# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1660 data_ip323 loop_ _publ_author_name 'Mei-Yuk Ckoi' 'Michael C.W. Chan' 'Shie-Ming Peng' 'Kung-Kai Cheung' 'Chi-Ming Che' #--------------------- #-------------------------------------------------------- _audit_creation_date 'Wed Jul 8 18:14:19 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- #---- _computing_data_collection 'MAR Data collection Software & DENZO' _computing_cell_refinement 'MAR Data Collection Software & DENZO' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ #----------- _cell_length_a 8.763(2) _cell_length_b 10.534(2) _cell_length_c 15.243(2) _cell_angle_alpha 90 _cell_angle_beta 97.31(2) _cell_angle_gamma 90 _cell_volume 1395.6(5) _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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '-x,1/2+y,1/2-z' ' -x, -y, -z' '+x,1/2-y,1/2+z' #----------------------------------------------------------- #------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 589.79 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H44 N6 Ru' _chemical_formula_moiety 'C30 H44 N6 Ru' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 620.00 _exptl_absorpt_coefficient_mu 0.592 _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 'Image Plate Detector' _diffrn_measurement_device 'MAR IPDS' _diffrn_measurement_method 'oscillation' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 2741 _reflns_number_total 2741 _reflns_number_observed 1532 _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 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.98 _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 C 0 60 0.003 0.002 'International Tables' H 0 88 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' Ru 0 2 -1.259 0.836 '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) 0.0000 0.0000 0.0000 0.0366(2) Uij ? ? N(1) 0.1496(8) 0.1052(7) -0.0851(5) 0.059(2) Uij ? ? N(2) -0.0892(8) 0.1900(6) 0.0461(5) 0.059(2) Uij ? ? N(3) 0.5971(9) -0.0952(9) 0.3923(5) 0.069(3) Uij ? ? C(1) 0.304(1) 0.139(1) -0.0446(7) 0.081(4) Uij ? ? C(2) 0.068(1) 0.231(1) -0.1181(10) 0.120(5) Uij ? ? C(3) 0.051(2) 0.329(1) -0.052(1) 0.122(5) Uij ? ? C(4) -0.107(2) 0.289(1) -0.0296(9) 0.121(5) Uij ? ? C(5) 0.008(1) 0.258(1) 0.107(1) 0.148(5) Uij ? ? C(6) -0.253(1) 0.182(1) 0.053(1) 0.130(5) Uij ? ? C(7) -0.260(2) 0.092(2) 0.150(1) 0.126(6) Uij ? ? C(8) -0.168(1) -0.023(2) 0.1670(7) 0.110(5) Uij ? ? C(9) 0.1721(8) -0.0023(8) 0.1060(5) 0.042(2) Uij ? ? C(10) 0.2660(9) -0.0148(8) 0.1697(5) 0.044(2) Uij ? ? C(11) 0.3759(9) -0.0436(8) 0.2446(6) 0.041(2) Uij ? ? C(12) 0.406(1) 0.0402(8) 0.3161(7) 0.054(3) Uij ? ? C(13) 