# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'E. Alessio' 'Teresa Gianferrara' 'Elisabetta Iengo' 'Barbara Serli' 'Ennio Zangrando' _publ_contact_author_name 'Prof Enzo Alessio' _publ_contact_author_address ; Dipartimento di Scienze Chimiche Universita di Trieste Via L Giorgieri 1 Trieste 34127 ITALY ; _publ_contact_author_email ALESSI@UNIV.TRIESTE.IT _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Pyridylporphyrins peripherally coordinated to ruthenium-nitrosyls, including the water-soluble Na4[Zn*4'TPyP{RuCl4(NO)}4]: synthesis and structural characterization. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 265963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-nitrosyl-(5-(4'pyridyl)-10,15,20-trisphenyl-porphyrin)- tetrachloro-ruthenate(III) tetrabutylamonium dichloroform solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H29 Cl4 N6 O Ru, C16 H36 N, 2(C H Cl3)' _chemical_formula_sum 'C61 H67 Cl10 N7 O Ru' _chemical_formula_weight 1369.79 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.833(3) _cell_length_b 13.688(4) _cell_length_c 22.584(4) _cell_angle_alpha 96.46(2) _cell_angle_beta 96.06(3) _cell_angle_gamma 106.02(2) _cell_volume 3165.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7610 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18125 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11615 _reflns_number_gt 7410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.05 (Farrugia, 1999)' _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^)+(0.0871P)^2^+2.8311P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11615 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2005 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 1.14786(4) -0.15974(3) 0.13622(2) 0.04847(15) Uani 1 1 d . . . Cl1 Cl 1.35313(14) -0.03327(11) 0.14452(8) 0.0623(4) Uani 1 1 d . . . Cl2 Cl 0.94069(13) -0.28323(11) 0.12561(6) 0.0552(3) Uani 1 1 d . . . Cl3 Cl 1.20801(16) -0.26426(13) 0.06243(8) 0.0688(4) Uani 1 1 d . . . Cl4 Cl 1.06631(15) -0.07882(11) 0.06149(6) 0.0578(4) Uani 1 1 d . . . N1 N 1.2064(6) -0.2254(4) 0.1953(2) 0.0561(14) Uani 1 1 d . . . O1 O 1.2258(6) -0.2626(5) 0.2257(3) 0.0949(18) Uani 1 1 d . . . N5 N 0.8951(5) 0.2569(3) 0.3769(2) 0.0503(11) Uani 1 1 d . . . N2 N 0.7895(4) 0.3520(3) 0.4707(2) 0.0493(10) Uani 1 1 d . . . H2N H 0.8071 0.2933 0.4625 0.059 Uiso 1 1 calc R . . N3 N 0.7255(4) 0.1589(3) 0.5230(2) 0.0495(10) Uani 1 1 d . . . N4 N 0.8306(5) 0.0626(3) 0.4285(2) 0.0521(11) Uani 1 1 d . . . H4N H 0.8290 0.1254 0.4412 0.063 Uiso 1 1 calc R . . C1 C 0.9461(6) 0.1987(4) 0.3375(3) 0.0531(13) Uani 1 1 d . . . C2 C 1.0099(6) 0.2627(4) 0.2971(3) 0.0615(16) Uani 1 1 d . . . H2 H 1.0542 0.2424 0.2660 0.074 Uiso 1 1 calc R . . C3 C 0.9958(6) 0.3562(5) 0.3111(3) 0.0613(15) Uani 1 1 d . . . H3 H 1.0283 0.4141 0.2916 0.074 Uiso 1 1 calc R . . C4 C 0.9224(6) 0.3541(4) 0.3611(3) 0.0541(13) Uani 1 1 d . . . C5 C 0.8821(5) 0.4356(4) 0.3878(2) 0.0501(12) Uani 1 1 d . . . C6 C 0.8191(6) 0.4330(4) 0.4392(3) 0.0513(13) Uani 1 1 d . . . C7 C 0.7740(6) 0.5134(4) 0.4666(3) 0.0565(14) Uani 1 1 d . . . H7 H 0.7823 0.5784 0.4537 0.068 Uiso 1 1 calc R . . C8 C 0.7180(7) 0.4805(4) 0.5137(3) 0.0607(15) Uani 1 1 d . . . H8 H 0.6789 0.5180 0.5401 0.073 Uiso 1 1 calc R . . C9 C 0.7276(6) 0.3783(4) 0.5174(2) 0.0515(13) Uani 1 1 d . . . C10 C 0.6809(5) 0.3204(4) 0.5612(2) 0.0476(12) Uani 1 1 d . . . C11 C 0.6834(5) 0.2196(4) 0.5645(2) 0.0497(12) Uani 1 1 d . . . C12 C 0.6379(5) 0.1609(4) 0.6110(3) 0.0536(13) Uani 1 1 d . . . H12 H 0.6034 0.1842 0.6450 0.064 Uiso 1 1 calc R . . C13 C 0.6533(6) 0.0655(4) 0.5972(2) 0.0513(13) Uani 1 1 d . . . H13 H 0.6327 0.0106 0.6201 0.062 Uiso 1 1 calc R . . C14 C 0.7067(5) 0.0639(4) 0.5415(2) 0.0465(12) Uani 1 1 d . . . C15 C 0.7326(5) -0.0222(4) 0.5099(2) 0.0478(12) Uani 1 1 d . . . C16 C 0.7860(5) -0.0206(4) 0.4558(3) 0.0508(13) Uani 1 1 d . . . C17 C 0.8039(7) -0.1091(5) 0.4204(3) 0.0623(16) Uani 1 1 d . . . H17 H 0.7799 -0.1777 0.4290 0.075 Uiso 1 1 calc R . . C18 C 0.8610(6) -0.0764(4) 0.3730(3) 0.0617(15) Uani 1 1 d . . . H18 H 0.8851 -0.1176 0.3422 0.074 Uiso 1 1 calc R . . C19 C 0.8786(6) 0.0329(4) 0.3781(2) 0.0517(13) Uani 1 1 d . . . C20 C 0.9355(6) 0.0945(4) 0.3376(3) 0.0540(13) Uani 1 1 d . . . N6 N 0.3879(4) 0.2055(3) -0.0216(2) 0.0499(11) Uani 1 1 d . . . C21 C 0.3526(6) 0.2341(4) -0.0831(3) 0.0558(14) Uani 1 1 d . . . H21A H 0.3584 0.3081 -0.0777 0.067 Uiso 1 1 calc R . . H21B H 0.2610 0.1954 -0.0982 0.067 Uiso 1 1 calc R . . C22 C 0.4349(7) 0.2144(5) -0.1314(3) 0.0679(17) Uani 1 1 d . . . H22A H 0.4296 0.1406 -0.1385 0.082 Uiso 1 1 calc R . . H22B H 0.5269 0.2545 -0.1183 0.082 Uiso 1 1 calc R . . C23 C 0.3821(8) 0.2475(6) -0.1895(4) 0.084(2) Uani 1 1 d . . . H23A H 0.2863 0.2203 -0.1964 0.101 Uiso 1 1 calc R . . H23B H 0.4053 0.3234 -0.1845 0.101 Uiso 1 1 calc R . . C24 C 0.4348(10) 0.2097(8) -0.2432(4) 0.109(3) Uani 1 1 d . . . H24A H 0.5298 0.2349 -0.2362 0.164 Uiso 1 1 calc R . . H24B H 0.4021 0.2351 -0.2787 0.164 Uiso 