460(4) 0.1528(5) 0.0583 Uij ? ? C(14) 0.3552(4) -0.0535(4) 0.1235(6) 0.0660 Uij ? ? C(15) 0.3827(4) -0.1104(4) 0.1571(5) 0.0602 Uij ? ? C(16) 0.3647(5) -0.1610(4) 0.1115(5) 0.0765 Uij ? ? C(17) 0.3878(5) -0.2156(4) 0.1362(7) 0.0921 Uij ? ? C(18) 0.4320(5) -0.2212(4) 0.2064(6) 0.0775 Uij ? ? C(19) 0.4497(4) -0.1712(3) 0.2490(6) 0.0667 Uij ? ? C(20) 0.4267(4) -0.1159(4) 0.2260(5) 0.0596 Uij ? ? C(21) 0.5843(4) -0.0994(4) 0.1243(6) 0.0789 Uij ? ? C(22) 0.5925(5) -0.0854(5) 0.0282(6) 0.0904 Uij ? ? C(23) 0.5288(6) -0.1008(6) -0.0227(6) 0.1017 Uij ? ? C(24) 0.5201(7) -0.1647(7) -0.0320(8) 0.1552 Uij ? ? C(25) 0.7029(5) -0.1286(4) 0.1546(6) 0.0818 Uij ? ? C(26) 0.6886(6) -0.1947(5) 0.1573(7) 0.1077 Uij ? ? C(27) 0.752(1) -0.2306(8) 0.143(2) 0.2358 Uij ? ? C(28) 0.7931(10) -0.2302(10) 0.095(1) 0.2231 Uij ? ? C(29) 0.6699(4) -0.0265(4) 0.1729(6) 0.0760 Uij ? ? C(30) 0.6219(5) 0.0202(5) 0.2001(6) 0.0853 Uij ? ? C(31) 0.6550(6) 0.0804(5) 0.1873(6) 0.0938 Uij ? ? C(32) 0.6125(6) 0.1291(5) 0.2178(8) 0.1232 Uij ? ? C(33) 0.6218(4) -0.1025(4) 0.2723(6) 0.0695 Uij ? ? C(34) 0.6746(5) -0.0959(5) 0.3445(6) 0.0950 Uij ? ? C(35) 0.6461(5) -0.1139(6) 0.4314(6) 0.1016 Uij ? ? C(36) 0.654(1) -0.179(1) 0.430(1) 0.109(8) Uij ? ? C(36') 0.688(1) -0.1174(9) 0.503(1) 0.103(7) Uij ? ? H(1) 0.5593 0.0294 0.4799 0.0778 Uij ? ? H(2) 0.5829 0.1133 0.5645 0.0839 Uij ? ? H(3) 0.5376 0.2027 0.5259 0.0988 Uij ? ? H(4) 0.4644 0.2110 0.4078 0.0828 Uij ? ? H(5) 0.3189 0.1847 0.2089 0.0897 Uij ? ? H(6) 0.2307 0.1883 0.1116 0.1047 Uij ? ? H(7) 0.1949 0.1039 0.0408 0.1066 Uij ? ? H(8) 0.2513 0.0138 0.0643 0.0867 Uij ? ? H(9) 0.3358 -0.1577 0.0627 0.0921 Uij ? ? H(10) 0.3738 -0.2496 0.1054 0.1112 Uij ? ? H(11) 0.4490 -0.2585 0.2238 0.0928 Uij ? ? H(12) 0.4794 -0.1743 0.2972 0.0799 Uij ? ? H(13) 0.5724 -0.1398 0.1289 0.0945 Uij ? ? H(14) 0.5484 -0.0758 0.1457 0.0945 Uij ? ? H(15) 0.6017 -0.0447 0.0218 0.1081 Uij ? ? H(16) 0.6293 -0.1076 0.0058 0.1081 Uij ? ? H(17) 0.4908 -0.0851 0.0071 0.1215 Uij ? ? H(18) 0.5317 -0.0836 -0.0786 0.1215 Uij ? ? H(19) 0.5169 -0.1823 0.0239 0.1864 Uij ? ? H(20) 0.4800 -0.1727 -0.0637 0.1864 Uij ? ? H(21) 0.5578 -0.1808 -0.0619 0.1864 Uij ? ? H(22) 0.7147 -0.1186 0.0968 0.0986 Uij ? ? H(23) 0.7400 -0.1210 0.1918 0.0986 Uij ? ? H(24) 0.6701 -0.2045 0.2121 0.1284 Uij ? ? H(25) 0.6572 -0.2042 0.1129 0.1284 Uij ? ? H(26) 0.7747 -0.2257 0.1969 0.2853 Uij ? ? H(27) 0.7344 -0.2694 0.1397 0.2853 Uij ? ? H(28) 0.8244 -0.2604 0.1089 0.2630 Uij ? ? H(29) 0.7749 -0.2372 0.0390 0.2630 Uij ? ? H(30) 0.8151 -0.1933 0.0960 0.2630 Uij ? ? H(31) 0.7095 -0.0226 0.2070 0.0915 Uij ? ? H(32) 0.6805 -0.0201 0.1137 0.0915 Uij ? ? H(33) 0.5821 0.0179 0.1660 0.1025 Uij ? ? H(34) 0.6107 0.0151 0.2595 0.1025 Uij ? ? H(35) 0.6963 0.0811 0.2185 0.1128 Uij ? ? H(36) 0.6637 0.0858 0.1273 0.1128 Uij ? ? H(37) 0.6350 0.1654 0.2084 0.1484 Uij ? ? H(38) 0.5709 0.1290 0.1870 0.1484 Uij ? ? H(39) 0.6036 0.1245 0.2781 0.1484 Uij ? ? H(40) 0.5855 -0.0766 0.2853 0.0833 Uij ? ? H(41) 0.6060 -0.1419 0.2731 0.0833 Uij ? ? H(42) 0.7123 -0.1205 0.3318 0.1130 Uij ? ? H(43) 0.6890 -0.0562 0.3475 0.1130 Uij ? ? H(44) 0.6362 -0.1947 0.4824 0.1433 Uij ? ? H(45) 0.6279 -0.1938 0.3824 0.1433 Uij ? ? H(46) 0.6991 -0.1887 0.4233 0.1433 Uij ? ? H(47) 0.6658 -0.1419 0.5463 0.1218 Uij ? ? H(48) 0.7289 -0.1355 0.4875 0.1218 Uij ? ? H(49) 0.6950 -0.0801 0.5268 0.1218 Uij ? ? 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 Os(1) 0.0447(2) 0.0490(2) 0.0582(2) -0.0009(2) 0.0004(1) 0.0030(2) O(1) 0.050(3) 0.055(3) 0.081(4) 0.000(3) -0.013(3) -0.004(3) O(2) 0.057(4) 0.045(3) 0.080(4) 0.006(3) -0.001(3) -0.005(3) O(3) 0.117(6) 0.050(4) 0.125(6) -0.004(4) -0.039(5) 0.017(4) O(4) 0.106(5) 0.099(5) 0.059(4) 0.002(4) -0.006(4) -0.007(4) N(1) 0.062(4) 0.070(5) 0.067(4) 0.004(4) -0.005(4) 0.011(4) N(2) 0.058(5) 0.042(4) 0.070(4) 0.008(3) -0.005(4) 0.002(3) N(3) 0.055(4) 0.057(4) 0.055(4) -0.003(4) -0.011(3) -0.004(3) N(4) 0.041(4) 0.085(5) 0.072(5) -0.010(4) 0.012(4) -0.004(4) C(1) 0.046(5) 0.055(5) 0.065(5) -0.016(4) -0.001(4) 0.005(4) C(2) 0.058(6) 0.058(5) 0.080(6) -0.004(4) 0.008(5) 0.005(5) C(3) 0.069(6) 0.077(6) 0.064(6) -0.011(5) -0.003(5) 0.003(5) C(4) 0.092(7) 0.072(7) 0.084(7) -0.030(6) 0.013(6) -0.004(5) C(5) 0.086(7) 0.049(5) 0.071(6) -0.005(5) -0.001(5) 0.001(4) C(6) 0.065(5) 0.047(5) 0.057(5) -0.019(4) 0.001(4) 0.007(4) C(7) 0.071(6) 0.053(5) 0.075(6) 0.007(4) 0.000(5) 0.006(5) C(8) 0.049(5) 0.072(6) 0.067(6) 0.003(5) 0.006(4) 0.003(5) C(9) 0.068(6) 0.071(6) 0.086(6) 0.012(5) -0.007(5) 0.022(5) C(10) 0.081(7) 0.084(7) 0.096(7) 0.022(7) 0.003(7) 0.030(6) C(11) 0.045(5) 0.126(10) 0.095(8) 0.011(7) -0.008(5) 0.032(7) C(12) 0.061(6) 0.085(7) 0.071(6) -0.005(5) -0.009(5) 0.020(5) C(13) 0.045(5) 0.075(6) 0.055(5) -0.003(5) 0.004(4) 0.014(4) C(14) 0.059(6) 0.065(6) 0.074(6) -0.024(5) 0.006(5) -0.004(5) C(15) 0.057(6) 0.055(5) 0.069(6) -0.005(4) 0.011(5) -0.010(4) C(16) 0.075(7) 0.076(7) 0.079(6) -0.020(6) 0.006(5) -0.019(5) C(17) 0.095(8) 0.054(6) 0.127(9) -0.019(6) 0.022(7) -0.028(6) C(18) 0.075(7) 0.052(5) 0.106(8) -0.009(5) 0.007(6) -0.014(6) C(19) 0.066(6) 0.043(5) 0.091(6) -0.004(5) 0.016(5) -0.002(5) C(20) 0.054(6) 0.054(5) 0.070(6) -0.010(4) 0.013(4) -0.010(4) C(21) 0.056(6) 0.097(7) 0.084(7) -0.020(5) 0.015(5) -0.002(6) C(22) 0.087(8) 0.113(8) 0.071(6) -0.016(7) -0.002(6) 0.021(6) C(23) 