data_ic12707 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H44 N22 Ru5 S2' _chemical_formula_weight 1666.66 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.5330(7) _cell_length_b 10.5330(7) _cell_length_c 26.1558(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2901.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1462 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 21.19 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7377 _exptl_absorpt_correction_T_max 0.7856 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11354 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1726 _reflns_number_gt 1251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.1716P)^2^+30.0507P] 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 1726 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2791 _refine_ls_wR_factor_gt 0.2539 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.010 _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 Ru1 Ru 0.0000 0.0000 0.17390(5) 0.0424(5) Uani 1 4 d S . . Ru2 Ru 0.0000 0.0000 0.08635(4) 0.0333(5) Uani 1 4 d S . . Ru3 Ru 0.0000 0.0000 0.0000 0.0488(6) Uani 1 8 d S . . S1 S 0.0000 0.0000 0.36225(18) 0.0606(14) Uani 1 4 d S . . N3 N 0.0845(8) -0.1666(7) 0.0000 0.0267(16) Uani 1 2 d S . . N4 N 0.0000 0.0000 0.2558(5) 0.039(3) Uani 1 4 d S . . C8 C 0.2053(15) -0.3994(12) 0.0000 0.057(4) Uani 1 2 d S . . H8 H 0.2080 -0.4905 0.0000 0.068 Uiso 1 2 d SR . . C9 C 0.0000 0.0000 0.3004(8) 0.043(4) Uani 1 4 d S . . N1 N 0.1725(13) -0.0948(14) 0.1700(5) 0.030(3) Uiso 0.50 1 d P . 1 N2 N 0.1375(11) -0.1347(11) 0.0843(4) 0.027(2) Uiso 0.50 1 d P . 1 C1 C 0.232(3) -0.105(2) 0.2098(10) 0.038(7) Uiso 0.50 1 d P . 1 H1 H 0.1913 -0.0831 0.2410 0.045 Uiso 0.50 1 calc PR . 1 C2 C 0.359(2) -0.149(2) 0.2110(9) 0.033(5) Uiso 0.50 1 d P . 1 H2 H 0.4042 -0.1533 0.2423 0.039 Uiso 0.50 1 calc PR . 1 C3 C 0.4153(18) -0.1848(19) 0.1653(7) 0.042(4) Uiso 0.50 1 d P . 1 H3 H 0.5017 -0.2105 0.1645 0.050 Uiso 0.50 1 calc PR . 1 C4 C 0.3442(16) -0.1827(16) 0.1214(7) 0.041(3) Uiso 0.50 1 d P . 1 H4 H 0.3797 -0.2080 0.0896 0.049 Uiso 0.50 1 calc PR . 1 C5 C 0.2163(14) -0.1420(14) 0.1247(5) 0.031(3) Uiso 0.50 1 d P . 1 C6 C 0.1430(15) -0.2110(14) 0.0429(5) 0.028(3) Uiso 0.50 1 d P . 