1 1 calc R . . H24C H 0.4072 0.1344 -0.2500 0.164 Uiso 1 1 calc R . . C25 C 0.3920(5) 0.0937(4) -0.0275(3) 0.0513(13) Uani 1 1 d . . . H25A H 0.4648 0.0884 -0.0494 0.062 Uiso 1 1 calc R . . H25B H 0.4115 0.0774 0.0135 0.062 Uiso 1 1 calc R . . C26 C 0.2711(6) 0.0135(4) -0.0589(3) 0.0540(13) Uani 1 1 d . . . H26A H 0.2532 0.0250 -0.1011 0.065 Uiso 1 1 calc R . . H26B H 0.1962 0.0185 -0.0384 0.065 Uiso 1 1 calc R . . C27 C 0.2891(6) -0.0924(4) -0.0579(3) 0.0549(13) Uani 1 1 d . . . H27A H 0.3634 -0.0967 -0.0790 0.066 Uiso 1 1 calc R . . H27B H 0.3103 -0.1019 -0.0157 0.066 Uiso 1 1 calc R . . C28 C 0.1700(6) -0.1782(5) -0.0873(3) 0.0671(16) Uani 1 1 d . . . H28A H 0.0979 -0.1781 -0.0646 0.101 Uiso 1 1 calc R . . H28B H 0.1888 -0.2443 -0.0877 0.101 Uiso 1 1 calc R . . H28C H 0.1463 -0.1678 -0.1287 0.101 Uiso 1 1 calc R . . C29 C 0.2825(6) 0.2215(4) 0.0158(3) 0.0558(14) Uani 1 1 d . . . H29A H 0.2737 0.2910 0.0131 0.067 Uiso 1 1 calc R . . H29B H 0.1987 0.1711 -0.0024 0.067 Uiso 1 1 calc R . . C30 C 0.3070(7) 0.2108(5) 0.0810(3) 0.0688(17) Uani 1 1 d . . . H30A H 0.3788 0.2702 0.1022 0.083 Uiso 1 1 calc R . . H30B H 0.3327 0.1475 0.0849 0.083 Uiso 1 1 calc R . . C31 C 0.1844(8) 0.2058(5) 0.1093(4) 0.086(2) Uani 1 1 d . . . H31A H 0.1549 0.2663 0.1021 0.103 Uiso 1 1 calc R . . H31B H 0.1149 0.1433 0.0900 0.103 Uiso 1 1 calc R . . C32 C 0.2075(11) 0.2037(7) 0.1756(4) 0.121(4) Uani 1 1 d . . . H32A H 0.2424 0.1467 0.1829 0.181 Uiso 1 1 calc R . . H32B H 0.1254 0.1946 0.1920 0.181 Uiso 1 1 calc R . . H32C H 0.2697 0.2687 0.1954 0.181 Uiso 1 1 calc R . . C33 C 0.5218(5) 0.2716(4) 0.0085(3) 0.0515(13) Uani 1 1 d . . . H33A H 0.5869 0.2562 -0.0158 0.062 Uiso 1 1 calc R . . H33B H 0.5390 0.2513 0.0485 0.062 Uiso 1 1 calc R . . C34 C 0.5420(6) 0.3871(4) 0.0167(3) 0.0587(15) Uani 1 1 d . . . H34A H 0.4704 0.4030 0.0358 0.070 Uiso 1 1 calc R . . H34B H 0.5409 0.4108 -0.0231 0.070 Uiso 1 1 calc R . . C35 C 0.6718(7) 0.4436(5) 0.0560(3) 0.0720(18) Uani 1 1 d . . . H35A H 0.7401 0.4157 0.0415 0.086 Uiso 1 1 calc R . . H35B H 0.6945 0.5172 0.0512 0.086 Uiso 1 1 calc R . . C36 C 0.6711(8) 0.4348(6) 0.1223(4) 0.091(2) Uani 1 1 d . . . H36A H 0.6037 0.4621 0.1372 0.137 Uiso 1 1 calc R . . H36B H 0.7559 0.4741 0.1449 0.137 Uiso 1 1 calc R . . H36C H 0.6533 0.3624 0.1277 0.137 Uiso 1 1 calc R . . N1A N 1.0865(4) -0.0643(3) 0.20073(19) 0.0473(10) Uani 1 1 d . . . C2A C 1.1581(6) -0.0255(5) 0.2549(3) 0.0555(14) Uani 1 1 d . . . H2A H 1.2412 -0.0358 0.2629 0.067 Uiso 1 1 calc R . . C3A C 1.1143(6) 0.0294(5) 0.2997(3) 0.0575(14) Uani 1 1 d . . . H3A H 1.1678 0.0566 0.3373 0.069 Uiso 1 1 calc R . . C4A C 0.9922(6) 0.0444(4) 0.2894(2) 0.0529(13) Uani 1 1 d . . . C5A C 0.9212(6) 0.0070(5) 0.2321(3) 0.0574(14) Uani 1 1 d . . . H5A H 0.8394 0.0184 0.2222 0.069 Uiso 1 1 calc R . . C6A C 0.9716(6) -0.0469(5) 0.1898(3) 0.0555(14) Uani 1 1 d . . . H6A H 0.9218 -0.0727 0.1512 0.067 Uiso 1 1 calc R . . C1B C 0.9064(5) 0.5307(4) 0.3590(3) 0.0518(13) Uani 1 1 d . . . C2B C 0.8583(6) 0.5255(5) 0.2985(3) 0.0593(15) Uani 1 1 d . . . H2B H 0.8084 0.4611 0.2762 0.071 Uiso 1 1 calc R . . C3B C 0.8823(7) 0.6132(5) 0.2702(3) 0.0633(16) Uani 1 1 d . . . H3B H 0.8475 0.6087 0.2292 0.076 Uiso 1 1 calc R . . C4B C 0.9568(6) 0.7062(5) 0.3023(3) 0.0595(15) Uani 1 1 d . . . H4B H 0.9751 0.7657 0.2829 0.071 Uiso 1 1 calc R . . C5B C 1.0049(6) 0.7139(5) 0.3620(3) 0.0610(15) Uani 1 1 d . . . H5B H 1.0547 0.7787 0.3839 0.073 Uiso 1 1 calc R . . C6B C 0.9807(5) 0.6268(4) 0.3904(3) 0.0543(13) Uani 1 1 d . . . H6B H 1.0150 0.6325 0.4315 0.065 Uiso 1 1 calc R . . C1C C 0.6227(6) 0.3704(4) 0.6094(2) 0.0522(13) Uani 1 1 d . . . C2C C 0.6968(7) 0.4194(6) 0.6629(3) 0.081(2) Uani 1 1 d . . . H2C H 0.7856 0.4213 0.6696 0.097 Uiso 1 1 calc R . . C3C C 0.6454(8) 0.4657(7) 0.7069(4) 0.091(2) Uani 1 1 d . . . H3C H 0.6992 0.5003 0.7434 0.110 Uiso 1 1 calc R . . C4C C 0.5181(8) 0.4628(5) 0.6992(3) 0.0727(19) Uani 1 1 d . . . H4C H 0.4829 0.4949 0.7300 0.087 Uiso 1 1 calc R . . C5C C 0.4410(8) 0.4128(7) 0.6460(3) 0.089(2) Uani 1 1 d . . . H5C H 0.3516 0.4090 0.6399 0.107 Uiso 1 1 calc R . . C6C C 0.4960(7) 0.3676(7) 0.6013(3) 0.082(2) Uani 1 1 d . . . H6C H 0.4434 0.3342 0.5643 0.098 Uiso 1 1 calc R . . C1D C 0.7018(5) -0.1200(4) 0.5357(2) 0.0536(13) Uani 1 1 d . . . C2D C 0.5771(6) -0.1640(4) 0.5495(3) 0.0555(14) Uani 1 1 d . . . H2D H 0.5107 -0.1325 0.5408 0.067 Uiso 1 1 calc R . . C3D C 0.5496(6) -0.2527(4) 0.5758(3) 0.0568(14) Uani 1 1 d . . . H3D H 0.4653 -0.2809 0.5857 0.068 Uiso 1 1 calc R . . C4D C 0.6443(6) -0.3002(5) 0.5875(3) 0.0608(15) Uani 1 1 d . . . H4D H 0.6250 -0.3608 0.6058 0.073 Uiso 1 1 calc R . . C5D C 0.7680(6) -0.2602(5) 0.5728(3) 0.0583(14) Uani 1 1 d . . . H5D H 0.8326 -0.2938 0.5803 0.070 Uiso 1 1 calc R . . C6D C 0.7958(6) -0.1706(4) 0.5471(3) 0.0545(13) Uani 1 1 d . . . H6D H 0.8803 -0.1431 0.5371 0.065 Uiso 1 1 calc R . . C50 C 0.1294(8) 0.4943(5) 0.1041(4) 0.079(2) Uani 1 1 d . . . H50 H 0.1192 0.5636 0.0995 0.095 Uiso 1 1 calc R . . Cl5 Cl 