Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Roberta Sessoli' _publ_contact_author_address ; Dipartimento di Chimica Universita degli Studi di Firenze Via Della Lastruccia 3 50019 - Sesto Fiorentino Firenze 50019 ITALY ; _publ_contact_author_email ROBERTA.SESSOLI@UNIFI.IT _publ_section_title ; Ferromagnetic interactions in Ru(III)-Nitronyl Nitroxide radical complex: A potential 2p4d building block for molecular magnets ; loop_ _publ_author_name 'Roberta Sessoli' 'Kevin Bernot' 'Dante Gatteschi' 'Fabrice Pointillart' 'Lorenzo Sorace' data_RusalenN3 _database_code_depnum_ccdc_archive 'CCDC 629621' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H29 N5 O2 P Ru' _chemical_formula_sum 'C34 H29 N5 O2 P Ru' _chemical_formula_weight 671.66 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' P P 0.1023 0.0942 '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 'P 1 21/c 1' 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 11.052(3) _cell_length_b 22.395(7) _cell_length_c 12.428(4) _cell_angle_alpha 90 _cell_angle_beta 102.388(5) _cell_angle_gamma 90 _cell_volume 3004.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 13057 _cell_measurement_theta_min 3.93 _cell_measurement_theta_max 20.59 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; 'abspack(Crysalis RED,Oxford diffraction Ltd.)' ; _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_T_max 0.936 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13057 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 20.59 _reflns_number_total 3014 _reflns_number_gt 2516 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0832P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3014 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 0.44681(4) 0.159249(19) 0.16421(3) 0.0313(3) Uani 1 1 d . . . P1 P 0.30492(14) 0.09592(7) 0.22560(12) 0.0322(4) Uani 1 1 d . . . N1 N 0.3269(4) 0.22720(19) 0.1365(4) 0.0336(12) Uani 1 1 d . . . N2 N 0.5063(5) 0.2014(2) 0.3060(4) 0.0370(12) Uani 1 1 d . . . N3 N 0.5778(5) 0.2083(3) 0.0951(4) 0.0418(14) Uani 1 1 d . . . N4 N 0.6450(7) 0.2418(3) 0.1405(5) 0.0494(15) Uani 1 1 d . . . N5 N 0.7226(8) 0.2759(3) 0.1839(7) 0.095(2) Uani 1 1 d . . . O1 O 0.3827(4) 0.12956(17) 0.0097(3) 0.0417(10) Uani 1 1 d . . . O2 O 0.5763(4) 0.09583(16) 0.2085(3) 0.0403(10) Uani 1 1 d . . . C1 C 0.2728(6) 0.1413(3) -0.0488(5) 0.0390(16) Uani 1 1 d . . . C2 C 0.2226(7) 0.1029(3) -0.1379(5) 0.0564(19) Uani 1 1 d . . . C3 C 0.1090(8) 0.1129(4) -0.2042(5) 0.065(2) Uani 1 1 d . . . C4 C 0.0381(8) 0.1620(4) -0.1912(6) 0.066(2) Uani 1 1 d . . . C5 C 0.0834(6) 0.2010(3) -0.1080(6) 0.0540(19) Uani 1 1 d . . . C6 C 0.1981(6) 0.1914(3) -0.0334(5) 0.0409(16) Uani 1 1 d . . . C7 C 0.2350(6) 0.2329(3) 0.0534(6) 0.0456(17) Uani 1 1 d . . . C8 C 0.3611(6) 0.2751(3) 0.2203(5) 0.0512(18) Uani 1 1 d . . . C9 C 0.4187(6) 0.2460(3) 0.3295(5) 0.0432(16) Uani 1 1 d . . . C10 C 0.6125(7) 0.1938(3) 0.3720(5) 0.0502(18) Uani 1 1 d . . . C11 C 0.7028(6) 0.1491(3) 0.3627(5) 0.0491(18) Uani 1 1 d . . . C12 C 0.8134(7) 0.1498(4) 0.4428(6) 0.073(2) Uani 1 1 d . . . C13 C 0.9016(8) 0.1061(5) 0.4434(7) 0.090(3) Uani 1 1 d . . . C14 C 0.8810(8) 0.0620(4) 0.3646(8) 0.081(3) Uani 1 1 d . . . C15 C 0.7737(7) 0.0598(3) 0.2866(7) 0.064(2) Uani 1 1 d . . . C16 C 0.6799(6) 0.1028(3) 0.2828(5) 0.0433(17) Uani 1 1 d . . . C17 C 0.1407(5) 0.1134(2) 0.1765(5) 0.0319(14) Uani 1 1 d . . . C18 C 0.0655(6) 0.0781(3) 0.1002(5) 0.0418(16) Uani 1 1 d . . . C19 C -0.0564(6) 0.0931(3) 0.0587(5) 0.0519(18) Uani 1 1 d . . . C20 C -0.1041(6) 0.1442(3) 0.0969(6) 0.0582(19) Uani 1 1 d . . . C21 C -0.0311(6) 0.1794(3) 0.1721(5) 0.0510(19) Uani 1 1 d . . . C22 C 0.0926(6) 0.1650(3) 0.2117(5) 0.0416(17) Uani 1 1 d . . . C23 C 0.3168(5) 0.0173(2) 0.1906(5) 0.0351(15) Uani 1 1 d . . . C24 C 0.2630(6) -0.0257(3) 0.2461(5) 0.0464(16) Uani 1 1 d . . . C25 C 0.2735(7) -0.0860(3) 0.2233(6) 0.060(2) Uani 1 1 d . . . C26 C 0.3372(6) -0.1033(3) 0.1460(7) 0.061(2) Uani 1 1 d . . . C27 C 0.3890(6) -0.0612(3) 0.0886(6) 0.063(2) Uani 1 1 d . . . C28 C 0.3786(6) -0.0014(3) 0.1113(6) 0.0516(18) Uani 1 1 d . . . C29 C 0.3271(6) 0.0915(2) 0.3755(5) 0.0366(15) Uani 1 1 d . . . C30 C 0.4456(6) 0.0796(3) 0.4336(5) 0.0533(18) Uani 1 1 d . . . C31 C 0.4687(7) 0.0730(3) 0.5474(6) 0.064(2) Uani 1 1 d . . . C32 C 0.3759(9) 0.0771(3) 0.6017(6) 0.064(2) Uani 1 1 d . . . C33 C 0.2590(8) 0.0889(3) 0.5466(6) 0.069(2) Uani 1 1 d . . . C34 C 0.2342(6) 0.0966(3) 0.4333(5) 0.0527(18) Uani 1 1 d . . . H20 H 0.2684 0.0700 -0.1515 0.068 Uiso 1 1 calc R . . H30 H 0.0784 0.0857 -0.2599 0.078 Uiso 1 1 calc R . . H40 H -0.0385 0.1684 -0.2381 0.079 Uiso 1 1 calc R . . H50 H 0.0376 0.2349 -0.1000 0.065 Uiso 1 1 calc R . . H70 H 0.1885 0.2677 0.0502 0.055 Uiso 1 1 calc R . . H80 H 0.2880 0.2975 0.2270 0.061 Uiso 1 1 calc R . . H81 H 0.4197 0.3023 0.1984 0.061 Uiso 1 1 calc R . . H90 H 0.3555 0.2271 0.3612 0.052 Uiso 1 1 calc R . . H91 H 0.4614 0.2756 0.3810 0.052 Uiso 1 1 calc R . . H100 H 0.6325 0.2199 0.4314 0.060 Uiso 1 1 calc R . . H120 H 0.8275 0.1799 0.4957 0.088 Uiso 1 1 calc R . . H130 H 0.9747 0.1065 0.4969 0.109 Uiso 1 1 calc R . . H140 H 0.9415 0.0332 0.3646 0.098 Uiso 1 1 calc R . . H150 H 0.7621 0.0293 0.2347 0.077 Uiso 1 1 calc R . . H180 H 0.0973 0.0434 0.0759 0.050 Uiso 1 1 calc R . . H190 H -0.1061 0.0693 0.0057 0.062 Uiso 1 1 calc R . . H200 H -0.1868 0.1543 0.0706 0.070 Uiso 1 1 calc R . . H210 H -0.0639 0.2135 0.1976 0.061 Uiso 1 1 calc R . . H220 H 0.1430 0.1900 0.2620 0.050 Uiso 1 1 calc R . . H240 H 0.2197 -0.0140 0.2990 0.056 Uiso 1 1 calc R . . H250 H 0.2371 -0.1146 0.2607 0.071 Uiso 1 1 calc R . . H260 H 0.3458 -0.1437 0.1319 0.073 Uiso 1 1 calc R . . H270 H 0.4307 -0.0730 0.0347 0.075 Uiso 1 1 calc R . . H280 H 0.4139 0.0268 0.0725 0.062 Uiso 1 1 calc R . . H300 H 0.5101 0.0761 0.3967 0.064 Uiso 1 1 calc R . . H310 H 0.5489 0.0656 0.5864 0.077 Uiso 1 1 calc R . . H320 H 0.3923 0.0718 0.6776 0.077 Uiso 1 1 calc R . . H330 H 0.1954 0.0919 0.5846 0.083 Uiso 1 1 calc R . . H340 H 0.1540 0.1053 0.3958 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0292(4) 0.0326(4) 0.0326(4) -0.0026(2) 0.0076(3) 0.0021(2) P1 0.0273(10) 0.0348(9) 0.0346(9) -0.0004(7) 0.0071(7) 0.0027(7) N1 0.034(3) 0.030(3) 0.037(3) -0.002(2) 0.008(3) 0.002(2) N2 0.037(3) 0.043(3) 0.032(3) -0.006(2) 0.009(3) -0.003(3) N3 0.042(4) 0.051(4) 0.033(3) -0.005(3) 0.008(3) -0.014(3) N4 0.050(5) 0.047(4) 0.059(4) 0.008(3) 0.028(4) 0.007(3) N5 0.084(6) 0.069(5) 0.131(6) -0.014(5) 0.021(5) -0.015(5) O1 0.043(3) 0.050(3) 0.031(2) -0.010(2) 0.005(2) 0.006(2) O2 0.032(3) 0.038(2) 0.050(3) 0.002(2) 0.007(2) 0.008(2) C1 0.046(5) 0.044(4) 0.029(4) 0.000(3) 0.013(4) -0.012(4) C2 0.063(6) 0.063(5) 0.047(4) -0.010(4) 0.020(4) -0.016(4) C3 0.070(6) 0.080(6) 0.040(4) -0.006(4) -0.001(5) -0.027(5) C4 0.064(6) 0.085(6) 0.040(5) 0.011(4) -0.005(4) -0.029(5) C5 0.043(5) 0.061(5) 0.055(5) 0.027(4) 0.004(4) 0.000(4) C6 0.045(4) 0.050(4) 0.027(4) 0.001(3) 0.006(3) -0.006(4) C7 0.037(4) 0.044(4) 0.055(4) 0.019(4) 0.008(4) 0.007(3) C8 0.052(5) 0.040(4) 0.062(5) -0.015(4) 0.013(4) 0.005(3) C9 0.038(4) 0.051(4) 0.039(4) -0.015(3) 0.006(3) 0.003(3) C10 0.046(5) 0.060(5) 0.041(4) -0.017(4) 0.002(4) -0.006(4) C11 0.027(4) 0.069(5) 0.049(4) -0.004(4) 0.004(4) 0.002(4) C12 0.037(5) 0.116(7) 0.061(5) -0.010(5) -0.002(4) 0.003(5) C13 0.037(6) 0.140(9) 0.084(6) 0.017(6) -0.009(5) 0.008(6) C14 0.039(6) 0.082(6) 0.120(8) 0.025(6) 0.010(6) 0.023(5) C15 0.032(5) 0.060(5) 0.099(6) 0.010(4) 0.013(5) 0.011(4) C16 0.026(4) 0.047(4) 0.056(4) 0.018(4) 0.007(4) -0.003(4) C17 0.027(4) 0.033(3) 0.036(3) -0.003(3) 0.006(3) 0.006(3) C18 0.045(5) 0.042(4) 0.039(4) -0.003(3) 0.009(3) 0.007(4) C19 0.038(5) 0.057(5) 0.053(4) -0.009(4) -0.008(4) 0.006(4) C20 0.028(4) 0.075(5) 0.065(5) -0.009(4) -0.004(4) 0.009(4) C21 0.046(5) 0.052(4) 0.055(5) -0.008(4) 0.009(4) 0.015(4) C22 0.028(4) 0.056(4) 0.039(4) -0.004(3) 0.002(3) -0.001(3) C23 0.024(4) 0.034(4) 0.045(4) -0.007(3) 0.002(3) 0.002(3) C24 0.043(4) 0.037(4) 0.056(4) 0.001(3) 0.004(3) -0.009(3) C25 0.049(5) 0.047(5) 0.071(5) 0.011(4) -0.011(4) -0.009(4) C26 0.039(5) 0.036(4) 0.091(6) -0.008(4) -0.023(4) 0.001(4) C27 0.043(5) 0.056(5) 0.089(6) -0.027(4) 0.013(4) 0.005(4) C28 0.042(4) 0.036(4) 0.078(5) -0.011(4) 0.015(4) 0.005(3) C29 0.032(4) 0.037(4) 0.039(4) 0.001(3) 0.004(3) -0.005(3) C30 0.038(5) 0.075(5) 0.044(5) 0.006(4) 0.005(4) 0.007(4) C31 0.052(5) 0.077(5) 0.052(5) 0.012(4) -0.015(4) -0.005(4) C32 0.080(6) 0.074(5) 0.037(4) 0.011(4) 0.013(5) 0.004(5) C33 0.062(6) 0.103(6) 0.045(5) 0.010(4) 0.019(4) 0.003(5) C34 0.043(5) 0.078(5) 0.038(4) 0.006(4) 0.011(4) 0.007(4) _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 N2 1.983(5) . ? Ru1 N1 1.999(5) . ? Ru1 O2 2.008(4) . ? Ru1 O1 2.012(4) . ? Ru1 N3 2.139(5) . ? Ru1 P1 2.3591(16) . ? P1 C23 1.825(6) . ? P1 C17 1.829(6) . ? P1 C29 1.829(6) . ? N1 C7 1.290(7) . ? N2 C10 1.291(8) . ? N2 C9 1.463(7) . ? N3 N4 1.118(8) . ? N4 N5 1.189(9) . ? O1 C1 1.302(7) . ? O2 C16 1.317(7) . ? C1 C2 1.418(8) . ? C1 C6 1.430(9) . ? C2 C3 1.364(9) . ? C4 C5 1.363(9) . ? C4 C3 1.381(10) . ? C6 C7 1.416(9) . ? C6 C5 1.417(8) . ? C8 N1 1.486(7) . ? C9 C8 1.517(8) . ? C11 C12 1.401(9) . ? C11 C10 1.437(9) . ? C12 C13 1.380(11) . ? C14 C15 1.362(11) . ? C14 C13 1.375(12) . ? C16 C15 1.408(9) . ? C16 C11 1.420(9) . ? C17 C18 1.371(8) . ? C17 C22 1.381(7) . ? C18 C19 1.377(8) . ? C19 C20 1.385(9) . ? C21 C20 1.350(9) . ? C22 C21 1.388(8) . ? C23 C28 1.378(8) . ? C23 C24 1.391(8) . ? C24 C25 1.391(9) . ? C25 C26 1.364(9) . ? C27 C26 1.379(9) . ? C28 C27 1.378(9) . ? C29 C34 1.378(8) . ? C29 C30 1.378(8) . ? C30 C31 1.390(9) . ? C31 C32 1.346(10) . ? C33 C32 1.351(10) . ? C34 C33 1.386(9) . ? 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 N2 Ru1 N1 82.6(2) . . ? N2 Ru1 O2 90.72(18) . . ? N1 Ru1 O2 173.31(17) . . ? N2 Ru1 O1 170.87(17) . . ? N1 Ru1 O1 90.16(18) . . ? O2 Ru1 O1 96.43(16) . . ? N2 Ru1 N3 89.3(2) . . ? N1 Ru1 N3 91.18(19) . . ? O2 Ru1 N3 88.25(18) . . ? O1 Ru1 N3 85.21(19) . . ? N2 Ru1 P1 96.62(14) . . ? N1 Ru1 P1 92.92(13) . . ? O2 Ru1 P1 88.31(12) . . ? O1 Ru1 P1 89.29(12) . . ? N3 Ru1 P1 173.15(15) . . ? C23 P1 C17 104.1(3) . . ? C23 P1 C29 100.9(3) . . ? C17 P1 C29 105.0(3) . . ? C23 P1 Ru1 114.57(19) . . ? C17 P1 Ru1 116.35(19) . . ? C29 P1 Ru1 114.1(2) . . ? N4 N3 Ru1 125.1(4) . . ? C16 O2 Ru1 124.7(4) . . ? C5 C4 C3 118.2(8) . . ? C1 O1 Ru1 124.1(3) . . ? C18 C17 C22 118.9(5) . . ? C18 C17 P1 121.2(4) . . ? C22 C17 P1 119.7(5) . . ? N3 N4 N5 174.9(7) . . ? C10 N2 C9 120.9(5) . . ? C10 N2 Ru1 125.8(4) . . ? C9 N2 Ru1 113.3(4) . . ? C34 C29 C30 118.2(6) . . ? C34 C29 P1 125.0(5) . . ? C30 C29 P1 116.7(5) . . ? N2 C9 C8 106.5(5) . . ? C28 C23 C24 118.3(5) . . ? C28 C23 P1 122.4(5) . . ? C24 C23 P1 119.3(4) . . ? C25 C24 C23 120.6(6) . . ? C17 C22 C21 119.9(6) . . ? C29 C34 C33 120.8(7) . . ? C17 C18 C19 121.2(6) . . ? C29 C30 C31 120.0(6) . . ? C23 