0.517(1) 0.009(1) 0.3855(6) 0.068(3) Uij ? ? C(14) 0.565(1) -0.1770(9) 0.3255(6) 0.061(3) Uij ? ? C(15) 0.4602(9) -0.1543(8) 0.2523(6) 0.052(2) Uij ? ? H(1) 0.3583 0.0631 -0.0248 0.0994 Uij ? ? H(2) 0.3579 0.1795 -0.0871 0.0994 Uij ? ? H(3) 0.2987 0.1934 0.0041 0.0994 Uij ? ? H(4) 0.1246 0.2693 -0.1596 0.1094 Uij ? ? H(5) -0.0329 0.2124 -0.1438 0.1094 Uij ? ? H(6) 0.1289 0.3251 -0.0018 0.1094 Uij ? ? H(7) 0.0505 0.4137 -0.0754 0.1094 Uij ? ? H(8) -0.1636 0.2519 -0.0804 0.1094 Uij ? ? H(9) -0.1609 0.3605 -0.0115 0.1094 Uij ? ? H(10) 0.0334 0.2108 0.1580 0.1201 Uij ? ? H(11) 0.0995 0.2778 0.0804 0.1201 Uij ? ? H(12) -0.0407 0.3356 0.1188 0.1201 Uij ? ? H(13) -0.2964 0.2646 0.0580 0.1094 Uij ? ? H(14) -0.3071 0.1408 0.0025 0.1094 Uij ? ? H(15) -0.2278 0.1477 0.1982 0.1094 Uij ? ? H(16) -0.3632 0.0684 0.1510 0.1094 Uij ? ? H(17) -0.2160 -0.0738 0.2070 0.1094 Uij ? ? H(18) -0.0683 0.0009 0.1933 0.1094 Uij ? ? H(19) 0.3497 0.1173 0.3170 0.0659 Uij ? ? H(20) 0.5382 0.0696 0.4317 0.0813 Uij ? ? H(21) 0.6187 -0.2558 0.3290 0.0738 Uij ? ? H(22) 0.4454 -0.2157 0.2064 0.0628 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) 0.0332(5) 0.0389(5) 0.0348(5) -0.0003(5) -0.0062(3) -0.0008(5) N(1) 0.054(4) 0.083(5) 0.039(4) -0.015(4) 0.001(3) 0.021(4) N(2) 0.052(4) 0.044(4) 0.073(5) 0.011(3) -0.017(4) -0.020(4) N(3) 0.071(5) 0.079(6) 0.052(5) 0.005(5) -0.018(4) 0.008(4) C(1) 0.059(6) 0.108(9) 0.073(7) -0.040(6) 0.000(5) 0.008(6) C(2) 0.087(8) 0.12(1) 0.14(1) -0.046(8) -0.036(7) 0.101(9) C(3) 0.108(10) 0.054(7) 0.20(2) -0.011(7) 0.02(1) 0.040(9) C(4) 0.15(1) 0.052(8) 0.15(1) 0.018(8) -0.032(9) -0.004(7) C(5) 0.094(8) 0.075(7) 0.25(1) 0.022(7) -0.064(9) -0.085(8) C(6) 0.064(8) 0.12(1) 0.20(1) 0.025(8) 0.011(8) -0.082(10) C(7) 0.13(1) 0.15(1) 0.11(1) -0.039(9) 0.063(9) -0.053(9) C(8) 0.069(7) 0.21(2) 0.051(5) -0.039(8) 0.013(5) -0.009(7) C(9) 0.045(4) 0.040(4) 0.040(4) -0.012(5) -0.002(3) -0.003(5) C(10) 0.042(4) 0.045(5) 0.041(4) -0.001(4) -0.007(3) 0.001(4) C(11) 0.033(4) 0.051(5) 0.037(5) -0.004(3) -0.002(4) 0.003(3) C(12) 0.059(5) 0.050(5) 0.050(6) 0.001(4) -0.011(5) -0.006(4) C(13) 0.091(7) 0.067(7) 0.039(4) -0.011(6) -0.017(4) -0.005(5) C(14) 0.064(6) 0.060(6) 0.055(6) 0.009(5) -0.009(5) 0.007(5) C(15) 0.051(5) 0.050(5) 0.050(5) 0.004(4) -0.008(4) 0.000(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 1532 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0643 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0776 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.260 _refine_ls_shift/esd_max 0.0340 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.80 _refine_diff_density_max 1.43 #---------------------------------------------------------------------- #------- _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) N(1) 2.249(6) ? ? yes Ru(1) N(1) 2.249(6) ? ? yes Ru(1) N(2) 2.292(6) ? ? yes Ru(1) N(2) 2.292(6) ? ? yes Ru(1) C(9) 2.065(7) ? ? yes Ru(1) C(9) 2.065(7) ? ? yes N(1) C(1) 1.46(1) ? ? yes N(1) C(2) 1.56(2) ? ? yes N(1) C(8) 1.55(1) ? ? yes N(2) C(4) 1.55(1) ? ? yes N(2) C(5) 1.37(1) ? ? yes N(2) C(6) 1.46(1) ? ? yes N(3) C(13) 1.30(1) ? ? yes N(3) C(14) 1.34(1) ? ? yes C(2) C(3) 1.46(2) ? ? yes C(3) C(4) 1.53(2) ? ? yes C(6) C(7) 1.75(2) ? ? yes C(7) C(8) 1.46(2) ? ? yes C(9) C(10) 1.20(1) ? ? yes C(10) C(11) 1.43(1) ? ? yes C(11) C(12) 1.40(1) ? ? yes C(11) C(15) 1.38(1) ? ? yes C(12) C(13) 1.39(1) ? ? yes C(14) C(15) 1.37(1) ? ? yes #----------------------------------------------------------------------- #------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ru(1) N(1) 180.0 ? ? ? yes N(1) Ru(1) N(2) 89.6(3) ? ? ? yes N(1) Ru(1) N(2) 90.4(3) ? ? ? yes N(1) Ru(1) C(9) 92.0(3) ? ? ? yes N(1) Ru(1) C(9) 88.0(3) ? ? ? yes N(1) Ru(1) N(2) 90.4(3) ? ? ? yes N(1) Ru(1) N(2) 89.6(3) ? ? ? yes N(1) Ru(1) C(9) 88.0(3) ? ? ? yes N(1) Ru(1) C(9) 92.0(3) ? ? ? yes N(2) Ru(1) N(2) 180.0 ? ? ? yes N(2) Ru(1) C(9) 90.8(3) ? ? ? yes N(2) Ru(1) C(9) 89.2(3) ? ? ? yes N(2) Ru(1) C(9) 89.2(3) ? ? ? yes N(2) Ru(1) C(9) 90.8(3) ? ? ? yes C(9) Ru(1) C(9) 180.0 ? ? ? yes Ru(1) N(1) C(1) 116.9(6) ? ? ? yes Ru(1) N(1) C(2) 109.3(6) ? ? ? yes Ru(1) N(1) C(8) 108.5(6) ? ? ? yes C(1) N(1) C(2) 107.0(8) ? ? ? yes C(1) N(1) C(8) 106.9(8) ? ? ? yes C(2) N(1) C(8) 107.9(9) ? ? ? yes Ru(1) N(2) C(4) 111.4(6) ? ? ? yes Ru(1) N(2) C(5) 117.1(6) ? ? ? yes Ru(1) N(2) C(6) 110.4(6) ? ? ? yes C(4) N(2) C(5) 98.5(9) ? ? ? yes C(4) N(2) C(6) 95.1(9) ? ? ? yes C(5) N(2) C(6) 120.7(9) ? ? ? yes C(13) N(3) C(14) 115.3(8) ? ? ? yes N(1) C(2) C(3) 117(1) ? ? ? yes C(2) C(3) C(4) 98(1) ? ? ? yes N(2) C(4) C(3) 110.3(10) ? ? ? yes N(2) C(6) C(7) 103(1) ? ? ? yes C(6) C(7) C(8) 121.4(10) ? ? ? yes N(1) C(8) C(7) 115.6(10) ? ? ? yes Ru(1) C(9) C(10) 173.5(7) ? ? ? yes C(9) C(10) C(11) 174.1(9) ? ? ? yes C(10) C(11) C(12) 121.9(7) ? ? ? yes C(10) C(11) C(15) 123.2(8) ? ? ? yes C(12) C(11) C(15) 114.9(8) ? ? ? yes C(11) C(12) C(13) 119.3(8) ? ? ? yes N(3) C(13) C(12) 125.5(8) ? ? ? yes N(3) C(14) C(15) 124.1(8) ? ? ? yes C(11) C(15) C(14) 120.9(8) ? ? ? yes #----------------------------------------------------------------------- #------ _publ_section_references ; Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; data_ic5556 loop_ _publ_author_name 'Chi-Ming Che' 'Shie-Ming Peng' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H70 