0.101(9) 0.124(10) 0.080(7) -0.035(8) 0.000(6) 0.014(7) C(24) 0.16(1) 0.17(1) 0.13(1) -0.06(1) -0.003(10) 0.02(1) C(25) 0.063(6) 0.088(7) 0.095(7) -0.002(6) 0.001(6) -0.004(6) C(26) 0.101(9) 0.092(8) 0.130(9) 0.018(7) 0.001(7) -0.015(7) C(27) 0.23(2) 0.14(1) 0.33(3) 0.06(2) 0.16(2) -0.01(2) C(28) 0.18(2) 0.28(2) 0.21(2) 0.11(2) 0.07(1) 0.08(2) C(29) 0.061(6) 0.076(6) 0.091(7) -0.027(5) 0.012(5) -0.003(5) C(30) 0.073(7) 0.081(6) 0.101(8) -0.006(6) 0.013(6) 0.004(6) C(31) 0.106(9) 0.083(7) 0.093(8) 0.006(7) -0.007(7) -0.004(6) C(32) 0.14(1) 0.084(8) 0.15(1) 0.023(8) -0.022(9) 0.005(7) C(33) 0.049(5) 0.079(6) 0.080(6) -0.011(5) 0.004(5) 0.008(5) C(34) 0.085(8) 0.101(8) 0.099(8) -0.018(7) -0.020(6) -0.003(6) C(35) 0.097(8) 0.15(1) 0.054(6) -0.007(8) -0.012(5) 0.022(6) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.38445 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3047 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0315 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0409 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.289 _refine_ls_shift/esd_max 1.6070 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.58 _refine_diff_density_max 1.15 #------------------------------------------------------------------------------ _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 Os(1) O(1) 1.969(5) ? ? yes Os(1) O(2) 1.977(5) ? ? yes Os(1) N(1) 1.618(7) ? ? yes Os(1) N(2) 2.011(6) ? ? yes Os(1) N(3) 2.010(6) ? ? yes O(1) C(1) 1.347(9) ? ? yes O(2) C(20) 1.355(9) ? ? yes O(3) C(7) 1.227(9) ? ? yes O(4) C(14) 1.226(9) ? ? yes N(2) C(7) 1.39(1) ? ? yes N(2) C(8) 1.428(10) ? ? yes N(3) C(13) 1.424(10) ? ? yes N(3) C(14) 1.373(10) ? ? yes N(4) C(21) 1.52(1) ? ? yes N(4) C(25) 1.51(1) ? ? yes N(4) C(29) 1.51(1) ? ? yes N(4) C(33) 1.502(10) ? ? yes C(1) C(2) 1.40(1) ? ? yes C(1) C(6) 1.38(1) ? ? yes C(2) C(3) 1.40(1) ? ? yes C(3) C(4) 1.36(1) ? ? yes C(4) C(5) 1.40(1) ? ? yes C(5) C(6) 1.41(1) ? ? yes C(6) C(7) 1.49(1) ? ? yes C(8) C(9) 1.38(1) ? ? yes C(8) C(13) 1.40(1) ? ? yes C(9) C(10) 1.36(1) ? ? yes C(10) C(11) 1.37(1) ? ? yes C(11) C(12) 1.41(1) ? ? yes C(12) C(13) 1.37(1) ? ? yes C(14) C(15) 1.50(1) ? ? yes C(15) C(16) 1.39(1) ? ? yes C(15) C(20) 1.38(1) ? ? yes C(16) C(17) 1.38(1) ? ? yes C(17) C(18) 1.40(1) ? ? yes C(18) C(19) 1.36(1) ? ? yes C(19) C(20) 1.38(1) ? ? yes C(21) C(22) 1.53(1) ? ? yes C(22) C(23) 1.53(1) ? ? yes C(23) C(24) 1.47(2) ? ? yes C(25) C(26) 1.53(1) ? ? yes C(26) C(27) 1.51(2) ? ? yes C(27) C(28) 1.11(2) ? ? yes C(29) C(30) 1.49(1) ? ? yes C(30) C(31) 1.53(1) ? ? yes C(31) C(32) 1.47(1) ? ? yes C(33) C(34) 1.54(1) ? ? yes C(34) C(35) 1.51(1) ? ? yes C(35) C(36) 1.49(3) ? ? yes C(35) C(36') 1.38(2) ? ? 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) Os(1) O(2) 77.6(2) ? ? ? yes O(1) Os(1) N(1) 109.0(3) ? ? ? yes O(1) Os(1) N(2) 91.1(2) ? ? ? yes O(1) Os(1) N(3) 144.9(2) ? ? ? yes O(2) Os(1) N(1) 107.4(3) ? ? ? yes O(2) Os(1) N(2) 145.5(2) ? ? ? yes O(2) Os(1) N(3) 90.8(2) ? ? ? yes N(1) Os(1) N(2) 107.0(3) ? ? ? yes N(1) Os(1) N(3) 106.1(3) ? ? ? yes N(2) Os(1) N(3) 79.9(3) ? ? ? yes Os(1) O(1) C(1) 121.5(5) ? ? ? yes Os(1) O(2) C(20) 122.9(5) ? ? ? yes Os(1) N(2) C(7) 125.5(5) ? ? ? yes Os(1) N(2) C(8) 113.0(5) ? ? ? yes C(7) N(2) C(8) 121.4(7) ? ? ? yes Os(1) N(3) C(13) 112.7(5) ? ? ? yes Os(1) N(3) C(14) 126.6(6) ? ? ? yes C(13) N(3) C(14) 120.5(7) ? ? ? yes C(21) N(4) C(25) 110.2(7) ? ? ? yes C(21) N(4) C(29) 110.4(7) ? ? ? yes C(21) N(4) C(33) 105.3(6) ? ? ? yes C(25) N(4) C(29) 107.0(7) ? ? ? yes C(25) N(4) C(33) 111.9(7) ? ? ? yes C(29) N(4) C(33) 112.2(7) ? ? ? yes O(1) C(1) C(2) 115.6(7) ? ? ? yes O(1) C(1) C(6) 124.4(7) ? ? ? yes C(2) C(1) C(6) 119.9(7) ? ? ? yes C(1) C(2) C(3) 120.2(8) ? ? ? yes C(2) C(3) C(4) 119.3(8) ? ? ? yes C(3) C(4) C(5) 121.6(9) ? ? ? yes C(4) C(5) C(6) 119.4(8) ? ? ? yes C(1) C(6) C(5) 119.6(8) ? ? ? yes C(1) C(6) C(7) 125.4(7) ? ? ? yes C(5) C(6) C(7) 114.9(7) ? ? ? yes O(3) C(7) N(2) 121.3(8) ? ? ? yes O(3) C(7) C(6) 119.6(8) ? ? ? yes N(2) C(7) C(6) 119.2(7) ? ? ? yes N(2) C(8) C(9) 125.4(8) ? ? ? yes N(2) C(8) C(13) 114.2(7) ? ? ? yes C(9) C(8) C(13) 120.4(8) ? ? ? yes C(8) C(9) C(10) 119.8(9) ? ? ? yes C(9) C(10) C(11) 120.8(9) ? ? ? yes C(10) C(11) C(12) 120.2(9) ? ? ? yes C(11) C(12) C(13) 119.2(9) ? ? ? yes N(3) C(13) C(8) 114.8(7) ? ? ? yes N(3) C(13) C(12) 125.5(8) ? ? ? yes C(8) C(13) C(12) 119.6(8) ? ? ? yes O(4) C(14) N(3) 121.8(9) ? ? ? yes O(4) C(14) C(15) 119.0(8) ? ? ? yes N(3) C(14) C(15) 119.2(8) ? ? ? yes C(14) C(15) C(16) 116.5(8) ? ? ? yes C(14) C(15) C(20) 125.0(8) ? ? ? yes C(16) C(15) C(20) 118.4(8) ? ? ? yes C(15) C(16) C(17) 121.3(9) ? ? ? yes C(16) C(17) C(18) 120.3(8) ? ? ? yes C(17) C(18) C(19) 117.3(8) ? ? ? yes C(18) C(19) C(20) 123.4(9) ? ? ? yes O(2) C(20) C(15) 123.9(8) ? ? ? yes O(2) C(20) C(19) 116.8(8) ? ? ? yes C(15) C(20) C(19) 119.2(8) ? ? ? yes N(4) C(21) C(22) 116.8(7) ? ? ? yes C(21) C(22) C(23) 111.3(8) ? ? ? yes C(22) C(23) C(24) 112(1) ? ? ? yes N(4) C(25) C(26) 115.9(8) ? ? ? yes C(25) C(26) C(27) 112(1) ? ? ? yes C(26) C(27) C(28) 134(2) ? ? ? yes N(4) C(29) C(30) 116.3(8) ? ? ? yes C(29) C(30) C(31) 109.2(8) ? ? ? yes C(30) C(31) C(32) 112.8(10) ? ? ? yes N(4) C(33) C(34) 116.2(7) ? ? ? yes C(33) C(34) C(35) 111.3(8) ? ? ? yes C(34) C(35) C(36) 102(1) ? ? ? yes C(34) C(35) C(36') 119(1) ? ? ? yes C(36) C(35) C(36') 83(1) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_4a #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:59:09 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.074(2) _cell_length_b 13.118(2) _cell_length_c 13.648(2) _cell_angle_alpha 75.65(2) _cell_angle_beta 84.14(2) _cell_angle_gamma 86.46(2) _cell_volume 2081.