C28 C27 121.2(6) . . ? O1 C1 C2 118.4(6) . . ? O1 C1 C6 125.5(5) . . ? C2 C1 C6 116.1(6) . . ? C18 C19 C20 119.1(6) . . ? C20 C21 C22 120.4(6) . . ? O2 C16 C15 117.7(6) . . ? O2 C16 C11 125.1(6) . . ? C15 C16 C11 117.1(6) . . ? C7 C6 C5 118.1(6) . . ? C7 C6 C1 122.4(6) . . ? C5 C6 C1 119.4(6) . . ? C12 C11 C16 120.2(6) . . ? C12 C11 C10 116.7(7) . . ? C16 C11 C10 122.9(6) . . ? C26 C25 C24 119.8(7) . . ? N1 C8 C9 108.2(5) . . ? C4 C5 C6 122.1(7) . . ? C7 N1 C8 121.8(5) . . ? C7 N1 Ru1 126.3(4) . . ? C8 N1 Ru1 111.7(4) . . ? N2 C10 C11 126.4(6) . . ? C3 C2 C1 121.9(7) . . ? N1 C7 C6 126.4(6) . . ? C32 C33 C34 119.9(7) . . ? C21 C20 C19 120.4(7) . . ? C32 C31 C30 120.6(7) . . ? C2 C3 C4 122.1(7) . . ? C15 C14 C13 121.3(7) . . ? C28 C27 C26 119.7(7) . . ? C31 C32 C33 120.5(6) . . ? C25 C26 C27 120.3(6) . . ? C13 C12 C11 120.1(8) . . ? C14 C15 C16 121.4(7) . . ? C14 C13 C12 119.8(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 20.59 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.546 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.148 data_RusalenNITpPy _database_code_depnum_ccdc_archive 'CCDC 629622' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C46 H45 N5 O4 P Ru),(Cl O4),2(O)' _chemical_formula_sum 'C46 H45 Cl N5 O10 P Ru' _chemical_formula_weight 995.38 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 15.492(4) _cell_length_b 18.354(5) _cell_length_c 19.038(6) _cell_angle_alpha 112.120(4) _cell_angle_beta 93.650(5) _cell_angle_gamma 100.473(6) _cell_volume 4879(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 35387 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 21.72 _exptl_crystal_description cube _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.46827 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ; 'abspack(Crysalis RED,Oxford diffraction Ltd.)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35387 _diffrn_reflns_av_R_equivalents 0.1335 _diffrn_reflns_av_sigmaI/netI 0.3137 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 21.72 _reflns_number_total 11427 _reflns_number_gt 3466 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. One of the perchlorate anions has been found to be severely disordered. The positions of its constituent atoms have then been restrained to tetrahedral geometry before the last refinement cycles, and the position of one oxygen atom has been kept fixed. We found four water molecules per unit cell. Given the low diffracting power of the crystal it has not been possible to locate their hydrogen atoms on the difference maps. ; _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^)+(0.0718P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11427 _refine_ls_number_parameters 1108 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.2252 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2010 _refine_ls_wR_factor_gt 0.1532 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.859 _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 0.21350(7) 0.32905(7) 0.62775(6) 0.0642(5) Uani 1 1 d . . . Ru2 Ru 0.25016(8) 0.17505(7) 0.92726(7) 0.0707(5) Uani 1 1 d . . . P1 P 0.3454(3) 0.3864(2) 0.5947(2) 0.0725(13) Uani 1 1 d . . . P2 P 0.3689(3) 0.1150(2) 0.9386(2) 0.0732(13) Uani 1 1 d . . . O1 O 0.2815(5) 0.3356(6) 0.7251(5) 0.073(3) Uani 1 1 d . . . O2 O 0.2254(6) 0.2183(5) 0.5623(4) 0.070(3) Uani 1 1 d . . . O3 O -0.2286(7) 0.1442(9) 0.6604(8) 0.165(6) Uani 1 1 d . . . O4 O -0.0238(8) 0.0753(7) 0.7924(6) 0.112(4) Uani 1 1 d . . . O5 O 0.2798(6) 0.1790(6) 0.8272(5) 0.072(3) Uani 1 1 d . . . O6 O 0.3325(7) 0.2798(6) 0.9921(6) 0.077(4) Uani 1 1 d . . . O7 O -0.1504(9) 0.3076(14) 0.8822(16) 0.395(19) Uani 1 1 d . . . O8 O 0.0697(10) 0.4711(14) 0.851(2) 0.47(2) Uani 1 1 d . . . N1 N 0.1884(9) 0.4393(7) 0.6810(7) 0.071(4) Uani 1 1 d . . . N2 N 0.1326(7) 0.3315(9) 0.5454(7) 0.075(4) Uani 1 1 d . . . N3 N 0.1008(8) 0.2670(7) 0.6603(6) 0.057(3) Uani 1 1 d . . . N4 N -0.1933(12) 0.1134(9) 0.7021(8) 0.108(5) Uani 1 1 d . . . N5 N -0.0961(10) 0.0809(8) 0.7620(8) 0.084(4) Uani 1 1 d . . . N6 N 0.1666(8) 0.0675(8) 0.8701(10) 0.078(4) Uani 1 1 d . . . N7 N 0.1969(8) 0.1626(11) 1.0139(9) 0.080(4) Uani 1 1 d . . . N8 N 0.1558(8) 0.2442(7) 0.9167(6) 0.062(3) Uani 1 1 d . . . N9 N -0.1057(11) 0.3695(11) 0.8739(9) 0.133(6) Uani 1 1 d . . . N10 N -0.0038(10) 0.4400(9) 0.8532(11) 0.164(8) Uani 1 1 d . . . C1 C 0.3146(11) 0.4034(10) 0.7869(8) 0.067(5) Uani 1 1 d . . . C2 C 0.3763(10) 0.3967(11) 0.8402(9) 0.100(6) Uani 1 1 d . . . H20 H 0.3947 0.3487 0.8300 0.119 Uiso 1 1 calc R . . C3 C 0.4085(16) 0.4614(15) 0.9068(11) 0.130(10) Uani 1 1 d . . . H30 H 0.4502 0.4567 0.9414 0.156 Uiso 1 1 calc R . . C4 C 0.3843(17) 0.5293(17) 0.9250(13) 0.129(10) Uani 1 1 d . . . H40 H 0.4084 0.5719 0.9715 0.154 Uiso 1 1 calc R . . C5 C 0.3231(13) 0.5381(11) 0.8752(12) 0.112(6) Uani 1 1 d . . . H50 H 0.3050 0.5866 0.8888 0.134 Uiso 1 1 calc R . . C6 C 0.2859(11) 0.4729(11) 0.8015(9) 0.073(5) Uani 1 1 d . . . C7 C 0.2203(10) 0.4888(10) 0.7496(11) 0.088(5) Uani 1 1 d . . . H70 H 0.2021 0.5373 0.7687 0.105 Uiso 1 1 calc R . . C8 C 0.1236(9) 0.4573(9) 0.6369(10) 0.089(5) Uani 1 1 d . . . H80 H 0.1372 0.5147 0.6483 0.106 Uiso 1 1 calc R . . H81 H 0.0654 0.4434 0.6504 0.106 Uiso 1 1 calc R . . C9 C 0.1230(9) 0.4111(10) 0.5535(9) 0.082(5) Uani 1 1 d . . . H91 H 0.0677 0.4079 0.5244 0.098 Uiso 1 1 calc R . . H90 H 0.1717 0.4369 0.5353 0.098 Uiso 1 1 calc R . . C10 C 0.0878(9) 0.2680(10) 0.4893(8) 