1 C7 C 0.2044(19) -0.3298(17) 0.0422(6) 0.042(4) Uiso 0.50 1 d P . 1 H7 H 0.2454 -0.3602 0.0722 0.050 Uiso 0.50 1 calc PR . 1 N1' N 0.1794(13) -0.0529(15) 0.1673(5) 0.034(4) Uiso 0.50 1 d P . 2 N2' N 0.0202(11) -0.1824(11) 0.0838(4) 0.030(2) Uiso 0.50 1 d P . 2 C1' C 0.255(3) -0.108(3) 0.2069(11) 0.042(8) Uiso 0.50 1 d P . 2 H1' H 0.2188 -0.1125 0.2401 0.050 Uiso 0.50 1 calc PR . 2 C2' C 0.375(3) -0.153(3) 0.2014(13) 0.061(10) Uiso 0.50 1 d P . 2 H2' H 0.4167 -0.1952 0.2289 0.073 Uiso 0.50 1 calc PR . 2 C3' C 0.4300(18) -0.139(2) 0.1595(8) 0.045(4) Uiso 0.50 1 d P . 2 H3' H 0.5127 -0.1740 0.1553 0.053 Uiso 0.50 1 calc PR . 2 C4' C 0.3751(16) -0.0758(16) 0.1189(7) 0.044(4) Uiso 0.50 1 d P . 2 H4' H 0.4216 -0.0614 0.0884 0.053 Uiso 0.50 1 calc PR . 2 C5' C 0.2464(13) -0.0317(13) 0.1238(5) 0.031(3) Uiso 0.50 1 d P . 2 C6' C 0.0845(15) -0.2342(14) 0.0439(5) 0.027(3) Uiso 0.50 1 d P . 2 C7' C 0.1499(17) -0.3488(16) 0.0475(6) 0.035(3) Uiso 0.50 1 d P . 2 H7' H 0.1583 -0.3923 0.0791 0.042 Uiso 0.50 1 calc PR . 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 Ru1 0.0493(6) 0.0493(6) 0.0285(8) 0.000 0.000 0.000 Ru2 0.0367(5) 0.0367(5) 0.0265(8) 0.000 0.000 0.000 Ru3 0.0494(8) 0.0494(8) 0.0477(13) 0.000 0.000 0.000 S1 0.076(2) 0.076(2) 0.030(2) 0.000 0.000 0.000 N3 0.037(4) 0.020(4) 0.023(4) 0.000 0.000 0.008(3) N4 0.049(5) 0.049(5) 0.018(6) 0.000 0.000 0.000 C8 0.085(10) 0.036(6) 0.049(7) 0.000 0.000 0.028(6) C9 0.034(5) 0.034(5) 0.061(12) 0.000 0.000 0.000 _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 Ru1 N1' 1.978(14) 3 ? Ru1 N1' 1.978(14) 2 ? Ru1 N1' 1.978(14) . ? Ru1 N1' 1.978(14) 4 ? Ru1 N1 2.075(14) 3 ? Ru1 N1 2.075(14) 2 ? Ru1 N1 2.075(14) . ? Ru1 N1 2.075(14) 4 ? Ru1 N4 2.143(13) . ? Ru1 Ru2 2.2899(17) . ? Ru2 N2' 1.934(12) 2 ? Ru2 N2' 1.934(12) . ? Ru2 N2' 1.934(12) 3 ? Ru2 N2' 1.934(12) 4 ? Ru2 N2 2.028(11) 3 ? Ru2 N2 2.028(11) 2 ? Ru2 N2 2.028(11) 4 ? Ru2 N2 2.028(11) . ? Ru2 Ru3 2.2585(12) . ? Ru3 N3 1.967(7) 3 ? Ru3 N3 1.967(7) 11 ? Ru3 N3 1.967(7) 9 ? Ru3 N3 1.967(7) . ? Ru3 Ru2 2.2585(12) 9 ? S1 C9 1.62(2) . ? N3 C6' 1.352(13) 10 ? N3 C6' 1.352(13) . ? N3 C6 1.364(14) . ? N3 C6 1.364(14) 10 ? N4 C9 1.17(2) . ? C8 C7 1.326(18) . ? C8 C7 1.326(18) 10 ? C8 C7' 1.472(17) 10 ? C8 C7' 1.472(17) . ? N1 C1 1.22(3) . ? N1 