# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_try-1 #TrackingRef 'try-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37.5 N4.5 O P2 Ru S2' _chemical_formula_weight 868.92 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.436(5) _cell_length_b 12.863(5) _cell_length_c 13.394(5) _cell_angle_alpha 94.291(5) _cell_angle_beta 94.205(5) _cell_angle_gamma 104.931(5) _cell_volume 2054.9(14) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26178 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.03 _reflns_number_total 5733 _reflns_number_gt 3642 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1106P)^2^+0.3421P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5733 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.005 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 Ru01 Ru 0.79749(5) 0.32214(5) 0.75703(4) 0.0420(3) Uani 1 1 d . . . P2 P 0.73352(16) 0.48025(16) 0.78057(14) 0.0423(5) Uani 1 1 d . . . P1 P 0.83209(17) 0.14878(17) 0.73141(16) 0.0515(6) Uani 1 1 d . . . C221 C 0.6987(6) 0.5180(7) 0.9061(6) 0.046(2) Uani 1 1 d . . . C211 C 0.8368(7) 0.5977(6) 0.7510(6) 0.052(2) Uani 1 1 d . . . C231 C 0.6051(6) 0.4779(6) 0.7037(6) 0.046(2) Uani 1 1 d . . . C111 C 0.9700(6) 0.1520(6) 0.6953(6) 0.051(2) Uani 1 1 d . . . C131 C 0.8257(7) 0.0715(7) 0.8411(7) 0.061(2) Uani 1 1 d . . . C232 C 0.5416(7) 0.3880(7) 0.6482(6) 0.060(2) Uani 1 1 d . . . H232 H 0.5675 0.3262 0.6444 0.071 Uiso 1 1 calc R . . C222 C 0.7015(6) 0.6241(7) 0.9378(6) 0.059(2) Uani 1 1 d . . . H222 H 0.7304 0.6787 0.8977 0.070 Uiso 1 1 calc R . . C136 C 0.7711(7) 0.0931(7) 0.9208(7) 0.061(2) Uani 1 1 d . . . H136 H 0.7347 0.1478 0.9190 0.073 Uiso 1 1 calc R . . C234 C 0.4025(8) 0.4723(10) 0.6000(7) 0.075(3) Uani 1 1 d . . . H234 H 0.3349 0.4698 0.5641 0.090 Uiso 1 1 calc R . . C224 C 0.6251(7) 0.5717(9) 1.0879(6) 0.066(3) Uani 1 1 d . . . H224 H 0.6005 0.5889 1.1494 0.079 Uiso 1 1 calc R . . C226 C 0.6598(6) 0.4397(7) 0.9686(6) 0.051(2) Uani 1 1 d . . . H226 H 0.6579 0.3682 0.9495 0.062 Uiso 1 1 calc R . . C212 C 0.9268(7) 0.6494(7) 0.8202(7) 0.068(3) Uani 1 1 d . . . H212 H 0.9287 0.6253 0.8839 0.082 Uiso 1 1 calc R . . C121 C 0.7362(7) 0.0555(8) 0.6357(8) 0.069(3) Uani 1 1 d . . . C225 C 0.6236(7) 0.4665(8) 1.0593(6) 0.064(2) Uani 1 1 d . . . H225 H 0.5979 0.4130 1.1014 0.077 Uiso 1 1 calc R . . C223 C 0.6620(7) 0.6505(8) 1.0278(6) 0.063(2) Uani 1 1 d . . . H223 H 0.6610 0.7213 1.0465 0.075 Uiso 1 1 calc R . . C116 C 0.9926(8) 0.1198(7) 0.5996(7) 0.076(3) Uani 1 1 d . . . H116 H 0.9343 0.0948 0.5489 0.091 Uiso 1 1 calc R . . C216 C 0.8359(9) 0.6284(8) 0.6568(8) 0.088(3) Uani 1 1 d . . . H216 H 0.7776 0.5946 0.6082 0.106 Uiso 1 1 calc R . . C235 C 0.4609(9) 0.5640(10) 0.6538(8) 0.091(3) Uani 1 1 d . . . H235 H 0.4334 0.6247 0.6574 0.109 Uiso 1 1 calc R . . C233 C 0.4411(7) 0.3840(8) 0.5977(7) 0.070(3) Uani 1 1 d . . . H233 H 0.3993 0.3200 0.5616 0.084 Uiso 1 1 calc R . . C115 C 1.1016(9) 0.1248(9) 0.5792(8) 0.092(3) Uani 1 1 d . . . H115 H 1.1160 0.1015 0.5153 0.111 Uiso 1 1 calc R . . C113 C 1.1680(8) 0.1985(8) 0.7445(8) 0.078(3) Uani 1 1 d . . . H113 H 1.2272 0.2260 0.7939 0.094 Uiso 1 1 calc R . . C112 C 1.0621(7) 0.1932(8) 0.7648(7) 0.074(3) Uani 1 1 d . . . H112 H 1.0504 0.2185 0.8289 0.088 Uiso 1 1 calc R . . C236 C 0.5669(8) 0.5668(8) 0.7058(6) 0.075(3) Uani 1 1 d . . . H236 H 0.6096 0.6307 0.7414 0.091 Uiso 1 1 calc R . . C132 C 0.8750(9) -0.0128(8) 