F6 N10 O13 Re2 Ru S2' _chemical_formula_weight 1814.87 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3284(2) _cell_length_b 10.5843(3) _cell_length_c 20.8961(5) _cell_angle_alpha 84.370(1) _cell_angle_beta 84.973(1) _cell_angle_gamma 88.998(1) _cell_volume 1825.99(8) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6914 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method ? _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.647 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.3791 _exptl_absorpt_correction_T_max 0.6477 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20 _diffrn_reflns_number 21885 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7455 _reflns_number_observed 4349 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7455 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_obs 0.0649 _refine_ls_wR_factor_all 0.1660 _refine_ls_wR_factor_obs 0.1329 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.017 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.5000 0.5000 0.5000 0.0404(3) Uani 1 d S . Re Re 1.17785(5) 0.46928(5) 0.10878(2) 0.0527(2) Uani 1 d . . N1 N 1.0714(9) 0.4772(8) 0.2089(3) 0.039(2) Uani 1 d . . N2 N 1.3278(10) 0.3206(10) 0.1522(4) 0.058(3) Uani 1 d . . N3 N 1.3756(10) 0.5653(9) 0.1417(4) 0.048(2) Uani 1 d . . C1 C 1.0042(15) 0.3674(13) 0.0916(5) 0.067(3) Uani 1 d . . C2 C 1.2745(14) 0.4616(14) 0.0228(6) 0.081(4) Uani 1 d . . C3 C 1.0559(14) 0.6153(13) 0.0795(5) 0.063(3) Uani 1 d . . C4 C 0.6884(11) 0.4960(10) 0.4309(5) 0.047(3) Uani 1 d . . C5 C 0.7895(12) 0.4936(9) 0.3859(5) 0.046(2) Uani 1 d . . C6 C 0.8919(10) 0.4872(9) 0.3289(4) 0.038(2) Uani 1 d . . C7 C 0.9542(11) 0.5955(9) 0.2932(4) 0.044(2) Uani 1 d . . H7A H 0.9362(11) 0.6744(9) 0.3088(4) 0.052 Uiso 1 calc R . C8 C 1.0418(11) 0.5868(10) 0.2353(5) 0.044(2) Uani 1 d . . H8A H 1.0834(11) 0.6610(10) 0.2129(5) 0.053 Uiso 1 calc R . C9 C 1.0154(12) 0.3704(10) 0.2444(5) 0.046(2) Uani 1 d . . H9A H 1.0377(12) 0.2921(10) 0.2287(5) 0.056 Uiso 1 calc R . C10 C 0.9274(11) 0.3742(10) 0.3023(5) 0.047(2) Uani 1 d . . H10A H 0.8900(11) 0.2986(10) 0.3246(5) 0.057 Uiso 1 calc R . C11 C 1.2917(16) 0.1961(15) 0.1585(8) 0.088(5) Uani 1 d . . H11A H 1.2021(16) 0.1694(15) 0.1401(8) 0.105 Uiso 1 calc R . C12 C 1.3856(22) 0.1063(15) 0.1922(9) 0.112(6) Uani 1 d . . H12A H 1.3555(22) 0.0214(15) 0.1980(9) 0.134 Uiso 1 calc R . C13 C 1.5202(21) 0.1436(17) 0.2161(10) 0.121(6) Uani 1 d . . H13A H 1.5873(21) 0.0841(17) 0.2364(10) 0.145 Uiso 1 calc R . C14 C 1.5562(17) 0.2664(15) 0.2105(7) 0.088(4) Uani 1 d . . H14A H 1.6481(17) 0.2922(15) 0.2278(7) 0.105 Uiso 1 calc R . C15 C 1.4582(14) 