# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pdm142 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Br N4 O4 Ru2' _chemical_formula_weight 818.67 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.203(2) _cell_length_b 14.203(2) _cell_length_c 7.6293(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1539.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6056 _exptl_absorpt_correction_T_max 0.8543 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6945 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.97 _reflns_number_total 916 _reflns_number_gt 829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The nitrogen and oxygen atoms are equally disordered over two sites by symmetry. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+8.6699P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 916 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.0000 1.0000 0.0000 0.0449(3) Uani 1 8 d S . . Ru1 Ru 1.0000 1.0000 0.34938(7) 0.0249(2) Uani 1 4 d S . . C1 C 0.8289(3) 0.9203(3) 0.5000 0.0309(10) Uani 1 2 d S . . C2 C 0.7366(4) 0.8700(4) 0.5000 0.0394(12) Uani 1 2 d S A . C3 C 0.7341(4) 0.7721(4) 0.5000 0.0450(14) Uani 1 2 d S . . C4 C 0.6474(5) 0.7272(5) 0.5000 0.0599(18) Uani 1 2 d S A . H4 H 0.6454 0.6618 0.5000 0.072 Uiso 1 2 calc SR . . C5 C 0.5647(5) 0.7769(6) 0.5000 0.079(3) Uani 1 2 d S . . H5 H 0.5073 0.7455 0.5000 0.095 Uiso 1 2 calc SR A . C6 C 0.5678(5) 0.8732(6) 0.5000 0.099(3) Uani 1 2 d S A . H6 H 0.5121 0.9076 0.5000 0.119 Uiso 1 2 calc SR . . C7 C 0.6537(5) 0.9197(6) 0.5000 0.099(3) Uani 1 2 d S . . H7 H 0.6552 0.9852 0.5000 0.119 Uiso 1 2 calc SR A . C8 C 0.8238(5) 0.7150(5) 0.5000 0.075(3) Uani 1 2 d S A . H8A H 0.8706 0.7465 0.4306 0.112 Uiso 0.50 1 calc PR . . H8B H 0.8116 0.6539 0.4513 0.112 Uiso 0.50 1 calc PR . . H8C H 0.8462 0.7083 0.6180 0.112 Uiso 0.50 1 calc PR . . N1 N 0.8685(2) 0.9410(2) 0.3533(3) 0.0344(6) Uani 0.50 1 d P A 1 H1 H 0.8395 0.9300 0.2564 0.041 Uiso 0.50 1 calc PR A 1 O1 O 0.8685(2) 0.9410(2) 0.3533(3) 0.0344(6) Uani 0.50 1 d P A 2 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 Br1 0.0513(5) 0.0513(5) 0.0320(6) 0.000 0.000 0.000 Ru1 0.0243(2) 0.0243(2) 0.0261(3) 0.000 0.000 0.000 C1 0.024(2) 0.026(2) 0.042(3) 0.000 0.000 -0.0016(18) C2 0.028(3) 0.038(3) 0.052(3) 0.000 0.000 -0.010(2) C3 0.039(3) 0.038(3) 0.059(4) 0.000 0.000 -0.009(2) C4 0.053(4) 0.040(3) 0.086(5) 0.000 0.000 -0.017(3) C5 0.037(4) 0.063(5) 0.139(8) 0.000 0.000 -0.024(3) C6 0.030(2) 0.050(3) 0.217(9) 0.000 0.000 -0.005(2) C7 0.030(2) 0.050(3) 0.217(9) 0.000 0.000 -0.005(2) C8 0.049(4) 0.037(3) 0.138(8) 0.000 0.000 0.003(3) N1 0.0297(14) 0.0397(16) 0.0336(15) -0.0018(11) -0.0027(11) -0.0052(12) O1 0.0297(14) 0.0397(16) 0.0336(15) -0.0018(11) -0.0027(11) -0.0052(12) _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 Br1 Ru1 2.6655(7) . ? Br1 Ru1 2.6655(7) 9_775 ? Ru1 O1 2.048(3) 3_755 ? Ru1 N1 2.048(3) 3_755 ? Ru1 N1 2.048(3) . ? Ru1 O1 2.048(3) 2_775 ? Ru1 N1 2.048(3) 2_775 ? Ru1 O1 2.048(3) 4_575 ? Ru1 N1 2.048(3) 4_575 ? Ru1 Ru1 2.2983(11) 9_776 ? C1 O1 1.286(4) 10_556 ? C1 N1 1.286(4) 10_556 ? C1 N1 1.286(4) . ? C1 C2 1.493(7) . ? C2 C7 1.373(9) . ? C2 C3 1.392(8) . ? C3 C4 1.387(9) . ? C3 C8 1.509(9) . ? C4 C5 1.370(11) . ? C4 H4 0.9300 . ? C5 C6 1.369(11) . ? C5 H5 0.9300 . ? C6 C7 1.388(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 H1 0.8600 . ? 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 Ru1 Br1 Ru1 180.0 . 9_775 ? O1 Ru1 N1 0.00(16) 3_755 3_755 ? O1 Ru1 N1 89.987(3) 3_755 . ? N1 Ru1 N1 89.987(3) 3_755 . ? O1 Ru1 O1 89.987(4) 3_755 2_775 ? N1 Ru1 O1 89.987(4) 3_755 2_775 ? N1 Ru1 O1 178.34(15) . 2_775 ? O1 Ru1 N1 89.987(4) 3_755 2_775 ? N1 Ru1 N1 89.987(4) 3_755 2_775 ? N1 Ru1 N1 178.34(15) . 2_775 ? O1 Ru1 N1 0.0(2) 2_775 2_775 ? O1 Ru1 O1 178.34(15) 3_755 4_575 ? N1 Ru1 O1 178.34(15) 3_755 4_575 ? N1 Ru1 O1 89.988(3) . 4_575 ? O1 Ru1 O1 89.990(3) 2_775 4_575 ? N1 Ru1 O1 89.990(3) 2_775 4_575 ? O1 Ru1 N1 178.34(15) 3_755 4_575 ? N1 Ru1 N1 178.34(15) 3_755 4_575 ? N1 Ru1 N1 89.988(3) . 4_575 ? O1 Ru1 N1 89.990(3) 2_775 4_575 ? N1 Ru1 N1 89.990(3) 2_775 4_575 ? O1 Ru1 N1 0.0(2) 4_575 4_575 ? O1 Ru1 Ru1 89.17(7) 3_755 9_776 ? N1 Ru1 Ru1 89.17(7) 3_755 9_776 ? N1 Ru1 Ru1 89.17(7) . 9_776 ? O1 Ru1 Ru1 89.17(7) 2_775 9_776 ? N1 Ru1 Ru1 89.17(7) 2_775 9_776 ? O1 Ru1 Ru1 89.17(7) 4_575 9_776 ? N1 Ru1 Ru1 89.17(7) 4_575 9_776 ? O1 Ru1 Br1 90.83(7) 3_755 . ? N1 Ru1 Br1 90.83(7) 3_755 . ? N1 Ru1 Br1 90.83(7) . . ? O1 Ru1 Br1 90.83(7) 2_775 . ? N1 Ru1 Br1 90.83(7) 2_775 . ? O1 Ru1 Br1 90.83(7) 4_575 . ? N1 Ru1 Br1 90.83(7) 4_575 . ? Ru1 Ru1 Br1 180.0 9_776 . ? O1 C1 N1 0.00(12) 10_556 10_556 ? O1 C1 N1 121.0(4) 10_556 . ? N1 C1 N1 121.0(4) 10_556 . ? O1 C1 C2 119.5(2) 10_556 . ? N1 C1 C2 119.5(2) 10_556 . ? N1 C1 C2 119.5(2) . . ? C7 C2 C3 119.5(6) . . ? C7 C2 C1 120.5(5) . . ? C3 C2 C1 120.0(5) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 C8 121.0(5) . . ? C4 C3 C8 120.1(6) . . ? C5 C4 C3 121.7(6) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 119.2(7) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 120.2(7) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 120.7(7) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 N1 Ru1 120.3(3) . . ? C1 N1 H1 119.9 . . ? Ru1 N1 H1 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru1 Br1 Ru1 O1 64(6) 9_775 . . 3_755 ? Ru1 Br1 Ru1 N1 64(6) 9_775 . . 3_755 ? Ru1 Br1 Ru1 N1 -26(6) 9_775 . . . ? Ru1 Br1 Ru1 O1 154(6) 9_775 . . 2_775 ? Ru1 Br1 Ru1 N1 154(6) 9_775 . . 2_775 ? Ru1 Br1 Ru1 O1 -116(6) 9_775 . . 4_575 ? Ru1 Br1 Ru1 N1 -116(6) 9_775 . . 4_575 ? Ru1 Br1 Ru1 Ru1 2(3) 9_775 . . 9_776 ? O1 C1 C2 C7 90.5(4) 10_556 . . . ? N1 C1 C2 C7 90.5(4) 10_556 . . . ? N1 C1 C2 C7 -90.5(4) . . . . ? O1 C1 C2 C3 -89.5(4) 10_556 . . . ? N1 C1 C2 C3 -89.5(4) 10_556 . . . ? N1 C1 C2 C3 89.5(4) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 180.0 . . . . ? C7 C2 C3 C8 180.0 . . . . ? C1 C2 C3 C8 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C8 C3 C4 C5 180.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 180.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? O1 C1 N1 Ru1 4.0(7) 10_556 . . . ? N1 C1 N1 Ru1 4.0(7) 10_556 . . . ? C2 C1 N1 Ru1 -174.9(3) . . . . ? O1 Ru1 N1 C1 87.2(3) 3_755 . . . ? N1 Ru1 N1 C1 87.2(3) 3_755 . . . ? O1 Ru1 N1 C1 -1.9(3) 2_775 . . . ? N1 Ru1 N1 C1 -1.9(3) 2_775 . . . ? O1 Ru1 N1 C1 -91.2(3) 4_575 . . . ? N1 Ru1 N1 C1 -91.2(3) 4_575 . . . ? Ru1 Ru1 N1 C1 -2.0(3) 9_776 . . . ? Br1 Ru1 N1 C1 178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.929 _refine_diff_density_min -2.016 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 952770' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pdm145 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Br N4 O4 Ru2' _chemical_formula_weight 818.67 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.082(2) _cell_length_b 11.138(2) _cell_length_c 22.418(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.86(3) _cell_angle_gamma 90.00 _cell_volume 3235.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6081 _exptl_absorpt_correction_T_max 0.7774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23913 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5699 _reflns_number_gt 2965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some of the C-atoms were refined using geometric restraints and variable common C-C distances. All the phenyl rings have been refined as rigid bodys. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+40.0959P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5699 _refine_ls_number_parameters 322 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1726 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.3303 _refine_ls_wR_factor_gt 0.2353 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br3 Br 0.25835(14) 0.33380(17) 0.03913(10) 0.0848(7) Uani 1 1 d . . . C1 C -0.0530(13) 0.4543(13) 0.1080(4) 0.059(4) Uani 1 1 d D . . C2 C -0.0864(10) 0.4236(12) 0.1675(4) 0.075(5) Uani 1 1 d GD . . C3 C -0.0245(9) 0.3500(12) 0.2075(6) 0.095(6) Uani 1 1 d G . . H3 H 0.0389 0.3236 0.1982 0.114 Uiso 1 1 calc R . . C4 C -0.0574(13) 0.3157(14) 0.2614(5) 0.132(10) Uani 1 1 d GD . . C5 C -0.1522(15) 0.3551(18) 0.2753(6) 0.174(15) Uani 1 1 d G . . H5 H -0.1742 0.3322 0.3113 0.209 Uiso 1 1 calc R . . C6 C -0.2140(11) 0.4287(17) 0.2353(7) 0.168(14) Uani 1 1 d G . . H6 H -0.2774 0.4551 0.2446 0.202 Uiso 1 1 calc R . . C7 C -0.1812(10) 0.4630(13) 0.1814(6) 0.109(7) Uani 1 1 d G . . H7 H -0.2226 0.5122 0.1547 0.131 Uiso 1 1 calc R . . C8 C 0.008(2) 0.231(3) 0.3049(12) 0.200(18) Uani 1 1 d D . . H8A H 0.0338 0.2729 0.3412 0.300 Uiso 1 1 calc R . . H8B H 0.0655 0.2015 0.2863 0.300 Uiso 1 1 calc R . . H8C H -0.0331 0.1639 0.3144 0.300 Uiso 1 1 calc R . . C9 C 0.0891(13) 0.7055(10) 0.0401(7) 0.063(4) Uani 1 1 d D . . C10 C 0.1465(11) 0.8177(9) 0.0601(8) 0.115(6) Uani 1 1 d GD . . C11 C 0.2506(10) 0.8175(9) 0.0833(6) 0.081(5) Uani 1 1 d G . . H11 H 0.2877 0.7461 0.0857 0.098 Uiso 1 1 calc R . . C12 C 0.2993(8) 0.9241(12) 0.1029(7) 0.101(7) Uani 1 1 d GD . . C13 C 0.2438(12) 1.0310(9) 0.0993(8) 0.139(12) Uani 1 1 d G . . H13 H 0.2764 1.1023 0.1124 0.167 Uiso 1 1 calc R . . C14 C 0.1397(12) 1.0311(9) 0.0761(8) 0.115(6) Uani 1 1 d G . . H14 H 0.1026 1.1026 0.0737 0.138 Uiso 1 1 calc R . . C15 C 0.0910(9) 0.9245(12) 0.0565(8) 0.157(13) Uani 1 1 d G . . H15 H 0.0214 0.9246 0.0410 0.188 Uiso 1 1 calc R . . C16 C 0.4130(12) 0.927(3) 0.1320(17) 0.207(18) Uani 1 1 d D . . H16A H 0.4284 0.8547 0.1551 0.311 Uiso 1 1 calc R . . H16B H 0.4245 0.9952 0.1580 0.311 Uiso 1 1 calc R . . H16C H 0.4569 0.9313 0.1011 0.311 Uiso 1 1 calc R . . C17 C 0.5255(14) 0.5906(15) 0.1117(5) 0.069(4) Uani 1 1 d D . . C18 C 0.5359(12) 0.6441(13) 0.1737(5) 0.088(6) Uani 1 1 d GD . . C19 C 0.6225(11) 0.7132(15) 0.1934(7) 0.115(8) Uani 1 1 d G . . H19 H 0.6729 0.7249 0.1685 0.137 Uiso 1 1 calc R . . C20 C 0.6336(14) 0.7650(16) 0.2503(8) 0.192(11) Uani 1 1 d GD . . C21 C 0.5583(18) 0.7475(18) 0.2876(5) 0.192(11) Uani 1 1 d G . . H21 H 0.5658 0.7821 0.3257 0.231 Uiso 1 1 calc R . . C22 C 0.4718(15) 0.6784(18) 0.2679(6) 0.167(13) Uani 1 1 d G . . H22 H 0.4214 0.6667 0.2929 0.200 Uiso 1 1 calc R . . C23 C 0.4606(11) 0.6267(15) 0.2110(7) 0.130(9) Uani 1 1 d G . . H23 H 0.4027 0.5804 0.1978 0.157 Uiso 1 1 calc R . . C24 C 0.7287(18) 0.842(3) 0.2736(13) 0.192(11) Uani 1 1 d D . . H24A H 0.7191 0.8778 0.3113 0.288 Uiso 1 1 calc R . . H24B H 0.7374 0.9033 0.2448 0.288 Uiso 1 1 calc R . . H24C H 0.7890 0.7915 0.2792 0.288 Uiso 1 1 calc R . . C25 C 0.6048(11) 0.3045(11) 0.0376(7) 0.063(4) Uani 1 1 d D . . C26 C 0.6564(10) 0.1880(9) 0.0577(7) 0.080(5) Uani 1 1 d GDU . . C27 C 0.7554(10) 0.1869(11) 0.0893(8) 0.119(7) Uani 1 1 d GU . . H27 H 0.7896 0.2588 0.0994 0.143 Uiso 1 1 calc R . . C28 C 0.8035(10) 0.0783(15) 0.1059(9) 0.156(10) Uani 1 1 d GDU . . C29 C 0.7525(14) -0.0292(11) 0.0908(11) 0.152(11) Uani 1 1 d GU . . H29 H 0.7846 -0.1019 0.1018 0.182 Uiso 1 1 calc R . . C30 C 0.6534(13) -0.0281(10) 0.0591(11) 0.176(16) Uani 1 1 d G . . H30 H 0.6193 -0.1001 0.0490 0.212 Uiso 1 1 calc R . . C31 C 0.6053(9) 0.0805(13) 0.0425(9) 0.163(14) Uani 1 1 d G . . H31 H 0.5391 0.0812 0.0214 0.195 Uiso 1 1 calc R . . C32 C 0.9139(19) 0.072(3) 0.140(2) 0.30(2) Uani 1 1 d DU . . H32A H 0.9238 -0.0041 0.1601 0.454 Uiso 1 1 calc R . . H32B H 0.9243 0.1357 0.1686 0.454 Uiso 1 1 calc R . . H32C H 0.9625 0.0794 0.1115 0.454 Uiso 1 1 calc R . . N1 N 0.1113(11) 0.4859(11) -0.0703(6) 0.064(3) Uani 1 1 d . . . H1 H 0.1683 0.4590 -0.0802 0.076 Uiso 1 1 calc R . . N2 N 0.0034(11) 0.2951(11) -0.0179(6) 0.067(4) Uani 1 1 d . . . H2 H 0.0374 0.2288 -0.0153 0.080 Uiso 1 1 calc R . . N4 N 0.4476(11) 0.5255(11) 0.0934(6) 0.064(3) Uani 1 1 d . . . H4 H 0.4032 0.5109 0.1174 0.077 Uiso 1 1 calc R . . N3 N 0.5067(9) 0.3039(10) 0.0371(5) 0.054(3) Uani 1 1 d . . . H3A H 0.4760 0.2417 0.0490 0.065 Uiso 1 1 calc R . . O1 O 0.0359(10) 0.4172(10) 0.0959(5) 0.075(3) Uani 1 1 d . . . O2 O 0.1458(8) 0.6061(10) 0.0429(5) 0.074(3) Uani 1 1 d . . . O3 O 0.3455(8) 0.6032(11) -0.0231(5) 0.081(4) Uani 1 1 d . . . O4 O 0.4063(10) 0.3849(11) -0.0776(6) 0.085(4) Uani 1 1 d . . . Ru1 Ru 0.07660(10) 0.44996(11) 0.01282(6) 0.0584(4) Uani 1 1 d . . . Ru2 Ru 0.42475(10) 0.45371(11) 0.00765(6) 0.0597(4) Uani 1 1 d . . . 