0.0474(2) 0.44796(18) 0.16366(10) 0.0968(6) Uani 1 1 d . . . Cl6 Cl 0.2958(2) 0.50577(17) 0.12116(10) 0.0894(6) Uani 1 1 d . . . Cl7 Cl 0.0621(3) 0.41099(16) 0.03698(10) 0.1022(7) Uani 1 1 d . . . C60 C 0.5511(8) 0.1629(6) 0.2530(4) 0.087(2) Uani 1 1 d . . . H60 H 0.4693 0.1231 0.2259 0.104 Uiso 1 1 calc R . . Cl8 Cl 0.5377(3) 0.28360(19) 0.27985(12) 0.1228(9) Uani 1 1 d . . . Cl9 Cl 0.5759(2) 0.09299(17) 0.31154(11) 0.0978(6) Uani 1 1 d . . . Cl10 Cl 0.6809(3) 0.1793(2) 0.21130(12) 0.1136(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0457(3) 0.0476(3) 0.0527(3) 0.00259(19) 0.01230(18) 0.0145(2) Cl1 0.0482(8) 0.0533(8) 0.0799(10) -0.0043(7) 0.0165(7) 0.0087(7) Cl2 0.0482(8) 0.0552(8) 0.0592(8) 0.0042(6) 0.0113(6) 0.0104(6) Cl3 0.0682(10) 0.0676(10) 0.0715(10) 0.0098(8) 0.0182(8) 0.0188(8) Cl4 0.0674(9) 0.0574(8) 0.0521(8) 0.0077(6) 0.0139(6) 0.0221(7) N1 0.061(3) 0.053(3) 0.046(3) -0.003(2) 0.023(3) 0.002(3) O1 0.077(4) 0.104(5) 0.108(5) -0.013(4) 0.012(4) 0.046(4) N5 0.061(3) 0.044(2) 0.050(3) 0.0034(19) 0.013(2) 0.020(2) N2 0.053(3) 0.044(2) 0.054(3) 0.004(2) 0.012(2) 0.017(2) N3 0.049(3) 0.050(3) 0.049(3) 0.001(2) 0.008(2) 0.017(2) N4 0.058(3) 0.046(2) 0.053(3) 0.000(2) 0.014(2) 0.018(2) C1 0.056(3) 0.056(3) 0.053(3) 0.006(3) 0.017(3) 0.023(3) C2 0.075(4) 0.055(3) 0.060(4) 0.001(3) 0.029(3) 0.022(3) C3 0.076(4) 0.050(3) 0.060(4) 0.006(3) 0.028(3) 0.016(3) C4 0.054(3) 0.051(3) 0.056(3) 0.003(3) 0.015(3) 0.013(3) C5 0.053(3) 0.047(3) 0.049(3) 0.002(2) 0.011(2) 0.013(3) C6 0.052(3) 0.050(3) 0.052(3) 0.002(2) 0.012(2) 0.015(3) C7 0.063(4) 0.046(3) 0.064(4) 0.009(3) 0.022(3) 0.017(3) C8 0.083(4) 0.049(3) 0.058(4) 0.004(3) 0.026(3) 0.028(3) C9 0.055(3) 0.049(3) 0.051(3) 0.001(2) 0.012(3) 0.017(3) C10 0.046(3) 0.050(3) 0.048(3) 0.004(2) 0.011(2) 0.018(3) C11 0.046(3) 0.054(3) 0.049(3) 0.002(2) 0.011(2) 0.015(3) C12 0.052(3) 0.056(3) 0.051(3) 0.003(3) 0.014(2) 0.013(3) C13 0.059(3) 0.048(3) 0.050(3) 0.008(2) 0.012(2) 0.019(3) C14 0.047(3) 0.049(3) 0.045(3) 0.004(2) 0.006(2) 0.017(2) C15 0.046(3) 0.052(3) 0.044(3) 0.002(2) 0.003(2) 0.015(3) C16 0.052(3) 0.049(3) 0.052(3) 0.002(2) 0.010(2) 0.017(3) C17 0.082(5) 0.051(3) 0.054(3) 0.005(3) 0.021(3) 0.016(3) C18 0.075(4) 0.050(3) 0.058(4) -0.005(3) 0.014(3) 0.017(3) C19 0.055(3) 0.053(3) 0.048(3) 0.000(2) 0.007(2) 0.019(3) C20 0.060(4) 0.052(3) 0.049(3) -0.001(2) 0.012(3) 0.016(3) N6 0.048(3) 0.044(2) 0.059(3) 0.005(2) 0.010(2) 0.016(2) C21 0.057(4) 0.047(3) 0.068(4) 0.013(3) 0.005(3) 0.023(3) C22 0.068(4) 0.074(4) 0.071(4) 0.017(3) 0.012(3) 0.031(4) C23 0.093(6) 0.088(5) 0.088(5) 0.028(4) 0.031(4) 0.040(5) C24 0.107(7) 0.135(8) 0.085(6) 0.034(6) 0.022(5) 0.023(6) C25 0.047(3) 0.051(3) 0.055(3) 0.004(2) 0.009(2) 0.014(3) C26 0.052(3) 0.049(3) 0.063(4) 0.011(3) 0.010(3) 0.016(3) C27 0.051(3) 0.053(3) 0.059(3) 0.006(3) 0.007(3) 0.013(3) C28 0.064(4) 0.055(4) 0.073(4) 0.002(3) 0.014(3) 0.005(3) C29 0.047(3) 0.045(3) 0.080(4) 0.006(3) 0.016(3) 0.019(3) C30 0.065(4) 0.071(4) 0.074(4) 0.011(3) 0.031(3) 0.019(3) C31 0.092(6) 0.056(4) 0.122(7) 0.016(4) 0.063(5) 0.022(4) C32 0.166(10) 0.103(7) 0.109(7) 0.025(6) 0.088(7) 0.035(7) C33 0.042(3) 0.047(3) 0.064(4) 0.007(2) 0.008(2) 0.011(2) C34 0.056(4) 0.046(3) 0.075(4) 0.005(3) 0.016(3) 0.015(3) C35 0.062(4) 0.060(4) 0.086(5) -0.003(3) 0.013(3) 0.008(3) C36 0.084(5) 0.088(5) 0.083(5) -0.010(4) -0.005(4) 0.008(4) N1A 0.047(3) 0.049(2) 0.045(2) 0.0031(19) 0.0099(19) 0.012(2) C2A 0.054(3) 0.064(4) 0.054(3) 0.003(3) 0.009(3) 0.028(3) C3A 0.054(3) 0.063(4) 0.053(3) -0.003(3) 0.005(3) 0.019(3) C4A 0.063(4) 0.045(3) 0.047(3) 0.000(2) 0.015(3) 0.011(3) C5A 0.050(3) 0.068(4) 0.053(3) -0.003(3) 0.007(3) 0.020(3) C6A 0.048(3) 0.068(4) 0.052(3) -0.001(3) 0.009(2) 0.024(3) C1B 0.050(3) 0.053(3) 0.052(3) 0.003(2) 0.016(2) 0.014(3) C2B 0.071(4) 0.054(3) 0.052(3) 0.006(3) 0.013(3) 0.016(3) C3B 0.081(4) 0.064(4) 0.050(3) 0.009(3) 0.019(3) 0.026(3) C4B 0.070(4) 0.048(3) 0.069(4) 0.015(3) 0.027(3) 0.024(3) C5B 0.054(4) 0.055(3) 0.071(4) 0.002(3) 0.012(3) 0.013(3) C6B 0.049(3) 0.055(3) 0.059(3) 0.002(3) 0.010(3) 0.017(3) C1C 0.059(4) 0.050(3) 0.048(3) 0.004(2) 0.017(3) 0.016(3) C2C 0.060(4) 0.099(5) 0.070(4) -0.024(4) 0.011(3) 0.015(4) C3C 0.086(6) 0.103(6) 0.067(5) -0.027(4) 0.009(4) 0.014(5) C4C 0.103(6) 0.064(4) 0.066(4) 0.007(3) 0.039(4) 0.041(4) C5C 0.085(5) 0.129(7) 0.073(5) 0.001(5) 0.015(4) 0.068(5) C6C 0.069(4) 0.125(6) 0.056(4) -0.011(4) 0.007(3) 0.045(5) C1D 0.050(3) 0.059(3) 0.045(3) -0.005(2) 0.006(2) 0.009(3) C2D 0.056(3) 0.057(3) 0.051(3) -0.004(3) 0.006(3) 0.016(3) C3D 0.055(3) 0.052(3) 0.058(4) 0.002(3) 0.015(3) 0.008(3) C4D 0.073(4) 0.048(3) 0.055(4) 0.002(3) 0.014(3) 0.008(3) C5D 0.063(4) 0.054(3) 0.055(3) 0.001(3) 0.005(3) 0.017(3) C6D 0.054(3) 0.053(3) 0.056(3) 0.000(3) 0.013(3) 0.014(3) C50 0.085(5) 0.054(4) 0.094(5) 0.019(4) 0.011(4) 0.011(4) Cl5 0.0821(14) 0.1073(15) 0.0948(15) 0.0020(12) 0.0295(11) 0.0164(12) Cl6 0.0735(12) 0.0975(14) 0.0900(13) 0.0156(10) 0.0186(10) 0.0097(10) Cl7 0.1255(19) 0.0813(13) 