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 890.14 _chemical_formula_analytical ? _chemical_formula_sum 'C37 H47 Cl5 N4 O4 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 916.00 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 5737 _reflns_number_total 5737 _reflns_number_observed 3695 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.27 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 2 -1.259 0.836 'International Tables' Cl 0 10 0.148 0.159 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 74 0.003 0.002 'International Tables' H 0 94 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Ru(1) 0.09997(5) 0.09627(5) 0.17277(4) 0.0523 Uij ? ? Cl(1) 0.3164(2) 0.3797(2) -0.2915(2) 0.1097 Uij ? ? Cl(2) 0.2665(2) 0.1599(2) -0.3324(2) 0.0984 Uij ? ? Cl(3) 0.3409(3) -0.0009(3) 0.4838(3) 0.1457 Uij ? ? Cl(4) 0.1294(4) -0.0662(4) 0.5800(3) 0.1757 Uij ? ? Cl(5) 0.2559(4) -0.1924(3) 0.4616(4) 0.1989 Uij ? ? O(1) 0.1470(4) 0.1239(4) 0.2967(3) 0.0619 Uij ? ? O(2) 0.1036(4) -0.0444(4) 0.2641(3) 0.0655 Uij ? ? O(3) 0.2830(5) 0.3684(4) 0.0658(4) 0.0785 Uij ? ? O(4) 0.1969(5) -0.0984(4) -0.0210(4) 0.0827 Uij ? ? N(1) -0.0288(4) 0.1339(5) 0.1645(5) 0.0670 Uij ? ? N(2) 0.1874(4) 0.2159(4) 0.0884(4) 0.0520 Uij ? ? N(3) 0.1478(4) 0.0378(4) 0.0530(4) 0.0512 Uij ? ? N(4) 0.5977(5) 0.2730(5) 0.1510(5) 0.0666 Uij ? ? C(1) 0.1565(6) 0.2226(6) 0.3070(5) 0.0580 Uij ? ? C(2) 0.1356(7) 0.2378(7) 0.4063(6) 0.0723 Uij ? ? C(3) 0.1440(8) 0.3344(7) 0.4234(6) 0.0818 Uij ? ? C(4) 0.1716(8) 0.4217(7) 0.3427(7) 0.0832 Uij ? ? C(5) 0.1931(6) 0.4055(6) 0.2478(6) 0.0672 Uij ? ? C(6) 0.1880(6) 0.3075(6) 0.2259(5) 0.0559 Uij ? ? C(7) 0.2227(6) 0.3013(6) 0.1199(6) 0.0570 Uij ? ? C(8) 0.2131(5) 0.2111(6) -0.0154(5) 0.0540 Uij ? ? C(9) 0.2522(6) 0.2917(6) -0.0967(6) 0.0662 Uij ? ? C(10) 0.2679(7) 0.2753(7) -0.1937(6) 0.0740 Uij ? ? C(11) 0.2442(7) 0.1813(7) -0.2123(5) 0.0689 Uij ? ? C(12) 0.2061(6) 0.1009(6) -0.1331(6) 0.0666 Uij ? ? C(13) 0.1894(5) 0.1145(6) -0.0336(5) 0.0567 Uij ? ? C(14) 0.1505(6) -0.0673(6) 0.0514(5) 0.0572 Uij ? ? C(15) 0.0962(6) -0.1439(6) 0.1377(6) 0.0588 Uij ? ? C(16) 0.0684(6) -0.2397(7) 0.1196(6) 0.0681 Uij ? ? C(17) 0.0244(7) -0.3197(7) 0.1967(8) 0.0856 Uij ? ? C(18) 0.0064(7) -0.3053(7) 0.2936(7) 0.0826 Uij ? ? C(19) 0.0312(7) -0.2147(7) 0.3146(6) 0.0749 Uij ? ? C(20) 0.0767(6) -0.1319(6) 0.2370(6) 0.0635 Uij ? ? C(21) 0.5616(6) 0.3342(6) 0.0482(7) 0.0770 Uij ? ? C(22) 0.6206(8) 0.3043(7) -0.0440(7) 0.0893 Uij ? ? C(23) 0.5792(8) 0.3687(8) -0.1408(8) 0.1010 Uij ? ? C(24) 0.634(1) 0.3408(10) -0.2346(9) 0.1288 Uij ? ? C(25) 0.5845(6) 0.1561(6) 0.1656(6) 0.0683 Uij ? ? C(26) 0.4659(8) 0.1234(8) 0.1651(8) 0.1042 Uij ? ? C(27) 0.469(1) -0.001(1) 0.193(1) 0.1636 Uij ? ? C(28) 0.383(3) -0.043(2) 0.185(2) 0.18(1) Uij ? ? C(28') 0.485(3) -0.030(3) 0.105(3) 0.16(1) Uij ? ? C(29) 0.5239(7) 0.3140(8) 0.2312(8) 0.0907 Uij ? ? C(30) 0.5438(9) 0.261(1) 0.3399(9) 0.1276 Uij ? ? C(31) 0.463(1) 0.297(1) 0.422(1) 0.1668 Uij ? ? C(32) 0.492(2) 0.389(1) 0.436(2) 0.2286 Uij ? ? C(33) 0.7209(6) 0.2868(6) 0.1565(6) 0.0720 Uij ? ? C(34) 0.7521(8) 0.3991(8) 0.1414(10) 0.1229 Uij ? ? C(35) 0.8769(9) 0.4042(9) 0.162(1) 0.1239 Uij ? ? C(36) 0.889(2) 0.376(2) 0.266(2) 0.120(7) Uij ? ? C(36') 0.937(2) 0.430(2) 0.076(2) 0.131(9) Uij ? ? C(37) 0.221(1) -0.0652(9) 0.4752(9) 0.1166 Uij ? ? H(1) 0.1152 0.1801 0.4614 0.0865 Uij ? ? H(2) 0.1309 0.3430 0.4907 0.0980 Uij ? ? H(3) 0.1753 0.4896 0.3545 0.0994 Uij ? ? H(4) 0.2126 0.4642 0.1936 0.0803 Uij ? ? H(5) 0.2676 0.3578 -0.0857 0.0788 Uij ? ? H(6) 0.1914 0.0353 -0.1457 0.0802 Uij ? ? H(7) 0.0804 -0.2500 0.0527 0.0813 Uij ? ? H(8) 0.0060 -0.3842 0.1836 0.1029 Uij ? ? H(9) -0.0241 -0.3603 0.3470 0.0988 Uij ? ? H(10) 0.0180 -0.2068 0.3823 0.0896 Uij ? ? H(11) 0.4844 0.3246 0.0480 0.0918 Uij ? ? H(12) 0.5736 0.4067 0.0417 0.0918 Uij ? ? H(13) 0.6979 0.3145 -0.0453 0.1073 Uij ? ? H(14) 0.6087 0.2323 -0.0390 0.1073 Uij ? ? H(15) 0.5015 0.3594 -0.1383 0.1201 Uij ? ? H(16) 0.5919 0.4407 -0.1455 0.1201 Uij ? ? H(17) 0.6219 0.2693 -0.2315 0.1537 Uij ? ? H(18) 0.6035 0.3847 -0.2926 0.1537 Uij ? ? H(19) 0.7119 0.3509 -0.2390 0.1537 Uij ? ? H(20) 0.6291 0.1343 0.1126 0.0815 Uij ? ? H(21) 0.6105 0.1209 0.2292 0.0815 Uij ? ? H(22) 0.4177 0.1492 0.2135 0.1238 Uij ? ? H(23) 0.4406 0.1504 0.0993 0.1238 Uij ? ? H(24) 0.5360 0.3869 0.2206 0.1082 Uij ? ? H(25) 0.4486 0.3045 0.2224 0.1082 Uij ? ? H(26) 0.5373 0.1874 0.3488 0.1540 Uij ? ? H(27) 0.6181 0.2746 0.3496 0.1540 Uij ? ? H(28) 0.3899 0.3011 0.4040 0.1956 Uij ? ? H(29) 0.4689 0.2462 0.4856 0.1956 Uij ? ? H(30) 0.5639 0.3893 0.4538 0.2515 Uij ? ? H(31) 0.4853 0.4442 0.3717 0.2515 Uij ? ? H(32) 0.4395 0.4125 0.4851 0.2515 Uij ? ? H(33) 0.7407 0.2482 0.2213 0.0867 Uij ? ? H(34) 0.7620 0.2589 0.1052 0.0867 Uij ? ? H(35) 0.7411 0.4369 0.0740 0.1475 Uij ? ? H(36) 0.7058 0.4304 0.1878 0.1475 Uij ? ? H(37) 0.8441 0.4238 0.2966 0.1418 Uij ? ? H(38) 0.8630 0.3067 0.2928 0.1418 Uij ? ? H(39) 0.9638 0.3788 0.2765 0.1418 Uij ? ? H(40) 1.0131 0.4332 0.0877 0.1520 Uij ? ? H(41) 0.9309 0.3803 0.0370 0.1520 Uij ? ? H(42) 0.9126 0.4981 0.0385 0.1520 Uij ? ? H(43) 0.1838 -0.0288 0.4170 0.1462 Uij ? ? 