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 Br3 0.0754(12) 0.0766(12) 0.1049(15) 0.0266(11) 0.0211(10) -0.0101(9) C1 0.078(11) 0.052(9) 0.044(8) 0.004(7) 0.003(8) -0.013(8) C2 0.103(14) 0.077(11) 0.051(10) 0.004(8) 0.027(9) -0.004(10) C3 0.127(17) 0.084(13) 0.080(13) 0.024(11) 0.034(12) 0.017(12) C4 0.19(3) 0.14(2) 0.080(16) 0.045(15) 0.048(17) 0.04(2) C5 0.23(4) 0.21(3) 0.10(2) 0.08(2) 0.11(2) 0.08(3) C6 0.20(3) 0.23(3) 0.100(19) 0.05(2) 0.10(2) 0.09(3) C7 0.118(18) 0.13(2) 0.086(15) 0.022(13) 0.040(13) 0.017(15) C8 0.27(4) 0.21(3) 0.14(3) 0.10(3) 0.09(3) 0.12(3) C9 0.097(14) 0.040(8) 0.052(9) -0.012(7) 0.014(9) -0.014(8) C10 0.137(14) 0.062(8) 0.132(14) 0.002(8) -0.030(11) -0.014(9) C11 0.100(14) 0.062(11) 0.087(13) -0.007(9) 0.032(11) -0.015(10) C12 0.118(17) 0.086(14) 0.098(15) -0.012(12) 0.010(13) -0.048(13) C13 0.16(2) 0.072(15) 0.16(2) 0.008(14) -0.06(2) -0.036(15) C14 0.137(14) 0.062(8) 0.132(14) 0.002(8) -0.030(11) -0.014(9) C15 0.17(3) 0.095(17) 0.18(3) 0.004(18) -0.07(2) -0.016(18) C16 0.14(3) 0.17(3) 0.30(5) -0.05(3) 0.00(3) -0.08(2) C17 0.077(12) 0.071(11) 0.061(11) 0.004(8) 0.020(9) -0.009(9) C18 0.103(15) 0.101(14) 0.055(11) -0.006(10) -0.010(11) 0.013(12) C19 0.109(17) 0.14(2) 0.091(15) -0.032(14) -0.014(13) 0.010(15) C20 0.25(3) 0.193(19) 0.113(16) -0.061(15) -0.051(15) 0.012(19) C21 0.25(3) 0.193(19) 0.113(16) -0.061(15) -0.051(15) 0.012(19) C22 0.25(4) 0.16(3) 0.083(18) -0.020(17) 0.01(2) 0.05(3) C23 0.16(2) 0.17(3) 0.067(14) -0.016(15) 0.030(15) 0.00(2) C24 0.25(3) 0.193(19) 0.113(16) -0.061(15) -0.051(15) 0.012(19) C25 0.046(9) 0.090(12) 0.053(9) 0.007(8) 0.005(7) 0.001(8) C26 0.074(11) 0.072(11) 0.100(14) 0.018(10) 0.032(10) 0.002(9) C27 0.078(13) 0.102(15) 0.170(19) -0.019(14) -0.009(13) 0.017(11) C28 0.099(16) 0.105(16) 0.25(2) -0.023(18) -0.035(17) 0.033(14) C29 0.108(18) 0.086(16) 0.26(3) 0.028(19) 0.01(2) 0.007(14) C30 0.12(2) 0.11(2) 0.29(5) 0.08(2) -0.02(3) -0.013(17) C31 0.13(2) 0.070(15) 0.28(4) 0.06(2) 0.03(2) 0.011(15) C32 0.20(3) 0.19(3) 0.47(6) -0.08(4) -0.14(4) 0.10(3) N1 0.078(9) 0.070(8) 0.049(7) 0.001(6) 0.029(7) -0.015(7) N2 0.079(9) 0.054(7) 0.065(9) 0.000(6) 0.003(7) -0.020(7) N4 0.079(9) 0.067(9) 0.052(8) 0.008(6) 0.025(7) -0.009(7) N3 0.053(8) 0.047(7) 0.059(7) 0.020(5) 0.001(6) -0.018(5) O1 0.085(8) 0.073(7) 0.064(7) 0.006(6) 0.002(6) -0.020(7) O2 0.071(7) 0.063(7) 0.084(8) 0.004(6) 0.000(6) -0.014(6) O3 0.066(7) 0.081(8) 0.099(9) 0.015(7) 0.025(6) -0.043(6) O4 0.097(9) 0.085(9) 0.071(8) -0.009(7) 0.002(7) -0.015(7) Ru1 0.0670(9) 0.0575(8) 0.0528(8) 0.0013(6) 0.0156(6) -0.0183(6) Ru2 0.0630(8) 0.0578(8) 0.0597(8) 0.0058(6) 0.0137(6) -0.0132(6) _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 Br3 Ru1 2.700(2) . ? Br3 Ru2 2.728(2) . ? C1 N1 1.250(18) 3_565 ? C1 O1 1.296(18) . ? C1 C2 1.500(5) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 C8 1.538(5) . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N2 1.245(19) 3_565 ? C9 O2 1.328(19) . ? C9 C10 1.495(5) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 C16 1.540(5) . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O4 1.281(19) 3_665 ? C17 N4 1.272(19) . ? C17 C18 1.501(5) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 C21 1.3900 . ? C20 C24 1.540(5) . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O3 1.281(17) 3_665 ? C25 N3 1.283(18) . ? C25 C26 1.503(5) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 C32 1.539(5) . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N1 C1 1.250(18) 3_565 ? N1 Ru1 2.018(12) . ? N1 H1 0.8600 . ? N2 C9 1.245(19) 3_565 ? N2 Ru1 2.045(12) . ? N2 H2 0.8600 . ? N4 Ru2 2.065(13) . ? N4 H4 0.8600 . ? N3 Ru2 2.044(11) . ? N3 H3A 0.8600 . ? O1 Ru1 2.040(12) . ? O2 Ru1 2.033(11) . ? O3 C25 1.281(17) 3_665 ? O3 Ru2 2.031(13) . ? O4 C17 1.281(19) 3_665 ? O4 Ru2 2.043(12) . ? Ru1 Ru1 2.297(3) 3_565 ? Ru2 Ru2 2.290(2) 3_665 ? 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 Ru1 Br3 Ru2 114.77(8) . . ? N1 C1 O1 120.8(10) 3_565 . ? N1 C1 C2 119.8(14) 3_565 . ? O1 C1 C2 119.5(13) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 119.6(11) . . ? C7 C2 C1 120.3(11) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C8 119.4(15) . . ? C3 C4 C8 120.5(15) . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 O2 121.4(10) 3_565 . ? N2 C9 C10 123.0(15) 3_565 . ? O2 C9 C10 115.4(14) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 122.5(12) . . ? C15 C10 C9 117.5(12) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 C16 121.5(15) . . ? C13 C12 C16 118.4(15) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 N4 121.4(11) 3_665 . ? O4 C17 C18 119.0(14) 3_665 . ? N4 C17 C18 119.6(14) . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 118.8(12) . . ? C23 C18 C17 121.2(12) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 C24 118.7(17) . . ? C19 C20 C24 121.3(17) . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 N3 123.0(11) 3_665 . ? O3 C25 C26 123.2(13) 3_665 . ? N3 C25 C26 113.9(12) . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 120.6(11) . . ? C31 C26 C25 119.4(11) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 C32 117.8(17) . . ? C27 C28 C32 122.2(18) . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1 Ru1 122.3(10) 3_565 . ? C1 N1 H1 118.8 3_565 . ? Ru1 N1 H1 118.8 . . ? C9 N2 Ru1 121.6(10) 3_565 . ? C9 N2 H2 119.2 3_565 . ? Ru1 N2 H2 119.2 . . ? C17 N4 Ru2 122.0(10) . . ? C17 N4 H4 119.0 . . ? Ru2 N4 H4 119.0 . . ? C25 N3 Ru2 118.5(8) . . ? C25 N3 H3A 120.7 . . ? Ru2 N3 H3A 120.7 . . ? C1 O1 Ru1 119.2(8) . . ? C9 O2 Ru1 118.5(8) . . ? C25 O3 Ru2 119.4(9) 3_665 . ? C17 O4 Ru2 118.4(9) 3_665 . ? N1 Ru1 O1 177.7(5) . . ? N1 Ru1 O2 89.4(5) . . ? O1 Ru1 O2 90.6(5) . . ? N1 Ru1 N2 90.6(5) . . ? O1 Ru1 N2 89.3(5) . . ? O2 Ru1 N2 178.5(5) . . ? N1 Ru1 Ru1 88.4(4) . 3_565 ? O1 Ru1 Ru1 89.3(4) . 3_565 ? O2 Ru1 Ru1 90.1(3) . 3_565 ? N2 Ru1 Ru1 88.5(4) . 3_565 ? N1 Ru1 Br3 89.6(4) . . ? O1 Ru1 Br3 92.7(4) . . ? O2 Ru1 Br3 89.9(3) . . ? N2 Ru1 Br3 91.5(4) . . ? Ru1 Ru1 Br3 178.02(10) 3_565 . ? O3 Ru2 O4 90.0(5) . . ? O3 Ru2 N3 178.7(5) . . ? O4 Ru2 N3 89.2(5) . . ? O3 Ru2 N4 90.1(5) . . ? O4 Ru2 N4 178.3(5) . . ? N3 Ru2 N4 90.7(5) . . ? O3 Ru2 Ru2 89.4(3) . 3_665 ? O4 Ru2 Ru2 91.3(4) . 3_665 ? N3 Ru2 Ru2 89.6(3) . 3_665 ? N4 Ru2 Ru2 87.0(4) . 3_665 ? O3 Ru2 Br3 95.8(3) . . ? O4 Ru2 Br3 93.6(4) . . ? N3 Ru2 Br3 85.3(3) . . ? N4 Ru2 Br3 88.2(4) . . ? Ru2 Ru2 Br3 172.89(10) 3_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 175.5(12) 3_565 . . . ? O1 C1 C2 C3 -3.7(18) . . . . ? N1 C1 C2 C7 -1.1(19) 3_565 . . . ? O1 C1 C2 C7 179.7(12) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 -176.6(14) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C2 C3 C4 C8 178(2) . . . . ? C3 C4 C5 C6 0.0 . . . . ? C8 C4 C5 C6 -178(2) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 176.5(14) . . . . ? N2 C9 C10 C11 -178.1(13) 3_565 . . . ? O2 C9 C10 C11 -4(2) . . . . ? N2 C9 C10 C15 4(2) 3_565 . . . ? O2 C9 C10 C15 178.3(11) . . . . ? C15 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C12 -178.1(16) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C16 177(2) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C16 C12 C13 C14 -177(2) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C9 C10 C15 C14 178.2(16) . . . . ? O4 C17 C18 C19 -3(2) 3_665 . . . ? N4 C17 C18 C19 178.8(13) . . . . ? O4 C17 C18 C23 175.8(13) 3_665 . . . ? N4 C17 C18 C23 -2(2) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C17 C18 C19 C20 179.3(14) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C18 C19 C20 C24 180(2) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C24 C20 C21 C22 -179.8(19) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C19 C18 C23 C22 0.0 . . . . ? C17 C18 C23 C22 -179.3(15) . . . . ? O3 C25 C26 C27 32(2) 3_665 . . . ? N3 C25 C26 C27 -147.0(13) . . . . ? O3 C25 C26 C31 -146.0(15) 3_665 . . . ? N3 C25 C26 C31 35.1(19) . . . . ? C31 C26 C27 C28 0.0 . . . . ? C25 C26 C27 C28 -177.8(16) . . . . ? C26 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C32 179(3) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C32 C28 C29 C30 -179(3) . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C26 0.0 . . . . ? C27 C26 C31 C30 0.0 . . . . ? C25 C26 C31 C30 177.9(15) . . . . ? O4 C17 N4 Ru2 0(2) 3_665 . . . ? C18 C17 N4 Ru2 177.7(11) . . . . ? O3 C25 N3 Ru2 4(2) 3_665 . . . ? C26 C25 N3 Ru2 -177.6(10) . . . . ? N1 C1 O1 Ru1 -3.2(19) 3_565 . . . ? C2 C1 O1 Ru1 176.0(9) . . . . ? N2 C9 O2 Ru1 -2(2) 3_565 . . . ? C10 C9 O2 Ru1 -177.0(11) . . . . ? C1 N1 Ru1 O1 3(12) 3_565 . . . ? C1 N1 Ru1 O2 -88.4(12) 3_565 . . . ? C1 N1 Ru1 N2 90.2(13) 3_565 . . . ? C1 N1 Ru1 Ru1 1.7(12) 3_565 . . 3_565 ? C1 N1 Ru1 Br3 -178.3(12) 3_565 . . . ? C1 O1 Ru1 N1 0(12) . . . . ? C1 O1 Ru1 O2 91.6(11) . . . . ? C1 O1 Ru1 N2 -87.0(11) . . . . ? C1 O1 Ru1 Ru1 1.5(10) . . . 3_565 ? C1 O1 Ru1 Br3 -178.5(10) . . . . ? C9 O2 Ru1 N1 89.4(12) . . . . ? C9 O2 Ru1 O1 -88.2(11) . . . . ? C9 O2 Ru1 N2 -3(20) . . . . ? C9 O2 Ru1 Ru1 1.1(11) . . . 3_565 ? C9 O2 Ru1 Br3 179.1(11) . . . . ? C9 N2 Ru1 N1 -86.9(13) 3_565 . . . ? C9 N2 Ru1 O1 90.7(13) 3_565 . . . ? C9 N2 Ru1 O2 5(20) 3_565 . . . ? C9 N2 Ru1 Ru1 1.4(13) 3_565 . . 3_565 ? C9 N2 Ru1 Br3 -176.6(13) 3_565 . . . ? Ru2 Br3 Ru1 N1 46.8(4) . . . . ? Ru2 Br3 Ru1 O1 -133.3(3) . . . . ? Ru2 Br3 Ru1 O2 -42.7(3) . . . . ? Ru2 Br3 Ru1 N2 137.4(4) . . . . ? Ru2 Br3 Ru1 Ru1 48(3) . . . 3_565 ? C25 O3 Ru2 O4 -94.2(12) 3_665 . . . ? C25 O3 Ru2 N3 -41(20) 3_665 . . . ? C25 O3 Ru2 N4 84.0(12) 3_665 . . . ? C25 O3 Ru2 Ru2 -2.9(12) 3_665 . . 3_665 ? C25 O3 Ru2 Br3 172.2(12) 3_665 . . . ? C17 O4 Ru2 O3 89.2(13) 3_665 . . . ? C17 O4 Ru2 N3 -89.7(13) 3_665 . . . ? C17 O4 Ru2 N4 -2(17) 3_665 . . . ? C17 O4 Ru2 Ru2 -0.2(13) 3_665 . . 3_665 ? C17 O4 Ru2 Br3 -175.0(13) 3_665 . . . ? C25 N3 Ru2 O3 38(20) . . . . ? C25 N3 Ru2 O4 90.4(12) . . . . ? C25 N3 Ru2 N4 -87.9(12) . . . . ? C25 N3 Ru2 Ru2 -0.9(11) . . . 3_665 ? C25 N3 Ru2 Br3 -176.0(12) . . . . ? C17 N4 Ru2 O3 -89.4(13) . . . . ? C17 N4 Ru2 O4 2(17) . . . . ? C17 N4 Ru2 N3 89.5(13) . . . . ? C17 N4 Ru2 Ru2 0.0(13) . . . 