0.0812(14) 0.0183(10) -0.0094(12) 0.0058(12) C60 0.095(6) 0.082(5) 0.072(5) 0.001(4) 0.021(4) 0.008(4) Cl8 0.180(3) 0.0949(16) 0.1050(18) 0.0121(13) 0.0539(18) 0.0482(18) Cl9 0.1048(16) 0.0916(14) 0.0981(15) 0.0192(11) 0.0352(12) 0.0208(12) Cl10 0.1067(18) 0.143(2) 0.1055(17) 0.0334(15) 0.0523(14) 0.0405(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 1.843(6) . ? Ru N1A 2.127(4) . ? Ru Cl3 2.3360(18) . ? Ru Cl4 2.3455(16) . ? Ru Cl2 2.3774(16) . ? Ru Cl1 2.3855(17) . ? N1 O1 0.939(7) . ? N5 C4 1.377(7) . ? N5 C1 1.385(7) . ? N2 C6 1.367(7) . ? N2 C9 1.374(7) . ? N3 C14 1.378(7) . ? N3 C11 1.379(7) . ? N4 C16 1.352(7) . ? N4 C19 1.369(7) . ? C1 C20 1.400(8) . ? C1 C2 1.433(8) . ? C2 C3 1.337(8) . ? C3 C4 1.446(8) . ? C4 C5 1.405(7) . ? C5 C6 1.406(8) . ? C5 C1B 1.492(8) . ? C6 C7 1.427(7) . ? C7 C8 1.342(8) . ? C8 C9 1.443(8) . ? C9 C10 1.387(8) . ? C10 C11 1.397(7) . ? C10 C1C 1.505(7) . ? C11 C12 1.439(8) . ? C12 C13 1.368(7) . ? C13 C14 1.438(7) . ? C14 C15 1.419(7) . ? C15 C16 1.405(8) . ? C15 C1D 1.488(8) . ? C16 C17 1.444(8) . ? C17 C18 1.350(8) . ? C18 C19 1.445(8) . ? C19 C20 1.389(8) . ? C20 C4A 1.496(7) . ? N6 C33 1.521(7) . ? N6 C21 1.523(7) . ? N6 C25 1.534(7) . ? N6 C29 1.537(7) . ? C21 C22 1.527(9) . ? C22 C23 1.540(10) . ? C23 C24 1.494(11) . ? C25 C26 1.503(8) . ? C26 C27 1.517(8) . ? C27 C28 1.513(8) . ? C29 C30 1.500(9) . ? C30 C31 1.523(9) . ? C31 C32 1.496(13) . ? C33 C34 1.521(7) . ? C34 C35 1.531(9) . ? C35 C36 1.517(11) . ? N1A C6A 1.334(7) . ? N1A C2A 1.344(7) . ? C2A C3A 1.393(8) . ? C3A C4A 1.394(8) . ? C4A C5A 1.397(8) . ? C5A C6A 1.390(8) . ? C1B C2B 1.395(8) . ? C1B C6B 1.403(8) . ? C2B C3B 1.398(8) . ? C3B C4B 1.378(9) . ? C4B C5B 1.377(9) . ? C5B C6B 1.391(8) . ? C1C C6C 1.354(9) . ? C1C C2C 1.367(9) . ? C2C C3C 1.369(10) . ? C3C C4C 1.361(11) . ? C4C C5C 1.377(11) . ? C5C C6C 1.396(9) . ? C1D C6D 1.400(8) . ? C1D C2D 1.403(8) . ? C2D C3D 1.384(8) . ? C3D C4D 1.376(9) . ? C4D C5D 1.390(9) . ? C5D C6D 1.387(8) . ? C50 Cl7 1.745(8) . ? C50 Cl6 1.763(8) . ? C50 Cl5 1.771(8) . ? C60 Cl8 1.745(8) . ? C60 Cl10 1.752(8) . ? C60 Cl9 1.756(8) . ? 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 Ru N1A 91.5(2) . . ? N1 Ru Cl3 90.58(17) . . ? N1A Ru Cl3 177.59(13) . . ? N1 Ru Cl4 178.13(17) . . ? N1A Ru Cl4 87.92(12) . . ? Cl3 Ru Cl4 89.99(6) . . ? N1 Ru Cl2 89.00(17) . . ? N1A Ru Cl2 89.17(13) . . ? Cl3 Ru Cl2 89.59(6) . . ? Cl4 Ru Cl2 89.22(6) . . ? N1 Ru Cl1 92.79(18) . . ? N1A Ru Cl1 90.76(13) . . ? Cl3 Ru Cl1 90.41(6) . . ? Cl4 Ru Cl1 88.99(6) . . ? Cl2 Ru Cl1 178.21(6) . . ? O1 N1 Ru 173.1(7) . . ? C4 N5 C1 107.3(5) . . ? C6 N2 C9 108.0(4) . . ? C14 N3 C11 107.6(4) . . ? C16 N4 C19 108.5(4) . . ? N5 C1 C20 124.9(5) . . ? N5 C1 C2 108.7(5) . . ? C20 C1 C2 126.4(5) . . ? C3 C2 C1 107.8(5) . . ? C2 C3 C4 108.2(5) . . ? N5 C4 C5 125.7(5) . . ? N5 C4 C3 108.0(5) . . ? C5 C4 C3 126.2(5) . . ? C4 C5 C6 124.5(5) . . ? C4 C5 C1B 117.4(5) . . ? C6 C5 C1B 118.0(5) . . ? N2 C6 C5 125.2(5) . . ? N2 C6 C7 108.9(5) . . ? C5 C6 C7 125.9(5) . . ? C8 C7 C6 107.5(5) . . ? C7 C8 C9 108.1(5) . . ? N2 C9 C10 128.3(5) . . ? N2 C9 C8 107.5(5) . . ? C10 C9 C8 124.1(5) . . ? C9 C10 C11 125.5(5) . . ? C9 C10 C1C 117.2(5) . . ? C11 C10 C1C 117.2(5) . . ? N3 C11 C10 126.0(5) . . ? N3 C11 C12 108.7(5) . . ? C10 C11 C12 125.3(5) . . ? C13 C12 C11 107.5(5) . . ? C12 C13 C14 107.2(5) . . ? N3 C14 C15 125.4(5) . . ? N3 C14 C13 109.0(4) . . ? C15 C14 C13 125.7(5) . . ? C16 C15 C14 124.1(5) . . ? C16 C15 C1D 118.0(5) . . ? C14 C15 C1D 117.9(5) . . ? N4 C16 C15 126.4(5) . . ? N4 C16 C17 108.6(5) . . ? C15 C16 C17 125.0(5) . . ? C18 C17 C16 107.4(5) . . ? C17 C18 C19 107.1(5) . . ? N4 C19 C20 127.5(5) . . ? N4 C19 C18 108.3(5) . . ? C20 C19 C18 124.2(5) . . ? C19 C20 C1 126.8(5) . . ? C19 C20 C4A 116.7(5) . . ? C1 C20 C4A 116.5(5) . . ? C33 N6 C21 111.6(4) . . ? C33 N6 C25 106.5(4) . . ? C21 N6 C25 110.8(4) . . ? C33 N6 C29 111.0(4) . . ? C21 N6 C29 105.9(4) . . ? C25 N6 C29 111.2(4) . . ? N6 C21 C22 116.5(4) . . ? C21 C22 C23 107.8(5) . . ? C24 C23 C22 112.2(6) . . ? C26 C25 N6 116.4(4) . . ? C25 C26 C27 109.5(5) . . ? C28 C27 C26 113.0(5) . . ? C30 C29 N6 115.1(5) . . ? C29 C30 C31 109.5(6) . . ? C32 C31 C30 111.3(8) . . ? N6 C33 C34 115.7(4) . . ? C33 C34 C35 110.5(5) . . ? C36 C35 C34 113.7(6) . . ? C6A N1A C2A 118.2(5) . . ? C6A N1A Ru 120.5(4) . . ? C2A N1A Ru 121.1(4) . . ? N1A C2A C3A 122.0(5) . . ? C2A C3A C4A 120.1(5) . . ? C3A C4A C5A 117.1(5) . . ? C3A C4A C20 122.3(5) . . ? C5A C4A C20 120.6(5) . . ? C6A C5A C4A 119.3(5) . . ? N1A C6A C5A 123.2(5) . . ? C2B C1B C6B 117.9(5) . . ? C2B C1B C5 120.3(5) . . ? C6B C1B C5 121.8(5) . . ? C1B C2B C3B 121.3(6) . . ? C4B C3B C2B 119.3(6) . . ? C5B C4B C3B 120.7(6) . . ? C4B C5B C6B 120.0(6) . . ? C5B C6B C1B 120.8(6) . . ? C6C C1C C2C 118.3(6) . . ? C6C C1C C10 121.2(5) . . ? C2C C1C C10 120.5(6) . . ? C1C C2C C3C 121.1(7) . . ? C4C C3C C2C 120.9(7) . . ? C3C C4C C5C 119.1(6) . . ? C4C C5C C6C 119.1(7) . . ? C1C C6C C5C 121.6(7) . . ? C6D C1D C2D 118.0(6) . . ? C6D C1D C15 121.3(5) . . ? C2D C1D C15 120.7(5) . . ? C3D C2D C1D 120.8(6) . . ? C4D C3D C2D 120.1(6) . . ? C3D C4D C5D 120.6(6) . . ? C6D C5D C4D 119.3(6) . . ? C5D C6D C1D 121.2(6) . . ? Cl7 C50 Cl6 110.6(5) . . ? Cl7 C50 Cl5 109.9(4) . . ? Cl6 C50 Cl5 109.5(4) . . ? Cl8 C60 Cl10 108.7(4) . . ? Cl8 C60 Cl9 112.2(4) . . ? Cl10 C60 Cl9 109.