0.8413(9) 0.093(3) Uani 1 1 d . . . H132 H 0.9104 -0.0308 0.7862 0.112 Uiso 1 1 calc R . . C135 C 0.7677(8) 0.0375(8) 1.0033(8) 0.086(3) Uani 1 1 d . . . H135 H 0.7327 0.0567 1.0581 0.103 Uiso 1 1 calc R . . C214 C 1.0138(12) 0.7623(10) 0.7089(15) 0.128(6) Uani 1 1 d . . . H214 H 1.0742 0.8166 0.6939 0.154 Uiso 1 1 calc R . . C134 C 0.8171(10) -0.0488(10) 1.0056(10) 0.111(4) Uani 1 1 d . . . H134 H 0.8128 -0.0894 1.0605 0.133 Uiso 1 1 calc R . . C215 C 0.9282(14) 0.7153(11) 0.6329(11) 0.128(5) Uani 1 1 d . . . H215 H 0.9302 0.7389 0.5690 0.154 Uiso 1 1 calc R . . C126 C 0.6740(11) -0.0400(10) 0.6533(9) 0.124(5) Uani 1 1 d . . . H126 H 0.6807 -0.0591 0.7186 0.149 Uiso 1 1 calc R . . C114 C 1.1866(8) 0.1636(8) 0.6519(10) 0.085(3) Uani 1 1 d . . . H114 H 1.2593 0.1661 0.6378 0.103 Uiso 1 1 calc R . . C133 C 0.8710(10) -0.0717(9) 0.9267(13) 0.121(5) Uani 1 1 d . . . H133 H 0.9062 -0.1273 0.9284 0.146 Uiso 1 1 calc R . . C213 C 1.0124(10) 0.7328(10) 0.8009(11) 0.106(4) Uani 1 1 d . . . H213 H 1.0683 0.7680 0.8512 0.128 Uiso 1 1 calc R . . S1 S 0.89318(17) 0.35417(17) 0.91452(14) 0.0515(6) Uani 1 1 d . . . N1 N 0.9421(5) 0.4035(5) 0.7174(4) 0.0424(15) Uani 1 1 d . . . N11 N 0.6431(5) 0.2352(5) 0.7888(5) 0.0504(17) Uani 1 1 d . . . C2 C 1.0327(6) 0.4403(6) 0.7839(6) 0.052(2) Uani 1 1 d . . . C1 C 1.0177(6) 0.4209(6) 0.8802(6) 0.057(2) Uani 1 1 d . . . H1 H 1.0780 0.4452 0.9290 0.068 Uiso 1 1 calc R . . N2 N 0.9532(5) 0.4247(5) 0.6214(5) 0.0549(18) Uani 1 1 d . . . C4 C 1.1431(7) 0.5010(8) 0.7498(7) 0.091(3) Uani 1 1 d . . . H4A H 1.1603 0.4602 0.6931 0.137 Uiso 1 1 calc R . . H4B H 1.2011 0.5111 0.8038 0.137 Uiso 1 1 calc R . . H4C H 1.1377 0.5702 0.7310 0.137 Uiso 1 1 calc R . . C124 C 0.5906(9) -0.0857(10) 0.4931(14) 0.123(6) Uani 1 1 d . . . H124 H 0.5405 -0.1336 0.4451 0.148 Uiso 1 1 calc R . . C123 C 0.6505(10) 0.0124(12) 0.4609(9) 0.114(5) Uani 1 1 d . . . H123 H 0.6418 0.0278 0.3945 0.137 Uiso 1 1 calc R . . C125 C 0.5978(14) -0.1162(13) 0.5822(11) 0.160(8) Uani 1 1 d . . . H125 H 0.5564 -0.1828 0.5987 0.192 Uiso 1 1 calc R . . N3 N 0.8547(6) 0.3969(6) 0.4676(5) 0.076(2) Uani 1 1 d . . . H3A H 0.7948 0.3725 0.4272 0.092 Uiso 1 1 calc R . . H3B H 0.9151 0.4328 0.4455 0.092 Uiso 1 1 calc R . . C3 C 0.8538(7) 0.3793(7) 0.5635(6) 0.053(2) Uani 1 1 d . . . O1 O 0.7618(4) 0.3249(4) 0.5964(3) 0.0545(14) Uani 1 1 d . . . C11 C 0.5555(7) 0.1869(6) 0.8049(6) 0.046(2) Uani 1 1 d . . . C122 C 0.7253(9) 0.0871(9) 0.5349(9) 0.093(3) Uani 1 1 d . . . H122 H 0.7659 0.1541 0.5188 0.112 Uiso 1 1 calc R . . S11 S 0.4307(2) 0.1164(2) 0.8279(2) 0.0839(8) Uani 1 1 d . . . C6 C 0.3953(14) 0.8056(12) 0.7963(14) 0.038(4) Uani 0.50 1 d P . . N4 N 0.3307(12) 0.7709(11) 0.7389(12) 0.054(4) Uani 0.50 1 d P . . C5 C 0.4839(14) 0.8486(12) 0.8710(12) 0.052(4) Uani 0.50 1 d P . . 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 Ru01 0.0399(4) 0.0426(5) 0.0451(4) 0.0017(3) 0.0082(3) 0.0136(3) P2 0.0434(12) 0.0416(13) 0.0435(12) 0.0031(10) 0.0085(9) 0.0130(10) P1 0.0464(13) 0.0462(14) 0.0632(14) -0.0041(11) 0.0062(10) 0.0169(11) C221 0.044(5) 0.048(5) 0.050(5) 0.001(4) 0.005(4) 0.020(4) C211 0.055(5) 0.043(5) 0.065(6) 0.017(5) 0.024(5) 0.017(4) C231 0.052(5) 0.040(5) 0.054(5) 0.006(4) 0.011(4) 0.026(4) C111 0.049(5) 0.037(5) 0.070(6) -0.001(4) 0.011(4) 0.019(4) C131 0.049(5) 0.043(6) 0.100(7) 0.017(5) 0.020(5) 0.018(5) C232 0.053(6) 0.047(6) 0.074(6) -0.003(5) -0.005(5) 