3_665 ? C17 N4 Ru2 Br3 174.8(13) . . . . ? Ru1 Br3 Ru2 O3 2.8(4) . . . . ? Ru1 Br3 Ru2 O4 -87.6(4) . . . . ? Ru1 Br3 Ru2 N3 -176.5(3) . . . . ? Ru1 Br3 Ru2 N4 92.7(4) . . . . ? Ru1 Br3 Ru2 Ru2 139.4(8) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.942 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.307 _vrf_PLAT220_pdm145 ; Due to the low quality of the data collected, reflected in a poor final model. ; _vrf_PLAT342_pdm145 ; Due to the low quality of the data collected, reflected in a poor final model. ; _database_code_depnum_ccdc_archive 'CCDC 952771' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3-pdm126 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Br N4 O4 Ru2' _chemical_formula_weight 818.67 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.942(6) _cell_length_b 10.424(2) _cell_length_c 13.010(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.32(3) _cell_angle_gamma 90.00 _cell_volume 3355.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6514 _exptl_absorpt_correction_T_max 0.7994 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14504 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3669 _reflns_number_gt 2297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+16.0446P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3669 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.0000 0.30578(10) 0.7500 0.0577(3) Uani 1 2 d S . . C1 C 0.1020(3) 0.5729(6) 0.6253(5) 0.0446(16) Uani 1 1 d . . . C2 C 0.1572(3) 0.6200(7) 0.6963(6) 0.0523(18) Uani 1 1 d . . . C3 C 0.1819(4) 0.7092(10) 0.6562(8) 0.080(3) Uani 1 1 d . . . H3 H 0.1646 0.7370 0.5826 0.096 Uiso 1 1 calc R . . C4 C 0.2321(4) 0.7600(12) 0.7221(10) 0.099(4) Uani 1 1 d . . . H4 H 0.2475 0.8215 0.6920 0.118 Uiso 1 1 calc R . . C5 C 0.2594(4) 0.7214(11) 0.8303(8) 0.078(3) Uani 1 1 d . . . C6 C 0.2354(4) 0.6300(11) 0.8694(8) 0.086(3) Uani 1 1 d . . . H6 H 0.2536 0.6006 0.9423 0.103 Uiso 1 1 calc R . . C7 C 0.1847(4) 0.5779(9) 0.8051(7) 0.074(2) Uani 1 1 d . . . H7 H 0.1696 0.5157 0.8351 0.088 Uiso 1 1 calc R . . C8 C 0.3133(4) 0.7797(13) 0.9034(10) 0.119(5) Uani 1 1 d . . . H8A H 0.3078 0.8464 0.9487 0.178 Uiso 1 1 calc R . . H8B H 0.3301 0.8151 0.8571 0.178 Uiso 1 1 calc R . . H8C H 0.3362 0.7146 0.9509 0.178 Uiso 1 1 calc R . . C9 C 0.0367(2) 0.2896(6) 0.4340(5) 0.0371(14) Uani 1 1 d . . . C10 C 0.0591(3) 0.1744(7) 0.4011(5) 0.0433(15) Uani 1 1 d . . . C11 C 0.0799(3) 0.1822(8) 0.3192(6) 0.060(2) Uani 1 1 d . . . H11 H 0.0783 0.2591 0.2818 0.072 Uiso 1 1 calc R . . C12 C 0.1032(4) 0.0749(9) 0.2934(8) 0.074(3) Uani 1 1 d . . . H12 H 0.1163 0.0815 0.2375 0.089 Uiso 1 1 calc R . . C13 C 0.1076(4) -0.0406(8) 0.3468(8) 0.068(2) Uani 1 1 d . . . C14 C 0.0843(4) -0.0481(8) 0.4257(8) 0.071(2) Uani 1 1 d . . . H14 H 0.0845 -0.1259 0.4608 0.085 Uiso 1 1 calc R . . C15 C 0.0611(3) 0.0571(7) 0.4520(7) 0.060(2) Uani 1 1 d . . . H15 H 0.0464 0.0493 0.5055 0.072 Uiso 1 1 calc R . . C16 C 0.1341(5) -0.1546(10) 0.3184(10) 0.110(4) Uani 1 1 d . . . H16A H 0.1132 -0.1809 0.2428 0.165 Uiso 1 1 calc R . . H16B H 0.1362 -0.2239 0.3685 0.165 Uiso 1 1 calc R . . H16C H 0.1699 -0.1316 0.3259 0.165 Uiso 1 1 calc R . . N1 N 0.0753(2) 0.5005(5) 0.6665(4) 0.0407(12) Uani 1 1 d . . . H1 H 0.0906 0.4757 0.7350 0.049 Uiso 1 1 calc R . . N2 N 0.0255(2) 0.2859(4) 0.5209(4) 0.0366(12) Uani 1 1 d . . . H2 H 0.0297 0.2152 0.5576 0.044 Uiso 1 1 calc R . . O1 O -0.0799(2) 0.3894(5) 0.4777(4) 0.0544(12) Uani 1 1 d . . . O2 O -0.0300(2) 0.6052(5) 0.6218(4) 0.0586(14) Uani 1 1 d . . . Ru1 Ru -0.00206(2) 0.44334(5) 0.57406(4) 0.0383(2) Uani 1 1 d . . . 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 Br1 0.0976(9) 0.0466(6) 0.0386(5) 0.000 0.0372(6) 0.000 C1 0.050(4) 0.045(4) 0.037(3) -0.004(3) 0.015(3) 0.005(3) C2 0.050(4) 0.061(5) 0.042(4) -0.005(3) 0.014(3) 0.003(4) C3 0.062(6) 0.112(8) 0.057(5) 0.015(5) 0.012(4) -0.020(5) C4 0.064(6) 0.129(9) 0.096(8) 0.004(7) 0.025(6) -0.034(6) C5 0.050(5) 0.113(8) 0.070(6) -0.010(6) 0.023(5) -0.002(5) C6 0.065(6) 0.118(9) 0.056(5) 0.001(6) 0.003(5) 0.003(6) C7 0.061(5) 0.092(7) 0.057(5) 0.009(5) 0.012(4) -0.002(5) C8 0.055(6) 0.184(13) 0.103(9) -0.035(9) 0.016(6) -0.023(7) C9 0.033(3) 0.040(4) 0.037(3) 0.000(3) 0.012(3) 0.008(3) C10 0.044(4) 0.047(4) 0.037(3) -0.003(3) 0.015(3) 0.005(3) C11 0.082(6) 0.052(4) 0.058(5) 0.004(4) 0.041(4) 0.007(4) C12 0.096(7) 0.073(6) 0.076(6) -0.005(5) 0.057(6) 0.009(5) C13 0.071(6) 0.055(5) 0.082(6) -0.013(4) 0.035(5) 0.007(4) C14 0.099(7) 0.039(4) 0.083(6) 0.004(4) 0.045(6) 0.014(4) C15 0.082(6) 0.048(4) 0.063(5) 0.003(4) 0.043(5) 0.006(4) C16 0.123(10) 0.088(8) 0.143(10) -0.020(7) 0.080(9) 0.036(7) N1 0.045(3) 0.044(3) 0.027(3) 0.007(2) 0.008(2) -0.001(3) N2 0.059(3) 0.024(2) 0.033(3) 0.0064(19) 0.024(3) 0.004(2) O1 0.061(3) 0.061(3) 0.041(3) 0.006(2) 0.019(2) 0.000(3) O2 0.088(4) 0.051(3) 0.040(3) 0.009(2) 0.029(3) 0.014(3) Ru1 0.0495(3) 0.0394(3) 0.0256(3) 0.0011(2) 0.0144(2) 0.0013(2) _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 Br1 Ru1 2.6829(8) . ? Br1 Ru1 2.6830(8) 2_556 ? C1 N1 1.296(8) . ? C1 O1 1.293(8) 5_566 ? C1 C2 1.490(10) . ? C2 C3 1.362(11) . ? C2 C7 1.383(11) . ? C3 C4 1.388(13) . ? C4 C5 1.365(14) . ? C5 C6 1.357(14) . ? C5 C8 1.513(13) . ? C6 C7 1.400(12) . ? C9 N2 1.282(8) . ? C9 O2 1.288(8) 5_566 ? C9 C10 1.481(9) . ? C10 C15 1.382(10) . ? C10 C11 1.389(9) . ? C11 C12 1.386(11) . ? C12 C13 1.370(12) . ? C13 C14 1.402(12) . ? C13 C16 1.507(11) . ? C14 C15 1.370(10) . ? N1 Ru1 2.039(5) . ? N2 Ru1 2.032(5) . ? O1 C1 1.293(8) 5_566 ? O1 Ru1 2.051(5) . ? O2 C9 1.288(8) 5_566 ? O2 Ru1 2.041(5) . ? Ru1 Ru1 2.3000(10) 5_566 ? 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 Ru1 Br1 Ru1 115.39(4) . 2_556 ? N1 C1 O1 120.2(6) . 5_566 ? N1 C1 C2 121.2(6) . . ? O1 C1 C2 118.6(6) 5_566 . ? C3 C2 C7 117.6(8) . . ? C3 C2 C1 120.5(7) . . ? C7 C2 C1 121.8(8) . . ? C2 C3 C4 121.9(9) . . ? C5 C4 C3 121.3(10) . . ? C6 C5 C4 116.8(9) . . ? C6 C5 C8 121.8(10) . . ? C4 C5 C8 121.4(10) . . ? C5 C6 C7 123.0(9) . . ? C2 C7 C6 119.3(9) . . ? N2 C9 O2 119.6(5) . 5_566 ? N2 C9 C10 119.7(6) . . ? O2 C9 C10 120.7(6) 5_566 . ? C15 C10 C11 117.9(7) . . ? C15 C10 C9 121.5(6) . . ? C11 C10 C9 120.6(6) . . ? C12 C11 C10 119.8(7) . . ? C13 C12 C11 122.9(8) . . ? C12 C13 C14 116.4(7) . . ? C12 C13 C16 121.6(9) . . ? C14 C13 C16 121.9(8) . . ? C15 C14 C13 121.3(8) . . ? C14 C15 C10 121.6(7) . . ? C1 N1 Ru1 122.1(4) . . ? C9 N2 Ru1 121.4(4) . . ? C1 O1 Ru1 119.3(5) 5_566 . ? C9 O2 Ru1 121.3(4) 5_566 . ? N2 Ru1 O2 177.75(18) . . ? N2 Ru1 N1 90.6(2) . . ? O2 Ru1 N1 89.6(2) . . ? N2 Ru1 O1 89.6(2) . . ? O2 Ru1 O1 90.1(2) . . ? N1 Ru1 O1 178.40(19) . . ? N2 Ru1 Ru1 89.13(13) . 5_566 ? O2 Ru1 Ru1 88.64(13) . 5_566 ? N1 Ru1 Ru1 88.12(14) . 5_566 ? O1 Ru1 Ru1 90.31(13) . 5_566 ? N2 Ru1 Br1 88.36(13) . . ? O2 Ru1 Br1 93.88(13) . . ? N1 Ru1 Br1 88.96(14) . . ? O1 Ru1 Br1 92.63(13) . . ? Ru1 Ru1 Br1 176.13(4) 5_566 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -171.3(8) . . . . ? O1 C1 C2 C3 5.5(11) 5_566 . . . ? N1 C1 C2 C7 7.1(11) . . . . ? O1 C1 C2 C7 -176.0(7) 5_566 . . . ? C7 C2 C3 C4 -1.9(15) . . . . ? C1 C2 C3 C4 176.6(9) . . . . ? C2 C3 C4 C5 0.7(18) . . . . ? C3 C4 C5 C6 1.0(18) . . . . ? C3 C4 C5 C8 -178.0(11) . . . . ? C4 C5 C6 C7 -1.5(16) . . . . ? C8 C5 C6 C7 177.5(10) . . . . ? C3 C2 C7 C6 1.4(14) . . . . ? C1 C2 C7 C6 -177.1(8) . . . . ? C5 C6 C7 C2 0.4(15) . . . . ? N2 C9 C10 C15 9.4(10) . . . . ? O2 C9 C10 C15 -172.8(7) 5_566 . . . ? N2 C9 C10 C11 -169.1(7) . . . . ? O2 C9 C10 C11 8.7(10) 5_566 . . . ? C15 C10 C11 C12 -1.8(12) . . . . ? C9 C10 C11 C12 176.8(8) . . . . ? C10 C11 C12 C13 -1.1(14) . . . . ? C11 C12 C13 C14 3.7(15) . . . . ? C11 C12 C13 C16 -178.7(10) . . . . ? C12 C13 C14 C15 -3.6(14) . . . . ? C16 C13 C14 C15 178.8(10) . . . . ? C13 C14 C15 C10 0.9(14) . . . . ? C11 C10 C15 C14 1.9(12) . . . . ? C9 C10 C15 C14 -176.7(8) . . . . ? O1 C1 N1 Ru1 -0.6(9) 5_566 . . . ? C2 C1 N1 Ru1 176.2(5) . . . . ? O2 C9 N2 Ru1 -0.6(9) 5_566 . . . ? C10 C9 N2 Ru1 177.2(4) . . . . ? C9 N2 Ru1 O2 8(6) . . . . ? C9 N2 Ru1 N1 -87.5(5) . . . . ? C9 N2 Ru1 O1 90.9(5) . . . . ? C9 N2 Ru1 Ru1 0.6(5) . . . 5_566 ? C9 N2 Ru1 Br1 -176.5(5) . . . . ? C9 O2 Ru1 N2 -7(6) 5_566 . . . ? C9 O2 Ru1 N1 88.0(5) 5_566 . . . ? C9 O2 Ru1 O1 -90.4(5) 5_566 . . . ? C9 O2 Ru1 Ru1 -0.1(5) 5_566 . . 5_566 ? C9 O2 Ru1 Br1 176.9(5) 5_566 . . . ? C1 N1 Ru1 N2 89.1(5) . . . . ? C1 N1 Ru1 O2 -88.7(5) . . . . ? C1 N1 Ru1 O1 -11(8) . . . . ? C1 N1 Ru1 Ru1 0.0(5) . . . 5_566 ? C1 N1 Ru1 Br1 177.5(5) . . . . ? C1 O1 Ru1 N2 -88.4(5) 5_566 . . . ? C1 O1 Ru1 O2 89.4(5) 5_566 . . . ? C1 O1 Ru1 N1 11(8) 5_566 . . . ? C1 O1 Ru1 Ru1 0.7(5) 5_566 . . 5_566 ? C1 O1 Ru1 Br1 -176.8(5) 5_566 . . . ? Ru1 Br1 Ru1 N2 159.73(15) 2_556 . . . ? Ru1 Br1 Ru1 O2 -20.44(16) 2_556 . . . ? Ru1 Br1 Ru1 N1 69.08(15) 2_556 . . . ? Ru1 Br1 Ru1 O1 -110.70(15) 2_556 . . . ? Ru1 Br1 Ru1 Ru1 110.1(6) 2_556 . . 5_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.017 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 952772' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3pdm121 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 I N4 O4 Ru2' _chemical_formula_weight 865.66 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 11.8852(7) _cell_length_b 13.4489(8) _cell_length_c 20.6974(12) _cell_angle_alpha 94.4770(10) _cell_angle_beta 94.7350(10) _cell_angle_gamma 90.3450(10) _cell_volume 3286.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4064 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.58 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7637 _exptl_absorpt_correction_T_max 0.9279 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25323 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11265 _reflns_number_gt 6817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.8283P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11265 _refine_ls_number_parameters 764 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3806(6) 0.5202(6) 0.1038(3) 0.0376(19) Uani 1 1 d . . . C2 C 0.3216(7) 0.5368(6) 0.1652(3) 0.044(2) Uani 1 1 d . . . C3 C 0.3540(8) 0.6112(6) 0.2109(4) 0.057(2) Uani 1 1 d . . . C4 C 0.2983(9) 0.6197(8) 0.2677(5) 0.082(3) Uani 1 1 d . . . H4 H 0.3160 0.6726 0.2986 0.099 Uiso 1 1 calc R . . C5 C 0.2194(10) 0.5524(8) 0.2782(5) 0.081(3) Uani 1 1 d . . . H5 H 0.1844 0.5583 0.3168 0.097 Uiso 1 1 calc R . . C6 C 0.1901(9) 0.4763(8) 0.2335(5) 0.091(4) Uani 1 1 d . . . H6 H 0.1359 0.4298 0.2416 0.110 Uiso 1 1 calc R . . C7 C 0.2409(8) 0.4675(7) 0.1755(5) 0.074(3) Uani 1 1 d . . . H7 H 0.2209 0.4157 0.1442 0.089 Uiso 1 1 calc R . . C8 C 0.4559(9) 0.6793(7) 0.2038(5) 0.090(3) Uani 1 1 d . . . H8A H 0.5228 0.6400 0.2020 0.135 Uiso 1 1 calc R . . H8B H 0.4649 0.7280 0.2404 0.135 Uiso 1 1 calc R . . H8C H 0.4435 0.7126 0.1645 0.135 Uiso 1 1 calc R . . C9 C 0.6659(6) 0.6034(6) 0.0692(3) 0.0330(18) Uani 1 1 d . . . C10 C 0.7595(7) 0.6593(6) 0.1106(4) 0.045(2) Uani 1 1 d . . . C11 C 0.8684(8) 0.6240(7) 0.1170(5) 0.063(3) Uani 1 1 d . . . C12 C 0.9488(9) 0.6768(9) 0.1613(6) 0.096(4) Uani 1 1 d . . . H12 H 1.0229 0.6548 0.1653 0.115 Uiso 1 1 calc R . . C13 C 0.9195(12) 0.7591(10) 0.1977(7) 0.117(5) Uani 1 1 d . . . H13 H 0.9732 0.7922 0.2271 0.141 Uiso 1 1 calc R . . C14 C 0.8108(10) 0.7942(8) 0.1918(5) 0.094(4) Uani 1 1 d . . . H14 H 0.7906 0.8508 0.2168 0.113 Uiso 1 1 calc R . . C15 C 0.7328(8) 0.7438(6) 0.1480(4) 0.066(3) Uani 1 1 d . . . H15 H 0.6595 0.7676 0.1435 0.079 Uiso 1 1 calc R . . C16 C 0.9057(8) 0.5341(8) 0.0758(5) 0.100(4) Uani 1 1 d . . . H16A H 0.8871 0.4743 0.0953 0.150 Uiso 1 1 calc R . . H16B H 0.9858 0.5377 0.0730 0.150 Uiso 1 1 calc R . . H16C H 0.8677 0.5331 0.0329 0.150 Uiso 1 1 calc R . . C17 C 0.2995(6) 0.0888(6) 0.0041(4) 0.042(2) Uani 1 1 d . . . C18 C 0.1900(7) 0.1361(6) 0.0133(4) 0.052(2) Uani 1 1 d . . . C19 C 0.1748(9) 0.1920(7) 0.0729(6) 0.077(3) Uani 1 1 d . . . C20 C 0.0709(12) 0.2373(9) 0.0796(7) 0.106(4) Uani 1 1 d . . . H20 H 0.0590 0.2757 0.1178 0.127 Uiso 1 1 calc R . . C21 C -0.0131(11) 0.2261(11) 0.0310(9) 0.119(5) Uani 1 1 d . . . H21 H -0.0821 0.2564 0.0366 0.143 Uiso 1 1 calc R . . C22 C 0.0020(10) 0.1700(11) -0.0271(8) 0.120(5) Uani 1 1 d . . . H22 H -0.0557 0.1645 -0.0605 0.144 Uiso 1 1 calc R . . C23 C 0.1038(9) 0.1224(8) -0.0347(6) 0.089(3) Uani 1 1 d . . . H23 H 0.1133 0.0814 -0.0721 0.106 Uiso 1 1 calc R . . C24 C 0.2655(10) 0.2037(9) 0.1288(5) 0.124(5) Uani 1 1 d . . . H24A H 0.2990 0.1401 0.1354 0.185 Uiso 1 1 calc R . . H24B H 0.2326 0.2286 0.1676 0.185 Uiso 1 1 calc R . . H24C H 0.3224 0.2498 0.1188 0.185 Uiso 1 1 calc R . . C25 C 0.5248(7) 0.0353(6) -0.1224(4) 0.044(2) Uani 1 1 d . . . C26 C 0.5452(9) 0.0496(6) -0.1920(4) 0.057(2) Uani 1 1 d . . . C27 C 0.6529(11) 0.0790(8) -0.2076(5) 0.084(4) Uani 1 1 d . . . C28 C 0.6653(15) 0.0897(9) -0.2735(6) 0.133(6) Uani 1 1 d . . . H28 H 0.7360 0.1080 -0.2852 0.159 Uiso 1 1 calc R . . C29 C 0.5819(16) 0.0752(10) -0.3202(7) 0.133(6) Uani 1 1 d . . . H29 H 0.5947 0.0835 -0.3631 0.159 Uiso 1 1 calc R . . C30 C 0.4758(13) 0.0475(8) -0.3045(5) 0.121(5) Uani 1 1 d . . . H30 H 0.4166 0.0392 -0.3369 0.145 Uiso 1 1 calc R . . C31 C 0.4573(10) 0.0319(6) -0.2389(4) 0.077(3) Uani 1 1 d . . . H31 H 0.3873 0.0101 -0.2280 0.092 Uiso 1 1 calc R . . C32 C 0.7512(10) 0.0985(10) -0.1591(7) 0.133(5) Uani 1 1 d . . . H32A H 0.8066 0.0478 -0.1654 0.199 Uiso 1 1 calc R . . H32B H 0.7268 0.0978 -0.1160 0.199 Uiso 1 1 calc R . . H32C H 0.7838 0.1626 -0.1643 0.199 Uiso 1 1 calc R . . C33 C 0.0520(6) 0.9509(6) 0.6209(3) 0.0327(18) Uani 1 1 d . . . C34 C 0.0845(7) 0.9254(5) 0.6895(3) 0.0364(18) Uani 1 1 d . . . C35 C 0.1776(8) 0.8665(6) 0.7049(4) 0.052(2) Uani 1 1 d . . . C36 C 0.1997(8) 0.8471(8) 0.7704(5) 0.077(3) Uani 1 1 d . . . H36 H 0.2615 0.8084 0.7821 0.093 Uiso 1 1 calc R . . C37 C 0.1336(9) 0.8830(8) 0.8172(5) 0.079(3) Uani 1 1 d . . . H37 H 0.1501 0.8682 0.8600 0.095 Uiso 1 1 calc R . . C38 C 0.0425(8) 0.9411(7) 0.8013(4) 0.068(3) Uani 1 1 d . . . H38 H -0.0025 0.9661 0.8334 0.081 Uiso 1 1 calc R . . C39 C 0.0184(7) 0.9621(6) 0.7380(4) 0.054(2) Uani 1 1 d . . . H39 H -0.0432 1.0017 0.7273 0.065 Uiso 1 1 calc R . . C40 C 0.2556(8) 0.8226(8) 0.6553(5) 0.089(3) Uani 1 1 d . . . H40A H 0.2182 0.7676 0.6297 0.134 Uiso 1 1 calc R . . H40B H 0.3235 0.7999 0.6776 0.134 Uiso 1 1 calc R . . H40C H 0.2742 0.8729 0.6273 0.134 Uiso 1 1 calc R . . C41 C 0.2054(7) 1.0884(6) 0.5095(3) 0.0389(19) Uani 1 1 d . . . C42 C 0.3172(7) 1.1366(6) 0.5207(4) 0.048(2) Uani 1 1 d . . . C43 C 0.3452(8) 1.2079(6) 0.5732(4) 0.059(2) Uani 1 1 d . . . C44 C 0.4533(10) 1.2509(8) 0.5775(6) 0.090(4) Uani 1 1 d . . . H44 H 0.4731 1.2997 0.6109 0.108 Uiso 1 1 calc R . . C45 C 0.5298(10) 1.2241(10) 0.5350(8) 0.107(5) Uani 1 1 d . . . H45 H 0.6016 1.2529 0.5410 0.128 Uiso 1 1 calc R . . C46 C 0.5047(9) 1.1566(10) 0.4841(7) 0.099(4) Uani 1 1 d . . . H46 H 0.5573 1.1403 0.4542 0.119 Uiso 1 1 calc R . . C47 C 0.3956(8) 1.1112(7) 0.4773(5) 0.068(3) Uani 1 1 d . . . H47 H 0.3771 1.0636 0.4430 0.081 Uiso 1 1 calc R . . C48 C 0.2651(9) 1.2360(8) 0.6229(5) 0.093(4) Uani 1 1 d . . . H48A H 0.2163 1.2876 0.6079 0.140 Uiso 1 1 calc R . . H48B H 0.3068 1.2600 0.6629 0.140 Uiso 1 1 calc R . . H48C H 0.2206 1.1788 0.6301 0.140 Uiso 1 1 calc R . . C49 C 0.1566(6) 0.5184(6) 0.6002(3) 0.0364(18) Uani 1 1 d . . . C50 C 0.2422(6) 0.5313(6) 0.6570(3) 0.042(2) Uani 1 1 d . . . C51 C 0.2109(8) 0.5531(7) 0.7189(4) 0.063(3) Uani 1 1 d . . . C56 C 0.0893(9) 0.5668(10) 0.7313(5) 0.119(5) Uani 1 1 d . . . H56A H 0.0531 0.6059 0.6989 0.179 Uiso 1 1 calc R . . H56B H 0.0844 0.6006 0.7736 0.179 Uiso 1 1 calc R . . H56C H 0.0524 0.5028 0.7294 0.179 Uiso 1 1 calc R . . C52 C 0.2924(10) 0.5640(8) 0.7695(4) 0.083(3) Uani 1 1 d . . . H52 H 0.2712 0.5767 0.8116 0.100 Uiso 1 1 calc R . . C53 C 0.4035(10) 0.5567(8) 0.7597(5) 0.083(3) Uani 1 1 d . . . H53 H 0.4578 0.5692 0.7945 0.100 Uiso 1 1 calc R . . C54 C 0.4361(8) 0.5309(8) 0.6984(5) 0.089(4) Uani 1 1 d . . . H54 H 0.5115 0.5198 0.6917 0.107 Uiso 1 1 calc R . . C55 C 0.3524(7) 0.5217(7) 0.6464(4) 0.062(3) Uani 1 1 d . . . H55 H 0.3729 0.5088 0.6042 0.074 Uiso 1 1 calc R . . C57 C 0.1376(6) 0.3860(5) 0.4312(3) 0.0307(17) Uani 1 1 d . . . C58 C 0.2138(6) 0.3234(5) 0.3928(3) 0.0387(19) Uani 1 1 d . . . C59 C 0.3294(7) 0.3464(6) 0.3966(4) 0.050(2) Uani 1 1 d . . . C60 C 0.3946(8) 0.2841(7) 0.3581(4) 0.065(3) Uani 1 1 d . . . H60 H 0.4721 0.2960 0.3606 0.078 Uiso 1 1 calc R . . C61 C 0.3510(9) 0.2060(7) 0.3166(5) 0.076(3) Uani 1 1 d . . . H61 H 0.3973 0.1675 0.2908 0.091 Uiso 1 1 calc R . . C62 C 0.2380(9) 0.1864(7) 0.3144(5) 0.079(3) Uani 1 1 d . . . H62 H 0.2063 0.1342 0.2865 0.095 Uiso 1 1 calc R . . C63 C 0.1712(7) 0.2431(6) 0.3529(4) 0.055(2) Uani 1 1 d . . . H63 H 0.0948 0.2270 0.3521 0.066 Uiso 1 1 calc R . . C64 C 0.3819(7) 0.4289(7) 0.4418(4) 0.075(3) Uani 1 1 d . . . H64A H 0.4612 0.4171 0.4499 0.113 Uiso 1 1 calc R . . H64B H 0.3470 0.4314 0.4822 0.113 Uiso 1 1 calc R . . H64C H 0.3712 0.4912 0.4226 0.113 Uiso 1 1 calc R . . I1 I 0.65651(4) 0.25725(4) 0.06500(2) 0.04408(15) Uani 1 1 d . . . I2 I 0.13265(4) 0.74404(3) 0.42506(2) 0.04075(15) Uani 1 1 d . . . O1 O 0.4429(4) 0.4429(4) 0.0980(2) 0.0404(13) Uani 1 1 d . . . O2 O 0.6619(4) 0.5093(4) 0.0729(2) 0.0409(13) Uani 1 1 d . . . O3 O 0.3884(4) 0.1434(4) 0.0135(2) 0.0441(13) Uani 1 1 d . . . O4 O 0.5546(4) 0.1056(4) -0.0795(2) 0.0461(14) Uani 1 1 d . . . O5 O 0.0684(4) 0.8855(3) 0.5743(2) 0.0423(13) Uani 1 1 d . . . O6 O -0.1181(4) 0.8576(4) 0.4784(2) 0.0418(13) Uani 1 1 d . . . O7 O 0.1592(4) 0.5795(4) 0.5544(2) 0.0489(14) Uani 1 1 d . . . O8 O 0.1398(4) 0.4800(3) 0.4256(2) 0.0353(12) Uani 1 1 d . . . N1 N 0.6277(5) 0.4171(4) -0.0592(3) 0.0360(11) Uani 1 1 d . . . H1 H 0.6741 0.3686 -0.0631 0.043 Uiso 1 1 calc R . . N2 N 0.4069(5) 0.3513(4) -0.0324(3) 0.0360(11) Uani 1 1 d . . . H2 H 0.4004 0.2880 -0.0298 0.043 Uiso 1 1 calc R . . N3 N 0.6927(5) 0.0062(5) 0.0118(3) 0.0440(17) Uani 1 1 d . . . H3 H 0.7539 0.0406 0.0213 0.053 Uiso 1 1 calc R . . N4 N 0.5247(5) 0.0459(4) 0.1082(3) 0.0454(17) Uani 1 1 d . . . H4A H 0.5506 0.0880 0.1393 0.054 Uiso 1 1 calc R . . N5 N -0.0062(5) 0.9657(4) 0.3906(3) 0.0349(15) Uani 1 1 d . . . H5A H 0.0072 0.9250 0.3580 0.042 Uiso 1 1 calc R . . N6 N 0.1892(5) 0.9949(4) 0.4895(3) 0.0395(16) Uani 1 1 d . . . H6A H 0.2468 0.9607 0.4791 0.047 Uiso 1 1 calc R . . N7 N -0.0679(5) 0.6529(4) 0.5315(3) 0.0366(15) Uani 1 1 d . . . H7A H -0.0668 0.7165 0.5295 0.044 Uiso 1 1 calc R . . N8 N -0.0828(4) 0.5514(4) 0.4031(2) 0.0243(13) Uani 1 1 d . . . H8 H -0.0840 0.5919 0.3729 0.029 Uiso 1 1 calc R . . Ru1 Ru 0.53659(5) 0.42810(4) 0.01942(3) 0.03012(16) Uani 1 1 d . . . Ru2 Ru 0.54280(5) 0.07654(4) 0.01528(3) 0.03689(17) Uani 1 1 d . . . Ru3 Ru 0.03650(5) 0.92469(4) 0.48143(3) 0.03294(16) Uani 1 1 d . . . Ru4 Ru 0.03739(5) 0.56832(4) 0.47849(3) 0.02685(15) Uani 1 1 d . . . 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 C1 0.043(5) 0.037(5) 0.033(4) 0.001(4) 0.004(4) -0.002(4) C2 0.052(5) 0.052(5) 0.033(4) 0.013(4) 0.018(4) 0.019(4) C3 0.077(7) 0.049(6) 0.046(5) 0.000(4) 0.023(5) 0.002(5) C4 0.108(9) 0.079(8) 0.063(7) -0.009(6) 0.041(6) 0.017(7) C5 0.106(9) 0.087(9) 0.057(7) 0.016(6) 0.041(6) 0.023(7) C6 0.100(9) 0.093(9) 0.091(8) 0.012(7) 0.066(7) -0.006(7) C7 0.073(7) 0.072(7) 0.080(7) -0.008(6) 0.045(6) -0.019(6) C8 0.116(9) 0.068(7) 0.086(8) -0.010(6) 0.025(7) -0.002(7) C9 0.039(5) 0.038(5) 0.022(4) 0.003(3) 0.000(3) 0.001(4) C10 0.049(6) 0.041(5) 0.047(5) 0.004(4) 0.009(4) -0.003(4) C11 0.047(6) 0.059(6) 0.081(7) 0.007(5) -0.007(5) -0.006(5) C12 0.057(7) 0.095(9) 0.129(10) 0.022(8) -0.041(7) -0.013(7) C13 0.098(11) 0.103(11) 0.140(12) -0.024(9) -0.024(9) -0.042(9) C14 0.093(9) 0.095(9) 0.085(8) -0.043(7) 0.004(7) -0.035(8) C15 0.059(6) 0.060(6) 0.074(6) -0.008(5) -0.015(5) -0.007(5) C16 0.054(7) 0.099(9) 0.140(10) -0.022(8) -0.004(7) 0.018(6) C17 0.033(5) 0.039(5) 0.058(5) 0.019(4) 0.003(4) 0.004(4) C18 0.042(6) 0.048(6) 0.070(6) 0.022(5) 0.018(5) 0.008(4) C19 0.067(7) 0.064(7) 0.106(9) 0.013(6) 0.039(7) 0.025(6) C20 0.101(10) 0.087(9) 0.141(12) 0.024(9) 0.059(10) 0.032(9) C21 0.050(8) 0.124(13) 0.190(17) 0.024(12) 0.035(10) 0.018(8) C22 0.053(8) 0.133(13) 0.172(14) 0.019(11) -0.018(9) 0.018(8) C23 0.047(7) 0.096(9) 0.121(10) 0.018(7) -0.014(7) 0.010(6) C24 0.129(12) 0.143(12) 0.093(9) -0.027(8) 0.013(9) 0.036(10) C25 0.051(5) 0.036(5) 0.045(5) 0.009(4) 0.000(4) 0.014(4) C26 0.094(8) 0.037(5) 0.042(5) 0.015(4) 0.007(5) 0.013(5) C27 0.122(11) 0.071(7) 0.072(7) 0.040(6) 0.048(7) 0.036(7) C28 0.262(19) 0.076(6) 0.076(8) 0.035(7) 0.073(9) 0.063(9) C29 0.262(19) 0.076(6) 0.076(8) 0.035(7) 0.073(9) 0.063(9) C30 0.233(17) 0.069(8) 0.053(8) -0.005(6) -0.031(9) 0.038(10) C31 0.140(10) 0.059(6) 0.031(5) 0.007(5) -0.001(6) 0.008(6) C32 0.069(9) 0.176(15) 0.163(14) 0.041(11) 0.043(9) 0.013(9) C33 0.035(5) 0.037(5) 0.027(4) 0.011(4) -0.003(3) -0.010(4) C34 0.047(5) 0.028(4) 0.035(4) 0.007(3) 0.001(4) 0.001(4) C35 0.065(6) 0.044(5) 0.049(5) 0.012(4) 0.004(5) 0.005(5) C36 0.069(7) 0.102(9) 0.060(7) 0.023(6) -0.015(6) 0.028(6) C37 0.098(9) 0.098(9) 0.044(6) 0.025(6) -0.005(6) 0.017(7) C38 0.074(7) 0.089(8) 0.041(6) 0.007(5) 0.007(5) 0.008(6) C39 0.049(6) 0.062(6) 0.051(6) 0.012(5) 0.000(5) 0.001(5) C40 0.070(7) 0.111(9) 0.087(8) 0.012(7) -0.001(6) 0.027(7) C41 0.039(5) 0.035(5) 0.044(5) 0.014(4) 0.001(4) 0.000(4) C42 0.040(5) 0.038(5) 0.069(6) 0.025(4) -0.001(5) 0.004(4) C43 0.064(7) 0.042(5) 0.069(6) 0.013(5) -0.010(5) 0.000(5) C44 0.064(8) 0.071(8) 0.129(11) 0.005(7) -0.026(7) -0.022(7) C45 0.057(8) 0.104(11) 0.159(14) 0.047(10) -0.022(9) -0.023(8) C46 0.056(8) 0.109(11) 0.143(12) 0.055(9) 0.024(8) 0.010(7) C47 0.053(6) 0.076(7) 0.075(7) 0.016(6) 0.007(5) -0.008(5) C48 0.089(8) 0.088(8) 0.092(8) -0.026(7) -0.029(7) 0.009(7) C49 0.036(5) 0.044(5) 0.029(4) 0.003(4) 0.004(4) 0.003(4) C50 0.040(5) 0.050(5) 0.035(5) 0.009(4) -0.012(4) -0.010(4) C51 0.054(6) 0.097(8) 0.036(5) 0.011(5) -0.010(5) -0.005(5) C56 0.094(9) 0.203(14) 0.057(7) -0.036(8) 0.032(6) -0.009(9) C52 0.088(8) 0.120(10) 0.039(6) 0.012(6) -0.015(6) -0.011(8) C53 0.096(9) 0.096(8) 0.052(7) 0.011(6) -0.039(6) -0.017(7) C54 0.052(7) 0.130(10) 0.082(8) 0.023(7) -0.027(6) 0.011(7) C55 0.041(6) 0.094(8) 0.049(5) 0.015(5) -0.011(4) -0.001(5) C57 0.032(4) 0.026(4) 0.035(4) 0.002(3) 0.006(3) 0.000(3) C58 0.047(5) 0.033(4) 0.039(4) 0.009(4) 0.018(4) 0.003(4) C59 0.049(6) 0.048(5) 0.056(5) 0.008(4) 0.017(4) 0.002(4) C60 0.053(6) 0.065(7) 0.079(7) 0.001(6) 0.022(5) 0.008(5) C61 0.092(9) 0.061(7) 0.080(7) 0.000(6) 0.044(7) 0.023(6) C62 0.097(9) 0.058(6) 0.081(7) -0.031(5) 0.033(7) -0.008(6) C63 0.047(5) 0.048(5) 0.070(6) -0.009(5) 0.014(5) -0.005(4) C64 0.050(6) 0.084(7) 0.086(7) -0.025(6) 0.002(5) -0.007(5) I1 0.0467(3) 0.0319(3) 0.0516(3) 0.0080(2) -0.0126(3) 0.0036(2) I2 0.0465(3) 0.0286(3) 0.0501(3) 0.0064(2) 0.0185(3) 0.0002(2) O1 0.049(3) 0.042(3) 0.033(3) 0.012(2) 0.012(2) 0.011(3) O2 0.051(3) 0.034(3) 0.036(3) 0.008(2) -0.007(2) 0.002(3) O3 0.042(3) 0.036(3) 0.055(3) 0.010(3) 0.000(3) 0.006(3) O4 0.059(4) 0.034(3) 0.045(3) 0.009(3) 0.003(3) -0.003(3) O5 0.052(3) 0.032(3) 0.043(3) 0.006(3) -0.002(3) 0.002(3) O6 0.046(3) 0.031(3) 0.048(3) 0.006(2) 0.001(3) -0.006(3) O7 0.053(4) 0.052(4) 0.042(3) 0.012(3) -0.001(3) -0.005(3) O8 0.044(3) 0.027(3) 0.038(3) 0.008(2) 