0.068(4) Uani 1 1 d . . . H100 H 0.0489 0.2755 0.4547 0.082 Uiso 1 1 calc R . . C11 C 0.0925(11) 0.1891(12) 0.4759(9) 0.070(4) Uiso 1 1 d . . . C12 C 0.0243(14) 0.1246(14) 0.4231(10) 0.119(8) Uani 1 1 d . . . H120 H -0.0193 0.1359 0.3955 0.142 Uiso 1 1 calc R . . C13 C 0.0225(14) 0.0478(18) 0.4128(11) 0.140(9) Uani 1 1 d . . . H130 H -0.0229 0.0080 0.3773 0.169 Uiso 1 1 calc R . . C14 C 0.0824(14) 0.0232(11) 0.4505(10) 0.103(6) Uani 1 1 d . . . H140 H 0.0772 -0.0305 0.4432 0.123 Uiso 1 1 calc R . . C15 C 0.1513(10) 0.0846(12) 0.5005(8) 0.074(4) Uani 1 1 d . . . H150 H 0.1958 0.0715 0.5255 0.088 Uiso 1 1 calc R . . C16 C 0.1552(12) 0.1654(11) 0.5140(9) 0.078(5) Uani 1 1 d . . . C17 C 0.1156(9) 0.2156(10) 0.6930(7) 0.068(5) Uani 1 1 d . . . H170 H 0.1738 0.2110 0.7017 0.082 Uiso 1 1 calc R . . C18 C 0.0510(11) 0.1701(8) 0.7139(7) 0.065(4) Uani 1 1 d . . . H180 H 0.0665 0.1361 0.7361 0.078 Uiso 1 1 calc R . . C19 C -0.0378(11) 0.1733(9) 0.7030(8) 0.066(4) Uani 1 1 d . . . C20 C -0.0515(10) 0.2265(11) 0.6672(8) 0.089(5) Uani 1 1 d . . . H200 H -0.1090 0.2309 0.6554 0.107 Uiso 1 1 calc R . . C21 C 0.0194(13) 0.2727(9) 0.6492(8) 0.079(5) Uani 1 1 d . . . H210 H 0.0074 0.3088 0.6283 0.095 Uiso 1 1 calc R . . C22 C -0.1065(13) 0.1273(10) 0.7231(9) 0.074(5) Uani 1 1 d . . . C23 C -0.1827(14) 0.0383(13) 0.7742(13) 0.118(6) Uani 1 1 d . . . C24 C -0.1915(12) 0.0875(17) 0.8582(11) 0.266(17) Uani 1 1 d . . . H240 H -0.1939 0.1416 0.8647 0.398 Uiso 1 1 calc R . . H241 H -0.1413 0.0889 0.8913 0.398 Uiso 1 1 calc R . . H242 H -0.2449 0.0628 0.8710 0.398 Uiso 1 1 calc R . . C25 C -0.1830(11) -0.0494(13) 0.7516(19) 0.291(19) Uani 1 1 d . . . H252 H -0.1383 -0.0550 0.7854 0.437 Uiso 1 1 calc R . . H250 H -0.1708 -0.0719 0.6999 0.437 Uiso 1 1 calc R . . H251 H -0.2401 -0.0775 0.7552 0.437 Uiso 1 1 calc R . . C26 C -0.2537(14) 0.0555(13) 0.7253(13) 0.107(6) Uani 1 1 d . . . C27 C -0.3263(15) 0.0885(13) 0.7536(11) 0.191(10) Uani 1 1 d . . . H270 H -0.3623 0.0923 0.7128 0.287 Uiso 1 1 calc R . . H272 H -0.3047 0.1413 0.7934 0.287 Uiso 1 1 calc R . . H271 H -0.3611 0.0543 0.7739 0.287 Uiso 1 1 calc R . . C28 C -0.2913(15) -0.0213(14) 0.6557(12) 0.239(15) Uani 1 1 d . . . H282 H -0.2439 -0.0459 0.6351 0.359 Uiso 1 1 calc R . . H281 H -0.3222 -0.0090 0.6177 0.359 Uiso 1 1 calc R . . H280 H -0.3317 -0.0577 0.6700 0.359 Uiso 1 1 calc R . . C29 C 0.4437(9) 0.3486(11) 0.6112(8) 0.071(5) Uani 1 1 d . . . C30 C 0.5211(14) 0.3769(13) 0.5909(11) 0.141(8) Uani 1 1 d . . . H300 H 0.5256 0.4176 0.5726 0.170 Uiso 1 1 calc R . . C31 C 0.5905(17) 0.3454(17) 0.5977(16) 0.168(11) Uani 1 1 d . . . H310 H 0.6408 0.3622 0.5788 0.202 Uiso 1 1 calc R . . C32 C 0.5946(14) 0.2934(19) 0.6281(12) 0.153(10) Uani 1 1 d . . . H320 H 0.6472 0.2783 0.6364 0.183 Uiso 1 1 calc R . . C33 C 0.5135(18) 0.2609(14) 0.6479(10) 0.163(9) Uani 1 1 d . . . H330 H 0.5113 0.2220 0.6684 0.196 Uiso 1 1 calc R . . C34 C 0.4382(12) 0.2880(13) 0.6364(9) 0.123(7) Uani 1 1 d . . . H340 H 0.3840 0.2647 0.6458 0.147 Uiso 1 1 calc R . . C35 C 0.3791(10) 0.4960(9) 0.6457(9) 0.073(4) Uani 1 1 d . . . C36 C 0.4371(9) 0.5302(12) 0.7125(9) 0.089(6) Uani 1 1 d . . . H360 H 0.4663 0.4977 0.7281 0.107 Uiso 1 1 calc R . . C37 C 0.4538(11) 0.6141(12) 0.7586(10) 0.108(6) Uani 1 1 d . . . H370 H 0.4935 0.6376 0.8040 0.130 Uiso 1 1 calc R . . C38 C 0.4086(16) 0.6584(11) 0.7327(15) 0.141(8) Uani 1 1 d . . . H380 H 0.4170 0.7132 0.7627 0.169 Uiso 1 1 calc R . . C39 C 0.3521(12) 0.6273(15) 0.6660(14) 0.151(10) Uani 1 1 d . . . H390 H 0.3247 0.6601 0.6493 0.181 Uiso 1 1 calc R . . C40 C 0.3372(11) 0.5466(14) 0.6245(11) 0.118(7) Uani 1 1 d . . . H400 H 0.2968 0.5243 0.5796 0.141 Uiso 1 1 calc R . . C41 C 0.3390(10) 0.3669(13) 0.4941(8) 0.087(6) Uani 1 1 d . . . C42 C 0.3787(12) 0.4202(11) 0.4644(12) 0.142(7) Uani 1 1 d . . . H420 H 0.4062 0.4724 0.4980 0.170 Uiso 1 1 calc R . . C43 C 0.3795(16) 0.3978(17) 0.3817(14) 0.186(11) Uani 1 1 d . . . H430 H 0.4111 0.4337 0.3637 0.223 Uiso 1 1 calc R . . C44 C 0.3339(15) 0.3248(14) 0.3328(11) 0.130(8) Uani 1 1 d . . . H440 H 0.3295 0.3094 0.2800 0.156 Uiso 1 1 calc R . . C45 C 0.2958(12) 0.2762(12) 0.3630(12) 0.114(7) Uani 1 1 d . . . H450 H 0.2663 0.2246 0.3293 0.136 Uiso 1 1 calc R . . C46 C 0.2955(11) 0.2945(10) 0.4399(11) 0.095(6) Uani 1 1 d . . . H460 H 0.2644 0.2561 0.4553 0.114 Uiso 1 1 calc R . . C47 C 0.2720(13) 0.1167(11) 0.7619(11) 0.079(5) Uani 1 1 d . . . C48 C 0.3197(11) 0.1280(12) 0.7047(13) 0.099(6) Uani 1 1 d . . . H480 H 0.3558 0.1780 0.7141 0.119 Uiso 1 1 calc R . . C49 C 0.3129(14) 0.0658(19) 0.6361(13) 0.119(7) Uani 1 1 d . . . H490 H 0.3438 0.0731 0.5981 0.143 Uiso 1 1 calc R . . C50 C 0.2584(17) -0.0104(15) 0.6226(13) 0.117(7) Uani 1 1 d . . . H500 H 0.2566 -0.0529 0.5760 0.140 Uiso 1 1 calc R . . C51 C 0.2071(14) -0.0249(14) 0.6757(16) 0.123(8) Uani 1 1 d . . . H510 H 0.1686 -0.0742 0.6649 0.148 Uiso 1 1 calc R . . C52 C 0.2176(12) 0.0387(14) 0.7445(13) 0.080(5) Uani 1 1 d . . . C53 C 0.1639(13) 0.0211(10) 0.7982(15) 0.094(7) Uani 1 1 d . . . H530 H 0.1235 -0.0284 0.7795 0.113 Uiso 1 1 calc R . . C54 C 0.1036(10) 0.0437(10) 0.9197(11) 0.103(6) Uani 1 1 d . . . H540 H 0.0493 0.0618 0.9154 0.124 Uiso 1 1 calc R . . H541 H 0.0888 -0.0145 0.9030 0.124 Uiso 1 1 calc R . . C55 C 0.1477(11) 0.0814(11) 0.9998(11) 0.104(6) Uani 1 1 d . . . H551 H 0.1038 0.0840 1.0343 0.125 Uiso 1 1 calc R . . H550 H 0.1878 0.0498 1.0085 0.125 Uiso 1 1 calc R . . C56 C 0.2008(10) 