0.012(5) C222 0.059(6) 0.058(6) 0.060(6) 0.004(5) 0.010(4) 0.017(5) C136 0.052(5) 0.052(6) 0.083(7) 0.029(5) 0.015(5) 0.014(5) C234 0.055(6) 0.113(9) 0.055(6) 0.001(6) 0.003(5) 0.019(7) C224 0.059(6) 0.091(8) 0.048(6) -0.011(6) 0.010(4) 0.021(6) C226 0.048(5) 0.051(6) 0.050(5) -0.005(4) 0.010(4) 0.005(4) C212 0.052(6) 0.056(6) 0.091(7) 0.005(5) 0.012(5) 0.005(5) C121 0.053(6) 0.054(6) 0.097(8) -0.027(6) 0.000(5) 0.019(5) C225 0.057(6) 0.077(7) 0.054(6) 0.006(5) 0.007(4) 0.009(5) C223 0.069(6) 0.066(7) 0.056(6) -0.012(5) 0.012(5) 0.028(5) C116 0.059(6) 0.095(8) 0.069(7) -0.013(6) 0.007(5) 0.017(6) C216 0.104(8) 0.074(7) 0.092(8) 0.025(6) 0.035(6) 0.020(6) C235 0.106(9) 0.119(10) 0.077(7) 0.002(7) 0.012(6) 0.085(8) C233 0.052(6) 0.065(7) 0.092(7) 0.008(5) -0.002(5) 0.017(5) C115 0.072(8) 0.124(10) 0.087(8) -0.009(7) 0.033(6) 0.034(7) C113 0.051(6) 0.099(8) 0.087(8) -0.010(6) 0.006(5) 0.028(6) C112 0.055(6) 0.098(8) 0.070(6) -0.014(5) 0.006(5) 0.032(6) C236 0.078(7) 0.073(7) 0.071(6) -0.005(5) -0.010(5) 0.020(6) C132 0.093(8) 0.073(7) 0.130(10) 0.041(7) 0.038(7) 0.035(7) C135 0.072(7) 0.079(8) 0.116(9) 0.043(7) 0.034(6) 0.022(6) C214 0.088(10) 0.069(9) 0.214(19) 0.000(11) 0.054(12) -0.009(8) C134 0.087(9) 0.105(10) 0.147(12) 0.059(9) 0.043(8) 0.016(8) C215 0.163(14) 0.104(11) 0.142(13) 0.070(10) 0.088(11) 0.044(11) C126 0.142(11) 0.093(10) 0.091(9) -0.015(7) 0.024(8) -0.048(9) C114 0.046(6) 0.089(8) 0.129(10) 0.014(7) 0.024(7) 0.027(6) C133 0.092(9) 0.080(9) 0.212(15) 0.076(10) 0.031(10) 0.037(7) C213 0.083(9) 0.085(10) 0.134(12) 0.010(8) 0.029(8) -0.014(7) S1 0.0548(13) 0.0542(14) 0.0458(12) 0.0056(10) 0.0066(9) 0.0145(11) N1 0.036(4) 0.056(4) 0.040(4) 0.011(3) 0.012(3) 0.016(3) N11 0.038(4) 0.045(4) 0.067(5) 0.004(3) 0.009(3) 0.008(4) C2 0.036(5) 0.065(6) 0.055(5) 0.021(4) 0.005(4) 0.009(4) C1 0.050(5) 0.054(6) 0.064(6) 0.018(4) 0.001(4) 0.009(4) N2 0.044(4) 0.074(5) 0.050(4) 0.008(4) 0.006(3) 0.020(4) C4 0.045(6) 0.128(9) 0.089(7) 0.034(7) -0.008(5) 0.001(6) C124 0.048(7) 0.060(9) 0.238(19) -0.059(10) 0.022(9) -0.011(6) C123 0.107(10) 0.139(12) 0.098(9) -0.070(9) -0.036(7) 0.070(10) C125 0.200(18) 0.148(15) 0.082(10) 0.012(10) 0.045(11) -0.050(12) N3 0.052(5) 0.115(7) 0.053(5) 0.012(4) 0.011(4) 0.005(4) C3 0.057(6) 0.072(6) 0.040(5) 0.001(4) 0.015(4) 0.033(5) O1 0.057(4) 0.073(4) 0.042(3) 0.008(3) 0.013(3) 0.030(3) C11 0.041(5) 0.036(5) 0.060(5) 0.002(4) 0.001(4) 0.013(4) C122 0.099(9) 0.086(8) 0.100(9) -0.017(7) -0.002(7) 0.045(7) S11 0.0494(15) 0.0750(18) 0.121(2) 0.0107(16) 0.0239(14) 0.0007(13) C6 0.031(10) 0.010(9) 0.085(13) 0.019(9) 0.032(9) 0.014(8) N4 0.039(9) 0.025(9) 0.099(12) 0.001(8) 0.032(8) 0.008(7) C5 0.072(12) 0.030(9) 0.064(11) 0.004(8) 0.018(9) 0.026(9) _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 Ru01 N1 1.965(6) . ? Ru01 N11 2.051(7) . ? Ru01 O1 2.170(5) . ? Ru01 S1 2.299(2) . ? Ru01 P2 2.376(2) . ? Ru01 P1 2.383(2) . ? P2 C211 1.803(8) . ? P2 C231 1.828(8) . ? P2 C221 1.828(8) . ? P1 C111 1.807(8) . ? P1 C121 1.820(9) . ? P1 C131 1.829(9) . ? C221 C226 1.372(10) . ? C221 C222 1.391(10) . ? C211 C216 1.350(11) . ? C211 C212 1.388(11) . ? C231 C236 1.346(11) . ? C231 C232 1.352(10) . ? C111 C112 1.384(11) . ? C111 C116 1.388(10) . ? C131 C136 1.356(11) . ? C131 C132 1.377(12) . ? C232 C233 1.364(11) . ? C222 C223 1.386(10) . ? C136 C135 1.357(11) . ? C234 C235 1.339(13) . ? C234 C233 1.341(12) . ? C224 C223 