0.016(2) -0.001(2) N1 0.044(3) 0.031(3) 0.034(2) 0.012(2) 0.003(2) 0.009(2) N2 0.044(3) 0.031(3) 0.034(2) 0.012(2) 0.003(2) 0.009(2) N3 0.038(4) 0.037(4) 0.057(4) 0.013(3) -0.005(3) 0.001(3) N4 0.068(5) 0.031(4) 0.036(4) 0.005(3) -0.009(3) -0.003(4) N5 0.039(4) 0.031(4) 0.034(3) 0.005(3) 0.003(3) 0.006(3) N6 0.043(4) 0.027(4) 0.050(4) 0.006(3) 0.006(3) 0.001(3) N7 0.040(4) 0.022(3) 0.050(4) 0.006(3) 0.018(3) -0.004(3) N8 0.029(3) 0.025(3) 0.021(3) 0.017(2) -0.003(2) -0.005(3) Ru1 0.0373(4) 0.0291(3) 0.0245(3) 0.0061(3) 0.0011(3) 0.0060(3) Ru2 0.0419(4) 0.0295(4) 0.0397(4) 0.0088(3) -0.0004(3) 0.0015(3) Ru3 0.0387(4) 0.0252(3) 0.0360(4) 0.0079(3) 0.0040(3) 0.0011(3) Ru4 0.0295(3) 0.0247(3) 0.0269(3) 0.0058(2) 0.0028(3) -0.0030(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.284(8) . ? C1 N1 1.297(8) 2_665 ? C1 C2 1.503(9) . ? C2 C3 1.354(10) . ? C2 C7 1.374(11) . ? C3 C4 1.393(11) . ? C3 C8 1.537(12) . ? C4 C5 1.341(13) . ? C4 H4 0.9300 . ? C5 C6 1.349(13) . ? C5 H5 0.9300 . ? C6 C7 1.384(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O2 1.275(8) . ? C9 N2 1.293(8) 2_665 ? C9 C10 1.507(10) . ? C10 C11 1.381(11) . ? C10 C15 1.378(11) . ? C11 C12 1.415(12) . ? C11 C16 1.516(12) . ? C12 C13 1.354(15) . ? C12 H12 0.9300 . ? C13 C14 1.377(15) . ? C13 H13 0.9300 . ? C14 C15 1.379(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O3 1.276(8) . ? C17 N3 1.299(9) 2_655 ? C17 C18 1.472(10) . ? C18 C23 1.369(12) . ? C18 C19 1.419(12) . ? C19 C20 1.393(13) . ? C19 C24 1.512(14) . ? C20 C21 1.356(16) . ? C20 H20 0.9300 . ? C21 C22 1.395(17) . ? C21 H21 0.9300 . ? C22 C23 1.387(14) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O4 1.273(8) . ? C25 N4 1.303(9) 2_655 ? C25 C26 1.507(11) . ? C26 C31 1.372(12) . ? C26 C27 1.407(13) . ? C27 C28 1.401(13) . ? C27 C32 1.486(14) . ? C28 C29 1.33(2) . ? C28 H28 0.9300 . ? C29 C30 1.383(18) . ? C29 H29 0.9300 . ? C30 C31 1.427(13) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N5 1.280(8) 2_576 ? C33 O5 1.282(8) . ? C33 C34 1.506(9) . ? C34 C35 1.394(10) . ? C34 C39 1.388(10) . ? C35 C36 1.404(11) . ? C35 C40 1.528(11) . ? C36 C37 1.358(12) . ? C36 H36 0.9300 . ? C37 C38 1.371(12) . ? C37 H37 0.9300 . ? C38 C39 1.371(11) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O6 1.299(8) 2_576 ? C41 N6 1.301(8) . ? C41 C42 1.468(10) . ? C42 C47 1.373(11) . ? C42 C43 1.409(11) . ? C43 C44 1.399(12) . ? C43 C48 1.488(12) . ? C44 C45 1.348(15) . ? C44 H44 0.9300 . ? C45 C46 1.349(16) . ? C45 H45 0.9300 . ? C46 C47 1.422(13) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 N8 1.275(8) 2_566 ? C49 O7 1.304(8) . ? C49 C50 1.489(9) . ? C50 C51 1.374(10) . ? C50 C55 1.351(10) . ? C51 C52 1.364(11) . ? C51 C56 1.499(12) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C52 C53 1.355(13) . ? C52 H52 0.9300 . ? C53 C54 1.377(13) . ? C53 H53 0.9300 . ? C54 C55 1.401(11) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C57 O8 1.278(7) . ? C57 N7 1.311(8) 2_566 ? C57 C58 1.478(9) . ? C58 C63 1.374(10) . ? C58 C59 1.402(10) . ? C59 C60 1.394(11) . ? C59 C64 1.494(10) . ? C60 C61 1.373(12) . ? C60 H60 0.9300 . ? C61 C62 1.363(12) . ? C61 H61 0.9300 . ? C62 C63 1.366(11) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? I1 Ru2 2.8517(8) . ? I1 Ru1 2.8908(8) . ? I2 Ru3 2.8950(8) . ? I2 Ru4 2.9447(7) . ? O1 Ru1 2.045(4) . ? O2 Ru1 2.038(5) . ? O3 Ru2 2.048(5) . ? O4 Ru2 2.045(5) . ? O5 Ru3 2.039(5) . ? O6 C41 1.299(8) 2_576 ? O6 Ru3 2.037(5) . ? O7 Ru4 2.042(5) . ? O8 Ru4 2.031(4) . ? N1 C1 1.297(8) 2_665 ? N1 Ru1 2.024(6) . ? N1 H1 0.8600 . ? N2 C9 1.293(8) 2_665 ? N2 Ru1 2.032(6) . ? N2 H2 0.8600 . ? N3 C17 1.299(9) 2_655 ? N3 Ru2 2.027(6) . ? N3 H3 0.8600 . ? N4 C25 1.303(9) 2_655 ? N4 Ru2 2.026(6) . ? N4 H4A 0.8600 . ? N5 C33 1.280(8) 2_576 ? N5 Ru3 2.027(6) . ? N5 H5A 0.8600 . ? N6 Ru3 2.029(6) . ? N6 H6A 0.8600 . ? N7 C57 1.311(8) 2_566 ? N7 Ru4 2.028(5) . ? N7 H7A 0.8600 . ? N8 C49 1.275(8) 2_566 ? N8 Ru4 2.024(5) . ? N8 H8 0.8600 . ? Ru1 Ru1 2.3001(11) 2_665 ? Ru2 Ru2 2.3106(12) 2_655 ? Ru3 Ru3 2.3097(12) 2_576 ? Ru4 Ru4 2.3079(10) 2_566 ? 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 O1 C1 N1 120.9(7) . 2_665 ? O1 C1 C2 117.4(7) . . ? N1 C1 C2 121.7(7) 2_665 . ? C3 C2 C7 121.5(7) . . ? C3 C2 C1 121.3(7) . . ? C7 C2 C1 116.9(7) . . ? C2 C3 C4 118.1(9) . . ? C2 C3 C8 121.5(8) . . ? C4 C3 C8 120.1(8) . . ? C5 C4 C3 120.7(10) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.9(10) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 120.0(10) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 118.6(9) . . ? C6 C7 H7 120.7 . . ? C2 C7 H7 120.7 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 N2 122.0(6) . 2_665 ? O2 C9 C10 116.4(7) . . ? N2 C9 C10 121.6(7) 2_665 . ? C11 C10 C15 118.9(8) . . ? C11 C10 C9 122.4(7) . . ? C15 C10 C9 118.4(8) . . ? C10 C11 C12 118.7(9) . . ? C10 C11 C16 122.1(8) . . ? C12 C11 C16 119.2(9) . . ? C13 C12 C11 120.9(11) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.6(11) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 118.5(11) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C10 122.4(10) . . ? C14 C15 H15 118.8 . . ? C10 C15 H15 118.8 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 N3 120.1(7) . 2_655 ? O3 C17 C18 118.1(7) . . ? N3 C17 C18 121.8(7) 2_655 . ? C23 C18 C19 121.3(9) . . ? C23 C18 C17 119.4(9) . . ? C19 C18 C17 119.2(9) . . ? C18 C19 C20 117.8(11) . . ? C18 C19 C24 123.0(9) . . ? C20 C19 C24 119.2(11) . . ? C21 C20 C19 120.6(13) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 121.3(13) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 119.4(13) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C18 C23 C22 119.5(12) . . ? C18 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 N4 122.2(7) . 2_655 ? O4 C25 C26 117.9(7) . . ? N4 C25 C26 119.9(7) 2_655 . ? C31 C26 C27 121.8(9) . . ? C31 C26 C25 118.3(9) . . ? C27 C26 C25 119.9(9) . . ? C28 C27 C26 116.5(13) . . ? C28 C27 C32 119.5(13) . . ? C26 C27 C32 124.0(9) . . ? C29 C28 C27 123.7(17) . . ? C29 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? C28 C29 C30 119.7(14) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C31 120.0(13) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C26 C31 C30 118.3(11) . . ? C26 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 O5 120.7(6) 2_576 . ? N5 C33 C34 121.1(7) 2_576 . ? O5 C33 C34 118.1(7) . . ? C35 C34 C39 120.0(7) . . ? C35 C34 C33 122.0(7) . . ? C39 C34 C33 118.0(7) . . ? C34 C35 C36 117.1(8) . . ? C34 C35 C40 124.1(8) . . ? C36 C35 C40 118.8(9) . . ? C37 C36 C35 122.1(9) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C38 120.2(9) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 119.5(9) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C34 121.1(8) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O6 C41 N6 118.5(7) 2_576 . ? O6 C41 C42 117.7(7) 2_576 . ? N6 C41 C42 123.8(8) . . ? C47 C42 C43 119.8(8) . . ? C47 C42 C41 117.9(8) . . ? C43 C42 C41 122.3(8) . . ? C42 C43 C44 117.0(10) . . ? C42 C43 C48 122.2(8) . . ? C44 C43 C48 120.7(9) . . ? C45 C44 C43 122.4(11) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? C44 C45 C46 121.6(12) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C45 C46 C47 118.1(12) . . ? C45 C46 H46 120.9 . . ? C47 C46 H46 120.9 . . ? C42 C47 C46 121.0(10) . . ? C42 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N8 C49 O7 121.2(6) 2_566 . ? N8 C49 C50 120.1(7) 2_566 . ? O7 C49 C50 118.7(6) . . ? C51 C50 C55 120.3(7) . . ? C51 C50 C49 121.3(7) . . ? C55 C50 C49 118.4(7) . . ? C50 C51 C52 119.2(9) . . ? C50 C51 C56 121.0(8) . . ? C52 C51 C56 119.9(9) . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C52 C51 121.5(10) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 120.1(9) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 118.2(10) . . ? C55 C54 H54 120.9 . . ? C53 C54 H54 120.9 . . ? C50 C55 C54 120.6(9) . . ? C50 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? O8 C57 N7 120.7(6) . 2_566 ? O8 C57 C58 117.6(6) . . ? N7 C57 C58 121.7(6) 2_566 . ? C63 C58 C59 119.9(7) . . ? C63 C58 C57 120.1(7) . . ? C59 C58 C57 120.0(7) . . ? C60 C59 C58 116.1(7) . . ? C60 C59 C64 121.4(8) . . ? C58 C59 C64 122.5(7) . . ? C59 C60 C61 123.8(9) . . ? C59 C60 H60 118.1 . . ? C61 C60 H60 118.1 . . ? C62 C61 C60 118.2(9) . . ? C62 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? C61 C62 C63 120.2(9) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C58 C63 C62 121.7(8) . . ? C58 C63 H63 119.1 . . ? C62 C63 H63 119.1 . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Ru2 I1 Ru1 110.67(2) . . ? Ru3 I2 Ru4 110.16(2) . . ? C1 O1 Ru1 117.4(4) . . ? C9 O2 Ru1 119.0(4) . . ? C17 O3 Ru2 118.8(5) . . ? C25 O4 Ru2 116.5(5) . . ? C33 O5 Ru3 117.9(4) . . ? C41 O6 Ru3 119.2(4) 2_576 . ? C49 O7 Ru4 119.4(4) . . ? C57 O8 Ru4 118.6(4) . . ? C1 N1 Ru1 123.1(5) 2_665 . ? C1 N1 H1 118.5 2_665 . ? Ru1 N1 H1 118.5 . . ? C9 N2 Ru1 120.6(5) 2_665 . ? C9 N2 H2 119.7 2_665 . ? Ru1 N2 H2 119.7 . . ? C17 N3 Ru2 122.8(5) 2_655 . ? C17 N3 H3 118.6 2_655 . ? Ru2 N3 H3 118.6 . . ? C25 N4 Ru2 122.4(5) 2_655 . ? C25 N4 H4A 118.8 2_655 . ? Ru2 N4 H4A 118.8 . . ? C33 N5 Ru3 123.4(5) 2_576 . ? C33 N5 H5A 118.3 2_576 . ? Ru3 N5 H5A 118.3 . . ? C41 N6 Ru3 124.1(5) . . ? C41 N6 H6A 118.0 . . ? Ru3 N6 H6A 118.0 . . ? C57 N7 Ru4 122.3(5) 2_566 . ? C57 N7 H7A 118.8 2_566 . ? Ru4 N7 H7A 118.8 . . ? C49 N8 Ru4 121.0(5) 2_566 . ? C49 N8 H8 119.5 2_566 . ? Ru4 N8 H8 119.5 . . ? N1 Ru1 O2 91.4(2) . . ? N1 Ru1 O1 178.4(2) . . ? O2 Ru1 O1 88.49(19) . . ? N1 Ru1 N2 90.3(2) . . ? O2 Ru1 N2 177.6(2) . . ? O1 Ru1 N2 89.8(2) . . ? N1 Ru1 Ru1 86.81(17) . 2_665 ? O2 Ru1 Ru1 90.07(14) . 2_665 ? O1 Ru1 Ru1 91.60(14) . 2_665 ? N2 Ru1 Ru1 88.35(17) . 2_665 ? N1 Ru1 I1 88.14(17) . . ? O2 Ru1 I1 84.73(14) . . ? O1 Ru1 I1 93.43(14) . . ? N2 Ru1 I1 97.00(16) . . ? Ru1 Ru1 I1 172.66(4) 2_665 . ? N3 Ru2 N4 93.8(2) . . ? N3 Ru2 O4 87.7(2) . . ? N4 Ru2 O4 177.7(2) . . ? N3 Ru2 O3 176.6(2) . . ? N4 Ru2 O3 88.5(2) . . ? O4 Ru2 O3 89.9(2) . . ? N3 Ru2 Ru2 87.24(17) . 2_655 ? N4 Ru2 Ru2 86.51(17) . 2_655 ? O4 Ru2 Ru2 91.89(14) . 2_655 ? O3 Ru2 Ru2 90.47(14) . 2_655 ? N3 Ru2 I1 90.37(17) . . ? N4 Ru2 I1 88.37(17) . . ? O4 Ru2 I1 93.31(14) . . ? O3 Ru2 I1 92.14(14) . . ? Ru2 Ru2 I1 174.19(4) 2_655 . ? N6 Ru3 O6 176.8(2) . . ? N6 Ru3 N5 94.2(2) . . ? O6 Ru3 N5 88.1(2) . . ? N6 Ru3 O5 88.8(2) . . ? O6 Ru3 O5 88.85(19) . . ? N5 Ru3 O5 176.1(2) . . ? N6 Ru3 Ru3 86.77(17) . 2_576 ? O6 Ru3 Ru3 91.07(15) . 2_576 ? N5 Ru3 Ru3 86.54(17) . 2_576 ? O5 Ru3 Ru3 91.04(14) . 2_576 ? N6 Ru3 I2 91.17(17) . . ? O6 Ru3 I2 91.17(15) . . ? N5 Ru3 I2 89.17(17) . . ? O5 Ru3 I2 93.38(14) . . ? Ru3 Ru3 I2 175.09(4) 2_576 . ? O8 Ru4 N7 178.26(19) . . ? O8 Ru4 O7 89.9(2) . . ? N7 Ru4 O7 90.6(2) . . ? O8 Ru4 N8 88.71(19) . . ? N7 Ru4 N8 90.7(2) . . ? O7 Ru4 N8 177.8(2) . . ? O8 Ru4 Ru4 91.35(13) . 2_566 ? N7 Ru4 Ru4 87.02(15) . 2_566 ? O7 Ru4 Ru4 89.07(15) . 2_566 ? N8 Ru4 Ru4 89.22(14) . 