C5 1.364(19) . ? N2 C5 1.346(18) . ? N2 C6 1.349(17) . ? C1 C2 1.42(3) . ? C2 C3 1.39(3) . ? C3 C4 1.37(2) . ? C4 C5 1.42(2) . ? C6 C7 1.41(2) . ? N1' C5' 1.36(2) . ? N1' C1' 1.43(3) . ? N2' C6' 1.358(17) . ? N2' C5' 1.360(18) 4 ? C1' C2' 1.36(4) . ? C2' C3' 1.25(4) . ? C3' C4' 1.38(3) . ? C4' C5' 1.44(2) . ? C5' N2' 1.360(18) 3 ? C6' C7' 1.39(2) . ? 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' Ru1 N1' 89.57(7) 3 2 ? N1' Ru1 N1' 89.57(7) 3 . ? N1' Ru1 N1' 170.0(8) 2 . ? N1' Ru1 N1' 170.0(8) 3 4 ? N1' Ru1 N1' 89.57(7) 2 4 ? N1' Ru1 N1' 89.57(7) . 4 ? N1' Ru1 N1 12.5(5) 3 3 ? N1' Ru1 N1 102.1(5) 2 3 ? N1' Ru1 N1 77.4(5) . 3 ? N1' Ru1 N1 165.4(5) 4 3 ? N1' Ru1 N1 77.4(5) 3 2 ? N1' Ru1 N1 12.5(5) 2 2 ? N1' Ru1 N1 165.4(5) . 2 ? N1' Ru1 N1 102.1(5) 4 2 ? N1 Ru1 N1 89.86(4) 3 2 ? N1' Ru1 N1 102.1(5) 3 . ? N1' Ru1 N1 165.4(5) 2 . ? N1' Ru1 N1 12.5(5) . . ? N1' Ru1 N1 77.4(5) 4 . ? N1 Ru1 N1 89.86(4) 3 . ? N1 Ru1 N1 174.3(8) 2 . ? N1' Ru1 N1 165.4(5) 3 4 ? N1' Ru1 N1 77.4(5) 2 4 ? N1' Ru1 N1 102.1(5) . 4 ? N1' Ru1 N1 12.5(5) 4 4 ? N1 Ru1 N1 174.3(8) 3 4 ? N1 Ru1 N1 89.86(4) 2 4 ? N1 Ru1 N1 89.86(4) . 4 ? N1' Ru1 N4 95.0(4) 3 . ? N1' Ru1 N4 95.0(4) 2 . ? N1' Ru1 N4 95.0(4) . . ? N1' Ru1 N4 95.0(4) 4 . ? N1 Ru1 N4 92.8(4) 3 . ? N1 Ru1 N4 92.8(4) 2 . ? N1 Ru1 N4 92.8(4) . . ? N1 Ru1 N4 92.8(4) 4 . ? N1' Ru1 Ru2 85.0(4) 3 . ? N1' Ru1 Ru2 85.0(4) 2 . ? N1' Ru1 Ru2 85.0(4) . . ? N1' Ru1 Ru2 85.0(4) 4 . ? N1 Ru1 Ru2 87.2(4) 3 . ? N1 Ru1 Ru2 87.2(4) 2 . ? N1 Ru1 Ru2 87.2(4) . . ? N1 Ru1 Ru2 87.2(4) 4 . ? N4 Ru1 Ru2 180.0 . . ? N2' Ru2 N2' 176.0(7) 2 . ? N2' Ru2 N2' 89.93(2) 2 3 ? N2' Ru2 N2' 89.93(2) . 3 ? N2' Ru2 N2' 89.93(2) 2 4 ? N2' Ru2 N2' 89.93(2) . 4 ? N2' Ru2 N2' 176.0(7) 3 4 ? N2' Ru2 N2 50.7(5) 2 3 ? N2' Ru2 N2 129.2(5) . 3 ? N2' Ru2 N2 39.3(5) 3 3 ? N2' Ru2 N2 140.6(5) 4 3 ? N2' Ru2 N2 39.3(5) 2 2 ? N2' Ru2 N2 140.6(5) . 2 ? N2' Ru2 N2 129.2(5) 3 2 ? N2' Ru2 N2 50.7(5) 4 2 ? N2 Ru2 N2 89.961(16) 3 2 ? N2' Ru2 N2 129.2(5) 2 4 ? N2' Ru2 N2 50.7(5) . 