1.350(11) . ? C224 C225 1.374(11) . ? C226 C225 1.377(10) . ? C212 C213 1.358(13) . ? C121 C126 1.320(13) . ? C121 C122 1.445(13) . ? C116 C115 1.389(12) . ? C216 C215 1.455(15) . ? C235 C236 1.435(12) . ? C115 C114 1.349(13) . ? C113 C114 1.343(12) . ? C113 C112 1.350(11) . ? C132 C133 1.416(15) . ? C135 C134 1.402(14) . ? C214 C213 1.316(17) . ? C214 C215 1.397(18) . ? C134 C133 1.345(15) . ? C126 C125 1.419(16) . ? S1 C1 1.681(8) . ? N1 C2 1.343(9) . ? N1 N2 1.344(7) . ? N11 C11 1.151(9) . ? C2 C1 1.348(10) . ? C2 C4 1.515(11) . ? N2 C3 1.375(9) . ? C124 C125 1.288(18) . ? C124 C123 1.407(17) . ? C123 C122 1.426(13) . ? N3 C3 1.321(9) . ? C3 O1 1.304(9) . ? C11 S11 1.646(9) . ? C6 N4 1.053(18) . ? C6 C5 1.40(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 Ru01 N11 176.4(2) . . ? N1 Ru01 O1 77.5(2) . . ? N11 Ru01 O1 98.8(2) . . ? N1 Ru01 S1 82.89(18) . . ? N11 Ru01 S1 100.73(18) . . ? O1 Ru01 S1 160.42(16) . . ? N1 Ru01 P2 92.61(18) . . ? N11 Ru01 P2 87.69(18) . . ? O1 Ru01 P2 87.80(14) . . ? S1 Ru01 P2 92.28(7) . . ? N1 Ru01 P1 95.66(18) . . ? N11 Ru01 P1 83.87(18) . . ? O1 Ru01 P1 91.02(14) . . ? S1 Ru01 P1 91.74(8) . . ? P2 Ru01 P1 171.20(7) . . ? C211 P2 C231 105.7(4) . . ? C211 P2 C221 104.5(4) . . ? C231 P2 C221 101.3(3) . . ? C211 P2 Ru01 111.0(3) . . ? C231 P2 Ru01 115.2(3) . . ? C221 P2 Ru01 117.9(3) . . ? C111 P1 C121 105.0(4) . . ? C111 P1 C131 101.8(4) . . ? C121 P1 C131 103.3(5) . . ? C111 P1 Ru01 114.3(3) . . ? C121 P1 Ru01 114.7(3) . . ? C131 P1 Ru01 116.0(3) . . ? C226 C221 C222 118.0(7) . . ? C226 C221 P2 120.1(6) . . ? C222 C221 P2 121.6(6) . . ? C216 C211 C212 118.4(9) . . ? C216 C211 P2 120.3(8) . . ? C212 C211 P2 120.8(7) . . ? C236 C231 C232 117.4(7) . . ? C236 C231 P2 119.7(7) . . ? C232 C231 P2 122.9(6) . . ? C112 C111 C116 115.9(8) . . ? C112 C111 P1 119.5(7) . . ? C116 C111 P1 124.6(7) . . ? C136 C131 C132 119.2(8) . . ? C136 C131 P1 121.8(7) . . ? C132 C131 P1 119.0(8) . . ? C231 C232 C233 122.7(8) . . ? C223 C222 C221 121.5(8) . . ? C131 C136 C135 122.2(9) . . ? C235 C234 C233 120.3(9) . . ? C223 C224 C225 120.7(8) . . ? C221 C226 C225 120.4(8) . . ? C213 C212 C211 124.3(10) . . ? C126 C121 C122 117.4(10) . . ? C126 C121 P1 123.6(10) . . ? C122 C121 P1 119.0(8) . . ? C224 C225 C226 120.4(8) . . ? C224 C223 C222 119.0(8) . . ? C111 C116 C115 120.4(9) . . ? C211 C216 C215 118.6(11) . . ? C234 C235 C236 118.7(9) . . ? C234 C233 C232 120.1(9) . . ? C114 C115 C116 120.0(9) . . ? C114 C113 C112 119.1(9) . . ? C113 C112 C111 123.5(8) . . ? C231 C236 C235 120.7(9) . . ? C131 C132 C133 118.9(10) . . ? C136 C135 C134 119.8(10) . . ? C213 C214 C215 122.6(14) . . ? C133 C134 C135 118.6(11) . . ? C214 C215 C216 118.0(12) . . ? C121 C126 C125 126.3(12) . . ? C113 C114 C115 121.1(9) . . ? C134 C133 C132 121.2(11) . . ? C214 C213 C212 117.9(13) . . ? C1 S1 Ru01 97.1(3) . . ? C2 N1 N2 117.5(6) . . ? C2 N1 Ru01 122.1(5) . . ? N2 N1 Ru01 120.5(5) . . ? C11 N11 Ru01 178.7(6) . . ? N1 C2 C1 115.9(7) . . ? N1 C2 C4 120.3(7) . . ? C1 C2 C4 123.7(7) . . ? C2 C1 S1 122.0(6) . . ? N1 N2 C3 109.8(6) . . ? C125 C124 C123 126.8(14) . . ? C124 C123 C122 116.8(12) . . ? C124 C125 C126 114.6(14) . . ? O1 C3 N3 119.6(7) . . ? O1 C3 N2 125.4(7) . . ? N3 C3 N2 114.9(8) . . ? C3 O1 Ru01 106.7(5) . . ? N11 C11 S11 179.3(7) . . ? C123 C122 C121 118.1(11) . . ? N4 C6 C5 177.5(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.998 