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 Ru(1) 0.0537(4) 0.0514(4) 0.0520(4) 0.0025(3) -0.0028(3) -0.0148(3) Cl(1) 0.153(2) 0.109(2) 0.058(1) -0.030(2) 0.012(1) -0.005(1) Cl(2) 0.121(2) 0.124(2) 0.052(1) 0.009(2) -0.002(1) -0.030(1) Cl(3) 0.134(3) 0.140(3) 0.164(3) -0.010(2) -0.028(2) -0.031(2) Cl(4) 0.199(4) 0.200(4) 0.113(3) -0.069(3) 0.018(2) -0.007(2) Cl(5) 0.280(5) 0.113(3) 0.235(5) 0.050(3) -0.156(4) -0.062(3) O(1) 0.086(4) 0.050(3) 0.052(3) 0.001(3) -0.014(2) -0.014(2) O(2) 0.090(4) 0.049(3) 0.056(3) -0.007(3) -0.003(3) -0.009(2) O(3) 0.086(4) 0.080(4) 0.070(3) -0.033(3) 0.003(3) -0.015(3) O(4) 0.107(4) 0.069(4) 0.074(4) 0.014(3) 0.009(3) -0.031(3) N(1) 0.046(3) 0.077(4) 0.079(4) 0.008(3) 0.001(3) -0.028(4) N(2) 0.051(3) 0.059(4) 0.047(3) 0.000(3) -0.003(3) -0.015(3) N(3) 0.049(3) 0.045(4) 0.057(4) 0.001(3) 0.002(3) -0.010(3) N(4) 0.060(4) 0.061(4) 0.081(4) 0.015(3) -0.008(3) -0.023(4) C(1) 0.065(5) 0.059(5) 0.053(5) 0.007(4) -0.013(4) -0.018(4) C(2) 0.091(6) 0.071(6) 0.058(5) -0.014(5) 0.001(4) -0.021(4) C(3) 0.112(7) 0.076(6) 0.064(5) -0.010(5) -0.001(5) -0.031(5) C(4) 0.112(7) 0.067(6) 0.076(6) -0.005(5) 0.002(5) -0.033(5) C(5) 0.076(5) 0.055(5) 0.072(6) -0.001(4) -0.004(4) -0.020(4) C(6) 0.057(4) 0.059(5) 0.054(5) 0.002(4) -0.003(4) -0.020(4) C(7) 0.055(5) 0.058(5) 0.057(5) 0.003(4) -0.008(4) -0.013(4) C(8) 0.046(4) 0.060(5) 0.054(5) 0.002(4) -0.006(3) -0.013(4) C(9) 0.070(5) 0.072(5) 0.055(5) 0.000(4) -0.004(4) -0.013(4) C(10) 0.073(5) 0.090(7) 0.051(5) -0.005(5) 0.006(4) -0.007(5) C(11) 0.084(6) 0.076(6) 0.047(5) 0.015(5) -0.008(4) -0.019(4) C(12) 0.069(5) 0.070(6) 0.065(5) 0.012(4) -0.012(4) -0.025(5) C(13) 0.048(4) 0.071(5) 0.051(4) 0.012(4) -0.003(3) -0.020(4) C(14) 0.055(4) 0.066(5) 0.053(5) 0.009(4) -0.014(4) -0.019(4) C(15) 0.052(4) 0.061(5) 0.068(5) 0.006(4) -0.007(4) -0.025(4) C(16) 0.064(5) 0.064(5) 0.083(6) -0.002(4) -0.004(4) -0.034(5) C(17) 0.076(6) 0.065(6) 0.125(8) -0.009(5) -0.009(6) -0.038(6) C(18) 0.088(6) 0.064(6) 0.091(7) -0.014(5) 0.010(5) -0.014(5) C(19) 0.084(6) 0.063(6) 0.074(5) -0.016(5) 0.013(4) -0.015(4) C(20) 0.061(5) 0.051(5) 0.079(6) 0.005(4) -0.006(4) -0.019(4) C(21) 0.062(5) 0.059(5) 0.107(7) 0.005(4) -0.015(5) -0.013(5) C(22) 0.103(7) 0.075(6) 0.085(7) 0.011(5) -0.008(5) -0.015(5) C(23) 0.094(7) 0.107(8) 0.089(7) -0.003(6) -0.019(5) 0.006(6) C(24) 0.15(1) 0.127(10) 0.094(8) -0.019(8) -0.029(7) 0.010(7) C(25) 0.071(5) 0.053(5) 0.077(5) -0.003(4) -0.003(4) -0.011(4) C(26) 0.105(7) 0.072(6) 0.136(9) -0.010(6) -0.023(6) -0.020(6) C(27) 0.16(1) 0.10(1) 0.25(2) -0.046(9) -0.01(1) -0.06(1) C(29) 0.069(6) 0.101(7) 0.107(7) 0.021(5) -0.008(5) -0.041(6) C(30) 0.103(8) 0.18(1) 0.110(9) 0.053(8) -0.026(7) -0.069(8) C(31) 0.094(9) 0.25(2) 0.17(1) 0.03(1) 0.024(8) -0.08(1) C(32) 0.19(2) 0.20(2) 0.33(2) 0.01(1) 0.01(1) -0.17(2) C(33) 0.053(5) 0.069(6) 0.097(6) 0.011(4) -0.012(4) -0.026(5) C(34) 0.091(7) 0.078(7) 0.20(1) -0.012(6) -0.043(8) -0.021(8) C(35) 0.094(8) 0.091(8) 0.17(1) -0.027(6) -0.016(8) -0.003(8) C(37) 0.141(10) 0.090(8) 0.119(10) 0.002(7) -0.052(8) -0.011(7) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3695 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0557 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0760 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.520 _refine_ls_shift/esd_max 2.7230 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.51 _refine_diff_density_max 0.42 #------------------------------------------------------------------------------ _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 Ru(1) O(1) 1.960(4) ? ? yes Ru(1) O(2) 1.955(5) ? ? yes Ru(1) N(1) 1.609(6) ? ? yes Ru(1) N(2) 1.991(5) ? ? yes Ru(1) N(3) 1.992(6) ? ? yes Cl(1) C(10) 1.742(8) ? ? yes Cl(2) C(11) 1.722(8) ? ? yes Cl(3) C(37) 1.75(1) ? ? yes Cl(4) C(37) 1.71(1) ? ? yes Cl(5) C(37) 1.75(1) ? ? yes O(1) C(1) 1.348(8) ? ? yes O(2) C(20) 1.357(9) ? ? yes O(3) C(7) 1.224(8) ? ? yes O(4) C(14) 1.231(8) ? ? yes N(2) C(7) 1.399(9) ? ? yes N(2) C(8) 1.434(8) ? ? yes N(3) C(13) 1.419(8) ? ? yes N(3) C(14) 1.382(9) ? ? yes N(4) C(21) 1.53(1) ? ? yes N(4) C(25) 1.513(10) ? ? yes N(4) C(29) 1.52(1) ? ? yes N(4) C(33) 1.521(9) ? ? yes C(1) C(2) 1.413(10) ? ? yes C(1) C(6) 1.402(9) ? ? yes C(2) C(3) 1.36(1) ? ? yes C(3) C(4) 1.41(1) ? ? yes C(4) C(5) 1.36(1) ? ? yes C(5) C(6) 1.40(1) ? ? yes C(6) C(7) 1.486(10) ? ? yes C(8) C(9) 1.395(9) ? ? yes C(8) C(13) 1.402(10) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(10) C(11) 1.37(1) ? ? yes C(11) C(12) 1.37(1) ? ? yes C(12) C(13) 1.41(1) ? ? yes C(14) C(15) 1.471(10) ? ? yes C(15) C(16) 1.41(1) ? ? yes C(15) C(20) 1.40(1) ? ? yes C(16) C(17) 1.38(1) ? ? yes C(17) C(18) 1.38(1) ? ? yes C(18) C(19) 1.35(1) ? ? yes C(19) C(20) 1.41(1) ? ? yes C(21) C(22) 1.51(1) ? ? yes C(22) C(23) 1.50(1) ? ? yes C(23) C(24) 1.50(2) ? ? yes C(25) C(26) 1.52(1) ? ? yes C(26) C(27) 1.58(1) ? ? yes C(27) C(28) 1.22(3) ? ? yes C(27) C(28') 1.34(4) ? ? yes C(28) C(28') 1.54(4) ? ? yes C(29) C(30) 1.51(1) ? ? yes C(30) C(31) 1.55(2) ? ? yes C(31) C(32) 1.34(2) ? ? yes C(33) C(34) 1.50(1) ? ? yes C(34) C(35) 1.57(1) ? ? yes C(35) C(36) 1.39(2) ? ? yes C(35) C(36') 1.30(3) ? ? 