0.3582(12) 0.1790(6) 0.062(3) Uani 1 d . . C16 C 1.4830(12) 0.4942(12) 0.1742(5) 0.056(3) Uani 1 d . . C17 C 1.6139(14) 0.5500(14) 0.1987(6) 0.072(4) Uani 1 d . . H17A H 1.6895(14) 0.4991(14) 0.2195(6) 0.087 Uiso 1 calc R . C18 C 1.6300(18) 0.6775(15) 0.1922(7) 0.089(4) Uani 1 d . . H18A H 1.7150(18) 0.7147(15) 0.2093(7) 0.106 Uiso 1 calc R . C19 C 1.5224(16) 0.7498(13) 0.1610(7) 0.083(4) Uani 1 d . . H19A H 1.5300(16) 0.8379(13) 0.1566(7) 0.099 Uiso 1 calc R . C20 C 1.3957(14) 0.6880(15) 0.1346(7) 0.081(4) Uani 1 d . . H20A H 1.3239(14) 0.7378(15) 0.1112(7) 0.097 Uiso 1 calc R . C22 C 0.5904(28) 0.7873(18) 0.4589(11) 0.150(8) Uani 1 d . . C23 C 0.4327(18) 0.7135(17) 0.3866(7) 0.103(5) Uani 1 d . . C25 C 0.3569(16) 0.4955(19) 0.3634(6) 0.107(6) Uani 1 d . . C26 C 0.4193(21) 0.2908(16) 0.4129(9) 0.112(5) Uani 1 d . . N4 N 0.4464(18) 0.7020(14) 0.4583(7) 0.057(4) Uiso 0.60 d P 1 N5 N 0.3467(19) 0.4201(15) 0.4279(8) 0.062(4) Uiso 0.60 d P 1 C21 C 0.3865(29) 0.1768(23) 0.4688(12) 0.086(7) Uiso 0.60 d P 1 C24 C 0.3089(29) 0.6333(22) 0.3613(11) 0.080(6) Uiso 0.60 d P 1 C27 C 0.2871(30) 0.7576(22) 0.4895(12) 0.089(7) Uiso 0.60 d P 1 C28 C 0.1723(27) 0.4024(21) 0.4545(11) 0.079(6) Uiso 0.60 d P 1 N4' N 0.3497(31) 0.5733(24) 0.4191(13) 0.073(7) Uiso 0.40 d P 2 N5' N 0.4289(40) 0.2926(31) 0.4862(17) 0.099(9) Uiso 0.40 d P 2 C21' C 0.2397(92) 0.3613(67) 0.4001(36) 0.199(26) Uiso 0.40 d P 2 C24' C 0.4048(86) 0.8280(64) 0.4307(34) 0.181(24) Uiso 0.40 d P 2 C27' C 0.1772(46) 0.6067(34) 0.4432(18) 0.094(11) Uiso 0.40 d P 2 C28' C 0.5581(55) 0.2077(41) 0.4716(22) 0.116(14) Uiso 0.40 d P 2 O1 O 0.8964(13) 0.3057(11) 0.0824(5) 0.111(4) Uani 1 d . . O2 O 1.3353(12) 0.4536(12) -0.0289(4) 0.120(4) Uani 1 d . . O3 O 0.9830(12) 0.7049(11) 0.0638(5) 0.102(3) Uani 1 d . . S S 0.9372(8) 0.9668(5) 0.2607(4) 0.162(3) Uani 1 d . . C29 C 0.9798(36) 0.9921(22) 0.3455(16) 0.174(13) Uani 1 d . . F1 F 0.8410(26) 1.0470(15) 0.3567(13) 0.283(12) Uani 1 d . . F2 F 0.9975(19) 0.8847(13) 0.3790(8) 0.208(7) Uani 1 d . . F3 F 1.1019(18) 1.0601(12) 0.3444(8) 0.211(7) Uani 1 d . . O4 O 0.7940(15) 0.8922(9) 0.2730(9) 0.176(7) Uani 1 d . . O5 O 1.0853(20) 0.8918(14) 0.2379(15) 0.298(15) Uani 1 d . . O6 O 0.9243(17) 1.0901(10) 0.2315(8) 0.166(6) Uani 1 d . . O7 O 0.5000 0.0000 0.0000 0.528(41) Uiso 1 d S . C30 C 0.7749(60) 0.0219(44) 0.0549(25) 0.411(29) Uiso 1 d . . H30A H 0.8904(60) 0.0260(44) 0.0503(25) 0.617 Uiso 1 calc R . H30B H 0.7416(60) -0.0496(44) 0.0847(25) 0.617 Uiso 1 calc R . H30C H 0.7313(60) 0.0985(44) 0.0708(25) 0.617 Uiso 1 calc R . C31 C 0.7142(57) 0.0074(44) -0.0096(23) 0.361(25) Uiso 1 d . . H31A H 0.7584(57) -0.0695(44) -0.0262(23) 