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Ru N1 O1 71(6) . . . . ? Cl3 Ru N1 O1 -108(6) . . . . ? Cl4 Ru N1 O1 0(11) . . . . ? Cl2 Ru N1 O1 -18(6) . . . . ? Cl1 Ru N1 O1 162(6) . . . . ? C4 N5 C1 C20 -178.2(6) . . . . ? C4 N5 C1 C2 1.6(7) . . . . ? N5 C1 C2 C3 -1.1(8) . . . . ? C20 C1 C2 C3 178.7(6) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? C1 N5 C4 C5 176.6(6) . . . . ? C1 N5 C4 C3 -1.5(7) . . . . ? C2 C3 C4 N5 0.9(7) . . . . ? C2 C3 C4 C5 -177.2(6) . . . . ? N5 C4 C5 C6 7.2(10) . . . . ? C3 C4 C5 C6 -175.1(6) . . . . ? N5 C4 C5 C1B -171.9(5) . . . . ? C3 C4 C5 C1B 5.8(9) . . . . ? C9 N2 C6 C5 -179.5(6) . . . . ? C9 N2 C6 C7 -0.3(7) . . . . ? C4 C5 C6 N2 0.7(10) . . . . ? C1B C5 C6 N2 179.8(5) . . . . ? C4 C5 C6 C7 -178.3(6) . . . . ? C1B C5 C6 C7 0.8(9) . . . . ? N2 C6 C7 C8 -0.1(7) . . . . ? C5 C6 C7 C8 179.1(6) . . . . ? C6 C7 C8 C9 0.5(7) . . . . ? C6 N2 C9 C10 -179.5(6) . . . . ? C6 N2 C9 C8 0.5(7) . . . . ? C7 C8 C9 N2 -0.6(7) . . . . ? C7 C8 C9 C10 179.4(6) . . . . ? N2 C9 C10 C11 -3.0(10) . . . . ? C8 C9 C10 C11 177.0(6) . . . . ? N2 C9 C10 C1C 176.9(5) . . . . ? C8 C9 C10 C1C -3.1(9) . . . . ? C14 N3 C11 C10 -177.4(5) . . . . ? C14 N3 C11 C12 0.6(6) . . . . ? C9 C10 C11 N3 -4.0(9) . . . . ? C1C C10 C11 N3 176.0(5) . . . . ? C9 C10 C11 C12 178.3(6) . . . . ? C1C C10 C11 C12 -1.7(8) . . . . ? N3 C11 C12 C13 0.2(7) . . . . ? C10 C11 C12 C13 178.2(5) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C11 N3 C14 C15 177.3(5) . . . . ? C11 N3 C14 C13 -1.2(6) . . . . ? C12 C13 C14 N3 1.3(6) . . . . ? C12 C13 C14 C15 -177.2(5) . . . . ? N3 C14 C15 C16 2.4(9) . . . . ? C13 C14 C15 C16 -179.4(5) . . . . ? N3 C14 C15 C1D -177.8(5) . . . . ? C13 C14 C15 C1D 0.4(8) . . . . ? C19 N4 C16 C15 178.0(6) . . . . ? C19 N4 C16 C17 -1.1(7) . . . . ? C14 C15 C16 N4 6.0(9) . . . . ? C1D C15 C16 N4 -173.8(5) . . . . ? C14 C15 C16 C17 -174.9(5) . . . . ? C1D C15 C16 C17 5.3(9) . . . . ? N4 C16 C17 C18 1.0(7) . . . . ? C15 C16 C17 C18 -178.2(6) . . . . ? C16 C17 C18 C19 -0.4(7) . . . . ? C16 N4 C19 C20 -178.9(6) . . . . ? C16 N4 C19 C18 0.9(7) . . . . ? C17 C18 C19 N4 -0.3(7) . . . . ? C17 C18 C19 C20 179.5(6) . . . . ? N4 C19 C20 C1 -5.6(10) . . . . ? C18 C19 C20 C1 174.7(6) . . . . ? N4 C19 C20 C4A 174.0(5) . . . . ? C18 C19 C20 C4A -5.8(9) . . . . ? N5 C1 C20 C19 -3.1(10) . . . . ? C2 C1 C20 C19 177.1(6) . . . . ? N5 C1 C20 C4A 177.3(5) . . . . ? C2 C1 C20 C4A -2.4(9) . . . . ? C33 N6 C21 C22 65.2(6) . . . . ? C25 N6 C21 C22 -53.2(7) . . . . ? C29 N6 C21 C22 -173.9(5) . . . . ? N6 C21 C22 C23 179.4(5) . . . . ? C21 C22 C23 C24 -166.8(7) . . . . ? C33 N6 C25 C26 -177.2(5) . . . . ? C21 N6 C25 C26 -55.7(6) . . . . ? C29 N6 C25 C26 61.8(6) . . . . ? N6 C25 C26 C27 -177.1(5) . . . . ? C25 C26 C27 C28 178.5(5) . . . . ? C33 N6 C29 C30 -51.2(6) . . . . ? C21 N6 C29 C30 -172.5(5) . . . . ? C25 N6 C29 C30 67.1(6) . . . . ? N6 C29 C30 C31 -168.1(5) . . . . ? C29 C30 C31 C32 -175.3(6) . . . . ? C21 N6 C33 C34 56.6(6) . . . . ? C25 N6 C33 C34 177.6(5) . . . . ? C29 N6 C33 C34 -61.2(6) . . . . ? N6 C33 C34 C35 171.0(5) . . . . ? C33 C34 C35 C36 -74.5(7) . . . . ? N5 Ru N1A C6A -136.0(5) . . . . ? Cl3 Ru N1A C6A 12(3) . . . . ? Cl4 Ru N1A C6A 42.3(4) . . . . ? Cl2 Ru N1A C6A -47.0(4) . . . . ? Cl1 Ru N1A C6A 131.2(4) . . . . ? N5 Ru N1A C2A 39.7(5) . . . . ? Cl3 Ru N1A C2A -172(3) . . . . ? Cl4 Ru N1A C2A -142.1(4) . . . . ? Cl2 Ru N1A C2A 128.7(4) . . . . ? Cl1 Ru N1A C2A -53.1(4) . . . . ? C6A N1A C2A C3A 1.7(9) . . . . ? Ru N1A C2A C3A -174.1(4) . . . . ? N1A C2A C3A C4A 0.8(9) . . . . ? C2A C3A C4A C5A -3.2(9) . . . . ? C2A C3A C4A C20 174.5(5) . . . . ? C19 C20 C4A C3A -80.6(7) . . . . ? C1 C20 C4A C3A 99.0(7) . . . . ? C19 C20 C4A C5A 96.9(7) . . . . ? C1 C20 C4A C5A -83.4(7) . . . . ? C3A C4A C5A C6A 3.2(9) . . . . ? C20 C4A C5A C6A -174.5(5) . . . . ? C2A N1A C6A C5A -1.7(9) . . . . ? Ru N1A C6A C5A 174.1(5) . . . . ? C4A C5A C6A N1A -0.8(10) . . . . ? C4 C5 C1B C2B 56.4(8) . . . . ? C6 C5 C1B C2B -122.8(6) . . . . ? C4 C5 C1B C6B -121.6(6) . . . . ? C6 C5 C1B C6B 59.2(8) . . . . ? C6B C1B C2B C3B -0.6(9) . . . . ? C5 C1B C2B C3B -178.6(5) . . . . ? C1B C2B C3B C4B 1.2(9) . . . . ? C2B C3B C4B C5B -1.5(9) . . . . ? C3B C4B C5B C6B 1.3(9) . . . . ? C4B C5B C6B C1B -0.6(9) . . . . ? C2B C1B C6B C5B 0.3(8) . . . . ? C5 C1B C6B C5B 178.3(5) . . . . ? C9 C10 C1C C6C 86.5(8) . . . . ? C11 C10 C1C C6C -93.5(8) . . . . ? C9 C10 C1C C2C -94.0(8) . . . . ? C11 C10 C1C C2C 86.0(8) . . . . ? C6C C1C C2C C3C -0.9(12) . . . . ? C10 C1C C2C C3C 179.6(7) . . . . ? C1C C2C C3C C4C 1.1(13) . . . . ? C2C C3C C4C C5C -0.2(13) . . . . ? C3C C4C C5C C6C -0.9(12) . . . . ? C2C C1C C6C C5C -0.3(12) . . . . ? C10 C1C C6C C5C 179.2(7) . . . . ? C4C C5C C6C C1C 1.2(13) . . . . ? C16 C15 C1D C6D 54.4(7) . . . . ? C14 C15 C1D C6D -125.3(6) . . . . ? C16 C15 C1D C2D -125.8(6) . . . . ? C14 C15 C1D C2D 54.4(7) . . . . ? C6D C1D C2D C3D 2.3(8) . . . . ? C15 C1D C2D C3D -177.4(5) . . . . ? C1D C2D C3D C4D -1.3(9) . . . . ? C2D C3D C4D C5D -0.4(9) . . . . ? C3D C4D C5D C6D 1.1(9) . . . . ? C4D C5D C6D C1D -0.1(9) . . . . ? C2D C1D C6D C5D -1.6(8) . . . . ? C15 C1D C6D C5D 178.