2_566 ? O8 Ru4 I2 89.20(12) . . ? N7 Ru4 I2 92.44(15) . . ? O7 Ru4 I2 90.54(14) . . ? N8 Ru4 I2 91.19(14) . . ? Ru4 Ru4 I2 179.33(4) 2_566 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 108.7(9) . . . . ? N1 C1 C2 C3 -69.1(11) 2_665 . . . ? O1 C1 C2 C7 -65.2(10) . . . . ? N1 C1 C2 C7 117.0(9) 2_665 . . . ? C7 C2 C3 C4 -4.0(14) . . . . ? C1 C2 C3 C4 -177.5(8) . . . . ? C7 C2 C3 C8 170.9(9) . . . . ? C1 C2 C3 C8 -2.7(13) . . . . ? C2 C3 C4 C5 3.9(16) . . . . ? C8 C3 C4 C5 -171.0(10) . . . . ? C3 C4 C5 C6 -1.6(18) . . . . ? C4 C5 C6 C7 -0.7(18) . . . . ? C5 C6 C7 C2 0.6(17) . . . . ? C3 C2 C7 C6 1.8(15) . . . . ? C1 C2 C7 C6 175.6(9) . . . . ? O2 C9 C10 C11 42.2(10) . . . . ? N2 C9 C10 C11 -138.5(8) 2_665 . . . ? O2 C9 C10 C15 -131.6(8) . . . . ? N2 C9 C10 C15 47.8(10) 2_665 . . . ? C15 C10 C11 C12 -0.8(13) . . . . ? C9 C10 C11 C12 -174.6(8) . . . . ? C15 C10 C11 C16 -177.6(9) . . . . ? C9 C10 C11 C16 8.7(13) . . . . ? C10 C11 C12 C13 1.5(17) . . . . ? C16 C11 C12 C13 178.3(11) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C10 0.6(17) . . . . ? C11 C10 C15 C14 -0.2(14) . . . . ? C9 C10 C15 C14 173.8(8) . . . . ? O3 C17 C18 C23 128.7(9) . . . . ? N3 C17 C18 C23 -52.7(12) 2_655 . . . ? O3 C17 C18 C19 -53.6(11) . . . . ? N3 C17 C18 C19 125.0(9) 2_655 . . . ? C23 C18 C19 C20 -3.5(14) . . . . ? C17 C18 C19 C20 178.9(8) . . . . ? C23 C18 C19 C24 176.1(10) . . . . ? C17 C18 C19 C24 -1.5(14) . . . . ? C18 C19 C20 C21 1.3(17) . . . . ? C24 C19 C20 C21 -178.3(12) . . . . ? C19 C20 C21 C22 -1(2) . . . . ? C20 C21 C22 C23 2(2) . . . . ? C19 C18 C23 C22 4.8(15) . . . . ? C17 C18 C23 C22 -177.6(9) . . . . ? C21 C22 C23 C18 -3.9(19) . . . . ? O4 C25 C26 C31 -129.8(8) . . . . ? N4 C25 C26 C31 48.4(11) 2_655 . . . ? O4 C25 C26 C27 51.2(11) . . . . ? N4 C25 C26 C27 -130.7(9) 2_655 . . . ? C31 C26 C27 C28 0.4(14) . . . . ? C25 C26 C27 C28 179.4(8) . . . . ? C31 C26 C27 C32 -179.6(10) . . . . ? C25 C26 C27 C32 -0.6(15) . . . . ? C26 C27 C28 C29 1.0(18) . . . . ? C32 C27 C28 C29 -179.1(13) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C28 C29 C30 C31 -2(2) . . . . ? C27 C26 C31 C30 -2.4(14) . . . . ? C25 C26 C31 C30 178.6(8) . . . . ? C29 C30 C31 C26 3.2(16) . . . . ? N5 C33 C34 C35 -147.6(7) 2_576 . . . ? O5 C33 C34 C35 34.5(10) . . . . ? N5 C33 C34 C39 32.5(10) 2_576 . . . ? O5 C33 C34 C39 -145.3(7) . . . . ? C39 C34 C35 C36 0.1(12) . . . . ? C33 C34 C35 C36 -179.7(7) . . . . ? C39 C34 C35 C40 -179.9(8) . . . . ? C33 C34 C35 C40 0.3(12) . . . . ? C34 C35 C36 C37 0.4(14) . . . . ? C40 C35 C36 C37 -179.6(10) . . . . ? C35 C36 C37 C38 -0.7(17) . . . . ? C36 C37 C38 C39 0.4(16) . . . . ? C37 C38 C39 C34 0.2(14) . . . . ? C35 C34 C39 C38 -0.4(12) . . . . ? C33 C34 C39 C38 179.4(7) . . . . ? O6 C41 C42 C47 -141.6(8) 2_576 . . . ? N6 C41 C42 C47 39.6(11) . . . . ? O6 C41 C42 C43 37.5(11) 2_576 . . . ? N6 C41 C42 C43 -141.4(8) . . . . ? C47 C42 C43 C44 1.0(13) . . . . ? C41 C42 C43 C44 -178.0(8) . . . . ? C47 C42 C43 C48 -178.0(9) . . . . ? C41 C42 C43 C48 3.0(13) . . . . ? C42 C43 C44 C45 -2.0(16) . . . . ? C48 C43 C44 C45 177.0(11) . . . . ? C43 C44 C45 C46 3(2) . . . . ? C44 C45 C46 C47 -2.1(19) . . . . ? C43 C42 C47 C46 -0.7(14) . . . . ? C41 C42 C47 C46 178.4(8) . . . . ? C45 C46 C47 C42 1.2(16) . . . . ? N8 C49 C50 C51 -62.1(11) 2_566 . . . ? O7 C49 C50 C51 118.0(9) . . . . ? N8 C49 C50 C55 118.2(9) 2_566 . . . ? O7 C49 C50 C55 -61.7(10) . . . . ? C55 C50 C51 C52 -0.5(14) . . . . ? C49 C50 C51 C52 179.8(9) . . . . ? C55 C50 C51 C56 178.3(10) . . . . ? C49 C50 C51 C56 -1.4(14) . . . . ? C50 C51 C52 C53 1.9(16) . . . . ? C56 C51 C52 C53 -176.9(11) . . . . ? C51 C52 C53 C54 -4.7(18) . . . . ? C52 C53 C54 C55 5.8(17) . . . . ? C51 C50 C55 C54 1.8(14) . . . . ? C49 C50 C55 C54 -178.5(8) . . . . ? C53 C54 C55 C50 -4.4(16) . . . . ? O8 C57 C58 C63 -126.5(8) . . . . ? N7 C57 C58 C63 51.8(10) 2_566 . . . ? O8 C57 C58 C59 52.8(10) . . . . ? N7 C57 C58 C59 -128.9(8) 2_566 . . . ? C63 C58 C59 C60 0.1(12) . . . . ? C57 C58 C59 C60 -179.2(7) . . . . ? C63 C58 C59 C64 -176.3(8) . . . . ? C57 C58 C59 C64 4.3(12) . . . . ? C58 C59 C60 C61 2.1(13) . . . . ? C64 C59 C60 C61 178.7(9) . . . . ? C59 C60 C61 C62 -2.0(15) . . . . ? C60 C61 C62 C63 -0.4(16) . . . . ? C59 C58 C63 C62 -2.5(13) . . . . ? C57 C58 C63 C62 176.8(8) . . . . ? C61 C62 C63 C58 2.7(15) . . . . ? N1 C1 O1 Ru1 4.3(9) 2_665 . . . ? C2 C1 O1 Ru1 -173.5(5) . . . . ? N2 C9 O2 Ru1 -0.2(9) 2_665 . . . ? C10 C9 O2 Ru1 179.2(4) . . . . ? N3 C17 O3 Ru2 -8.2(10) 2_655 . . . ? C18 C17 O3 Ru2 170.4(5) . . . . ? N4 C25 O4 Ru2 8.9(10) 2_655 . . . ? C26 C25 O4 Ru2 -173.0(6) . . . . ? N5 C33 O5 Ru3 7.1(9) 2_576 . . . ? C34 C33 O5 Ru3 -175.0(5) . . . . ? N8 C49 O7 Ru4 3.5(9) 2_566 . . . ? C50 C49 O7 Ru4 -176.6(5) . . . . ? N7 C57 O8 Ru4 2.3(9) 2_566 . . . ? C58 C57 O8 Ru4 -179.4(5) . . . . ? O6 C41 N6 Ru3 -4.3(9) 2_576 . . . ? C42 C41 N6 Ru3 174.5(5) . . . . ? C1 N1 Ru1 O2 -92.4(5) 2_665 . . . ? C1 N1 Ru1 O1 -6(8) 2_665 . . . ? C1 N1 Ru1 N2 85.9(6) 2_665 . . . ? C1 N1 Ru1 Ru1 -2.4(5) 2_665 . . 2_665 ? C1 N1 Ru1 I1 -177.1(5) 2_665 . . . ? C9 O2 Ru1 N1 85.3(5) . . . . ? C9 O2 Ru1 O1 -93.1(5) . . . . ? C9 O2 Ru1 N2 -50(5) . . . . ? C9 O2 Ru1 Ru1 -1.5(5) . . . 2_665 ? C9 O2 Ru1 I1 173.3(5) . . . . ? C1 O1 Ru1 N1 1(8) . . . . ? C1 O1 Ru1 O2 88.0(5) . . . . ? C1 O1 Ru1 N2 -90.4(5) . . . . ? C1 O1 Ru1 Ru1 -2.1(5) . . . 2_665 ? C1 O1 Ru1 I1 172.6(5) . . . . ? C9 N2 Ru1 N1 -84.0(5) 2_665 . . . ? C9 N2 Ru1 O2 51(5) 2_665 . . . ? C9 N2 Ru1 O1 94.4(5) 2_665 . . . ? C9 N2 Ru1 Ru1 2.8(5) 2_665 . . 2_665 ? C9 N2 Ru1 I1 -172.2(5) 2_665 . . . ? Ru2 I1 Ru1 N1 -88.86(16) . . . . ? Ru2 I1 Ru1 O2 179.55(14) . . . . ? Ru2 I1 Ru1 O1 91.39(14) . . . . ? Ru2 I1 Ru1 N2 1.21(15) . . . . ? Ru2 I1 Ru1 Ru1 -135.4(3) . . . 2_665 ? C17 N3 Ru2 N4 86.7(6) 2_655 . . . ? C17 N3 Ru2 O4 -91.6(6) 2_655 . . . ? C17 N3 Ru2 O3 -47(4) 2_655 . . . ? C17 N3 Ru2 Ru2 0.4(6) 2_655 . . 2_655 ? C17 N3 Ru2 I1 175.1(6) 2_655 . . . ? C25 N4 Ru2 N3 -89.1(6) 2_655 . . . ? C25 N4 Ru2 O4 43(6) 2_655 . . . ? C25 N4 Ru2 O3 88.5(6) 2_655 . . . ? C25 N4 Ru2 Ru2 -2.1(6) 2_655 . . 2_655 ? C25 N4 Ru2 I1 -179.3(6) 2_655 . . . ? C25 O4 Ru2 N3 81.3(6) . . . . ? C25 O4 Ru2 N4 -51(6) . . . . ? C25 O4 Ru2 O3 -96.3(5) . . . . ? C25 O4 Ru2 Ru2 -5.8(5) . . . 2_655 ? C25 O4 Ru2 I1 171.6(5) . . . . ? C17 O3 Ru2 N3 54(4) . . . . ? C17 O3 Ru2 N4 -80.1(6) . . . . ? C17 O3 Ru2 O4 98.3(5) . . . . ? C17 O3 Ru2 Ru2 6.4(5) . . . 2_655 ? C17 O3 Ru2 I1 -168.4(5) . . . . ? Ru1 I1 Ru2 N3 146.93(17) . . . . ? Ru1 I1 Ru2 N4 -119.27(18) . . . . ? Ru1 I1 Ru2 O4 59.17(15) . . . . ? Ru1 I1 Ru2 O3 -30.80(14) . . . . ? Ru1 I1 Ru2 Ru2 -147.4(4) . . . 2_655 ? C41 N6 Ru3 O6 -48(4) . . . . ? C41 N6 Ru3 N5 86.3(6) . . . . ? C41 N6 Ru3 O5 -91.1(6) . . . . ? C41 N6 Ru3 Ru3 0.0(6) . . . 2_576 ? C41 N6 Ru3 I2 175.5(6) . . . . ? C41 O6 Ru3 N6 54(4) 2_576 . . . ? C41 O6 Ru3 N5 -80.8(5) 2_576 . . . ? C41 O6 Ru3 O5 96.7(5) 2_576 . . . ? C41 O6 Ru3 Ru3 5.7(5) 2_576 . . 2_576 ? C41 O6 Ru3 I2 -169.9(5) 2_576 . . . ? C33 N5 Ru3 N6 -85.5(6) 2_576 . . . ? C33 N5 Ru3 O6 92.2(6) 2_576 . . . ? C33 N5 Ru3 O5 53(3) 2_576 . . . ? C33 N5 Ru3 Ru3 1.0(5) 2_576 . . 2_576 ? C33 N5 Ru3 I2 -176.6(5) 2_576 . . . ? C33 O5 Ru3 N6 80.5(5) . . . . ? C33 O5 Ru3 O6 -97.3(5) . . . . ? C33 O5 Ru3 N5 -58(3) . . . . ? C33 O5 Ru3 Ru3 -6.3(5) . . . 2_576 ? C33 O5 Ru3 I2 171.6(5) . . . . ? Ru4 I2 Ru3 N6 138.92(16) . . . . ? Ru4 I2 Ru3 O6 -38.85(14) . . . . ? Ru4 I2 Ru3 N5 -126.94(15) . . . . ? Ru4 I2 Ru3 O5 50.07(14) . . . . ? Ru4 I2 Ru3 Ru3 -156.0(5) . . . 2_576 ? C57 O8 Ru4 N7 -21(7) . . . . ? C57 O8 Ru4 O7 87.4(5) . . . . ? C57 O8 Ru4 N8 -90.9(5) . . . . ? C57 O8 Ru4 Ru4 -1.7(5) . . . 2_566 ? C57 O8 Ru4 I2 177.9(5) . . . . ? C57 N7 Ru4 O8 19(7) 2_566 . . . ? C57 N7 Ru4 O7 -89.3(6) 2_566 . . . ? C57 N7 Ru4 N8 88.9(6) 2_566 . . . ? C57 N7 Ru4 Ru4 -0.3(5) 2_566 . . 2_566 ? C57 N7 Ru4 I2 -179.9(5) 2_566 . . . ? C49 O7 Ru4 O8 -94.3(5) . . . . ? C49 O7 Ru4 N7 84.0(5) . . . . ? C49 O7 Ru4 N8 -43(5) . . . . ? C49 O7 Ru4 Ru4 -3.0(5) . . . 2_566 ? C49 O7 Ru4 I2 176.5(5) . . . . ? C49 N8 Ru4 O8 91.7(5) 2_566 . . . ? C49 N8 Ru4 N7 -86.7(5) 2_566 . . . ? C49 N8 Ru4 O7 40(5) 2_566 . . . ? C49 N8 Ru4 Ru4 0.3(5) 2_566 . . 2_566 ? C49 N8 Ru4 I2 -179.1(5) 2_566 . . . ? Ru3 I2 Ru4 O8 -177.43(13) . . . . ? Ru3 I2 Ru4 N7 3.14(16) . . . . ? Ru3 I2 Ru4 O7 -87.53(15) . . . . ? Ru3 I2 Ru4 N8 93.88(15) . . . . ? Ru3 I2 Ru4 Ru4 -33(4) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.732 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 952773' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2pdm119 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 I N4 O4 Ru2' _chemical_formula_weight 865.66 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.076(2) _cell_length_b 22.551(4) _cell_length_c 13.443(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.303(4) _cell_angle_gamma 90.00 _cell_volume 3343.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2409 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 19.45 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 1.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6525 _exptl_absorpt_correction_T_max 0.9291 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24955 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.1264 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5874 _reflns_number_gt 2903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some of the C-atoms were refined using geometric restraints and variable common C-C distances. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1370P)^2^+25.5144P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5874 _refine_ls_number_parameters 316 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2893 _refine_ls_wR_factor_gt 0.1972 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4119(12) 0.5907(5) -0.1048(11) 0.034(4) Uani 1 1 d D . . C2 C 0.3665(18) 0.6446(6) -0.1621(12) 0.062(5) Uani 1 1 d D . . C3 C 0.3320(15) 0.6445(8) -0.2631(11) 0.047(4) Uani 1 1 d . . . H3A H 0.3350 0.6094 -0.2989 0.056 Uiso 1 1 calc R . . C4 C 0.293(3) 0.6962(10) -0.3125(13) 0.108(5) Uani 1 1 d D . . C5 C 0.305(3) 0.7487(10) -0.2658(17) 0.108(5) Uani 1 1 d . . . H5 H 0.2967 0.7840 -0.3016 0.130 Uiso 1 1 calc R . . C6 C 0.332(3) 0.7491(10) -0.1639(17) 0.108(5) Uani 1 1 d . . . H6 H 0.3222 0.7840 -0.1287 0.130 Uiso 1 1 calc R . . C7 C 0.373(3) 0.6995(10) -0.1135(18) 0.108(5) Uani 1 1 d . . . H7 H 0.4040 0.7021 -0.0471 0.130 Uiso 1 1 calc R . . C8 C 0.254(2) 0.6949(11) -0.4224(14) 0.098(8) Uani 1 1 d D . . H8A H 0.1698 0.6839 -0.4328 0.147 Uiso 1 1 calc R . . H8B H 0.3019 0.6664 -0.4543 0.147 Uiso 1 1 calc R . . H8C H 0.2647 0.7334 -0.4504 0.147 Uiso 1 1 calc R . . C9 C 0.2814(15) 0.4485(7) -0.0221(14) 0.052(5) Uani 1 1 d D . . C10 C 0.1580(18) 0.4208(14) -0.039(2) 0.127(4) Uani 1 1 d D . . C11 C 0.131(3) 0.3855(14) -0.117(2) 0.127(4) Uani 1 1 d . . . H11 H 0.1913 0.3772 -0.1593 0.153 Uiso 1 1 calc R . . C12 C 0.016(3) 0.3604(13) -0.139(2) 0.127(4) Uani 1 1 d D . . C13 C -0.067(3) 0.3722(13) -0.075(2) 0.127(4) Uani 1 1 d . . . H13 H -0.1458 0.3580 -0.0902 0.153 Uiso 1 1 calc R . . C14 C -0.045(2) 0.4035(13) 0.012(2) 0.127(4) Uani 1 1 d . . . H14 H -0.1021 0.4082 0.0580 0.153 Uiso 1 1 calc R . . C15 C 0.073(2) 0.4283(14) 0.026(2) 0.127(4) Uani 1 1 d . . . H15 H 0.0932 0.4510 0.0826 0.153 Uiso 1 1 calc R . . C16 C -0.003(2) 0.3153(13) -0.222(2) 0.127(4) Uani 1 1 d D . . H16A H -0.0696 0.2899 -0.2094 0.191 Uiso 1 1 calc R . . H16B H 0.0693 0.2919 -0.2233 0.191 Uiso 1 1 calc R . . H16C H -0.0202 0.3351 -0.2844 0.191 Uiso 1 1 calc R . . C17 C 0.4310(16) 0.3957(6) 0.4178(13) 0.049(4) Uani 1 1 d D . . C18 C 0.3974(15) 0.3375(6) 0.3691(13) 0.050(4) Uani 1 1 d D . . C19 C 0.3428(18) 0.3357(8) 0.2734(14) 0.060(5) Uani 1 1 d . . . H19 H 0.3284 0.3713 0.2393 0.072 Uiso 1 1 calc R . . C20 C 0.308(2) 0.2835(11) 0.2253(15) 0.092(8) Uani 1 1 d D . . C21 C 0.340(3) 0.2332(12) 0.271(2) 