0.433 Uiso 1 calc R . H31B H 0.7480(57) 0.0791(44) -0.0401(23) 0.433 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0316(6) 0.0579(8) 0.0312(6) -0.0069(5) 0.0021(5) 0.0034(5) Re 0.0376(3) 0.0888(4) 0.0323(3) -0.0130(2) 0.0012(2) 0.0005(2) N1 0.043(5) 0.046(5) 0.028(4) -0.002(4) -0.006(3) 0.003(4) N2 0.042(5) 0.079(7) 0.058(6) -0.038(5) 0.002(4) 0.010(5) N3 0.040(5) 0.055(6) 0.046(5) 0.001(4) 0.001(4) -0.006(4) C1 0.051(7) 0.105(10) 0.045(7) -0.015(7) -0.006(6) 0.002(7) C2 0.046(7) 0.147(13) 0.055(8) -0.024(8) -0.003(6) -0.015(8) C3 0.055(7) 0.088(10) 0.046(7) 0.000(6) -0.007(6) 0.000(7) C4 0.036(5) 0.063(7) 0.044(6) -0.012(5) -0.001(5) -0.001(5) C5 0.038(5) 0.050(7) 0.051(6) -0.014(5) 0.002(5) 0.000(5) C6 0.029(5) 0.050(6) 0.035(5) -0.008(5) -0.003(4) 0.000(4) C7 0.051(6) 0.041(6) 0.039(6) -0.015(5) 0.000(5) 0.000(5) C8 0.038(5) 0.046(6) 0.047(6) -0.004(5) -0.001(5) -0.006(5) C9 0.051(6) 0.046(6) 0.042(6) -0.007(5) -0.001(5) 0.009(5) C10 0.045(6) 0.052(7) 0.044(6) -0.002(5) 0.002(5) -0.007(5) C11 0.053(8) 0.081(11) 0.135(14) -0.049(9) 0.000(8) 0.011(8) C12 0.101(13) 0.063(10) 0.169(18) -0.024(10) 0.015(12) 0.015(10) C13 0.089(12) 0.079(13) 0.194(20) 0.005(12) -0.041(13) 0.016(10) C14 0.070(9) 0.081(11) 0.110(12) 0.004(9) -0.014(8) 0.016(8) C15 0.051(7) 0.075(9) 0.063(8) -0.020(6) -0.005(6) 0.006(6) C16 0.042(6) 0.083(9) 0.043(6) -0.012(6) -0.008(5) 0.006(6) C17 0.053(7) 0.094(11) 0.075(9) -0.013(7) -0.023(6) -0.004(7) C18 0.082(10) 0.084(11) 0.108(12) -0.029(9) -0.025(9) -0.018(9) C19 0.074(9) 0.062(9) 0.110(12) 0.008(8) -0.006(8) -0.012(8) C20 0.044(7) 0.109(12) 0.087(10) 0.001(9) 0.002(7) -0.006(8) C22 0.180(21) 0.114(15) 0.151(19) -0.017(13) 0.026(16) -0.048(14) C23 0.086(10) 0.146(14) 0.065(9) 0.038(9) -0.003(8) 0.028(10) C25 0.073(9) 0.220(19) 0.032(7) -0.028(9) -0.018(6) 0.042(11) C26 0.110(13) 0.113(13) 0.120(14) -0.049(11) -0.006(11) -0.002(10) O1 0.096(8) 0.147(10) 0.095(8) -0.015(7) -0.031(6) -0.036(7) O2 0.081(7) 0.236(13) 0.046(6) -0.042(7) 0.022(5) -0.014(7) O3 0.100(8) 0.123(9) 0.078(7) 0.009(6) -0.018(6) 0.037(7) S 0.140(5) 0.068(3) 0.287(8) 0.011(4) -0.094(5) -0.028(3) C29 0.169(23) 0.082(16) 0.275(34) 0.068(19) -0.124(26) -0.053(16) F1 0.245(21) 0.136(13) 0.431(31) 0.069(16) 0.071(22) -0.008(14) F2 0.257(17) 0.142(11) 0.236(16) 0.020(10) -0.125(13) 0.016(10) F3 0.191(13) 0.145(10) 0.314(19) -0.005(11) -0.121(13) -0.054(10) O4 0.121(10) 0.054(7) 0.366(22) -0.024(9) -0.096(12) -0.012(7) O5 0.130(13) 0.096(11) 0.651(48) -0.035(17) 0.055(20) 0.029(10) O6 0.176(13) 0.053(7) 0.280(18) -0.001(8) -0.103(12) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C4 2.040(10) . ? Ru C4 