0.2204(14) 1.0757(12) 0.075(5) Uani 1 1 d . . . H560 H 0.1659 0.2103 1.1105 0.090 Uiso 1 1 calc R . . C57 C 0.2532(14) 0.3013(13) 1.0997(11) 0.080(6) Uani 1 1 d . . . C58 C 0.2454(11) 0.3556(15) 1.1725(14) 0.096(6) Uani 1 1 d . . . H580 H 0.2018 0.3383 1.1977 0.115 Uiso 1 1 calc R . . C59 C 0.2959(16) 0.4313(16) 1.2097(10) 0.110(8) Uani 1 1 d . . . H590 H 0.2904 0.4634 1.2596 0.132 Uiso 1 1 calc R . . C60 C 0.3556(14) 0.4582(9) 1.1697(13) 0.098(6) Uani 1 1 d . . . H600 H 0.3880 0.5113 1.1910 0.117 Uiso 1 1 calc R . . C61 C 0.3684(11) 0.4054(13) 1.0957(11) 0.087(5) Uani 1 1 d . . . H610 H 0.4122 0.4249 1.0720 0.104 Uiso 1 1 calc R . . C62 C 0.3170(11) 0.3227(13) 1.0548(12) 0.074(5) Uani 1 1 d . . . C63 C 0.1817(9) 0.2988(8) 0.8892(7) 0.061(4) Uani 1 1 d . . . H630 H 0.2391 0.3053 0.8770 0.073 Uiso 1 1 calc R . . C64 C 0.1305(10) 0.3459(8) 0.8775(7) 0.060(4) Uani 1 1 d . . . H640 H 0.1533 0.3864 0.8612 0.072 Uiso 1 1 calc R . . C65 C 0.0412(10) 0.3330(9) 0.8903(6) 0.056(4) Uani 1 1 d . . . C66 C 0.0103(9) 0.2737(8) 0.9176(8) 0.073(4) Uani 1 1 d . . . H660 H -0.0480 0.2621 0.9264 0.088 Uiso 1 1 calc R . . C67 C 0.0722(11) 0.2340(8) 0.9303(7) 0.070(4) Uani 1 1 d . . . H670 H 0.0541 0.1959 0.9507 0.084 Uiso 1 1 calc R . . C68 C -0.0206(11) 0.3798(11) 0.8721(7) 0.063(4) Uani 1 1 d . . . C69 C -0.1506(13) 0.4283(11) 0.8592(9) 0.083(5) Uani 1 1 d . . . C70 C -0.1968(12) 0.4654(12) 0.9260(10) 0.184(10) Uani 1 1 d . . . H701 H -0.2437 0.4250 0.9288 0.277 Uiso 1 1 calc R . . H700 H -0.2212 0.5075 0.9197 0.277 Uiso 1 1 calc R . . H702 H -0.1552 0.4878 0.9723 0.277 Uiso 1 1 calc R . . C71 C -0.2213(11) 0.3755(9) 0.7891(10) 0.150(8) Uani 1 1 d . . . H712 H -0.1927 0.3503 0.7459 0.225 Uiso 1 1 calc R . . H711 H -0.2566 0.4085 0.7775 0.225 Uiso 1 1 calc R . . H710 H -0.2588 0.3346 0.8003 0.225 Uiso 1 1 calc R . . C72 C -0.0748(11) 0.4780(12) 0.8419(10) 0.083(5) Uani 1 1 d . . . C73 C -0.0512(14) 0.5668(12) 0.8991(10) 0.180(10) Uani 1 1 d . . . H730 H -0.0477 0.5691 0.9504 0.270 Uiso 1 1 calc R . . H731 H -0.0962 0.5935 0.8906 0.270 Uiso 1 1 calc R . . H732 H 0.0050 0.5930 0.8918 0.270 Uiso 1 1 calc R . . C74 C -0.0768(12) 0.4790(12) 0.7669(9) 0.169(9) Uani 1 1 d . . . H741 H -0.0236 0.5140 0.7650 0.253 Uiso 1 1 calc R . . H740 H -0.1274 0.4982 0.7557 0.253 Uiso 1 1 calc R . . H742 H -0.0806 0.4254 0.7297 0.253 Uiso 1 1 calc R . . C75 C 0.3834(9) 0.0968(12) 1.0256(9) 0.070(4) Uani 1 1 d . . . C76 C 0.3896(8) 0.1666(11) 1.0922(12) 0.089(5) Uani 1 1 d . . . H760 H 0.3841 0.2146 1.0882 0.107 Uiso 1 1 calc R . . C77 C 0.4041(9) 0.1644(11) 1.1646(10) 0.092(5) Uani 1 1 d . . . H770 H 0.4059 0.2099 1.2087 0.110 Uiso 1 1 calc R . . C78 C 0.4157(9) 0.0929(14) 1.1693(11) 0.080(5) Uani 1 1 d . . . H780 H 0.4277 0.0909 1.2169 0.096 Uiso 1 1 calc R . . C79 C 0.4097(9) 0.0274(10) 1.1056(11) 0.075(5) Uani 1 1 d . . . H790 H 0.4155 -0.0206 1.1092 0.090 Uiso 1 1 calc R . . C80 C 0.3951(9) 0.0294(9) 1.0348(10) 0.080(5) Uani 1 1 d . . . H800 H 0.3932 -0.0170 0.9916 0.096 Uiso 1 1 calc R . . C81 C 0.4769(9) 0.1763(8) 0.9431(9) 0.062(4) Uani 1 1 d . . . C82 C 0.4870(10) 0.2218(9) 0.9009(9) 0.083(5) Uani 1 1 d . . . H820 H 0.4376 0.2250 0.8727 0.100 Uiso 1 1 calc R . . C83 C 0.5734(14) 0.2649(9) 0.8998(10) 0.102(6) Uani 1 1 d . . . H830 H 0.5815 0.2938 0.8689 0.123 Uiso 1 1 calc R . . C84 C 0.6434(12) 0.2625(13) 0.9452(13) 0.130(9) Uani 1 1 d . . . H840 H 0.6998 0.2921 0.9474 0.156 Uiso 1 1 calc R . . C85 C 0.6313(17) 0.2177(14) 0.9863(12) 0.126(9) Uani 1 1 d . . . H850 H 0.6801 0.2159 1.0162 0.152 Uiso 1 1 calc R . . C86 C 0.5518(13) 0.1753(10) 0.9863(10) 0.095(6) Uani 1 1 d . . . H860 H 0.5465 0.1446 1.0157 0.115 Uiso 1 1 calc R . . C87 C 0.3659(11) 0.0187(10) 0.8610(9) 0.069(4) Uani 1 1 d . . . C88 C 0.3073(10) -0.0506(13) 0.8562(10) 0.088(5) Uani 1 1 d . . . H880 H 0.2728 -0.0491 0.8948 0.105 Uiso 1 1 calc R . . C89 C 0.3010(12) -0.1217(11) 0.7932(16) 0.106(7) Uani 1 1 d . . . H890 H 0.2636 -0.1687 0.7908 0.127 Uiso 1 1 calc R . . C90 C 0.3486(18) -0.1244(17) 0.7345(12) 0.129(9) Uani 1 1 d . . . H900 H 0.3404 -0.1722 0.6913 0.155 Uiso 1 1 calc R . . C91 C 0.4093(14) -0.0559(17) 0.7388(12) 0.105(6) Uani 1 1 d . . . H910 H 0.4447 -0.0575 0.7009 0.127 Uiso 1 1 calc R . . C92 C 0.4139(11) 0.0131(12) 0.8013(13) 0.086(5) Uani 1 1 d . . . H920 H 0.4521 0.0598 0.8040 0.103 Uiso 1 1 calc R . . Cl1 Cl 0.9153(9) 0.1789(6) 0.0798(6) 0.192(4) Uani 1 1 d . . . O9 O 0.938(3) 0.2402(12) 0.0700(18) 0.53(3) Uani 1 1 d . . . O10 O 0.9566(15) 0.1274(16) 0.0310(13) 0.271(11) Uani 1 1 d . . . O11 O 0.918(2) 0.1688(13) 0.1454(12) 0.346(17) Uani 1 1 d . . . O12 O 0.833(2) 0.155(3) 0.067(2) 0.49(3) Uani 1 1 d . . . Cl2 Cl 0.8485(12) 0.3532(9) 0.5084(9) 0.495(8) Uiso 1 1 d D . . O13 O 0.8324(13) 0.4267(9) 0.5518(10) 0.310(10) Uiso 1 1 d D . . O14 O 0.852(4) 0.3547(18) 0.4309(15) 0.90(5) Uiso 1 1 d D . . O15 O 0.926(3) 0.348(2) 0.558(4) 1.48(13) Uiso 1 1 d D . . O16 O 0.7901 0.2813 0.4943 0.65(3) Uiso 1 1 d D . . O17 O -0.081(3) 0.246(2) 0.327(2) 0.59(2) Uiso 1 1 d . . . O18 O 0.076(3) 0.229(3) 0.246(2) 0.63(2) Uiso 1 1 d . . . O19 O 0.134(3) 0.656(3) 0.756(2) 0.61(2) Uiso 1 1 d . . . O20 O 0.165(4) 0.668(4) 0.896(3) 0.77(3) Uiso 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 Ru1 0.0526(9) 0.0674(10) 0.0662(8) 0.0268(7) 0.0010(7) -0.0003(7) Ru2 0.0529(9) 0.0679(10) 0.1081(10) 0.0509(8) 0.0131(8) 0.0181(8) P1 0.063(3) 0.071(3) 0.080(3) 0.037(2) 0.003(2) -0.008(2) P2 0.062(3) 0.069(3) 0.106(3) 