4 ? N2' Ru2 N2 140.6(5) 3 4 ? N2' Ru2 N2 39.3(5) 4 4 ? N2 Ru2 N2 177.0(6) 3 4 ? N2 Ru2 N2 89.961(16) 2 4 ? N2' Ru2 N2 140.6(5) 2 . ? N2' Ru2 N2 39.3(5) . . ? N2' Ru2 N2 50.7(5) 3 . ? N2' Ru2 N2 129.2(5) 4 . ? N2 Ru2 N2 89.961(16) 3 . ? N2 Ru2 N2 177.0(6) 2 . ? N2 Ru2 N2 89.961(16) 4 . ? N2' Ru2 Ru3 88.0(3) 2 . ? N2' Ru2 Ru3 88.0(3) . . ? N2' Ru2 Ru3 88.0(3) 3 . ? N2' Ru2 Ru3 88.0(3) 4 . ? N2 Ru2 Ru3 88.5(3) 3 . ? N2 Ru2 Ru3 88.5(3) 2 . ? N2 Ru2 Ru3 88.5(3) 4 . ? N2 Ru2 Ru3 88.5(3) . . ? N2' Ru2 Ru1 92.0(3) 2 . ? N2' Ru2 Ru1 92.0(3) . . ? N2' Ru2 Ru1 92.0(3) 3 . ? N2' Ru2 Ru1 92.0(3) 4 . ? N2 Ru2 Ru1 91.5(3) 3 . ? N2 Ru2 Ru1 91.5(3) 2 . ? N2 Ru2 Ru1 91.5(3) 4 . ? N2 Ru2 Ru1 91.5(3) . . ? Ru3 Ru2 Ru1 180.0 . . ? N3 Ru3 N3 180.0 3 11 ? N3 Ru3 N3 90.0 3 9 ? N3 Ru3 N3 90.0 11 9 ? N3 Ru3 N3 90.0 3 . ? N3 Ru3 N3 90.0 11 . ? N3 Ru3 N3 180.0(4) 9 . ? N3 Ru3 Ru2 90.0 3 9 ? N3 Ru3 Ru2 90.0 11 9 ? N3 Ru3 Ru2 90.0 9 9 ? N3 Ru3 Ru2 90.0 . 9 ? N3 Ru3 Ru2 90.0 3 . ? N3 Ru3 Ru2 90.0 11 . ? N3 Ru3 Ru2 90.0 9 . ? N3 Ru3 Ru2 90.0 . . ? Ru2 Ru3 Ru2 180.0 9 . ? C6' N3 C6' 116.4(13) 10 . ? C6' N3 C6 121.3(9) 10 . ? C6' N3 C6 28.3(7) . . ? C6' N3 C6 28.3(7) 10 10 ? C6' N3 C6 121.3(9) . 10 ? C6 N3 C6 110.8(13) . 10 ? C6' N3 Ru3 118.0(7) 10 . ? C6' N3 Ru3 118.0(7) . . ? C6 N3 Ru3 120.7(7) . . ? C6 N3 Ru3 120.7(7) 10 . ? C9 N4 Ru1 180.000(1) . . ? C7 C8 C7 112.8(18) . 10 ? C7 C8 C7' 120.0(12) . 10 ? C7 C8 C7' 25.1(8) 10 10 ? C7 C8 C7' 25.1(8) . . ? C7 C8 C7' 120.0(12) 10 . ? C7' C8 C7' 115.0(15) 10 . ? N4 C9 S1 180.000(1) . . ? C1 N1 C5 122.4(18) . . ? C1 N1 Ru1 116.7(16) . . ? C5 N1 Ru1 120.9(10) . . ? C5 N2 C6 124.7(12) . . ? C5 N2 Ru2 117.3(9) . . ? C6 N2 Ru2 117.9(9) . . ? N1 C1 C2 122(2) . . ? C3 C2 C1 118(2) . . ? C4 C3 C2 118.8(18) . . ? C3 C4 C5 118.3(16) . . ? N2 C5 N1 116.9(13) . . ? N2 C5 C4 123.8(13) . . ? N1 C5 C4 119.0(13) . . ? N2 C6 N3 115.9(12) . . ? N2 C6 C7 124.0(13) . . ? N3 C6 C7 120.1(12) . . ? C8 C7 C6 120.4(15) . . ? C5' N1' C1' 112.5(16) . . ? C5' N1' Ru1 121.5(11) . . ? C1' N1' Ru1 125.8(15) . . ? C6' N2' C5' 126.3(13) . 4 ? C6' N2' Ru2 118.8(9) . . ? C5' N2' Ru2 114.9(9) 4 . ? C2' C1' N1' 126(3) . . ? C3' C2' C1' 119(3) . . ? C2' C3' C4' 123(2) . . ? C3' C4' C5' 118.9(16) . . ? N1' C5' N2' 117.0(13) . 3 ? N1' C5' C4' 120.7(14) . . ? N2' C5' C4' 122.0(13) 3 . ? N3 C6' N2' 116.1(12) . . ? N3 C6' C7' 120.9(12) . . ? N2' C6' C7' 123.0(13) . . ? C6' C7' C8 117.0(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.644 _refine_diff_density_min -3.830 _refine_diff_density_rms 0.275