2.040(10) 2_666 ? Ru N4' 2.26(3) 2_666 ? Ru N4' 2.26(3) . ? Ru N4 2.280(15) . ? Ru N4 2.280(15) 2_666 ? Ru N5 2.29(2) 2_666 ? Ru N5 2.29(2) . ? Ru N5' 2.34(3) 2_666 ? Ru N5' 2.34(3) . ? Re C1 1.899(13) . ? Re C2 1.911(13) . ? Re C3 1.914(14) . ? Re N3 2.148(8) . ? Re N2 2.171(9) . ? Re N1 2.208(7) . ? N1 C8 1.342(12) . ? N1 C9 1.356(12) . ? N2 C15 1.348(13) . ? N2 C11 1.35(2) . ? N3 C20 1.30(2) . ? N3 C16 1.346(13) . ? C1 O1 1.159(13) . ? C2 O2 1.164(13) . ? C3 O3 1.153(13) . ? C4 C5 1.207(13) . ? C5 C6 1.410(13) . ? C6 C10 1.384(13) . ? C6 C7 1.388(13) . ? C7 C8 1.368(12) . ? C9 C10 1.363(13) . ? C11 C12 1.40(2) . ? C12 C13 1.35(2) . ? C13 C14 1.33(2) . ? C14 C15 1.41(2) . ? C15 C16 1.45(2) . ? C16 C17 1.407(15) . ? C17 C18 1.35(2) . ? C18 C19 1.34(2) . ? C19 C20 1.43(2) . ? C22 N5' 1.36(3) 2_666 ? C22 N4 1.51(2) . ? C22 C21 1.62(3) 2_666 ? C22 C24' 1.73(7) . ? C22 C28' 1.83(5) 2_666 ? C23 N4 1.51(2) . ? C23 C24 1.51(3) . ? C23 C24' 1.60(7) . ? C23 N4' 1.70(3) . ? C25 N4' 1.49(3) . ? C25 N5 1.49(2) . ? C25 C24 1.50(3) . ? C25 C21' 1.81(7) . ? C26 N5 1.54(2) . ? C26 N5' 1.54(4) . ? C26 C21 1.60(3) . ? C26 C21' 1.69(7) . ? C26 C28' 1.90(5) . ? N4 C27 1.56(3) . ? N5 C28 1.52(3) . ? C21 C22 1.62(3) 2_666 ? N4' C27' 1.53(4) . ? N5' C22 1.36(3) 2_666 ? N5' C28' 1.42(5) . ? C28' C22 1.83(5) 2_666 ? S O6 1.392(11) . ? S O4 1.432(13) . ? S O5 1.52(2) . ? S C29 1.88(3) . ? C29 F3 1.25(2) . ? C29 F2 1.29(2) . ? C29 F1 1.30(3) . ? O7 C31 1.78(5) 2_655 ? O7 C31 1.78(5) . ? C30 C31 1.50(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Ru C4 180.000(2) . 2_666 ? C4 Ru N4' 93.6(7) . 2_666 ? C4 Ru N4' 86.4(7) 2_666 2_666 ? C4 Ru N4' 86.4(7) . . ? C4 Ru N4' 93.6(7) 2_666 . ? N4' Ru N4' 179.998(5) 2_666 . ? C4 Ru N4 88.0(5) . . ? C4 Ru N4 92.0(5) 2_666 . ? C4 Ru N4 92.0(5) . 2_666 ? C4 Ru N4 88.0(5) 2_666 2_666 ? N4 Ru N4 179.998(3) . 2_666 ? C4 Ru N5 93.3(5) . 2_666 ? C4 Ru N5 86.7(5) 2_666 2_666 ? N4 Ru N5 89.4(5) . 2_666 ? N4 Ru N5 90.6(5) 2_666 2_666 ? C4 Ru N5 86.7(5) . . ? C4 Ru N5 93.3(5) 2_666 . ? N4 Ru N5 90.6(5) . . ? N4 Ru N5 89.4(5) 2_666 . ? N5 Ru N5 179.998(2) 2_666 . ? C4 Ru N5' 88.4(9) . 2_666 ? C4 Ru N5' 91.6(9) 2_666 2_666 ? N4' Ru N5' 89.7(11) 2_666 2_666 ? N4' Ru N5' 90.3(11) . 2_666 ? C4 Ru N5' 91.6(9) . . ? C4 Ru N5' 88.4(9) 2_666 . ? N4' Ru N5' 90.3(11) 2_666 . ? N4' Ru N5' 89.7(11) . . ? N5' Ru N5' 179.999(4) 2_666 . ? C1 Re C2 90.8(5) . . ? C1 Re C3 88.1(5) . . ? C2 Re C3 89.6(6) . . ? C1 Re N3 171.1(4) . . ? C2 Re N3 95.3(4) . . ? C3 Re N3 98.4(4) . . ? C1 Re N2 98.6(5) . . ? C2 Re N2 95.3(5) . . ? C3 Re N2 171.7(4) . . ? N3 Re N2 74.5(4) . . ? C1 Re N1 90.1(4) . . ? C2 Re N1 178.7(4) . . ? C3 