0.051(3) 0.006(2) 0.020(2) O1 0.071(7) 0.068(8) 0.071(6) 0.030(6) -0.009(5) -0.004(6) O2 0.070(7) 0.055(7) 0.058(5) 0.006(5) -0.006(5) -0.009(6) O3 0.055(9) 0.230(16) 0.249(15) 0.163(13) -0.004(9) -0.012(9) O4 0.064(8) 0.148(11) 0.161(10) 0.103(8) 0.022(8) 0.016(8) O5 0.081(8) 0.047(7) 0.092(7) 0.033(6) 0.020(6) 0.014(6) O6 0.081(8) 0.074(9) 0.084(7) 0.032(7) 0.021(7) 0.035(7) O7 0.073(11) 0.54(3) 0.95(5) 0.67(4) 0.160(18) 0.136(15) O8 0.058(11) 0.41(3) 1.23(7) 0.66(4) 0.02(2) 0.023(15) N1 0.073(10) 0.063(10) 0.054(8) 0.007(7) 0.003(7) -0.006(8) N2 0.049(9) 0.065(11) 0.091(9) 0.023(8) -0.008(7) -0.011(8) N3 0.031(9) 0.065(10) 0.057(7) 0.006(6) 0.010(7) 0.004(7) N4 0.063(13) 0.121(14) 0.148(13) 0.082(10) -0.002(11) -0.021(11) N5 0.057(12) 0.066(11) 0.114(11) 0.030(9) 0.031(10) -0.011(10) N6 0.034(9) 0.073(11) 0.140(12) 0.056(10) -0.005(10) 0.021(8) N7 0.062(10) 0.086(14) 0.120(12) 0.065(10) 0.021(9) 0.028(10) N8 0.058(9) 0.077(10) 0.090(8) 0.063(7) 0.024(7) 0.037(8) N9 0.072(13) 0.182(17) 0.245(17) 0.175(14) 0.068(12) 0.054(12) N10 0.022(10) 0.123(14) 0.41(3) 0.196(17) -0.019(12) -0.018(10) C1 0.087(13) 0.038(12) 0.042(10) -0.008(9) 0.012(10) -0.019(10) C2 0.077(13) 0.152(19) 0.049(10) 0.050(13) -0.025(9) -0.037(11) C3 0.14(2) 0.14(2) 0.050(14) -0.003(16) -0.025(12) -0.034(19) C4 0.13(2) 0.15(3) 0.066(15) 0.024(17) -0.007(14) -0.03(2) C5 0.121(18) 0.085(16) 0.113(16) 0.018(15) 0.056(13) 0.019(14) C6 0.095(14) 0.029(12) 0.054(11) -0.018(10) 0.007(10) -0.009(11) C7 0.073(13) 0.088(15) 0.117(15) 0.065(14) 0.015(12) -0.002(11) C8 0.046(11) 0.070(13) 0.131(15) 0.019(12) -0.006(11) 0.019(9) C9 0.070(12) 0.055(13) 0.099(13) 0.026(11) -0.029(9) -0.009(9) C10 0.044(10) 0.075(13) 0.090(11) 0.040(10) -0.015(9) 0.014(9) C12 0.115(17) 0.117(18) 0.106(15) 0.039(16) -0.009(12) 0.005(17) C13 0.108(19) 0.17(3) 0.086(14) 0.024(19) -0.019(12) -0.02(2) C14 0.137(19) 0.069(14) 0.094(13) 0.041(12) -0.015(12) -0.001(14) C15 0.072(13) 0.083(14) 0.062(10) 0.025(10) 0.011(9) 0.014(11) C16 0.114(16) 0.054(14) 0.079(12) 0.039(11) 0.023(11) 0.016(12) C17 0.030(10) 0.098(14) 0.064(10) 0.027(9) -0.004(8) 0.001(10) C18 0.055(12) 0.044(10) 0.097(11) 0.029(8) 0.043(10) 0.003(9) C19 0.047(13) 0.045(11) 0.092(12) 0.015(9) 0.012(10) -0.001(10) C20 0.049(13) 0.112(16) 0.102(12) 0.047(11) -0.019(10) 0.007(11) C21 0.063(13) 0.077(13) 0.111(12) 0.049(10) 0.026(12) 0.021(11) C22 0.047(14) 0.072(14) 0.102(13) 0.038(10) 0.034(11) -0.005(12) C23 0.078(16) 0.116(18) 0.18(2) 0.091(16) 0.053(16) 0.001(14) C24 0.120(19) 0.48(5) 0.127(16) 0.11(2) 0.045(15) -0.10(2) C25 0.045(13) 0.14(2) 0.77(6) 0.29(3) -0.02(2) 0.001(13) C26 0.066(15) 0.115(18) 0.170(19) 0.095(16) 0.054(15) -0.005(14) C27 0.19(2) 0.26(3) 0.24(2) 0.16(2) 0.15(2) 0.14(2) C28 0.23(3) 0.18(2) 0.20(2) 0.03(2) 0.01(2) -0.12(2) C29 0.023(10) 0.109(15) 0.067(10) 0.024(9) -0.013(8) 0.008(10) C30 0.050(14) 0.18(2) 0.24(2) 0.121(18) 0.044(16) 0.027(16) C31 0.09(2) 0.20(3) 0.27(3) 0.15(2) 0.04(2) 0.036(19) C32 0.047(15) 0.27(4) 0.147(18) 0.063(19) 0.041(13) 0.07(2) C33 0.14(2) 0.27(3) 0.183(19) 0.172(19) 0.043(19) 0.10(2) C34 0.098(17) 0.19(2) 0.137(15) 0.121(15) 0.005(12) 0.047(15) C35 0.046(11) 0.080(14) 0.093(12) 0.037(11) 0.022(10) 0.010(11) C36 0.049(11) 0.117(18) 0.071(11) 0.031(11) -0.011(9) -0.033(11) C37 0.099(16) 0.043(13) 0.136(15) 0.016(13) -0.029(12) -0.038(12) C38 0.15(2) 0.056(16) 0.23(3) 0.063(18) 0.022(19) 0.035(16) C39 0.086(16) 0.10(2) 0.23(2) 0.064(18) -0.088(15) -0.017(14) C40 0.090(15) 0.070(16) 0.172(18) 0.053(15) -0.048(13) -0.024(13) C41 0.065(12) 0.134(18) 0.065(11) 0.071(13) 0.000(9) -0.035(12) C42 0.143(19) 0.099(17) 0.112(16) -0.010(13) 0.010(14) -0.031(14) C43 0.25(3) 0.20(3) 0.097(16) 0.075(17) 0.058(18) -0.02(2) C44 0.17(2) 0.100(19) 0.092(15) 0.033(15) -0.032(15) -0.014(16) C45 0.147(19) 0.090(17) 0.095(17) 0.032(13) 0.024(13) 0.011(13) C46 0.125(17) 0.083(15) 0.067(12) 0.026(11) 0.020(12) 0.005(12) C47 0.098(15) 0.031(14) 0.104(16) 0.019(12) -0.019(14) 0.036(12) C48 0.111(16) 0.13(2) 0.078(13) 0.058(16) 0.029(13) 0.037(13) C49 0.119(19) 0.16(2) 0.090(17) 0.050(17) 0.033(14) 0.064(18) C50 0.11(2) 0.11(2) 0.115(19) 0.015(16) -0.015(16) 0.044(17) C51 0.082(17) 0.13(2) 0.123(18) 0.01(2) -0.021(15) 0.030(15) C52 0.078(15) 0.058(16) 0.103(17) 0.030(14) -0.003(12) 0.027(13) C53 0.087(16) 0.039(13) 0.151(19) 0.052(14) -0.043(16) -0.010(11) C54 0.043(12) 0.140(17) 0.182(18) 0.117(15) 0.030(13) 0.033(11) C55 0.076(14) 0.111(16) 0.179(18) 0.115(15) 0.010(12) 0.028(12) C56 0.065(13) 0.083(18) 0.106(15) 0.056(13) 0.026(12) 0.043(13) C57 0.101(18) 0.052(15) 0.075(13) -0.004(13) -0.010(12) 0.054(14) C58 0.062(13) 0.085(16) 0.14(2) 0.048(15) -0.003(13) 0.025(13) C59 0.13(2) 0.15(3) 0.071(13) 0.046(16) 0.040(14) 0.076(18) C60 0.126(19) 0.048(12) 0.097(15) 0.002(13) -0.044(13) 0.045(12) C61 0.090(15) 0.081(15) 0.107(14) 0.054(12) 0.007(12) 0.030(14) C62 0.027(11) 0.10(2) 0.114(16) 0.066(17) -0.008(13) 0.000(12) C63 0.052(10) 0.068(12) 0.095(10) 0.060(9) 0.022(8) 0.029(9) C64 0.058(11) 0.048(10) 0.085(10) 0.035(8) 0.022(9) 0.013(9) C65 0.050(11) 0.059(11) 0.059(9) 0.024(8) -0.005(8) 0.016(9) C66 0.044(10) 0.064(11) 0.144(13) 0.072(11) 0.017(9) 0.020(9) C67 0.071(13) 0.050(11) 0.104(11) 0.044(9) 0.015(11) 0.017(10) C68 0.033(11) 0.089(14) 0.076(9) 0.048(9) 0.007(8) 0.001(10) C69 0.089(15) 0.103(15) 0.105(13) 0.073(12) 0.014(12) 0.065(13) C70 0.152(19) 0.27(3) 0.175(17) 0.072(18) 0.128(15) 0.154(19) C71 0.129(17) 