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.736 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.091 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 265964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-trichloro-cis-bis(5-(4'pyridyl)-10,15,20-trisphenyl-porphyrin)-nitrosyl- ruthenium(II) chloroform n-hexane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H58 Cl3 N11 O Ru, 2.5(C H Cl3), 0.5(C6 H14)' _chemical_formula_sum 'C91.50 H67.50 Cl10.50 N11 O Ru' _chemical_formula_weight 1810.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0074 0.0035 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.2413 0.3112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.5010 1.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 16.978(4) _cell_length_b 14.283(4) _cell_length_c 73.283(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.28(3) _cell_angle_gamma 90.00 _cell_volume 17767(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7392 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.0000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'CCD MarResearch' _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 47057 _diffrn_reflns_av_R_equivalents 0.1299 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -77 _diffrn_reflns_limit_l_max 76 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 31.96 _reflns_number_total 9229 _reflns_number_gt 5479 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.04 (Farrugia, 1999)' _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^)+(0.2000P)^2^] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9229 _refine_ls_number_parameters 848 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.3129 _refine_ls_wR_factor_gt 0.2747 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.215 _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 Ru Ru 0.84070(7) 0.57962(9) 0.379158(13) 0.0455(6) Uani 1 1 d D . . Cl1 Cl 0.7784(2) 0.7082(3) 0.36421(4) 0.0496(11) Uani 1 1 d . . . Cl2 Cl 0.8920(2) 0.4414(3) 0.39234(5) 0.0567(12) Uani 1 1 d . . . Cl3 Cl 0.9537(3) 0.5956(3) 0.36128(6) 0.0709(13) Uani 1 1 d . . . N1X N 0.8823(10) 0.6517(12) 0.3963(2) 0.076(5) Uani 1 1 d D . . O1X O 0.9057(9) 0.7041(10) 0.40408(18) 0.073(4) Uani 1 1 d D . . N1A N 0.7389(8) 0.5612(8) 0.39502(14) 0.040(3) Uani 1 1 d . . . C2A C 0.6664(10) 0.5658(12) 0.38751(19) 0.052(4) Uani 1 1 d . . . H2A H 0.6601 0.5792 0.3749 0.062 Uiso 1 1 calc R . . C3A C 0.6016(10) 0.5515(12) 0.39776(18) 0.053(4) Uani 1 1 d . . . H3A H 0.5507 0.5600 0.3924 0.064 Uiso 1 1 calc R . . C4A C 0.6086(10) 0.5242(10) 0.41625(16) 0.047(4) Uani 1 1 d . . . C5A C 0.6861(9) 0.5185(13) 0.42353(17) 0.057(5) Uani 1 1 d . . . H5A H 0.6948 0.5035 0.4360 0.069 Uiso 1 1 calc R . . C6A C 0.7488(10) 0.5348(13) 0.41252(18) 0.059(5) Uani 1 1 d . . . H6A H 0.8007 0.5271 0.4174 0.071 Uiso 1 1 calc R . . N1B N 0.7892(7) 0.4905(11) 0.35881(13) 0.050(4) Uani 1 1 d . . . C2B C 0.7604(9) 0.4063(11) 0.36236(19) 0.045(4) Uani 1 1 d . . . H2B H 0.7528 0.3891 0.3747 0.054 Uiso 1 1 calc R . . C3B C 0.7405(9) 0.3410(11) 0.34855(17) 0.046(4) Uani 1 1 d . . . H3B H 0.7192 0.2817 0.3517 0.055 Uiso 1 1 calc R . . C4B C 0.7522(9) 0.3640(9) 0.33035(16) 0.038(4) Uani 1 1 d . . . C5B C 0.7764(10) 0.4525(11) 0.32667(17) 0.051(4) Uani 1 1 d . . . H5B H 0.7810 0.4706 0.3143 0.061 Uiso 1 1 calc R . . C6B C 0.7955(9) 0.5199(11) 0.34052(18) 0.045(4) Uani 1 1 d . . . H6B H 0.8117 0.5816 0.3375 0.054 Uiso 1 1 calc R . . N1 N 0.4211(7) 0.5690(9) 0.44184(13) 0.046(3) Uani 1 1 d . . . H1N H 0.4029 0.5167 0.4465 0.055 Uiso 1 1 calc R . . N2 N 0.2832(8) 0.5165(9) 0.46305(13) 0.052(3) Uani 1 1 d . . . N3 N 0.3250(8) 0.3214(8) 0.46179(14) 0.049(3) Uani 1 1 d . . . H3N H 0.3439 0.3738 0.4573 0.058 Uiso 1 1 calc R . . N4 N 0.4700(8) 0.3739(9) 0.44278(15) 0.052(3) Uani 1 1 d . . . C1 C 0.4888(9) 0.5769(10) 0.43195(18) 0.045(4) Uiso 1 1 d . . . C2 C 0.4949(10) 0.6737(12) 0.4268(2) 0.056(4) Uiso 1 1 d . . . H2 H 0.5349 0.6998 0.4195 0.067 Uiso 1 1 calc R . . C3 C 0.4346(10) 0.7214(12) 0.43408(19) 0.056(4) Uiso 1 1 d . . . H3 H 0.4262 0.7870 0.4331 0.067 Uiso 1 1 calc R . . C4 C 0.3856(9) 0.6575(11) 0.44340(18) 0.046(4) Uiso 1 1 d . . . C5 C 0.3178(9) 0.6781(11) 0.45249(18) 0.051(4) Uiso 1 1 d . . . C6 C 0.2693(9) 0.6141(11) 0.46129(18) 0.049(4) Uiso 1 1 d . . . C7 C 0.1947(9) 0.6345(12) 0.46853(19) 0.054(4) Uiso 1 1 d . . . H7 H 0.1724 0.6954 0.4691 0.065 Uiso 1 1 calc R . . C8 C 0.1592(10) 0.5557(11) 0.47449(18) 0.049(4) Uiso 1 1 