0.115(10) Uani 1 1 d . . . H21 H 0.3226 0.1977 0.2371 0.138 Uiso 1 1 calc R . . C22 C 0.400(3) 0.2315(9) 0.369(2) 0.103(9) Uani 1 1 d . . . H22 H 0.4225 0.1956 0.3993 0.123 Uiso 1 1 calc R . . C23 C 0.424(2) 0.2848(9) 0.4164(17) 0.082(7) Uani 1 1 d . . . H23 H 0.4596 0.2849 0.4819 0.099 Uiso 1 1 calc R . . C24 C 0.247(3) 0.2845(12) 0.1209(16) 0.154(15) Uani 1 1 d D . . H24A H 0.2736 0.2510 0.0845 0.231 Uiso 1 1 calc R . . H24B H 0.2682 0.3204 0.0883 0.231 Uiso 1 1 calc R . . H24C H 0.1609 0.2827 0.1232 0.231 Uiso 1 1 calc R . . C25 C 0.7181(13) 0.4842(8) 0.4360(15) 0.057(5) Uani 1 1 d D . . C26 C 0.8430(12) 0.4721(9) 0.4063(13) 0.059(5) Uani 1 1 d D . . C27 C 0.9220(19) 0.4349(12) 0.4558(19) 0.091(4) Uani 1 1 d . . . H27 H 0.8984 0.4174 0.5135 0.109 Uiso 1 1 calc R . . C28 C 1.0379(19) 0.4203(11) 0.4273(16) 0.091(4) Uani 1 1 d D . . C29 C 1.071(2) 0.4494(11) 0.3474(18) 0.091(4) Uani 1 1 d . . . H29 H 1.1480 0.4426 0.3276 0.109 Uiso 1 1 calc R . . C30 C 0.9957(19) 0.4891(12) 0.2928(19) 0.091(4) Uani 1 1 d . . . H30 H 1.0226 0.5089 0.2384 0.109 Uiso 1 1 calc R . . C31 C 0.8764(19) 0.4990(11) 0.3215(15) 0.082(7) Uani 1 1 d . . . H31 H 0.8223 0.5232 0.2833 0.099 Uiso 1 1 calc R . . C32 C 1.122(2) 0.3774(12) 0.484(2) 0.128(11) Uani 1 1 d D . . H32A H 1.0947 0.3697 0.5479 0.192 Uiso 1 1 calc R . . H32B H 1.2025 0.3941 0.4920 0.192 Uiso 1 1 calc R . . H32C H 1.1243 0.3410 0.4468 0.192 Uiso 1 1 calc R . . I1 I 0.39207(12) 0.58423(5) 0.24325(8) 0.0593(4) Uani 1 1 d . . . O1 O 0.6410(12) 0.5630(5) 0.0879(9) 0.057(3) Uani 1 1 d . . . O2 O 0.5439(12) 0.4515(5) 0.1505(9) 0.066(4) Uani 1 1 d . . . O4 O 0.3037(11) 0.5327(6) 0.4713(10) 0.072(4) Uani 1 1 d . . . N3 N 0.5258(12) 0.6009(6) 0.4919(11) 0.047(3) Uani 1 1 d . . . H3 H 0.5190 0.6329 0.4571 0.057 Uiso 1 1 calc R . . N1 N 0.4094(11) 0.5933(5) -0.0122(8) 0.033(3) Uani 1 1 d . . . H1 H 0.3806 0.6239 0.0155 0.040 Uiso 1 1 calc R . . N2 N 0.3132(13) 0.4847(6) 0.0492(9) 0.047(3) Uani 1 1 d . . . H2 H 0.2608 0.4927 0.0906 0.056 Uiso 1 1 calc R . . O3 O 0.4213(11) 0.4422(5) 0.3604(9) 0.056(3) Uani 1 1 d . . . N4 N 0.6375(12) 0.5091(6) 0.3808(9) 0.043(3) Uani 1 1 d . . . H4 H 0.6532 0.5209 0.3225 0.052 Uiso 1 1 calc R . . Ru1 Ru 0.47498(13) 0.52358(6) 0.07114(9) 0.0418(4) Uani 1 1 d . . . Ru2 Ru 0.47131(12) 0.52248(6) 0.42465(10) 0.0423(4) Uani 1 1 d . . . 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 C1 0.032(8) 0.018(7) 0.053(10) -0.008(7) 0.011(7) 0.011(6) C2 0.099(16) 0.037(10) 0.048(12) -0.003(8) 0.000(11) 0.003(10) C3 0.054(11) 0.067(12) 0.021(8) 0.002(8) 0.006(7) 0.008(9) C4 0.206(15) 0.061(7) 0.056(7) 0.014(6) -0.002(9) 0.021(9) C5 0.206(15) 0.061(7) 0.056(7) 0.014(6) -0.002(9) 0.021(9) C6 0.206(15) 0.061(7) 0.056(7) 0.014(6) -0.002(9) 0.021(9) C7 0.206(15) 0.061(7) 0.056(7) 0.014(6) -0.002(9) 0.021(9) C8 0.103(19) 0.093(18) 0.091(19) 0.023(15) -0.022(15) -0.001(15) C9 0.067(12) 0.037(10) 0.053(12) 0.000(8) 0.013(10) -0.004(9) C10 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C11 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C12 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C13 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C14 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C15 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C16 0.094(8) 0.154(11) 0.137(11) -0.060(8) 0.027(7) -0.047(7) C17 0.054(11) 0.054(11) 0.039(11) -0.010(9) 0.008(8) -0.008(9) C18 0.050(11) 0.039(10) 0.061(12) -0.008(9) 0.013(9) 0.006(8) C19 0.089(14) 0.049(11) 0.044(11) -0.001(9) 0.013(10) -0.016(10) C20 0.13(2) 0.065(15) 0.075(17) -0.002(13) -0.015(15) -0.010(15) C21 0.19(3) 0.081(19) 0.077(19) -0.009(15) 0.00(2) -0.024(19) C22 0.15(2) 0.047(13) 0.11(2) -0.015(13) -0.009(19) -0.010(14) C23 0.117(19) 0.062(14) 0.065(15) -0.015(11) -0.005(13) -0.004(13) C24 0.26(4) 0.12(2) 0.068(19) -0.026(16) -0.04(2) -0.08(3) C25 0.059(12) 0.057(12) 0.061(13) -0.030(10) 0.039(11) -0.028(10) C26 0.040(10) 0.104(16) 0.034(10) -0.018(10) 0.003(8) 0.013(10) C27 0.060(7) 0.132(11) 0.084(9) -0.023(8) 0.027(6) 0.014(7) C28 0.060(7) 0.132(11) 0.084(9) -0.023(8) 0.027(6) 0.014(7) C29 0.060(7) 0.132(11) 0.084(9) -0.023(8) 0.027(6) 0.014(7) C30 0.060(7) 0.132(11) 0.084(9) -0.023(8) 0.027(6) 0.014(7) C31 0.071(15) 0.125(19) 0.053(13) 0.012(13) 0.014(11) 0.017(13) C32 0.059(16) 0.15(3) 0.18(3) -0.03(2) 0.021(18) 0.034(17) I1 0.0860(10) 0.0574(8) 0.0346(7) -0.0032(6) 0.0059(6) 0.0184(7) O1 0.074(9) 0.048(7) 0.047(7) -0.009(6) -0.001(7) -0.004(6) O2 0.097(10) 0.060(8) 0.041(7) -0.007(6) 0.014(7) 0.025(7) O4 0.057(8) 0.094(10) 0.063(9) -0.012(8) 0.003(7) 0.008(7) N3 0.044(8) 0.052(9) 0.047(9) -0.003(7) 0.008(7) 0.004(7) N1 0.054(8) 0.031(7) 0.015(6) -0.013(5) 0.002(5) 0.008(6) N2 0.065(9) 0.051(9) 0.025(7) -0.011(6) 0.006(7) 0.006(7) O3 0.065(8) 0.060(8) 0.043(7) -0.006(6) 0.007(6) -0.005(6) N4 0.047(8) 0.069(10) 0.015(7) 0.005(6) 0.007(6) 0.016(7) Ru1 0.0582(9) 0.0379(7) 0.0291(7) -0.0017(6) 0.0030(6) 0.0053(6) Ru2 0.0427(8) 0.0487(8) 0.0362(8) -0.0061(6) 0.0067(6) 0.0024(6) _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 C1 N1 1.249(17) . ? C1 O2 1.257(16) 3_665 ? C1 C2 1.499(5) . ? C2 C3 1.38(2) . ? C2 C7 1.40(3) . ? C3 C4 1.39(3) . ? C3 H3A 0.9300 . ? C4 C5 1.34(3) . ? C4 C8 1.500(5) . ? C5 C6 1.37(3) . ? C5 H5 0.9300 . ? C6 C7 1.36(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N2 1.28(2) . ? C9 O1 1.315(19) 3_665 ? C9 C10 1.500(5) . ? C10 C15 1.34(3) . ? C10 C11 1.34(3) . ? C11 C12 1.41(3) . ? C11 H11 0.9300 . ? C12 C13 1.35(3) . ? C12 C16 1.501(5) . ? C13 C14 1.36(4) . ? C13 H13 0.9300 . ? C14 C15 1.42(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O3 1.300(19) . ? C17 N3 1.27(2) 3_666 ? C17 C18 1.498(5) . ? C18 C23 1.37(3) . ? C18 C19 1.37(2) . ? C19 C20 1.38(3) . ? C19 H19 0.9300 . ? C20 C21 1.32(3) . ? C20 C24 1.500(5) . ? C21 C22 1.42(3) . ? C21 H21 0.9300 . ? C22 C23 1.38(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N4 1.24(2) . ? C25 O4 1.35(2) 3_666 ? C25 C26 1.500(5) . ? C26 C27 1.34(3) . ? C26 C31 1.37(3) . ? C27 C28 1.41(3) . ? C27 H27 0.9300 . ? C28 C29 1.34(3) . ? C28 C32 1.500(5) . ? C29 C30 1.39(3) . ? C29 H29 0.9300 . ? C30 C31 1.43(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? I1 Ru2 2.8741(18) . ? I1 Ru1 2.9085(17) . ? O1 C9 1.315(19) 3_665 ? O1 Ru1 2.035(12) . ? O2 C1 1.257(16) 3_665 ? O2 Ru1 2.053(12) . ? O4 C25 1.35(2) 3_666 ? O4 Ru2 2.027(13) . ? N3 C17 1.27(2) 3_666 ? N3 Ru2 2.050(13) . ? N3 H3 0.8600 . ? N1 Ru1 2.026(12) . ? N1 H1 0.8600 . ? N2 Ru1 1.993(14) . ? N2 H2 0.8600 . ? O3 Ru2 2.060(11) . ? N4 Ru2 2.007(12) . ? N4 H4 0.8600 . ? Ru1 Ru1 2.301(2) 3_665 ? Ru2 Ru2 2.302(3) 3_666 ? 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 N1 C1 O2 124.6(12) . 3_665 ? N1 C1 C2 115.9(12) . . ? O2 C1 C2 119.3(14) 3_665 . ? C3 C2 C7 117.3(14) . . ? C3 C2 C1 123.8(15) . . ? C7 C2 C1 118.5(15) . . ? C2 C3 C4 121.1(16) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 120.0(18) . . ? C5 C4 C8 119(2) . . ? C3 C4 C8 120.1(19) . . ? C4 C5 C6 118(2) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C7 C6 C5 121(2) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 120(2) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 O1 118.5(14) . 3_665 ? N2 C9 C10 123.9(18) . . ? O1 C9 C10 117.6(18) 3_665 . ? C15 C10 C11 118(2) . . ? C15 C10 C9 122(2) . . ? C11 C10 C9 120(2) . . ? C10 C11 C12 123(2) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 116(2) . . ? C13 C12 C16 124(2) . . ? C11 C12 C16 119(2) . . ? C12 C13 C14 125(3) . . ? C12 C13 H13 117.6 . . ? C14 C13 H13 117.6 . . ? C13 C14 C15 114(3) . . ? C13 C14 H14 123.0 . . ? C15 C14 H14 123.0 . . ? C10 C15 C14 124(3) . . ? C10 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 N3 121.5(13) . 3_666 ? O3 C17 C18 116.4(15) . . ? N3 C17 C18 122.0(16) 3_666 . ? C23 C18 C19 118.0(15) . . ? C23 C18 C17 121.5(17) . . ? C19 C18 C17 120.4(16) . . ? C18 C19 C20 122.9(17) . . ? C18 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C21 C20 C19 118(2) . . ? C21 C20 C24 121(2) . . ? C19 C20 C24 120(2) . . ? C20 C21 C22 122(2) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 118(2) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C18 C23 C22 121(2) . . ? C18 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 O4 120.1(12) . 3_666 ? N4 C25 C26 123.6(17) . . ? O4 C25 C26 116.3(18) 3_666 . ? C27 C26 C31 118.2(16) . . ? C27 C26 C25 123.8(19) . . ? C31 C26 C25 117.9(17) . . ? C26 C27 C28 125(2) . . ? C26 C27 H27 117.3 . . ? C28 C27 H27 117.3 . . ? C29 C28 C27 115(2) . . ? C29 C28 C32 121(2) . . ? C27 C28 C32 124(2) . . ? C28 C29 C30 123(2) . . ? C28 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C29 C30 C31 119(2) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C26 C31 C30 119(2) . . ? C26 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Ru2 I1 Ru1 110.67(5) . . ? C9 O1 Ru1 118.7(10) 3_665 . ? C1 O2 Ru1 119.3(10) 3_665 . ? C25 O4 Ru2 120.1(11) 3_666 . ? C17 N3 Ru2 123.1(11) 3_666 . ? C17 N3 H3 118.5 3_666 . ? Ru2 N3 H3 118.5 . . ? C1 N1 Ru1 118.4(9) . . ? C1 N1 H1 120.8 . . ? Ru1 N1 H1 120.8 . . ? C9 N2 Ru1 124.8(11) . . ? C9 N2 H2 117.6 . . ? Ru1 N2 H2 117.6 . . ? C17 O3 Ru2 117.1(9) . . ? C25 N4 Ru2 121.3(10) . . ? C25 N4 H4 119.3 . . ? Ru2 N4 H4 119.3 . . ? N2 Ru1 N1 89.3(5) . . ? N2 Ru1 O1 177.8(5) . . ? N1 Ru1 O1 89.8(5) . . ? N2 Ru1 O2 90.8(5) . . ? N1 Ru1 O2 177.7(4) . . ? O1 Ru1 O2 89.9(5) . . ? N2 Ru1 Ru1 87.5(4) . 3_665 ? N1 Ru1 Ru1 90.0(3) . 3_665 ? O1 Ru1 Ru1 90.5(3) . 3_665 ? O2 Ru1 Ru1 87.7(3) . 3_665 ? N2 Ru1 I1 88.8(4) . . ? N1 Ru1 I1 87.2(3) . . ? O1 Ru1 I1 93.2(3) . . ? O2 Ru1 I1 95.1(3) . . ? Ru1 Ru1 I1 175.39(10) 3_665 . ? N4 Ru2 O4 177.7(6) . . ? N4 Ru2 O3 87.9(5) . . ? O4 Ru2 O3 90.6(5) . . ? N4 Ru2 N3 91.1(5) . . ? O4 Ru2 N3 90.4(5) . . ? O3 Ru2 N3 177.9(5) . . ? N4 Ru2 Ru2 90.4(4) . 3_666 ? O4 Ru2 Ru2 87.9(4) . 3_666 ? O3 Ru2 Ru2 91.3(4) . 3_666 ? N3 Ru2 Ru2 86.9(4) . 3_666 ? N4 Ru2 I1 92.3(4) . . ? O4 Ru2 I1 89.5(4) . . ? O3 Ru2 I1 91.2(3) . . ? N3 Ru2 I1 90.6(4) . . ? Ru2 Ru2 I1 176.40(9) 3_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -161.8(17) . . . . ? O2 C1 C2 C3 22(3) 3_665 . . . ? N1 C1 C2 C7 26(3) . . . . ? O2 C1 C2 C7 -150(2) 3_665 . . . ? C7 C2 C3 C4 -7(3) . . . . ? C1 C2 C3 C4 -179(2) . . . . ? C2 C3 C4 C5 10(4) . . . . ? C2 C3 C4 C8 -179(2) . . . . ? C3 C4 C5 C6 -14(5) . . . . ? C8 C4 C5 C6 175(3) . . . . ? C4 C5 C6 C7 15(5) . . . . ? C5 C6 C7 C2 -12(5) . . . . ? C3 C2 C7 C6 7(4) . . . . ? C1 C2 C7 C6 180(2) . . . . ? N2 C9 C10 C15 -5(5) . . . . ? O1 C9 C10 C15 178(3) 3_665 . . . ? N2 C9 C10 C11 177(3) . . . . ? O1 C9 C10 C11 1(4) 3_665 . . . ? C15 C10 C11 C12 5(6) . . . . ? C9 C10 C11 C12 -177(3) . . . . ? C10 C11 C12 C13 -2(6) . . . . ? C10 C11 C12 C16 -172(3) . . . . ? C11 C12 C13 C14 -4(6) . . . . ? C16 C12 C13 C14 166(3) . . . . ? C12 C13 C14 C15 6(5) . . . . ? C11 C10 C15 C14 -3(6) . . . . ? C9 C10 C15 C14 179(3) . . . . ? C13 C14 C15 C10 -2(5) . . . . ? O3 C17 C18 C23 168.0(18) . . . . ? N3 C17 C18 C23 -7(3) 3_666 . . . ? O3 C17 C18 C19 -9(2) . . . . ? N3 C17 C18 C19 175.3(17) 3_666 . . . ? C23 C18 C19 C20 4(3) . . . . ? C17 C18 C19 C20 -179(2) . . . . ? C18 C19 C20 C21 -7(4) . . . . ? C18 C19 C20 C24 179(2) . . . . ? C19 C20 C21 C22 5(5) . . . . ? C24 C20 C21 C22 179(3) . . . . ? C20 C21 C22 C23 0(5) . . . . ? C19 C18 C23 C22 2(3) . . . . ? C17 C18 C23 C22 -176(2) . . . . ? C21 C22 C23 C18 -4(4) . . . . ? N4 C25 C26 C27 -166(2) . . . . ? O4 C25 C26 C27 15(3) 3_666 . . . ? N4 C25 C26 C31 12(3) . . . . ? O4 C25 C26 C31 -167.0(18) 3_666 . . . ? C31 C26 C27 C28 -1(4) . . . . ? C25 C26 C27 C28 177(2) . . . . ? C26 C27 C28 C29 4(4) . . . . ? C26 C27 C28 C32 -179(2) . . . . ? C27 C28 C29 C30 -3(4) . . . . ? C32 C28 C29 C30 180(2) . . . . ? C28 C29 C30 C31 -1(4) . . . . ? C27 C26 C31 C30 -4(3) . . . . ? C25 C26 C31 C30 178.7(19) . . . . ? C29 C30 C31 C26 5(4) . . . . ? O2 C1 N1 Ru1 -2(2) 3_665 . . . ? C2 C1 N1 Ru1 -177.8(11) . . . . ? O1 C9 N2 Ru1 -2(2) 3_665 . . . ? C10 C9 N2 Ru1 -178.5(19) . . . . ? N3 C17 O3 Ru2 -3(2) 3_666 . . . ? C18 C17 O3 Ru2 -178.4(11) . . . . ? O4 C25 N4 Ru2 -2(2) 3_666 . . . ? C26 C25 N4 Ru2 178.8(12) . . . . ? C9 N2 Ru1 N1 91.9(14) . . . . ? C9 N2 Ru1 O1 25(14) . . . . ? C9 N2 Ru1 O2 -85.8(14) . . . . ? C9 N2 Ru1 Ru1 1.9(14) . . . 