0.081(15) 0.22(2) 0.046(14) -0.031(16) 0.031(13) C72 0.056(12) 0.102(16) 0.122(15) 0.069(13) 0.015(11) 0.034(12) C73 0.26(3) 0.100(18) 0.151(16) 0.039(15) -0.008(17) 0.006(17) C74 0.18(2) 0.27(3) 0.142(15) 0.142(17) 0.090(15) 0.085(18) C75 0.061(11) 0.069(13) 0.091(13) 0.034(11) 0.019(9) 0.031(10) C76 0.054(11) 0.114(18) 0.108(13) 0.061(15) -0.018(10) 0.011(10) C77 0.053(11) 0.100(17) 0.126(17) 0.054(13) 0.015(10) 0.005(10) C78 0.055(11) 0.090(15) 0.116(16) 0.072(14) 0.000(10) 0.001(11) C79 0.101(14) 0.059(14) 0.087(12) 0.046(12) 0.012(11) 0.032(10) C80 0.088(12) 0.055(13) 0.117(15) 0.038(11) 0.035(10) 0.052(10) C81 0.038(11) 0.059(12) 0.102(12) 0.037(9) 0.030(10) 0.022(9) C82 0.051(13) 0.065(13) 0.120(13) 0.025(10) 0.012(10) 0.005(10) C83 0.084(15) 0.091(14) 0.134(15) 0.051(12) 0.058(13) -0.003(13) C84 0.024(12) 0.12(2) 0.18(2) 0.008(15) -0.027(13) -0.018(13) C85 0.13(2) 0.13(2) 0.172(19) 0.082(17) 0.042(18) 0.080(19) C86 0.044(12) 0.096(15) 0.169(16) 0.088(12) -0.006(13) -0.002(11) C87 0.040(11) 0.065(15) 0.102(13) 0.028(11) 0.008(10) 0.023(10) C88 0.067(13) 0.047(12) 0.139(15) 0.033(13) -0.017(11) 0.007(11) C89 0.105(17) 0.019(13) 0.18(2) 0.041(15) -0.023(16) 0.009(11) C90 0.11(2) 0.15(3) 0.112(18) 0.040(17) -0.016(16) 0.039(19) C91 0.083(17) 0.112(19) 0.120(18) 0.037(17) 0.006(13) 0.040(15) C92 0.080(15) 0.082(17) 0.108(14) 0.048(14) 0.001(13) 0.032(12) Cl1 0.259(12) 0.156(8) 0.226(9) 0.124(7) 0.120(8) 0.063(7) O9 0.95(7) 0.119(17) 0.66(5) 0.23(2) 0.56(5) 0.14(3) O10 0.27(2) 0.33(3) 0.31(2) 0.19(2) 0.150(19) 0.15(2) O11 0.60(5) 0.24(2) 0.214(19) 0.131(18) 0.05(2) 0.02(2) O12 0.29(3) 0.85(8) 0.71(7) 0.61(6) 0.37(4) 0.32(4) _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 N2 1.964(11) . ? Ru1 O2 1.994(9) . ? Ru1 N1 2.016(12) . ? Ru1 O1 2.024(8) . ? Ru1 N3 2.163(11) . ? Ru1 P1 2.358(4) . ? Ru2 N7 1.960(12) . ? Ru2 O6 1.992(10) . ? Ru2 N6 2.008(13) . ? Ru2 O5 2.012(9) . ? Ru2 N8 2.150(10) . ? Ru2 P2 2.348(4) . ? P1 C41 1.804(13) . ? P1 C35 1.828(16) . ? P1 C29 1.840(14) . ? P2 C81 1.816(14) . ? P2 C87 1.818(15) . ? P2 C75 1.817(14) . ? O1 C1 1.336(13) . ? O2 C16 1.338(16) . ? O3 N4 1.281(14) . ? O4 N5 1.267(14) . ? O5 C47 1.314(15) . ? O6 C62 1.225(19) . ? O7 N9 1.287(17) . ? O8 N10 1.188(15) . ? N1 C7 1.279(16) . ? N1 C8 1.431(15) . ? N2 C10 1.286(13) . ? N2 C9 1.447(15) . ? N3 C21 1.294(15) . ? N3 C17 1.355(14) . ? N4 C22 1.328(17) . ? N4 C26 1.498(18) . ? N5 C22 1.344(17) . ? N5 C23 1.502(18) . ? N6 C53 1.305(18) . ? N6 C54 1.519(16) . ? N7 C56 1.242(16) . ? N7 C55 1.461(17) . ? N8 C63 1.308(13) . ? N8 C67 1.330(14) . ? N9 C68 1.302(16) . ? N9 C69 1.485(17) . ? N10 C68 1.275(16) . ? N10 C72 1.451(17) . ? C1 C6 1.362(18) . ? C1 C2 1.405(18) . ? C2 C3 1.355(19) . ? C3 C4 1.29(3) . ? C4 C5 1.37(2) . ? C5 C6 1.454(19) . ? C6 C7 1.512(19) . ? C8 C9 1.490(15) . ? C10 C11 1.389(17) . ? C11 C16 1.400(18) . ? C11 C12 1.428(19) . ? C12 C13 1.34(2) . ? C13 C14 1.38(2) . ? C14 C15 1.394(17) . ? C15 C16 1.395(17) . ? C17 C18 1.362(16) . ? C18 C19 1.393(16) . ? C19 C22 1.400(18) . ? C19 C20 1.422(17) . ? C20 C21 1.404(17) . ? C23 C25 1.50(2) . ? C23 C26 1.55(2) . ? C23 C24 1.54(2) . ? C26 C27 1.41(2) . ? C26 C28 1.51(2) . ? C29 C30 1.356(19) . ? C29 C34 1.360(19) . ? C30 C31 1.33(2) . ? C31 C32 1.30(3) . ? C32 C33 1.43(2) . ? C33 C34 1.38(2) . ? C35 C36 1.366(15) . ? C35 C40 1.385(18) . ? C36 C37 1.421(18) . ? C37 C38 1.36(2) . ? C38 C39 1.35(2) . ? C39 C40 1.36(2) . ? C41 C46 1.356(17) . ? C41 C42 1.37(2) . ? C42 C43 1.47(2) . ? C43 C44 1.34(2) . ? C44 C45 1.309(19) . ? C45 C46 1.375(17) . ? C47 C48 1.41(2) . ? C47 C52 1.43(2) . ? C48 C49 1.35(2) . ? C49 C50 1.42(2) . ? C50 C51 1.40(2) . ? C51 C52 1.36(2) . ? C52 C53 1.45(2) . ? C54 C55 1.473(16) . ? C56 C57 1.44(2) . ? C57 C58 1.40(2) . ? C57 C62 1.44(2) . ? C58 C59 1.36(2) . ? C59 C60 1.37(2) . ? C60 C61 1.429(18) . ? C61 C62 1.46(2) . ? C63 C64 1.342(14) . ? C64 C65 1.413(15) . ? C65 C66 1.398(16) . ? C65 C68 1.501(17) . ? C66 C67 1.366(15) . ? C69 C72 1.487(19) . ? C69 C70 1.494(18) . ? C69 C71 1.540(17) . ? C72 C74 1.432(17) . ? C72 C73 1.539(19) . ? C75 C80 1.354(16) . ? C75 C76 1.406(17) . ? C76 C77 1.398(16) . ? C77 C78 1.391(17) . ? C78 C79 1.332(16) . ? C79 C80 1.367(15) . ? C81 C82 1.357(16) . ? C81 C86 1.385(16) . ? C82 C83 1.432(18) . ? C83 C84 1.36(2) . ? C84 C85 1.33(2) . ? C85 C86 1.33(2) . ? C87 C92 1.380(17) . ? C87 C88 1.389(17) . ? C88 C89 1.383(19) . ? C89 C90 1.37(2) . ? C90 C91 1.40(2) . ? C91 C92 1.359(18) . ? Cl1 O9 1.202(17) . ? Cl1 O12 1.24(3) . ? Cl1 O11 1.330(19) . ? Cl1 O10 1.34(2) . ? Cl2 O13 1.369(15) . ? Cl2 O16 1.380(15) . ? Cl2 O14 1.490(18) . ? Cl2 O15 1.52(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 N2 Ru1 O2 91.4(5) . . ? N2 Ru1 N1 80.2(6) . . ? O2 Ru1 N1 171.6(5) . . ? N2 Ru1 O1 169.7(4) . . ? O2 Ru1 O1 96.2(4) . . ? N1 Ru1 O1 92.1(5) . . ? N2 Ru1 N3 88.4(5) . . ? O2 Ru1 N3 84.6(4) . . ? N1 Ru1 N3 94.5(4) . . ? O1 Ru1 N3 85.3(4) . . ? N2 Ru1 P1 96.4(3) . . ? O2 Ru1 P1 90.9(3) . . ? N1 Ru1 P1 90.6(3) . . ? O1 Ru1 P1 90.5(3) . . ? N3 Ru1 P1 173.5(4) . . ? N7 Ru2 O6 94.0(6) . . ? N7 Ru2 N6 81.5(7) . . ? O6 Ru2 N6 175.1(6) . . ? N7 Ru2 O5 168.5(5) . . ? O6 Ru2 O5 94.9(4) . . ? N6 Ru2 O5 89.9(6) . . ? N7 Ru2 N8 89.3(5) . . ? O6 Ru2 N8 86.9(4) . . ? N6 Ru2 N8 94.9(5) . . ? O5 Ru2 N8 83.9(4) . . ? N7 Ru2 P2 96.0(4) . . ? O6 Ru2 P2 86.3(3) . . ? N6 Ru2 P2 92.3(3) . . ? O5 Ru2 P2 91.9(3) . . ? N8 Ru2 P2 171.7(4) . . ? C41 P1 C35 106.0(9) . . ? C41 