d . . . H8 H 0.1089 0.5504 0.4798 0.059 Uiso 1 1 calc R . . C9 C 0.2148(9) 0.4812(10) 0.47102(17) 0.044(3) Uiso 1 1 d . . . C10 C 0.2023(9) 0.3882(11) 0.47465(17) 0.043(4) Uiso 1 1 d . . . C11 C 0.2528(9) 0.3111(11) 0.47071(18) 0.047(4) Uiso 1 1 d . . . C12 C 0.2498(10) 0.2153(12) 0.4759(2) 0.056(4) Uiso 1 1 d . . . H12 H 0.2084 0.1872 0.4825 0.067 Uiso 1 1 calc R . . C13 C 0.3138(10) 0.1706(13) 0.4702(2) 0.061(4) Uiso 1 1 d . . . H13 H 0.3256 0.1061 0.4719 0.073 Uiso 1 1 calc R . . C14 C 0.3601(10) 0.2365(12) 0.46133(19) 0.054(4) Uiso 1 1 d . . . C15 C 0.4360(11) 0.2192(13) 0.4534(2) 0.066(5) Uiso 1 1 d . . . C16 C 0.4820(9) 0.2793(11) 0.44452(18) 0.050(4) Uiso 1 1 d . . . C17 C 0.5543(10) 0.2594(12) 0.43575(19) 0.056(4) Uiso 1 1 d . . . H17 H 0.5777 0.1991 0.4350 0.067 Uiso 1 1 calc R . . C18 C 0.5833(11) 0.3349(12) 0.4289(2) 0.063(4) Uiso 1 1 d . . . H18 H 0.6313 0.3397 0.4226 0.076 Uiso 1 1 calc R . . C19 C 0.5315(9) 0.4083(11) 0.43258(19) 0.048(4) Uiso 1 1 d . . . C20 C 0.5383(9) 0.5018(11) 0.42749(18) 0.047(4) Uiso 1 1 d . . . N5 N 0.6781(7) 0.2677(8) 0.28521(13) 0.041(3) Uani 1 1 d . . . H5N H 0.7062 0.2197 0.2816 0.049 Uiso 1 1 calc R . . N6 N 0.6781(7) 0.1453(8) 0.25341(12) 0.037(3) Uani 1 1 d . . . N7 N 0.7906(7) 0.0180(8) 0.27106(14) 0.043(3) Uani 1 1 d . . . H7N H 0.7732 0.0748 0.2733 0.051 Uiso 1 1 calc R . . N8 N 0.7926(7) 0.1450(8) 0.30272(14) 0.044(3) Uani 1 1 d . . . C21 C 0.6884(9) 0.3144(11) 0.30148(18) 0.046(4) Uiso 1 1 d . . . C22 C 0.6287(9) 0.3821(11) 0.30242(18) 0.047(4) Uiso 1 1 d . . . H22 H 0.6206 0.4233 0.3124 0.057 Uiso 1 1 calc R . . C23 C 0.5834(9) 0.3790(11) 0.28641(17) 0.045(4) Uiso 1 1 d . . . H23 H 0.5390 0.4170 0.2835 0.054 Uiso 1 1 calc R . . C24 C 0.6158(8) 0.3086(10) 0.27535(16) 0.035(3) Uiso 1 1 d . . . C25 C 0.5926(8) 0.2855(10) 0.25755(17) 0.039(3) Uiso 1 1 d . . . C26 C 0.6271(8) 0.2124(10) 0.24720(17) 0.038(3) Uiso 1 1 d . . . C27 C 0.6121(8) 0.1979(10) 0.22770(17) 0.040(3) Uiso 1 1 d . . . H27 H 0.5819 0.2379 0.2199 0.049 Uiso 1 1 calc R . . C28 C 0.6474(9) 0.1201(10) 0.22273(18) 0.042(3) Uiso 1 1 d . . . H28 H 0.6443 0.0916 0.2110 0.051 Uiso 1 1 calc R . . C29 C 0.6930(9) 0.0850(10) 0.23899(17) 0.039(3) Uiso 1 1 d . . . C30 C 0.7345(9) 0.0021(11) 0.24011(18) 0.049(4) Uiso 1 1 d . . . C31 C 0.7770(8) -0.0304(10) 0.25531(17) 0.039(3) Uiso 1 1 d . . . C32 C 0.8112(8) -0.1214(10) 0.25791(17) 0.042(3) Uiso 1 1 d . . . H32 H 0.8080 -0.1725 0.2496 0.050 Uiso 1 1 calc R . . C33 C 0.8487(9) -0.1209(10) 0.27433(17) 0.043(3) Uiso 1 1 d . . . H33 H 0.8791 -0.1710 0.2793 0.051 Uiso 1 1 calc R . . C34 C 0.8358(9) -0.0348(11) 0.28302(18) 0.045(4) Uiso 1 1 d . . . C35 C 0.8642(9) -0.0072(11) 0.30046(17) 0.044(4) Uiso 1 1 d . . . C36 C 0.8466(9) 0.0781(10) 0.30903(18) 0.045(4) Uiso 1 1 d . . . C37 C 0.8817(9) 0.1088(11) 0.32627(18) 0.047(4) Uiso 1 1 d . . . H37 H 0.9202 0.0764 0.3335 0.056 Uiso 1 1 calc R . . C38 C 0.8485(9) 0.1931(11) 0.3301(2) 0.053(4) Uiso 1 1 d . . . H38 H 0.8608 0.2317 0.3403 0.064 Uiso 1 1 calc R . . C39 C 0.7918(9) 0.2128(11) 0.31588(18) 0.046(4) Uiso 1 1 d . . . C40 C 0.7455(9) 0.2934(11) 0.31531(19) 0.050(4) Uiso 1 1 d . . . C1C C 0.2870(10) 0.7764(12) 0.4516(2) 0.060(5) Uani 1 1 d . . . C2C C 0.2642(12) 0.8151(14) 0.4350(3) 0.084(6) Uani 1 1 d . . . H2C H 0.2701 0.7819 0.4239 0.101 Uiso 1 1 calc R . . C3C C 0.2312(15) 0.9076(18) 0.4353(4) 0.108(9) Uani 1 1 d . . . H3C H 0.2084 0.9319 0.4243 0.129 Uiso 1 1 calc R . . C4C C 0.2309(15) 0.9611(18) 0.4501(6) 0.119(11) Uani 1 1 d . . . H4C H 0.2174 1.0256 0.4495 0.143 Uiso 1 1 calc R . . C5C C 0.2512(15) 0.9185(17) 0.4666(5) 0.109(9) Uani 1 1 d . . . H5C H 0.2434 0.9521 0.4776 0.131 Uiso 1 1 calc R . . C6C C 0.2825(12) 0.8280(14) 0.4677(3) 0.078(6) Uani 1 1 d . . . H6C H 0.3003 0.8026 0.4790 0.094 Uiso 1 1 calc R . . C1D C 0.1268(9) 0.3601(9) 0.48332(18) 0.042(4) Uani 1 1 d . . . C2D C 0.1023(11) 0.3934(11) 0.49994(18) 0.054(5) Uani 1 1 d . . . H2D H 0.1367 0.4340 0.5066 0.065 Uiso 1 1 calc R . . C3D C 0.0328(9) 0.3719(13) 0.50732(18) 0.053(4) Uani 1 1 d . . . H3D H 0.0200 0.3960 0.5190 0.064 Uiso 1 1 calc R . . C4D C -0.0181(11) 0.3165(13) 0.4983(2) 0.062(5) Uani 1 1 d . . . H4D H -0.0677 0.3025 0.5034 0.074 Uiso 1 1 calc R . . C5D C 0.0013(11) 0.2796(13) 0.48153(19) 0.061(5) Uani 1 1 d . . . H5D H -0.0344 0.2389 0.4753 0.073 Uiso 1 1 calc R . . C6D C 0.0723(10) 0.3017(12) 0.4739(2) 0.054(4) Uani 1 1 d . . . H6D H 0.0847 0.2776 0.4622 0.065 Uiso 1 1 calc R . . C1E C 0.4613(11) 0.1161(12) 0.4544(2) 0.063(5) Uani 1 1 d . . . C2E C 0.4917(13) 0.0815(14) 0.4698(3) 0.074(6) Uani 1 1 d . . . H2E H 0.4932 0.1179 0.4806 0.089 Uiso 1 1 calc R . . C3E C 0.5233(13) -0.0155(16) 0.4697(3) 0.089(6) Uani 1 1 d . . . H3E H 0.5429 -0.0447 0.4805 0.107 Uiso 1 1 calc R . . C4E C 0.5228(14) -0.0614(15) 0.4529(4) 0.088(7) Uani 1 1 d . . . H4E H 0.5454 -0.1221 0.4522 0.106 Uiso 1 1 calc R . . C5E C 0.4928(17) -0.0249(17) 0.4380(4) 0.106(8) Uani 1 1 d . . . H5E H 0.4934 -0.0601 0.4270 0.128 Uiso 1 1 calc R . . C6E C 