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 932348' ####################################################################### # # 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_try-2 #TrackingRef 'try-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37.5 N4.5 P2 Ru S3' _chemical_formula_weight 884.98 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' P P 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.509(5) _cell_length_b 12.844(5) _cell_length_c 13.672(5) _cell_angle_alpha 95.721(5) _cell_angle_beta 96.275(5) _cell_angle_gamma 104.012(5) _cell_volume 2100.3(14) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34097 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9547 _reflns_number_gt 5801 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0833P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9547 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1944 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _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 Ru1 Ru 0.28181(3) 0.30908(3) 0.25865(3) 0.03708(16) Uani 1 1 d . . . P1 P 0.22327(11) 0.47180(10) 0.27889(10) 0.0371(3) Uani 1 1 d . . . P2 P 0.31860(12) 0.13532(11) 0.24638(11) 0.0443(4) Uani 1 1 d . . . N11 N 0.1344(4) 0.2327(4) 0.3048(3) 0.0470(11) Uani 1 1 d . . . C121 C 0.0947(4) 0.4794(4) 0.2050(4) 0.0416(12) Uani 1 1 d . . . N1 N 0.4225(4) 0.3812(4) 0.2116(3) 0.0434(11) Uani 1 1 d . . . C211 C 0.4517(5) 0.1383(4) 0.2034(4) 0.0445(13) Uani 1 1 d . . . C231 C 0.3238(5) 0.0735(5) 0.3617(5) 0.0525(15) Uani 1 1 d . . . C111 C 0.3285(4) 0.5846(4) 0.2510(4) 0.0434(13) Uani 1 1 d . . . C131 C 0.1960(5) 0.5164(4) 0.4024(4) 0.0450(13) Uani 1 1 d . . . C221 C 0.2223(5) 0.0224(5) 0.1661(4) 0.0554(15) Uani 1 1 d . . . N2 N 0.4326(4) 0.3942(4) 0.1156(4) 0.0585(14) Uani 1 1 d . . . N3 N 0.3485(5) 0.3641(6) -0.0425(4) 0.094(2) Uani 1 1 d . . . H3A H 0.4111 0.3980 -0.0584 0.112 Uiso 1 1 calc R . . H3B H 0.2920 0.3385 -0.0876 0.112 Uiso 1 1 calc R . . C11 C 0.0491(5) 0.1857(4) 0.3246(4) 0.0487(14) Uani 1 1 d . . . C2 C 0.5177(5) 0.4224(5) 0.2732(4) 0.0506(14) Uani 1 1 d . . . C122 C 0.0751(5) 0.5751(5) 0.1864(5) 0.0658(18) Uani 1 1 d . . . H122 H 0.1310 0.6386 0.2055 0.079 Uiso 1 1 calc R . . C136 C 0.1683(5) 0.4431(5) 0.4701(4) 0.0515(14) Uani 1 1 d . . . H136 H 0.1708 0.3716 0.4546 0.062 Uiso 1 1 calc R . . C126 C 0.0098(5) 0.3872(5) 0.1756(4) 0.0519(15) Uani 1 1 d . . . H126 H 0.0215 0.3205 0.1872 0.062 Uiso 1 1 calc R . . C232 C 0.2742(5) 0.1037(5) 0.4390(5) 0.0566(16) Uani 1 1 d . . . H232 H 0.2413 0.1611 0.4353 0.068 Uiso 1 1 calc R . . C222 C 0.1116(5) 0.0179(5) 0.1427(4) 0.0633(17) Uani 1 1 d . . . H222 H 0.0849 0.0765 0.1646 0.076 Uiso 1 1 calc R . . C116 C 0.3317(6) 0.6069(5) 0.1547(5) 0.0644(17) Uani 1 1 d . . . H116 H 0.2755 0.5666 0.1057 0.077 Uiso 1 1 calc R . . C133 C 0.1598(6) 0.6562(6) 0.5182(5) 0.078(2) Uani 1 1 d . . . H133 H 0.1561 0.7273 0.5337 0.094 Uiso 1 1 calc R . . C236 C 0.3735(6) -0.0158(6) 0.3685(5) 0.076(2) Uani 1 1 d . . . H236 H 0.4098 -0.0393 0.3182 0.091 Uiso 1 1 calc R . . C1 C 0.5107(5) 0.4132(5) 0.3725(4) 0.0561(15) Uani 1 1 d . . . H1 H 0.5747 0.4398 0.4183 0.067 Uiso 1 1 calc R . . C125 C -0.0921(5) 0.3917(5) 0.1296(5) 0.0617(17) Uani 1 1 d . . . H125 H -0.1482 0.3281 0.1111 0.074 Uiso 1 1 calc R . . C216 C 0.4604(6) 0.1237(5) 0.1044(5) 0.0672(18) Uani 1 1 d . . . H216 H 0.3966 0.1093 0.0582 0.081 Uiso 1 1 calc R . . C233 C 0.2705(5) 