P1 C29 102.0(7) . . ? C35 P1 C29 105.1(8) . . ? C41 P1 Ru1 113.5(5) . . ? C35 P1 Ru1 113.4(4) . . ? C29 P1 Ru1 115.7(7) . . ? C81 P2 C87 104.1(8) . . ? C81 P2 C75 101.7(7) . . ? C87 P2 C75 105.0(9) . . ? C81 P2 Ru2 113.9(5) . . ? C87 P2 Ru2 115.4(4) . . ? C75 P2 Ru2 115.1(5) . . ? C1 O1 Ru1 125.2(10) . . ? C16 O2 Ru1 119.5(10) . . ? C47 O5 Ru2 126.3(11) . . ? C62 O6 Ru2 121.4(12) . . ? C7 N1 C8 120.3(14) . . ? C7 N1 Ru1 125.9(12) . . ? C8 N1 Ru1 113.7(9) . . ? C10 N2 C9 121.1(13) . . ? C10 N2 Ru1 123.9(11) . . ? C9 N2 Ru1 115.0(9) . . ? C21 N3 C17 116.7(13) . . ? C21 N3 Ru1 125.8(13) . . ? C17 N3 Ru1 117.5(10) . . ? O3 N4 C22 123.9(16) . . ? O3 N4 C26 117.7(17) . . ? C22 N4 C26 118.4(16) . . ? O4 N5 C22 127.1(15) . . ? O4 N5 C23 119.6(17) . . ? C22 N5 C23 113.0(16) . . ? C53 N6 C54 121.7(17) . . ? C53 N6 Ru2 125.6(13) . . ? C54 N6 Ru2 112.7(11) . . ? C56 N7 C55 121.7(16) . . ? C56 N7 Ru2 122.6(14) . . ? C55 N7 Ru2 115.7(11) . . ? C63 N8 C67 116.6(12) . . ? C63 N8 Ru2 116.3(10) . . ? C67 N8 Ru2 127.0(10) . . ? O7 N9 C68 121.6(17) . . ? O7 N9 C69 121.0(16) . . ? C68 N9 C69 117.1(15) . . ? O8 N10 C68 122.3(16) . . ? O8 N10 C72 117.8(16) . . ? C68 N10 C72 119.5(16) . . ? O1 C1 C6 123.3(16) . . ? O1 C1 C2 115.2(17) . . ? C6 C1 C2 121.3(14) . . ? C3 C2 C1 118.8(18) . . ? C4 C3 C2 124(3) . . ? C3 C4 C5 120(3) . . ? C4 C5 C6 121(2) . . ? C1 C6 C5 115.5(16) . . ? C1 C6 C7 127.0(14) . . ? C5 C6 C7 117.5(19) . . ? N1 C7 C6 123.8(16) . . ? N1 C8 C9 110.2(12) . . ? N2 C9 C8 106.0(12) . . ? N2 C10 C11 125.7(15) . . ? C10 C11 C16 125.9(17) . . ? C10 C11 C12 118.9(19) . . ? C16 C11 C12 115.0(18) . . ? C13 C12 C11 121(2) . . ? C12 C13 C14 125(2) . . ? C13 C14 C15 115.2(18) . . ? C14 C15 C16 121.6(16) . . ? O2 C16 C15 115.7(16) . . ? O2 C16 C11 122.1(17) . . ? C15 C16 C11 122.1(17) . . ? N3 C17 C18 124.3(13) . . ? C17 C18 C19 121.6(15) . . ? C18 C19 C22 123.6(17) . . ? C18 C19 C20 112.8(14) . . ? C22 C19 C20 123.6(17) . . ? C21 C20 C19 121.8(14) . . ? N3 C21 C20 122.7(15) . . ? N4 C22 N5 105.7(15) . . ? N4 C22 C19 128.3(18) . . ? N5 C22 C19 125.6(18) . . ? C25 C23 N5 109.5(17) . . ? C25 C23 C26 114.6(19) . . ? N5 C23 C26 104.2(16) . . ? C25 C23 C24 117(2) . . ? N5 C23 C24 104.5(15) . . ? C26 C23 C24 105.4(19) . . ? C27 C26 N4 109.6(19) . . ? C27 C26 C28 107.0(18) . . ? N4 C26 C28 109.3(16) . . ? C27 C26 C23 124.2(19) . . ? N4 C26 C23 98.0(15) . . ? C28 C26 C23 108(2) . . ? C30 C29 C34 119.5(17) . . ? C30 C29 P1 118.8(18) . . ? C34 C29 P1 121.4(15) . . ? C31 C30 C29 119(2) . . ? C32 C31 C30 126(3) . . ? C31 C32 C33 116(2) . . ? C34 C33 C32 119(2) . . ? C29 C34 C33 119.8(19) . . ? C36 C35 C40 117.2(16) . . ? C36 C35 P1 121.0(15) . . ? C40 C35 P1 121.1(15) . . ? C35 C36 C37 121.7(16) . . ? C38 C37 C36 116.3(17) . . ? C39 C38 C37 124(2) . . ? C38 C39 C40 118(2) . . ? C39 C40 C35 123.2(17) . . ? C46 C41 C42 113.7(14) . . ? C46 C41 P1 121.1(14) . . ? C42 C41 P1 125.2(17) . . ? C41 C42 C43 122.7(16) . . ? C44 C43 C42 118.7(19) . . ? C45 C44 C43 117(2) . . ? C44 C45 C46 125.9(19) . . ? C41 C46 C45 122.0(15) . . ? O5 C47 C48 117.8(19) . . ? O5 C47 C52 124(2) . . ? C48 C47 C52 117.7(17) . . ? C49 C48 C47 119.9(19) . . ? C48 C49 C50 120(2) . . ? C51 C50 C49 123(2) . . ? C52 C51 C50 115(2) . . ? C51 C52 C47 124(2) . . ? C51 C52 C53 113(2) . . ? C47 C52 C53 122(2) . . ? N6 C53 C52 126.7(18) . . ? C55 C54 N6 108.5(14) . . ? N7 C55 C54 108.1(13) . . ? N7 C56 C57 127.3(19) . . ? C58 C57 C56 116(2) . . ? C58 C57 C62 122(2) . . ? C56 C57 C62 121.8(17) . . ? C59 C58 C57 126(2) . . ? C58 C59 C60 116.5(19) . . ? C59 C60 C61 120.7(18) . . ? C60 C61 C62 124.1(17) . . ? O6 C62 C57 127.9(18) . . ? O6 C62 C61 121.0(18) . . ? C57 C62 C61 111.1(18) . . ? N8 C63 C64 123.9(13) . . ? C63 C64 C65 118.9(13) . . ? C66 C65 C64 118.8(13) . . ? C66 C65 C68 120.4(14) . . ? C64 C65 C68 120.8(14) . . ? C67 C66 C65 114.9(13) . . ? N8 C67 C66 126.8(13) . . ? N10 C68 N9 102.7(16) . . ? N10 C68 C65 129.6(15) . . ? N9 C68 C65 127.7(16) . . ? N9 C69 C72 100.0(14) . . ? N9 C69 C70 108.5(13) . . ? C72 C69 C70 120.5(17) . . ? N9 C69 C71 103.7(14) . . ? C72 C69 C71 113.9(14) . . ? C70 C69 C71 108.5(15) . . ? C74 C72 N10 107.9(16) . . ? C74 C72 C69 119.6(15) . . ? N10 C72 C69 100.6(14) . . ? C74 C72 C73 106.5(15) . . ? N10 C72 C73 108.5(14) . . ? C69 C72 C73 113.2(16) . . ? C80 C75 C76 117.4(15) . . ? C80 C75 P2 129.9(16) . . ? C76 C75 P2 112.5(14) . . ? C77 C76 C75 120.3(16) . . ? C78 C77 C76 118.8(17) . . ? C79 C78 C77 119.9(16) . . ? C78 C79 C80 121.2(15) . . ? C75 C80 C79 122.2(15) . . ? C82 C81 C86 118.1(14) . . ? C82 C81 P2 120.3(13) . . ? C86 C81 P2 121.6(14) . . ? C81 C82 C83 120.1(15) . . ? C84 C83 C82 118.3(17) . . ? C85 C84 C83 120(2) . . ? C84 C85 C86 122(2) . . ? C85 C86 C81 120.9(17) . . ? C92 C87 C88 117.9(15) . . ? C92 C87 P2 121.6(18) . . ? C88 C87 P2 120.2(16) . . ? C89 C88 C87 119.0(17) . . ? C90 C89 C88 121(2) . . ? C89 C90 C91 121(2) . . ? C92 C91 C90 117(2) . . ? C91 C92 C87 124.4(19) . . ? O9 Cl1 O12 111(3) . . ? O9 Cl1 O11 128(2) . . ? O12 Cl1 O11 90.9(19) . . ? O9 Cl1 O10 103.8(17) . . ? O12 Cl1 O10 113(3) . . ? O11 Cl1 O10 109.4(19) . . ? O13 Cl2 O16 122.9(17) . . ? O13 Cl2 O14 104.0(16) . . ? O16 Cl2 O14 103.8(16) . . ? O13 Cl2 O15 102.5(18) . . ? O16 Cl2 O15 100.8(17) . . ? O14 Cl2 O15 125(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 21.72 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.502 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.071