3_665 ? C9 N2 Ru1 I1 179.1(14) . . . . ? C1 N1 Ru1 N2 -86.1(12) . . . . ? C1 N1 Ru1 O1 91.9(12) . . . . ? C1 N1 Ru1 O2 8(14) . . . . ? C1 N1 Ru1 Ru1 1.4(11) . . . 3_665 ? C1 N1 Ru1 I1 -174.9(11) . . . . ? C9 O1 Ru1 N2 -23(14) 3_665 . . . ? C9 O1 Ru1 N1 -90.3(12) 3_665 . . . ? C9 O1 Ru1 O2 87.4(12) 3_665 . . . ? C9 O1 Ru1 Ru1 -0.3(12) 3_665 . . 3_665 ? C9 O1 Ru1 I1 -177.5(12) 3_665 . . . ? C1 O2 Ru1 N2 88.1(13) 3_665 . . . ? C1 O2 Ru1 N1 -6(14) 3_665 . . . ? C1 O2 Ru1 O1 -89.8(13) 3_665 . . . ? C1 O2 Ru1 Ru1 0.7(12) 3_665 . . 3_665 ? C1 O2 Ru1 I1 177.0(12) 3_665 . . . ? Ru2 I1 Ru1 N2 97.3(4) . . . . ? Ru2 I1 Ru1 N1 -173.3(3) . . . . ? Ru2 I1 Ru1 O1 -83.6(3) . . . . ? Ru2 I1 Ru1 O2 6.6(4) . . . . ? Ru2 I1 Ru1 Ru1 133.2(11) . . . 3_665 ? C25 N4 Ru2 O4 -42(14) . . . . ? C25 N4 Ru2 O3 -91.5(14) . . . . ? C25 N4 Ru2 N3 86.7(14) . . . . ? C25 N4 Ru2 Ru2 -0.2(14) . . . 3_666 ? C25 N4 Ru2 I1 177.4(13) . . . . ? C25 O4 Ru2 N4 46(14) 3_666 . . . ? C25 O4 Ru2 O3 94.7(13) 3_666 . . . ? C25 O4 Ru2 N3 -83.5(13) 3_666 . . . ? C25 O4 Ru2 Ru2 3.4(12) 3_666 . . 3_666 ? C25 O4 Ru2 I1 -174.1(12) 3_666 . . . ? C17 O3 Ru2 N4 92.7(12) . . . . ? C17 O3 Ru2 O4 -85.6(12) . . . . ? C17 O3 Ru2 N3 33(14) . . . . ? C17 O3 Ru2 Ru2 2.4(12) . . . 3_666 ? C17 O3 Ru2 I1 -175.1(12) . . . . ? C17 N3 Ru2 N4 -90.4(14) 3_666 . . . ? C17 N3 Ru2 O4 87.8(14) 3_666 . . . ? C17 N3 Ru2 O3 -31(14) 3_666 . . . ? C17 N3 Ru2 Ru2 -0.1(13) 3_666 . . 3_666 ? C17 N3 Ru2 I1 177.3(13) 3_666 . . . ? Ru1 I1 Ru2 N4 43.0(4) . . . . ? Ru1 I1 Ru2 O4 -135.6(4) . . . . ? Ru1 I1 Ru2 O3 -45.0(3) . . . . ? Ru1 I1 Ru2 N3 134.1(4) . . . . ? Ru1 I1 Ru2 Ru2 -180(100) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.866 _refine_diff_density_min -1.654 _refine_diff_density_rms 0.223 _vrf_PLAT220_2pdm119 ; Due to the low quality of the data collected, refleted in a poor final model. ; _vrf_PLAT342_2pdm119 ; Due to the low quality of the data collected, refleted in a poor final model. ; _database_code_depnum_ccdc_archive 'CCDC 952774' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pdm355 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 I N4 O4 Ru2' _chemical_formula_weight 865.66 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 13.470(4) _cell_length_b 18.229(6) _cell_length_c 15.637(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.823(7) _cell_angle_gamma 90.00 _cell_volume 3589(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7008 _exptl_absorpt_correction_T_max 0.8453 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9904 _diffrn_reflns_av_R_equivalents 0.1222 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3143 _reflns_number_gt 1540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The phenyl ring C18-C23 has been refinad as a rigid body. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1103P)^2^+121.6602P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3143 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1885 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2959 _refine_ls_wR_factor_gt 0.2057 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1314(14) 0.1123(10) 0.0695(12) 0.047(4) Uani 1 1 d . . . C2 C 0.2013(14) 0.1770(9) 0.1038(13) 0.049(5) Uani 1 1 d . . . C3 C 0.1609(17) 0.2441(11) 0.1173(18) 0.078(7) Uani 1 1 d . . . H3 H 0.0885 0.2487 0.1060 0.094 Uiso 1 1 calc R . . C4 C 0.224(2) 0.3022(11) 0.1464(17) 0.081(7) Uani 1 1 d . . . H4 H 0.1942 0.3459 0.1566 0.097 Uiso 1 1 calc R . . C5 C 0.333(2) 0.3005(13) 0.1624(17) 0.079(7) Uani 1 1 d . . . C6 C 0.3755(16) 0.2336(12) 0.1521(16) 0.074(7) Uani 1 1 d . . . H6 H 0.4481 0.2289 0.1653 0.089 Uiso 1 1 calc R . . C7 C 0.3089(15) 0.1732(12) 0.1218(16) 0.068(6) Uani 1 1 d . . . H7 H 0.3382 0.1287 0.1136 0.082 Uiso 1 1 calc R . . C8 C 0.403(2) 0.3658(14) 0.198(2) 0.126(12) Uani 1 1 d . . . H8A H 0.4392 0.3608 0.2629 0.189 Uiso 1 1 calc R . . H8B H 0.3605 0.4095 0.1857 0.189 Uiso 1 1 calc R . . H8C H 0.4543 0.3691 0.1685 0.189 Uiso 1 1 calc R . . C9 C 0.0262(15) -0.0447(10) 0.1683(15) 0.053(5) Uani 1 1 d . . . C10 C 0.0396(13) -0.0703(9) 0.2646(9) 0.073(6) Uani 1 1 d G . . C11 C -0.0222(12) -0.0388(8) 0.3095(13) 0.081(7) Uani 1 1 d G . . H11 H -0.0699 -0.0016 0.2814 0.097 Uiso 1 1 calc R . . C12 C -0.0127(16) -0.0629(12) 0.3964(13) 0.106(10) Uani 1 1 d G . . H12 H -0.0540 -0.0418 0.4265 0.128 Uiso 1 1 calc R . . C13 C 0.0586(18) -0.1185(13) 0.4384(10) 0.124(12) Uani 1 1 d G . . C14 C 0.1203(16) -0.1500(11) 0.3934(14) 0.163(17) Uani 1 1 d G . . H14 H 0.1680 -0.1873 0.4215 0.195 Uiso 1 1 calc R . . C15 C 0.1109(14) -0.1259(11) 0.3065(13) 0.127(12) Uani 1 1 d G . . H15 H 0.1522 -0.1470 0.2765 0.153 Uiso 1 1 calc R . . C16 C 0.084(3) -0.150(3) 0.536(2) 0.20(2) Uani 1 1 d . . . H16A H 0.0883 -0.2023 0.5337 0.307 Uiso 1 1 calc R . . H16B H 0.0298 -0.1357 0.5584 0.307 Uiso 1 1 calc R . . H16C H 0.1515 -0.1306 0.5751 0.307 Uiso 1 1 calc R . . I1 I -0.2500 0.12912(12) 0.0000 0.0848(9) Uani 1 2 d S . . O1 O 0.1686(10) 0.0497(7) 0.0538(10) 0.065(4) Uani 1 1 d . . . N2 N 0.0856(12) -0.0687(8) 0.1289(10) 0.051(4) Uani 1 1 d . . . H2 H 0.1344 -0.0998 0.1568 0.061 Uiso 1 1 calc R . . N1 N 0.0327(10) 0.1207(6) 0.0501(8) 0.033(3) Uani 1 1 d . . . H1 H 0.0086 0.1626 0.0588 0.040 Uiso 1 1 calc R . . O2 O -0.0495(11) 0.0001(8) 0.1297(10) 0.068(4) Uani 1 1 d . . . Ru1 Ru -0.07003(11) 0.03628(7) -0.00155(11) 0.0447(5) Uani 1 1 d . . . 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 C1 0.051(11) 0.052(11) 0.047(12) -0.003(9) 0.027(9) -0.001(9) C2 0.048(11) 0.044(10) 0.063(13) -0.011(9) 0.030(10) -0.012(8) C3 0.058(13) 0.050(12) 0.13(2) -0.018(13) 0.040(14) -0.005(10) C4 0.107(19) 0.042(12) 0.11(2) -0.027(12) 0.061(16) -0.010(12) C5 0.091(18) 0.069(15) 0.096(18) -0.033(13) 0.059(15) -0.042(13) C6 0.053(12) 0.076(15) 0.095(18) -0.033(13) 0.029(12) -0.037(11) C7 0.048(12) 0.066(13) 0.092(17) -0.021(12) 0.026(11) -0.004(10) C8 0.15(3) 0.09(2) 0.17(3) -0.07(2) 0.10(2) -0.08(2) C9 0.047(11) 0.038(10) 0.075(15) -0.001(10) 0.023(10) -0.008(9) C10 0.067(14) 0.074(15) 0.079(18) -0.003(13) 0.026(13) -0.014(12) C11 0.100(17) 0.087(17) 0.074(17) -0.024(14) 0.054(14) -0.046(15) C12 0.15(3) 0.09(2) 0.08(2) -0.018(16) 0.038(19) -0.03(2) C13 0.14(3) 0.15(3) 0.11(3) -0.01(2) 0.08(2) -0.07(3) C14 0.18(4) 0.24(4) 0.07(2) 0.08(3) 0.04(2) 0.03(3) C15 0.13(3) 0.17(3) 0.09(2) 0.04(2) 0.05(2) 0.02(3) C16 0.21(5) 0.33(6) 0.08(3) 0.05(3) 0.06(3) 0.05(5) I1 0.0618(13) 0.0577(13) 0.149(2) 0.000 0.0547(14) 0.000 O1 0.051(7) 0.054(9) 0.101(11) -0.016(7) 0.039(8) -0.005(6) N2 0.046(9) 0.055(9) 0.047(10) -0.001(8) 0.012(8) -0.002(7) N1 0.040(8) 0.021(6) 0.040(8) -0.009(6) 0.015(6) 0.005(5) O2 0.071(9) 0.066(9) 0.086(11) -0.026(8) 0.053(9) -0.017(8) Ru1 0.0409(8) 0.0380(8) 0.0641(10) -0.0083(8) 0.0294(7) -0.0071(6) _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 C1 N1 1.26(2) . ? C1 O1 1.30(2) . ? C1 C2 1.49(2) . ? C2 C3 1.39(3) . ? C2 C7 1.38(2) . ? C3 C4 1.33(3) . ? C4 C5 1.40(3) . ? C5 C6 1.38(3) . ? C5 C8 1.50(3) . ? C6 C7 1.39(3) . ? C9 N2 1.25(2) . ? C9 O2 1.28(2) . ? C9 C10 1.52(2) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 C16 1.54(3) . ? C14 C15 1.3900 . ? I1 Ru1 2.9636(19) 2_455 ? I1 Ru1 2.9636(19) . ? O1 Ru1 2.029(12) 5 ? N2 Ru1 2.015(15) 5 ? N1 Ru1 2.034(12) . ? O2 Ru1 2.078(15) . ? Ru1 N2 2.015(15) 5 ? Ru1 O1 2.029(12) 5 ? Ru1 Ru1 2.290(3) 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 N1 C1 O1 120.2(16) . . ? N1 C1 C2 118.0(16) . . ? O1 C1 C2 121.7(16) . . ? C3 C2 C7 117.1(17) . . ? C3 C2 C1 121.5(17) . . ? C7 C2 C1 121.4(17) . . ? C4 C3 C2 121(2) . . ? C3 C4 C5 123(2) . . ? C6 C5 C4 116.7(18) . . ? C6 C5 C8 121(2) . . ? C4 C5 C8 122(2) . . ? C7 C6 C5 119.8(19) . . ? C6 C7 C2 122.3(19) . . ? N2 C9 O2 122.3(19) . . ? N2 C9 C10 120.5(17) . . ? O2 C9 C10 117.2(18) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 119.4(14) . . ? C15 C10 C9 120.6(14) . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 C16 112(2) . . ? C12 C13 C16 128(2) . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? Ru1 I1 Ru1 110.35(8) 2_455 . ? C1 O1 Ru1 120.7(11) . 5 ? C9 N2 Ru1 121.6(14) . 5 ? C1 N1 Ru1 120.9(11) . . ? C9 O2 Ru1 118.2(13) . . ? N2 Ru1 O1 90.3(6) 5 5 ? N2 Ru1 N1 89.3(5) 5 . ? O1 Ru1 N1 178.1(5) 5 . ? N2 Ru1 O2 177.9(6) 5 . ? O1 Ru1 O2 89.5(6) 5 . ? N1 Ru1 O2 90.9(5) . . ? N2 Ru1 Ru1 89.2(5) 5 5 ? O1 Ru1 Ru1 88.8(4) 5 5 ? N1 Ru1 Ru1 89.4(3) . 5 ? O2 Ru1 Ru1 88.7(4) . 5 ? N2 Ru1 I1 92.4(5) 5 . ? O1 Ru1 I1 91.4(3) 5 . ? N1 Ru1 I1 90.5(3) . . ? O2 Ru1 I1 89.7(4) . . ? Ru1 Ru1 I1 178.37(11) 5 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2(3) . . . . ? O1 C1 C2 C3 178(2) . . . . ? N1 C1 C2 C7 -176.6(19) . . . . ? O1 C1 C2 C7 -1(3) . . . . ? C7 C2 C3 C4 0(4) . . . . ? C1 C2 C3 C4 -179(2) . . . . ? C2 C3 C4 C5 2(4) . . . . ? C3 C4 C5 C6 -4(4) . . . . ? C3 C4 C5 C8 -178(3) . . . . ? C4 C5 C6 C7 4(4) . . . . ? C8 C5 C6 C7 178(2) . . . . ? C5 C6 C7 C2 -2(4) . . . . ? C3 C2 C7 C6 0(3) . . . . ? C1 C2 C7 C6 179(2) . . . . ? N2 C9 C10 C11 175.3(14) . . . . ? O2 C9 C10 C11 -7(2) . . . . ? N2 C9 C10 C15 -6(2) . . . . ? O2 C9 C10 C15 171.7(13) . . . . ? C15 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C12 178.4(15) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C11 C12 C13 C16 177(3) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C16 C13 C14 C15 -177(2) . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C9 C10 C15 C14 -178.4(15) . . . . ? N1 C1 O1 Ru1 -2(2) . . . 5 ? C2 C1 O1 Ru1 -177.2(13) . . . 5 ? O2 C9 N2 Ru1 2(2) . . . 5 ? C10 C9 N2 Ru1 179.8(11) . . . 5 ? O1 C1 N1 Ru1 2(2) . . . . ? C2 C1 N1 Ru1 177.8(12) . . . . ? N2 C9 O2 Ru1 -2(2) . . . . ? C10 C9 O2 Ru1 180.0(11) . . . . ? C1 N1 Ru1 N2 -90.7(14) . . . 5 ? C1 N1 Ru1 O1 -13(18) . . . 5 ? C1 N1 Ru1 O2 87.1(14) . . . . ? C1 N1 Ru1 Ru1 -1.5(13) . . . 5 ? C1 N1 Ru1 I1 176.9(13) . . . . ? C9 O2 Ru1 N2 6(15) . . . 5 ? C9 O2 Ru1 O1 89.9(13) . . . 5 ? C9 O2 Ru1 N1 -88.2(13) . . . . ? C9 O2 Ru1 Ru1 1.2(12) . . . 5 ? C9 O2 Ru1 I1 -178.7(12) . . . . ? Ru1 I1 Ru1 N2 112.8(4) 2_455 . . 5 ? Ru1 I1 Ru1 O1 22.4(4) 2_455 . . 5 ? Ru1 I1 Ru1 N1 -157.9(4) 2_455 . . . ? Ru1 I1 Ru1 O2 -67.1(4) 2_455 . . . ? Ru1 I1 Ru1 Ru1 -74(3) 2_455 . . 5 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.804 _refine_diff_density_min -1.808 _refine_diff_density_rms 0.216 _vrf_PLAT220_pdm355 ; Due to the low quality of the data collected, reflected in a poor final model. ; _vrf_PLAT222_pdm355 ; Due to the low quality of the data collected, reflected in a poor final model. ; _vrf_PLAT342_pdm355 ; Due to the low quality of the data collected, reflected in a poor final model. ; _database_code_depnum_ccdc_archive 'CCDC 952775'