0.0527(6) 0.5228(5) 0.0707(19) Uani 1 1 d . . . H233 H 0.2370 0.0770 0.5748 0.085 Uiso 1 1 calc R . . C112 C 0.4140(6) 0.6431(5) 0.3233(5) 0.0681(18) Uani 1 1 d . . . C135 C 0.1372(5) 0.4757(6) 0.5603(5) 0.0686(19) Uani 1 1 d . . . H135 H 0.1192 0.4266 0.6052 0.082 Uiso 1 1 calc R . . C134 C 0.1330(6) 0.5833(8) 0.5828(5) 0.080(2) Uani 1 1 d . . . H134 H 0.1116 0.6052 0.6429 0.096 Uiso 1 1 calc R . . C212 C 0.5487(5) 0.1672(5) 0.2704(5) 0.0650(17) Uani 1 1 d . . . H212 H 0.5447 0.1823 0.3377 0.078 Uiso 1 1 calc R . . C124 C -0.1117(6) 0.4861(6) 0.1111(5) 0.0680(19) Uani 1 1 d . . . H124 H -0.1810 0.4882 0.0801 0.082 Uiso 1 1 calc R . . C223 C 0.0385(6) -0.0734(6) 0.0865(5) 0.071(2) Uani 1 1 d . . . H223 H -0.0354 -0.0732 0.0691 0.086 Uiso 1 1 calc R . . C3 C 0.3389(6) 0.3507(5) 0.0544(4) 0.0598(17) Uani 1 1 d . . . C132 C 0.1927(6) 0.6236(5) 0.4283(5) 0.0643(17) Uani 1 1 d . . . H132 H 0.2128 0.6740 0.3849 0.077 Uiso 1 1 calc R . . C123 C -0.0292(6) 0.5799(6) 0.1381(5) 0.074(2) Uani 1 1 d . . . H123 H -0.0417 0.6459 0.1249 0.089 Uiso 1 1 calc R . . C213 C 0.6515(6) 0.1740(6) 0.2391(7) 0.081(2) Uani 1 1 d . . . H213 H 0.7162 0.1935 0.2847 0.097 Uiso 1 1 calc R . . C226 C 0.2542(6) -0.0723(5) 0.1375(5) 0.073(2) Uani 1 1 d . . . H226 H 0.3271 -0.0747 0.1569 0.087 Uiso 1 1 calc R . . C224 C 0.0717(7) -0.1603(6) 0.0574(5) 0.079(2) Uani 1 1 d . . . H224 H 0.0209 -0.2201 0.0205 0.095 Uiso 1 1 calc R . . C215 C 0.5600(8) 0.1300(6) 0.0727(6) 0.087(2) Uani 1 1 d . . . H215 H 0.5636 0.1196 0.0049 0.105 Uiso 1 1 calc R . . C234 C 0.3159(6) -0.0340(7) 0.5302(6) 0.085(2) Uani 1 1 d . . . H234 H 0.3127 -0.0691 0.5865 0.102 Uiso 1 1 calc R . . C225 C 0.1806(7) -0.1633(6) 0.0811(6) 0.085(2) Uani 1 1 d . . . H225 H 0.2045 -0.2240 0.0603 0.102 Uiso 1 1 calc R . . C113 C 0.5004(6) 0.7239(6) 0.3009(7) 0.089(2) Uani 1 1 d . . . C214 C 0.6563(7) 0.1514(6) 0.1390(8) 0.093(3) Uani 1 1 d . . . H214 H 0.7237 0.1506 0.1167 0.112 Uiso 1 1 calc R . . C235 C 0.3642(7) -0.0663(6) 0.4560(7) 0.094(3) Uani 1 1 d . . . H235 H 0.3939 -0.1256 0.4613 0.112 Uiso 1 1 calc R . . C115 C 0.4163(8) 0.6878(7) 0.1276(7) 0.092(3) Uani 1 1 d . . . C114 C 0.5008(8) 0.7455(7) 0.2051(10) 0.113(4) Uani 1 1 d . . . S11 S -0.06817(16) 0.11644(15) 0.34985(18) 0.0869(6) Uani 1 1 d . . . S1 S 0.39395(12) 0.35717(12) 0.41228(10) 0.0464(4) Uani 1 1 d . . . S2 S 0.21448(14) 0.28225(14) 0.08606(11) 0.0598(4) Uani 1 1 d . . . C4 C 0.6253(5) 0.4763(6) 0.2403(5) 0.089(2) Uani 1 1 d . . . H4A H 0.6517 0.4235 0.2018 0.133 Uiso 1 1 calc R . . H4B H 0.6792 0.5087 0.2974 0.133 Uiso 1 1 calc R . . H4C H 0.6140 0.5313 0.2005 0.133 Uiso 1 1 calc R . . C6 C 0.1015(10) 0.2019(8) 0.7124(8) 0.039(2) Uani 0.50 1 d P . . N4 N 0.1765(9) 0.2357(8) 0.7617(7) 0.054(3) Uani 0.50 1 d P . . C5 C -0.0054(10) 0.1523(8) 0.6513(8) 0.047(3) Uani 0.50 1 d P . . 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 0.0358(3) 0.0372(3) 0.0376(3) 0.00034(18) 0.00356(18) 0.01056(19) P1 0.0386(8) 0.0353(7) 0.0364(8) 0.0009(6) 0.0038(6) 0.0097(6) P2 0.0380(8) 0.0387(8) 0.0542(9) -0.0038(7) 0.0008(7) 0.0126(6) N11 0.043(3) 0.040(3) 0.060(3) 0.009(2) 0.006(2) 0.012(2) C121 0.044(3) 0.045(3) 0.040(3) 0.006(2) 0.008(2) 0.017(3) N1 0.045(3) 0.055(3) 0.037(2) 0.009(2) 0.012(2) 0.021(2) C211 0.046(3) 0.037(3) 0.051(4) 0.002(2) 0.006(3) 0.014(3) C231 0.046(3) 0.046(3) 0.067(4) 0.018(3) 0.008(3) 0.010(3) C111 0.043(3) 0.040(3) 0.049(3) 0.005(3) 0.011(3) 