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) Ru(1) O(2) 77.7(2) ? ? ? yes O(1) Ru(1) N(1) 108.3(3) ? ? ? yes O(1) Ru(1) N(2) 90.5(2) ? ? ? yes O(1) Ru(1) N(3) 144.9(2) ? ? ? yes O(2) Ru(1) N(1) 107.3(3) ? ? ? yes O(2) Ru(1) N(2) 146.9(2) ? ? ? yes O(2) Ru(1) N(3) 91.3(2) ? ? ? yes N(1) Ru(1) N(2) 105.8(3) ? ? ? yes N(1) Ru(1) N(3) 106.8(3) ? ? ? yes N(2) Ru(1) N(3) 80.8(2) ? ? ? yes Ru(1) O(1) C(1) 122.1(4) ? ? ? yes Ru(1) O(2) C(20) 123.1(5) ? ? ? yes Ru(1) N(2) C(7) 126.8(5) ? ? ? yes Ru(1) N(2) C(8) 114.0(4) ? ? ? yes C(7) N(2) C(8) 119.1(6) ? ? ? yes Ru(1) N(3) C(13) 113.5(4) ? ? ? yes Ru(1) N(3) C(14) 126.0(5) ? ? ? yes C(13) N(3) C(14) 120.4(6) ? ? ? yes C(21) N(4) C(25) 110.8(6) ? ? ? yes C(21) N(4) C(29) 106.6(6) ? ? ? yes C(21) N(4) C(33) 110.3(6) ? ? ? yes C(25) N(4) C(29) 110.6(6) ? ? ? yes C(25) N(4) C(33) 106.0(6) ? ? ? yes C(29) N(4) C(33) 112.6(6) ? ? ? yes O(1) C(1) C(2) 116.6(6) ? ? ? yes O(1) C(1) C(6) 123.5(6) ? ? ? yes C(2) C(1) C(6) 119.8(7) ? ? ? yes C(1) C(2) C(3) 120.4(7) ? ? ? yes C(2) C(3) C(4) 120.8(7) ? ? ? yes C(3) C(4) C(5) 118.1(7) ? ? ? yes C(4) C(5) C(6) 123.6(7) ? ? ? yes C(1) C(6) C(5) 117.2(7) ? ? ? yes C(1) C(6) C(7) 125.8(7) ? ? ? yes C(5) C(6) C(7) 117.0(7) ? ? ? yes O(3) C(7) N(2) 123.4(7) ? ? ? yes O(3) C(7) C(6) 119.0(7) ? ? ? yes N(2) C(7) C(6) 117.6(7) ? ? ? yes N(2) C(8) C(9) 127.3(7) ? ? ? yes N(2) C(8) C(13) 113.5(6) ? ? ? yes C(9) C(8) C(13) 119.1(7) ? ? ? yes C(8) C(9) C(10) 119.9(8) ? ? ? yes Cl(1) C(10) C(9) 117.4(7) ? ? ? yes Cl(1) C(10) C(11) 121.3(6) ? ? ? yes C(9) C(10) C(11) 121.4(7) ? ? ? yes Cl(2) C(11) C(10) 121.4(6) ? ? ? yes Cl(2) C(11) C(12) 119.1(7) ? ? ? yes C(10) C(11) C(12) 119.5(7) ? ? ? yes C(11) C(12) C(13) 120.7(7) ? ? ? yes N(3) C(13) C(8) 115.3(6) ? ? ? yes N(3) C(13) C(12) 125.3(7) ? ? ? yes C(8) C(13) C(12) 119.3(7) ? ? ? yes O(4) C(14) N(3) 121.5(7) ? ? ? yes O(4) C(14) C(15) 119.0(7) ? ? ? yes N(3) C(14) C(15) 119.5(7) ? ? ? yes C(14) C(15) C(16) 116.9(7) ? ? ? yes C(14) C(15) C(20) 125.4(7) ? ? ? yes C(16) C(15) C(20) 117.6(7) ? ? ? yes C(15) C(16) C(17) 121.6(8) ? ? ? yes C(16) C(17) C(18) 119.3(8) ? ? ? yes C(17) C(18) C(19) 121.3(8) ? ? ? yes C(18) C(19) C(20) 120.4(8) ? ? ? yes O(2) C(20) C(15) 122.8(7) ? ? ? yes O(2) C(20) C(19) 117.4(7) ? ? ? yes C(15) C(20) C(19) 119.8(7) ? ? ? yes N(4) C(21) C(22) 116.5(7) ? ? ? yes C(21) C(22) C(23) 112.3(8) ? ? ? yes C(22) C(23) C(24) 114.3(9) ? ? ? yes N(4) C(25) C(26) 115.2(7) ? ? ? yes C(25) C(26) C(27) 106.9(9) ? ? ? yes C(26) C(27) C(28) 116(2) ? ? ? yes C(26) C(27) C(28') 106(2) ? ? ? yes C(28) C(27) C(28') 74(2) ? ? ? yes C(27) C(28) C(28') 56(1) ? ? ? yes C(27) C(28') C(28) 49(1) ? ? ? yes N(4) C(29) C(30) 115.2(8) ? ? ? yes C(29) C(30) C(31) 115.2(10) ? ? ? yes C(30) C(31) C(32) 111(1) ? ? ? yes N(4) C(33) C(34) 114.3(7) ? ? ? yes C(33) C(34) C(35) 110.5(8) ? ? ? yes C(34) C(35) C(36) 110(1) ? ? ? yes C(34) C(35) C(36') 109(1) ? ? ? yes C(36) C(35) C(36') 139(1) ? ? ? yes Cl(3) C(37) Cl(4) 109.5(7) ? ? ? yes Cl(3) C(37) Cl(5) 110.0(7) ? ? ? yes Cl(4) C(37) Cl(5) 111.8(7) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_5a #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 18:01:13 1998' _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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.817(2) _cell_length_b 10.165(2) _cell_length_c 19.091(3) _cell_angle_alpha 90 _cell_angle_beta 100.57(2) _cell_angle_gamma 90 _cell_volume 2254.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 546.83 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H21 Cl3 N5 O2 Ru ' _chemical_formula_moiety 'C18 H21 Cl3 N5 O2 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1100.00 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4128 _reflns_number_total 4128 _reflns_number_observed 2986 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.61 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 4 -1.259 0.836 'International Tables' Cl 0 12 0.148 0.159 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 20 0.006 0.003 'International Tables' C 0 72 0.003 0.002 'International Tables' H 0 84 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ 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 Ru(1) 0.23683(2) 0.06753(4) 0.64635(1) 0.0526 Uij ? ? Cl(1) 0.35464(10) 0.2475(1) 0.64086(5) 0.0707 Uij ? ? Cl(2) 0.08904(9) 0.1768(1) 0.56966(6) 0.0842 Uij ? ? Cl(3) 0.39861(9) -0.0584(1) 0.69395(6) 0.0673 Uij ? ? O(1) 0.2682(2) -0.0036(3) 0.5412(1) 0.0536 Uij ? ? O(2) 0.1747(3) -0.4083(3) 0.4062(2) 0.0641 Uij ? ? N(1) 0.1891(3) 0.0925(4) 0.7183(2) 0.0725 Uij ? ? N(2) 0.1511(2) -0.1167(3) 0.6269(2) 0.0534 Uij ? ? N(3) 0.2100(2) -0.1481(3) 0.4509(1) 0.0424 Uij ? ? N(4) 0.3018(3) -0.2995(3) 0.3503(2) 0.0503 Uij ? ? N(5) 0.4462(3) -0.5007(3) 0.3709(2) 0.0616 Uij ? ? C(1) 0.1034(3) -0.1782(5) 0.6768(2) 0.0677 Uij ? ? C(2) 0.0599(4) -0.3028(6) 0.6667(2) 0.0783 Uij ? ? C(3) 0.0648(4) -0.3688(5) 0.6058(3) 0.0823 Uij ? ? C(4) 0.1147(3) -0.3072(5) 0.5541(2) 0.0672 Uij ? ? C(5) 0.1561(3) -0.1820(4) 0.5662(2) 0.0508 Uij ? ? C(6) 0.2170(3) -0.1043(4) 0.5167(2) 0.0444 Uij ? ? C(7) 0.3863(3) -0.0511(4) 0.4194(2) 0.0498 Uij ? ? C(8) 0.1904(3) 0.0490(4) 0.3764(2) 0.0576 Uij ? ? C(9) 0.2587(3) -0.0785(3) 0.3939(2) 0.0409 Uij ? ? C(10) 0.2408(3) -0.1752(4) 0.3283(2) 0.0451 Uij ? ? C(11) 