Re N1 91.4(4) . . ? N3 Re N1 83.8(3) . . ? N2 Re N1 83.7(3) . . ? C8 N1 C9 116.3(8) . . ? C8 N1 Re 122.8(6) . . ? C9 N1 Re 120.4(6) . . ? C15 N2 C11 118.7(11) . . ? C15 N2 Re 116.7(8) . . ? C11 N2 Re 124.3(8) . . ? C20 N3 C16 117.7(10) . . ? C20 N3 Re 124.7(8) . . ? C16 N3 Re 117.6(7) . . ? O1 C1 Re 178.4(11) . . ? O2 C2 Re 178.0(14) . . ? O3 C3 Re 177.7(11) . . ? C5 C4 Ru 174.0(9) . . ? C4 C5 C6 172.9(11) . . ? C10 C6 C7 115.5(8) . . ? C10 C6 C5 122.5(9) . . ? C7 C6 C5 121.8(9) . . ? C8 C7 C6 120.3(9) . . ? N1 C8 C7 123.8(9) . . ? N1 C9 C10 122.0(9) . . ? C9 C10 C6 122.0(9) . . ? N2 C11 C12 121.6(13) . . ? C13 C12 C11 119.4(15) . . ? C14 C13 C12 119.4(16) . . ? C13 C14 C15 121.4(14) . . ? N2 C15 C14 119.4(12) . . ? N2 C15 C16 115.6(10) . . ? C14 C15 C16 125.0(11) . . ? N3 C16 C17 121.1(11) . . ? N3 C16 C15 115.5(10) . . ? C17 C16 C15 123.3(11) . . ? C18 C17 C16 120.2(12) . . ? C19 C18 C17 119.4(13) . . ? C18 C19 C20 118.2(13) . . ? N3 C20 C19 123.4(13) . . ? N4 C22 C21 111.4(16) . 2_666 ? N5' C22 C24' 110.4(30) 2_666 . ? N5' C22 C28' 50.4(19) 2_666 2_666 ? C24' C22 C28' 71.7(28) . 2_666 ? N4 C23 C24 117.9(14) . . ? C24' C23 N4' 114.9(28) . . ? N5 C25 C24 117.4(14) . . ? N4' C25 C21' 99.3(27) . . ? N5 C26 C21 115.7(15) . . ? N5' C26 C21' 103.5(30) . . ? N5' C26 C28' 47.4(17) . . ? C21' C26 C28' 148.9(32) . . ? C23 N4 C22 98.4(14) . . ? C23 N4 C27 106.5(14) . . ? C22 N4 C27 113.4(15) . . ? C23 N4 Ru 113.3(10) . . ? C22 N4 Ru 111.3(12) . . ? C27 N4 Ru 113.1(12) . . ? C25 N5 C28 110.6(14) . . ? C25 N5 C26 103.4(13) . . ? C28 N5 C26 109.1(14) . . ? C25 N5 Ru 113.5(11) . . ? C28 N5 Ru 112.2(12) . . ? C26 N5 Ru 107.6(10) . . ? C26 C21 C22 114.9(17) . 2_666 ? C25 C24 C23 112.7(18) . . ? C25 N4' C27' 112.6(22) . . ? C25 N4' C23 103.4(18) . . ? C27' N4' C23 105.1(21) . . ? C25 N4' Ru 115.4(15) . . ? C27' N4' Ru 112.7(20) . . ? C23 N4' Ru 106.4(13) . . ? C22 N5' C28' 82.3(27) 2_666 . ? C22 N5' C26 139.5(27) 2_666 . ? C28' N5' C26 79.7(26) . . ? C22 N5' Ru 115.3(22) 2_666 . ? C28' N5' Ru 116.3(26) . . ? C26 N5' Ru 105.2(19) . . ? C26 C21' C25 85.6(36) . . ? C23 C24' C22 86.7(35) . . ? N5' C28' C22 47.4(20) . 2_666 ? N5' C28' C26 52.9(21) . . ? C22 C28' C26 93.6(23) 2_666 . ? O6 S O4 118.2(8) . . ? O6 S O5 115.8(12) . . ? O4 S O5 113.6(8) . . ? O6 S C29 102.9(10) . . ? O4 S C29 100.7(12) . . ? O5 S C29 102.0(16) . . ? F3 C29 F2 111.4(21) . . ? F3 C29 F1 116.6(25) . . ? F2 C29 F1 114.7(29) . . ? F3 C29 S 109.9(23) . . ? F2 C29 S 110.4(19) . . ? F1 C29 S 92.2(19) . . ? C31 O7 C31 180.0 2_655 . ? C30 C31 O7 108.7(39) . . ? _refine_diff_density_max 1.492 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.160