0.013(3) C131 0.044(3) 0.053(3) 0.039(3) -0.002(3) 0.004(2) 0.019(3) C221 0.049(4) 0.052(4) 0.062(4) -0.008(3) 0.003(3) 0.015(3) N2 0.050(3) 0.091(4) 0.045(3) 0.018(3) 0.013(2) 0.030(3) N3 0.074(4) 0.168(7) 0.048(3) 0.020(4) 0.011(3) 0.044(4) C11 0.048(4) 0.040(3) 0.058(4) 0.005(3) 0.006(3) 0.014(3) C2 0.033(3) 0.057(4) 0.058(4) 0.014(3) 0.001(3) 0.004(3) C122 0.056(4) 0.053(4) 0.086(5) 0.011(3) -0.008(3) 0.015(3) C136 0.043(3) 0.064(4) 0.045(3) -0.002(3) 0.011(3) 0.010(3) C126 0.053(4) 0.048(3) 0.052(4) 0.005(3) 0.002(3) 0.011(3) C232 0.041(3) 0.056(4) 0.074(4) 0.018(3) 0.008(3) 0.012(3) C222 0.062(4) 0.065(4) 0.055(4) -0.003(3) -0.001(3) 0.008(3) C116 0.058(4) 0.064(4) 0.073(5) 0.014(3) 0.018(3) 0.013(3) C133 0.089(6) 0.085(5) 0.064(5) -0.021(4) 0.013(4) 0.040(5) C236 0.081(5) 0.075(5) 0.083(5) 0.018(4) 0.014(4) 0.037(4) C1 0.050(4) 0.058(4) 0.056(4) 0.007(3) -0.002(3) 0.010(3) C125 0.045(4) 0.064(4) 0.069(4) 0.000(3) -0.006(3) 0.011(3) C216 0.063(5) 0.075(5) 0.060(4) 0.010(3) 0.014(3) 0.008(4) C233 0.055(4) 0.082(5) 0.083(5) 0.040(4) 0.020(3) 0.016(4) C112 0.053(4) 0.054(4) 0.090(5) -0.006(4) 0.003(4) 0.009(3) C135 0.054(4) 0.103(6) 0.042(4) 0.000(4) 0.011(3) 0.011(4) C134 0.058(5) 0.127(7) 0.047(4) -0.024(5) 0.007(3) 0.025(5) C212 0.046(4) 0.085(5) 0.064(4) 0.008(4) 0.009(3) 0.015(4) C124 0.050(4) 0.095(6) 0.061(4) 0.010(4) -0.003(3) 0.027(4) C223 0.062(5) 0.073(5) 0.062(4) 0.009(4) -0.014(3) -0.005(4) C3 0.066(4) 0.089(5) 0.033(3) 0.008(3) 0.010(3) 0.036(4) C132 0.081(5) 0.060(4) 0.055(4) -0.003(3) 0.016(3) 0.025(4) C123 0.076(5) 0.070(5) 0.085(5) 0.017(4) -0.002(4) 0.037(4) C213 0.046(4) 0.087(5) 0.111(7) 0.028(5) 0.009(4) 0.014(4) C226 0.072(5) 0.057(4) 0.084(5) -0.005(4) 0.000(4) 0.015(4) C224 0.091(6) 0.058(4) 0.072(5) -0.008(4) -0.017(4) 0.008(4) C215 0.103(7) 0.074(5) 0.082(6) 0.003(4) 0.048(5) 0.006(5) C234 0.075(5) 0.099(6) 0.091(6) 0.052(5) 0.028(4) 0.019(5) C225 0.096(6) 0.057(4) 0.087(5) -0.011(4) -0.016(5) 0.015(4) C113 0.068(5) 0.059(5) 0.130(7) -0.001(5) 0.032(5) -0.004(4) C214 0.075(6) 0.083(6) 0.133(8) 0.018(5) 0.063(6) 0.021(5) C235 0.110(7) 0.065(5) 0.122(7) 0.051(5) 0.019(6) 0.037(5) C115 0.090(6) 0.068(5) 0.136(8) 0.042(5) 0.058(6) 0.025(5) C114 0.083(7) 0.063(5) 0.203(12) 0.035(7) 0.065(7) 0.011(5) S11 0.0565(11) 0.0651(12) 0.1408(19) 0.0127(12) 0.0428(12) 0.0059(9) S1 0.0458(8) 0.0487(8) 0.0400(8) 0.0026(6) -0.0002(6) 0.0072(7) S2 0.0559(10) 0.0821(12) 0.0378(8) -0.0063(8) -0.0044(7) 0.0213(9) C4 0.048(4) 0.128(7) 0.084(5) 0.041(5) 0.005(4) 0.003(4) C6 0.057(7) 0.037(6) 0.032(6) 0.004(5) 0.011(5) 0.029(6) N4 0.062(7) 0.058(6) 0.048(6) 0.011(5) 0.018(5) 0.023(6) C5 0.064(8) 0.042(6) 0.038(6) 0.002(5) -0.007(5) 0.024(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 Ru1 N1 1.987(4) . ? Ru1 N11 2.064(5) . ? Ru1 S1 2.3321(15) . ? Ru1 P1 2.3772(15) . ? Ru1 S2 2.3788(17) . ? Ru1 P2 2.3791(16) . ? P1 C111 1.809(6) . ? P1 C131 1.823(6) . ? P1 C121 1.832(5) . ? P2 C221 1.818(6) . ? P2 C211 1.818(6) . ? P2 C231 1.837(6) . ? N11 C11 1.166(7) . ? C121 C122 1.353(7) . ? C121 C126 1.377(7) . ? N1 C2 1.339(7) . ? N1 N2 1.355(6) . ? C211 C216 1.368(8) . ? C211 C212 1.386(8) . ? C231 C232 1.353(8) . ? C231 C236 1.436(8) . ? C111 C116 1.377(8) . ? C111 C112 1.385(8) . ? C131 C136 1.396(7) . ? C131 C132 1.399(8) . ? C221 C222 1.373(8) . ? C221 C226 1.402(8) . ? N2 C3 1.326(8) . ? N3 C3 1.368(7) . ? C11 S11 1.614(6) . ? C2 C1 