0.1142(3) -0.2015(4) 0.2965(2) 0.0610 Uij ? ? C(12) 0.2995(3) -0.1184(4) 0.2691(2) 0.0565 Uij ? ? C(13) 0.2671(3) -0.4019(4) 0.3856(2) 0.0508 Uij ? ? C(14) 0.3539(3) -0.5091(4) 0.4016(2) 0.0527 Uij ? ? C(15) 0.3365(4) -0.6073(4) 0.4488(2) 0.0658 Uij ? ? C(16) 0.4198(5) -0.7030(4) 0.4637(2) 0.0756 Uij ? ? C(17) 0.5144(4) -0.6977(5) 0.4317(3) 0.0794 Uij ? ? C(18) 0.5251(4) -0.5969(5) 0.3862(3) 0.0764 Uij ? ? H(1) 0.359(4) -0.299(5) 0.343(3) 0.0876 Uij ? ? H(2) 0.0997 -0.1345 0.7202 0.0818 Uij ? ? H(3) 0.0266 -0.3441 0.7024 0.0937 Uij ? ? H(4) 0.0341 -0.4546 0.5983 0.0982 Uij ? ? H(5) 0.1198 -0.3514 0.5110 0.0799 Uij ? ? H(6) 0.4260 -0.1321 0.4302 0.0596 Uij ? ? H(7) 0.4164 -0.0070 0.3829 0.0596 Uij ? ? H(8) 0.3963 0.0023 0.4608 0.0596 Uij ? ? H(9) 0.1975 0.1016 0.4182 0.0691 Uij ? ? H(10) 0.2197 0.0959 0.3407 0.0691 Uij ? ? H(11) 0.1117 0.0284 0.3599 0.0691 Uij ? ? H(12) 0.0781 -0.1214 0.2789 0.0737 Uij ? ? H(13) 0.1098 -0.2624 0.2581 0.0737 Uij ? ? H(14) 0.0765 -0.2370 0.3318 0.0737 Uij ? ? H(15) 0.3785 -0.1024 0.2876 0.0678 Uij ? ? H(16) 0.2927 -0.1790 0.2308 0.0678 Uij ? ? H(17) 0.2631 -0.0378 0.2524 0.0678 Uij ? ? H(18) 0.2691 -0.6086 0.4697 0.0790 Uij ? ? H(19) 0.4118 -0.7720 0.4961 0.0902 Uij ? ? H(20) 0.5721 -0.7636 0.4412 0.0952 Uij ? ? H(21) 0.5908 -0.5940 0.3639 0.0915 Uij ? ? 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 Ru(1) 0.0465(2) 0.0788(3) 0.0341(2) 0.0047(1) 0.0113(1) -0.0016(1) Cl(1) 0.0815(7) 0.0801(8) 0.0530(6) -0.0106(5) 0.0192(5) -0.0108(5) Cl(2) 0.0619(7) 0.119(1) 0.0697(7) 0.0215(6) 0.0058(5) 0.0213(7) Cl(3) 0.0509(6) 0.0887(8) 0.0595(6) 0.0108(5) 0.0027(4) -0.0037(5) O(1) 0.060(2) 0.067(2) 0.037(1) -0.017(1) 0.017(1) -0.007(1) O(2) 0.067(2) 0.053(2) 0.076(2) -0.005(1) 0.020(1) 0.005(1) N(1) 0.071(2) 0.104(3) 0.048(2) 0.013(2) 0.025(2) 0.001(2) N(2) 0.041(2) 0.082(2) 0.038(2) 0.001(1) 0.011(1) 0.012(2) N(3) 0.045(2) 0.052(2) 0.031(1) 0.000(1) 0.010(1) 0.004(1) N(4) 0.060(2) 0.044(2) 0.047(2) 0.006(2) 0.012(2) 0.000(1) N(5) 0.069(2) 0.056(2) 0.056(2) 0.011(2) 0.001(2) -0.002(2) C(1) 0.053(2) 0.109(4) 0.044(2) 0.003(2) 0.018(2) 0.022(2) C(2) 0.067(3) 0.112(4) 0.058(3) -0.011(3) 0.018(2) 0.034(3) C(3) 0.083(3) 0.094(4) 0.067(3) -0.030(3) 0.007(2) 0.023(3) C(4) 0.072(3) 0.080(3) 0.049(2) -0.022(2) 0.007(2) 0.013(2) C(5) 0.040(2) 0.075(3) 0.037(2) -0.003(2) 0.006(1) 0.016(2) C(6) 0.037(2) 0.060(3) 0.037(2) 0.000(2) 0.007(1) 0.006(2) C(7) 0.051(2) 0.057(3) 0.043(2) -0.005(2) 0.012(2) -0.001(2) C(8) 0.068(3) 0.056(3) 0.050(2) 0.014(2) 0.014(2) 0.007(2) C(9) 0.047(2) 0.044(2) 0.033(2) 0.002(1) 0.010(1) 0.005(1) C(10) 0.051(2) 0.049(2) 0.035(2) 0.004(2) 0.007(1) 0.004(2) C(11) 0.063(2) 0.070(3) 0.046(2) -0.002(2) -0.001(2) -0.003(2) C(12) 0.074(3) 0.060(3) 0.038(2) 0.005(2) 0.017(2) 0.005(2) C(13) 0.062(3) 0.044(3) 0.044(2) -0.003(2) 0.004(2) -0.005(2) C(14) 0.072(3) 0.044(2) 0.039(2) -0.001(2) 0.001(2) -0.009(2) C(15) 0.091(3) 0.049(3) 0.057(3) 0.001(2) 0.012(2) -0.001(2) C(16) 0.113(4) 0.052(3) 0.058(3) 0.013(3) 0.008(3) 0.010(2) C(17) 0.101(4) 0.065(3) 0.064(3) 0.026(3) -0.006(3) 0.003(2) C(18) 0.075(3) 0.082(4) 0.071(3) 0.012(2) 0.010(2) -0.004(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2986 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0322 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0458 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.242 _refine_ls_shift/esd_max 0.0420 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.54 _refine_diff_density_max 0.58 #------------------------------------------------------------------------------ _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 Ru(1) Cl(1) 2.312(1) ? ? yes Ru(1) Cl(2) 2.343(1) ? ? yes Ru(1) Cl(3) 2.341(1) ? ? yes Ru(1) O(1) 2.227(3) ? ? yes Ru(1) N(1) 1.598(4) ? ? yes Ru(1) N(2) 2.129(3) ? ? yes O(1) C(6) 1.237(4) ? ? yes O(2) C(13) 1.229(5) ? ? yes N(2) C(1) 1.346(6) ? ? yes N(2) C(5) 1.347(5) ? ? yes N(3) C(6) 1.322(4) ? ? yes N(3) C(9) 1.499(4) ? ? yes N(4) C(10) 1.477(5) ? ? yes N(4) C(13) 1.344(5) ? ? yes N(5) C(14) 1.331(6) ? ? yes N(5) C(18) 1.346(6) ? ? yes C(1) C(2) 1.367(8) ? ? yes C(2) C(3) 1.352(7) ? ? yes C(3) C(4) 1.388(7) ? ? yes C(4) C(5) 1.369(6) ? ? yes C(5) C(6) 1.510(5) ? ? yes C(7) C(9) 1.523(5) ? ? yes C(8) C(9) 1.531(5) ? ? yes C(9) C(10) 1.576(5) ? ? yes C(10) C(11) 1.531(5) ? ? yes C(10) C(12) 1.542(6) ? ? yes C(13) C(14) 1.490(6) ? ? yes C(14) C(15) 1.385(6) ? ? yes C(15) C(16) 1.377(7) ? ? yes C(16) C(17) 1.369(8) ? ? yes C(17) C(18) 1.365(7) ? ? 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 Cl(1) Ru(1) Cl(2) 89.01(4) ? ? ? yes Cl(1) Ru(1) Cl(3) 89.68(4) ? ? ? yes Cl(1) Ru(1) O(1) 90.84(8) ? ? ? yes Cl(1) Ru(1) N(1) 102.9(1) ? ? ? yes Cl(1) Ru(1) N(2) 163.52(9) ? ? ? yes Cl(2) Ru(1) Cl(3) 164.52(4) ? ? ? yes Cl(2) Ru(1) O(1) 79.58(7) ? ? ? yes Cl(2) Ru(1) N(1) 97.0(1) ? ? ? yes Cl(2) Ru(1) N(2) 91.83(8) ? ? ? yes Cl(3) Ru(1) O(1) 85.02(7) ? ? ? yes Cl(3) Ru(1) N(1) 98.3(1) ? ? ? yes Cl(3) Ru(1) N(2) 85.13(8) ? ? ? yes O(1) Ru(1) N(1) 165.8(1) ? ? ? yes O(1) Ru(1) N(2) 73.2(1) ? ? ? yes N(1) Ru(1) N(2) 93.3(2) ? ? ? yes Ru(1) O(1) C(6) 117.3(2) ? ? ? yes Ru(1) N(2) C(1) 122.2(3) ? ? ? yes Ru(1) N(2) C(5) 119.2(3) ? ? ? yes C(1) N(2) C(5) 118.1(4) ? ? ? yes C(6) N(3) C(9) 124.5(3) ? ? ? yes C(10) N(4) C(13) 128.8(3) ? ? ? yes C(14) N(5) C(18) 116.7(4) ? ? ? yes N(2) C(1) C(2) 121.7(4) ? ? ? yes C(1) C(2) C(3) 120.5(5) ? ? ? yes C(2) C(3) C(4) 118.5(5) ? ? ? yes C(3) C(4) C(5) 119.1(4) ? ? ? yes N(2) C(5) C(4) 122.1(4) ? ? ? yes N(2) C(5) C(6) 112.5(3) ? ? ? yes C(4) C(5) C(6) 125.3(3) ? ? ? yes O(1) C(6) N(3) 125.4(3) ? ? ? yes O(1) C(6) C(5) 116.9(3) ? ? ? yes N(3) C(6) C(5) 117.7(3) ? ? ? yes N(3) C(9) C(7) 110.0(2) ? ? ? yes N(3) C(9) C(8) 107.5(3) ? ? ? yes N(3) C(9) C(10) 105.6(3) ? ? ? yes C(7) C(9) C(8) 111.5(3) ? ? ? yes C(7) C(9) C(10) 110.5(3) ? ? ? yes C(8) C(9) C(10) 111.5(3) ? ? ? yes N(4) C(10) C(9) 108.7(3) ? ? ? yes N(4) C(10) C(11) 110.7(3) ? ? ? yes N(4) C(10) C(12) 105.5(3) ? ? ? yes C(9) C(10) C(11) 113.7(3) ? ? ? yes C(9) C(10) C(12) 109.6(3) ? ? ? yes C(11) C(10) C(12) 108.3(3) ? ? ? yes O(2) C(13) N(4) 124.9(4) ? ? ? yes O(2) C(13) C(14) 120.9(4) ? ? ? yes N(4) C(13) C(14) 114.1(4) ? ? ? yes N(5) C(14) C(13) 116.8(3) ? ? ? yes N(5) C(14) C(15) 124.4(4) ? ? ? yes C(13) C(14) C(15) 118.8(4) ? ? ? yes C(14) C(15) C(16) 117.2(5) ? ? ? yes C(15) C(16) C(17) 119.5(4) ? ? ? yes C(16) C(17) C(18) 119.5(5) ? ? ? yes N(5) C(18) C(17) 122.8(5) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END data_Complex_5b #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 8 17:55:45 1998' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.825(2) _cell_length_b 10.276(4) _cell_length_c 19.011(1) _cell_angle_alpha 90 _cell_angle_beta 100.952(7) _cell_angle_gamma 90 _cell_volume 2267.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 35.7 _cell_measurement_theta_max 41.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 635.96 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H21 Cl3 N5 O2 Os ' _chemical_formula_moiety 'C18 H21 Cl3 N5 O2 Os ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1228.00 _exptl_absorpt_coefficient_mu 5.996 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.884 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -1.68 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4464 _reflns_number_total 4247 _reflns_number_observed 2944 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.17 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03200 _diffrn_orient_matrix_UB_12 0.00121 _diffrn_orient_matrix_UB_13 -0.05261 _diffrn_orient_matrix_UB_21 -0.02925 _diffrn_orient_matrix_UB_22 -0.09074 _diffrn_orient_matrix_UB_23 0.00304 _diffrn_orient_matrix_UB_31 -0.07443 _diffrn_orient_matrix_UB_32 0.03514 _diffrn_orient_matrix_UB_33 0.00965 #------------------------------------------------------------------------------ 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 Os 0 4 -1.216 7.603 'International Tables' N 0 20 0.006 0.003 'International Tables' C 0 72 0.003 0.002 'International Tables' H 0 84 0.000 0.000 'International Tables' O 0 8 0.011 0.006 'International Tables' Cl 0 12 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ 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 Os(1) 0.23595(2) 0.06585(3) 0.14704(1) 0.0469 Uij ? ? Cl(1) 0.3518(2) 0.2453(2) 0.13864(9) 0.0691 Uij ? ? Cl(2) 0.0868(2) 0.1713(2) 0.06907(10) 0.0786 Uij ? ? Cl(3) 0.4009(1) -0.0550(2) 0.19390(9) 0.0617 Uij ? ? O(1) 0.2669(3) -0.0049(4) 0.0415(2) 0.0498 Uij ? ? O(2) 0.1768(4) -0.4070(4) -0.0920(2) 0.0589 Uij ? ? N(1) 0.1898(5) 0.0893(6) 0.2205(3) 0.0650 Uij ? ? N(2) 0.1528(4) -0.1163(5) 0.1288(2) 0.0494 Uij ? ? N(3) 0.2104(4) -0.1507(4) -0.0485(2) 0.0363 Uij ? ? N(4) 0.3034(4) -0.3003(5) -0.1483(2) 0.0451 Uij ? ? N(5) 0.4468(5) -0.5007(6) -0.1291(3) 0.0579 Uij ? ? C(1) 0.1041(5) -0.1757(8) 0.1781(3) 0.0599 Uij ? ? C(2) 0.0600(6) -0.2992(8) 0.1689(4) 0.0699 Uij ? ? C(3) 0.0664(6) -0.3676(8) 0.1078(4) 0.0736 Uij ? ? C(4) 0.1163(6) -0.3064(7) 0.0556(3) 0.0621 Uij ? ? C(5) 0.1576(5) -0.1818(7) 0.0674(3) 0.0470 Uij ? ? C(6) 0.2159(5) -0.1069(6) 0.0174(3) 0.0407 Uij ? ? C(7) 0.1896(6) 0.0437(6) -0.1232(3) 0.0529 Uij ? ? C(8) 0.3860(5) -0.0516(6) -0.0801(3) 0.0464 Uij ? ? C(9) 0.2581(5) -0.0815(5) -0.1059(3) 0.0358 Uij ? ? C(10) 0.2412(5) -0.1786(6) -0.1710(3) 0.0416 Uij ? ? C(11) 0.1143(5) -0.2062(7) -0.2031(3) 0.0565 Uij ? ? C(12) 0.2976(6) -0.1226(6) -0.2306(3) 0.0556 Uij ? ? C(13) 0.2691(6) -0.4018(6) -0.1126(3) 0.0476 Uij ? ? C(14) 0.3563(6) -0.5084(6) -0.0979(3) 0.0485 Uij ? ? C(15) 0.3388(6) -0.6081(7) -0.0523(4) 0.0601 Uij ? ? C(16) 0.4221(7) -0.7032(7) -0.0382(4) 0.0730 Uij ? ? C(17) 0.5132(7) -0.6990(8) -0.0709(4) 0.0739 Uij ? ? C(18) 0.5241(7) -0.5966(8) -0.1158(4) 0.0753 Uij ? ? H(1) 0.372(5) -0.315(7) -0.156(3) 0.0778 Uij ? ? H(2) 0.1000 -0.1306 0.2212 0.0720 Uij ? ? H(3) 0.0248 -0.3374 0.2049 0.0839 Uij ? ? H(4) 0.0379 -0.4540 0.1013 0.0885 Uij ? ? H(5) 0.1219 -0.3506 0.0125 0.0747 Uij ? ? H(6) 0.1977 0.0961 -0.0814 0.0635 Uij ? ? H(7) 0.2177 0.0898 -0.1597 0.0635 Uij ? ? H(8) 0.1106 0.0232 -0.1394 0.0635 Uij ? ? H(9) 0.4272 -0.1307 -0.0690 0.0557 Uij ? ? H(10) 0.4149 -0.0072 -0.1168 0.0557 Uij ? ? H(11) 0.3953 0.0016 -0.0386 0.0557 Uij ? ? H(12) 0.0772 -0.1274 -0.2205 0.0678 Uij ? ? H(13) 0.1096 -0.2666 -0.2413 0.0678 Uij ? ? H(14) 0.0774 -0.2416 -0.1671 0.0678 Uij ? ? H(15) 0.3770 -0.1069 -0.2124 0.0667 Uij ? ? H(16) 0.2900 -0.1829 -0.2691 0.0667 Uij ? ? H(17) 0.2608 -0.0432 -0.2472 0.0667 Uij ? ? H(18) 0.2718 -0.6109 -0.0315 0.0720 Uij ? ? H(19) 0.4152 -0.7714 -0.0055 0.0875 Uij ? ? H(20) 0.5697 -0.7659 -0.0631 0.0885 Uij ? ? H(21) 0.5894 -0.5941 -0.1382 0.0903 Uij ? ? 