1.385(8) . ? C2 C4 1.495(8) . ? C122 C123 1.415(8) . ? C136 C135 1.389(8) . ? C126 C125 1.375(8) . ? C232 C233 1.375(8) . ? C222 C223 1.397(8) . ? C116 C115 1.402(9) . ? C133 C134 1.359(10) . ? C133 C132 1.395(9) . ? C236 C235 1.419(9) . ? C1 S1 1.640(6) . ? C125 C124 1.337(8) . ? C216 C215 1.350(10) . ? C233 C234 1.374(10) . ? C112 C113 1.389(9) . ? C135 C134 1.401(10) . ? C212 C213 1.385(9) . ? C124 C123 1.370(9) . ? C223 C224 1.322(9) . ? C3 S2 1.716(7) . ? C213 C214 1.381(11) . ? C226 C225 1.396(9) . ? C224 C225 1.376(10) . ? C215 C214 1.379(11) . ? C234 C235 1.318(10) . ? C113 C114 1.367(13) . ? C115 C114 1.418(13) . ? C6 N4 1.063(13) . ? C6 C5 1.459(16) . ? 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 N11 178.88(18) . . ? N1 Ru1 S1 81.91(13) . . ? N11 Ru1 S1 99.15(13) . . ? N1 Ru1 P1 93.08(13) . . ? N11 Ru1 P1 87.25(12) . . ? S1 Ru1 P1 90.87(5) . . ? N1 Ru1 S2 82.18(13) . . ? N11 Ru1 S2 96.75(13) . . ? S1 Ru1 S2 164.08(6) . . ? P1 Ru1 S2 90.54(5) . . ? N1 Ru1 P2 94.42(13) . . ? N11 Ru1 P2 85.25(12) . . ? S1 Ru1 P2 89.98(5) . . ? P1 Ru1 P2 172.50(5) . . ? S2 Ru1 P2 90.68(6) . . ? C111 P1 C131 104.1(3) . . ? C111 P1 C121 104.5(2) . . ? C131 P1 C121 99.8(2) . . ? C111 P1 Ru1 110.70(18) . . ? C131 P1 Ru1 116.96(18) . . ? C121 P1 Ru1 118.95(18) . . ? C221 P2 C211 103.6(3) . . ? C221 P2 C231 98.8(3) . . ? C211 P2 C231 105.0(3) . . ? C221 P2 Ru1 119.7(2) . . ? C211 P2 Ru1 111.80(17) . . ? C231 P2 Ru1 116.1(2) . . ? C11 N11 Ru1 175.5(5) . . ? C122 C121 C126 117.7(5) . . ? C122 C121 P1 121.9(5) . . ? C126 C121 P1 120.0(4) . . ? C2 N1 N2 113.3(5) . . ? C2 N1 Ru1 122.5(4) . . ? N2 N1 Ru1 124.2(4) . . ? C216 C211 C212 118.2(6) . . ? C216 C211 P2 121.2(5) . . ? C212 C211 P2 120.2(5) . . ? C232 C231 C236 118.0(6) . . ? C232 C231 P2 121.9(4) . . ? C236 C231 P2 119.9(5) . . ? C116 C111 C112 118.3(6) . . ? C116 C111 P1 120.3(5) . . ? C112 C111 P1 121.1(5) . . ? C136 C131 C132 118.3(5) . . ? C136 C131 P1 121.2(4) . . ? C132 C131 P1 120.3(4) . . ? C222 C221 C226 116.0(6) . . ? C222 C221 P2 122.4(5) . . ? C226 C221 P2 120.8(5) . . ? C3 N2 N1 113.1(5) . . ? N11 C11 S11 177.8(5) . . ? N1 C2 C1 115.2(5) . . ? N1 C2 C4 124.0(5) . . ? C1 C2 C4 120.8(5) . . ? C121 C122 C123 121.0(6) . . ? C135 C136 C131 120.8(6) . . ? C125 C126 C121 121.5(5) . . ? C231 C232 C233 122.4(6) . . ? C221 C222 C223 120.8(7) . . ? C111 C116 C115 122.8(7) . . ? C134 C133 C132 119.5(7) . . ? C235 C236 C231 116.6(7) . . ? C2 C1 S1 122.5(5) . . ? C124 C125 C126 120.9(6) . . ? C215 C216 C211 121.1(7) . . ? C234 C233 C232 120.6(7) . . ? C111 C112 C113 121.6(7) . . ? C136 C135 C134 119.3(7) . . ? C133 C134 C135 121.0(6) . . ? C213 C212 C211 121.3(7) . . ? C125 C124 C123 119.7(6) . . ? C224 C223 C222 121.7(7) . . ? N2 C3 N3 113.3(6) . . ? N2 C3 S2 126.6(4) . . ? N3 C3 S2 120.1(5) . . ? C133 C132 C131 121.1(6) . . ? C124 C123 C122 119.3(6) . . ? C214 C213 C212 118.8(7) . . ? C225 C226 C221 122.5(7) . . ? C223 C224 C225 120.8(7) . . ? C216 C215 C214 121.1(7) . . ? C235 C234 C233 118.7(7) . . ? C224 C225 C226 117.9(7) . . ? C114 C113 C112 119.0(8) . . ? C215 C214 C213 119.2(7) . . ? C234 C235 C236 123.7(7) . . ? C116 C115 C114 116.2(8) . . ? C113 C114 C115 122.2(8) . . ? C1 S1 Ru1 97.8(2) . . ? C3 S2 Ru1 93.8(2) . . ? N4 C6 C5 175.5(13) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.057 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.116 _database_code_depnum_ccdc_archive 'CCDC 932349'