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 Os(1) 0.0424(1) 0.0681(2) 0.0313(1) 0.0059(1) 0.0098(1) -0.0016(1) Cl(1) 0.080(1) 0.076(1) 0.0533(10) -0.007(1) 0.0174(9) -0.0091(9) Cl(2) 0.058(1) 0.109(2) 0.066(1) 0.021(1) 0.0030(9) 0.019(1) Cl(3) 0.0453(9) 0.079(1) 0.0577(10) 0.0113(9) 0.0026(7) -0.0041(9) O(1) 0.056(3) 0.063(3) 0.034(2) -0.009(2) 0.017(2) -0.003(2) O(2) 0.062(3) 0.047(3) 0.069(3) -0.001(2) 0.014(2) 0.010(2) N(1) 0.063(4) 0.087(5) 0.048(3) 0.009(3) 0.019(3) 0.002(3) N(2) 0.034(3) 0.078(4) 0.036(3) -0.003(3) 0.005(2) 0.016(3) N(3) 0.036(2) 0.047(3) 0.026(2) 0.004(2) 0.006(2) 0.007(2) N(4) 0.053(3) 0.044(3) 0.039(3) 0.004(3) 0.013(2) -0.002(2) N(5) 0.062(4) 0.054(4) 0.056(3) 0.015(3) 0.007(3) -0.006(3) C(1) 0.048(4) 0.098(6) 0.036(3) 0.002(4) 0.013(3) 0.022(4) C(2) 0.062(5) 0.095(6) 0.057(4) -0.014(4) 0.021(4) 0.029(4) C(3) 0.081(5) 0.072(5) 0.067(5) -0.026(4) 0.011(4) 0.015(4) C(4) 0.067(5) 0.071(5) 0.048(4) -0.018(4) 0.010(3) 0.011(4) C(5) 0.039(3) 0.068(4) 0.033(3) -0.004(3) 0.004(3) 0.011(3) C(6) 0.033(3) 0.049(4) 0.039(3) -0.004(3) 0.002(3) 0.005(3) C(7) 0.068(4) 0.048(4) 0.043(4) 0.012(3) 0.011(3) 0.004(3) C(8) 0.050(4) 0.055(4) 0.035(3) -0.007(3) 0.011(3) -0.004(3) C(9) 0.042(3) 0.039(3) 0.026(3) 0.002(3) 0.007(2) 0.008(2) C(10) 0.048(3) 0.042(4) 0.033(3) 0.001(3) 0.005(2) 0.000(3) C(11) 0.058(4) 0.066(5) 0.040(3) -0.001(3) -0.005(3) 0.000(3) C(12) 0.078(5) 0.057(4) 0.034(3) 0.010(4) 0.016(3) 0.004(3) C(13) 0.056(4) 0.044(4) 0.040(3) -0.004(3) 0.002(3) -0.004(3) C(14) 0.063(4) 0.037(4) 0.041(3) 0.001(3) -0.001(3) -0.010(3) C(15) 0.080(5) 0.042(4) 0.058(4) 0.006(4) 0.013(4) 0.003(3) C(16) 0.105(6) 0.049(5) 0.060(4) 0.014(4) 0.003(4) 0.007(4) C(17) 0.087(6) 0.067(5) 0.061(5) 0.034(5) -0.002(4) 0.003(4) C(18) 0.076(5) 0.080(6) 0.066(5) 0.026(5) 0.005(4) -0.003(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.50006 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2944 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0278 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0304 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.331 _refine_ls_shift/esd_max 0.0290 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.70 _refine_diff_density_max 0.88 #------------------------------------------------------------------------------ _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 Os(1) Cl(1) 2.321(2) ? ? yes Os(1) Cl(2) 2.342(2) ? ? yes Os(1) Cl(3) 2.341(2) ? ? yes Os(1) O(1) 2.229(4) ? ? yes Os(1) N(1) 1.612(5) ? ? yes Os(1) N(2) 2.112(5) ? ? yes O(1) C(6) 1.251(7) ? ? yes O(2) C(13) 1.230(7) ? ? yes N(2) C(1) 1.337(7) ? ? yes N(2) C(5) 1.357(7) ? ? yes N(3) C(6) 1.322(7) ? ? yes N(3) C(9) 1.499(6) ? ? yes N(4) C(10) 1.473(7) ? ? yes N(4) C(13) 1.347(8) ? ? yes N(5) C(14) 1.322(8) ? ? yes N(5) C(18) 1.335(8) ? ? yes C(1) C(2) 1.37(1) ? ? yes C(2) C(3) 1.372(10) ? ? yes C(3) C(4) 1.397(9) ? ? yes C(4) C(5) 1.373(9) ? ? yes C(5) C(6) 1.489(8) ? ? yes C(7) C(9) 1.522(8) ? ? yes C(8) C(9) 1.530(8) ? ? yes C(9) C(10) 1.573(7) ? ? yes C(10) C(11) 1.535(8) ? ? yes C(10) C(12) 1.532(8) ? ? yes C(13) C(14) 1.494(8) ? ? yes C(14) C(15) 1.383(9) ? ? yes C(15) C(16) 1.377(9) ? ? yes C(16) C(17) 1.34(1) ? ? yes C(17) C(18) 1.38(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Os(1) Cl(2) 88.40(7) ? ? ? yes Cl(1) Os(1) Cl(3) 89.29(7) ? ? ? yes Cl(1) Os(1) O(1) 89.9(1) ? ? ? yes Cl(1) Os(1) N(1) 104.0(2) ? ? ? yes Cl(1) Os(1) N(2) 162.8(1) ? ? ? yes Cl(2) Os(1) Cl(3) 163.50(6) ? ? ? yes Cl(2) Os(1) O(1) 79.3(1) ? ? ? yes Cl(2) Os(1) N(1) 98.1(2) ? ? ? yes Cl(2) Os(1) N(2) 92.0(1) ? ? ? yes Cl(3) Os(1) O(1) 84.4(1) ? ? ? yes Cl(3) Os(1) N(1) 98.3(2) ? ? ? yes Cl(3) Os(1) N(2) 85.5(1) ? ? ? yes O(1) Os(1) N(1) 165.9(2) ? ? ? yes O(1) Os(1) N(2) 73.4(2) ? ? ? yes N(1) Os(1) N(2) 93.0(2) ? ? ? yes Os(1) O(1) C(6) 116.9(4) ? ? ? yes Os(1) N(2) C(1) 122.6(5) ? ? ? yes Os(1) N(2) C(5) 119.1(4) ? ? ? yes C(1) N(2) C(5) 118.1(6) ? ? ? yes C(6) N(3) C(9) 124.8(5) ? ? ? yes C(10) N(4) C(13) 128.6(5) ? ? ? yes C(14) N(5) C(18) 117.0(6) ? ? ? yes N(2) C(1) C(2) 122.5(7) ? ? ? yes C(1) C(2) C(3) 120.0(6) ? ? ? yes C(2) C(3) C(4) 118.0(7) ? ? ? yes C(3) C(4) C(5) 119.3(7) ? ? ? yes N(2) C(5) C(4) 122.0(6) ? ? ? yes N(2) C(5) C(6) 113.1(6) ? ? ? yes C(4) C(5) C(6) 124.8(6) ? ? ? yes O(1) C(6) N(3) 124.4(5) ? ? ? yes O(1) C(6) C(5) 116.7(5) ? ? ? yes N(3) C(6) C(5) 118.9(5) ? ? ? yes N(3) C(9) C(7) 107.4(4) ? ? ? yes N(3) C(9) C(8) 110.3(4) ? ? ? yes N(3) C(9) C(10) 105.2(4) ? ? ? yes C(7) C(9) C(8) 110.6(5) ? ? ? yes C(7) C(9) C(10) 112.5(4) ? ? ? yes C(8) C(9) C(10) 110.5(4) ? ? ? yes N(4) C(10) C(9) 109.0(4) ? ? ? yes N(4) C(10) C(11) 110.8(5) ? ? ? yes N(4) C(10) C(12) 105.8(5) ? ? ? yes C(9) C(10) C(11) 113.4(5) ? ? ? yes C(9) C(10) C(12) 109.6(5) ? ? ? yes C(11) C(10) C(12) 107.8(5) ? ? ? yes O(2) C(13) N(4) 124.4(6) ? ? ? yes O(2) C(13) C(14) 122.1(6) ? ? ? yes N(4) C(13) C(14) 113.5(6) ? ? ? yes N(5) C(14) C(13) 117.4(6) ? ? ? yes N(5) C(14) C(15) 123.8(6) ? ? ? yes C(13) C(14) C(15) 118.7(6) ? ? ? yes C(14) C(15) C(16) 117.5(7) ? ? ? yes C(15) C(16) C(17) 119.6(7) ? ? ? yes C(16) C(17) C(18) 119.3(7) ? ? ? yes N(5) C(18) C(17) 122.8(7) ? ? ? yes #------------------------------------------------------------------------------ _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;