0.4599(14) 0.0640(14) 0.4378(3) 0.081(6) Uani 1 1 d . . . H6E H 0.4373 0.0894 0.4269 0.097 Uiso 1 1 calc R . . C1F C 0.5285(9) 0.3394(12) 0.24871(16) 0.047(4) Uani 1 1 d . . . C2F C 0.4634(9) 0.2950(11) 0.24107(17) 0.046(4) Uani 1 1 d . . . H2F H 0.4600 0.2287 0.2414 0.055 Uiso 1 1 calc R . . C3F C 0.4021(9) 0.3476(12) 0.23284(17) 0.049(4) Uani 1 1 d . . . H3F H 0.3570 0.3169 0.2278 0.059 Uiso 1 1 calc R . . C4F C 0.4078(10) 0.4444(11) 0.23205(17) 0.047(4) Uani 1 1 d . . . H4F H 0.3674 0.4801 0.2262 0.057 Uiso 1 1 calc R . . C5F C 0.4712(9) 0.4876(11) 0.23976(17) 0.042(4) Uani 1 1 d . . . H5F H 0.4738 0.5540 0.2396 0.050 Uiso 1 1 calc R . . C6F C 0.5317(10) 0.4376(10) 0.24776(16) 0.042(4) Uani 1 1 d . . . H6F H 0.5763 0.4698 0.2527 0.050 Uiso 1 1 calc R . . C1G C 0.7291(10) -0.0649(9) 0.22404(16) 0.041(4) Uani 1 1 d . . . C2G C 0.6553(10) -0.0918(10) 0.21739(16) 0.047(4) Uani 1 1 d . . . H2G H 0.6086 -0.0685 0.2226 0.056 Uiso 1 1 calc R . . C3G C 0.6518(11) -0.1551(11) 0.20254(19) 0.058(5) Uani 1 1 d . . . H3G H 0.6016 -0.1765 0.1984 0.069 Uiso 1 1 calc R . . C4G C 0.7160(9) -0.1865(10) 0.19406(19) 0.045(4) Uani 1 1 d . . . H4G H 0.7115 -0.2267 0.1838 0.054 Uiso 1 1 calc R . . C5G C 0.7906(10) -0.1578(11) 0.20095(18) 0.051(4) Uani 1 1 d . . . H5G H 0.8373 -0.1808 0.1956 0.062 Uiso 1 1 calc R . . C6G C 0.7951(9) -0.0967(10) 0.21534(17) 0.041(4) Uani 1 1 d . . . H6G H 0.8454 -0.0755 0.2195 0.049 Uiso 1 1 calc R . . C1H C 0.9155(9) -0.0762(10) 0.31066(17) 0.043(4) Uani 1 1 d . . . C2H C 0.9916(11) -0.0963(12) 0.3048(2) 0.060(5) Uani 1 1 d . . . H2H H 1.0100 -0.0670 0.2941 0.073 Uiso 1 1 calc R . . C3H C 1.0406(11) -0.1575(12) 0.3142(2) 0.061(5) Uani 1 1 d . . . H3H H 1.0932 -0.1682 0.3106 0.073 Uiso 1 1 calc R . . C4H C 1.0088(11) -0.2038(11) 0.32964(18) 0.055(5) Uani 1 1 d . . . H4H H 1.0395 -0.2497 0.3359 0.066 Uiso 1 1 calc R . . C5H C 0.9341(10) -0.1831(10) 0.33563(19) 0.046(4) Uani 1 1 d . . . H5H H 0.9138 -0.2139 0.3460 0.055 Uiso 1 1 calc R . . C6H C 0.8902(10) -0.1181(11) 0.32642(17) 0.046(4) Uani 1 1 d . . . H6H H 0.8403 -0.1010 0.3310 0.055 Uiso 1 1 calc R . . C50 C 0.7156(14) 0.8281(14) 0.4037(3) 0.091(7) Uani 1 1 d . . . H50 H 0.7239 0.7784 0.3944 0.109 Uiso 1 1 calc R . . Cl51 Cl 0.6232(6) 0.8727(8) 0.39945(12) 0.173(4) Uani 1 1 d . . . Cl52 Cl 0.7894(6) 0.9111(5) 0.40065(11) 0.145(3) Uani 1 1 d . . . Cl53 Cl 0.7203(5) 0.7737(6) 0.42445(9) 0.136(3) Uani 1 1 d . . . C60 C 0.5180(13) 0.6092(18) 0.3389(3) 0.102(7) Uani 1 1 d DU . . H60 H 0.4903 0.5496 0.3420 0.123 Uiso 1 1 calc R . . Cl61 Cl 0.6129(3) 0.5688(5) 0.33913(6) 0.0991(19) Uani 1 1 d DU . . Cl62 Cl 0.4814(3) 0.6243(5) 0.31686(7) 0.1003(19) Uani 1 1 d DU . . Cl63 Cl 0.4908(6) 0.6699(8) 0.35500(9) 0.178(4) Uani 1 1 d DU . . C70 C 0.369(2) 0.453(2) 0.1639(4) 0.095(13) Uiso 0.50 1 d PD . . H70 H 0.4173 0.4919 0.1656 0.114 Uiso 0.50 1 calc PR . . Cl71 Cl 0.3409(10) 0.4186(11) 0.18506(17) 0.136(5) Uani 0.50 1 d PDU . . Cl72 Cl 0.2965(7) 0.5248(9) 0.15436(16) 0.100(3) Uani 0.50 1 d PDU . . Cl73 Cl 0.3919(12) 0.3661(13) 0.1523(2) 0.164(6) Uani 0.50 1 d PDU . . C41 C -0.083(2) 0.262(2) 0.1207(4) 0.063(9) Uiso 0.50 1 d PD . . H41A H -0.1260 0.2437 0.1125 0.095 Uiso 0.50 1 calc PR . . H41B H -0.1033 0.2767 0.1328 0.095 Uiso 0.50 1 calc PR . . H41C H -0.0446 0.2106 0.1218 0.095 Uiso 0.50 1 calc PR . . C42 C -0.040(3) 0.351(3) 0.1129(6) 0.122(17) Uiso 0.50 1 d PD . . H42A H -0.0098 0.3267 0.1026 0.146 Uiso 0.50 1 calc PR . . H42B H -0.0838 0.3883 0.1073 0.146 Uiso 0.50 1 calc PR . . C43 C 0.013(3) 0.424(2) 0.1219(5) 0.096(13) Uiso 0.50 1 d PD . . H43A H 0.0618 0.3899 0.1259 0.115 Uiso 0.50 1 calc PR . . H43B H -0.0129 0.4439 0.1332 0.115 Uiso 0.50 1 calc PR . . C44 C 0.0406(15) 0.5126(16) 0.1124(3) 0.033(6) Uiso 0.50 1 d PD . . H44A H 0.0692 0.4930 0.1014 0.040 Uiso 0.50 1 calc PR . . H44B H -0.0072 0.5462 0.1081 0.040 Uiso 0.50 1 calc PR . . C45 C 0.092(2) 0.583(2) 0.1225(4) 0.083(11) Uiso 0.50 1 d PD . . H45A H 0.0645 0.6036 0.1336 0.100 Uiso 0.50 1 calc PR . . H45B H 0.1414 0.5514 0.1265 0.100 Uiso 0.50 1 calc PR . . C46 C 0.113(2) 0.668(2) 0.1114(5) 0.083(11) Uiso 0.50 1 d PD . . H46A H 0.1359 0.7158 0.1195 0.125 Uiso 0.50 1 calc PR . . H46B H 0.0651 0.6927 0.1054 0.125 Uiso 0.50 1 calc PR . . H46C H 0.1509 0.6504 0.1022 0.125 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0501(10) 0.0513(10) 0.0352(8) -0.0048(5) 0.0042(5) -0.0022(7) Cl1 0.055(2) 0.051(2) 0.0430(19) -0.0031(15) 0.0057(15) -0.001(2) Cl2 0.059(3) 0.066(3) 0.045(2) 0.0056(17) -0.0019(16) 0.007(2) Cl3 0.082(3) 0.062(3) 0.068(3) -0.0029(19) -0.003(2) 0.001(3) N1X 0.072(12) 0.081(14) 0.077(12) 0.021(9) 0.040(9) -0.004(11) O1X 0.079(10) 0.071(11) 0.069(9) 0.017(7) 0.022(7) 0.006(9) N1A 0.058(9) 0.024(6) 0.038(7) -0.012(5) 0.014(6) -0.010(6) C2A 0.054(12) 0.065(11) 0.038(8) -0.006(7) 0.007(8) -0.005(9) C3A 0.050(11) 0.071(12) 0.038(9) -0.006(7) -0.005(7) 0.000(9) C4A 0.079(12) 0.033(9) 0.031(8) -0.002(6) 0.017(7) -0.017(9) C5A 0.052(10) 0.100(14) 0.020(7) 0.002(7) -0.008(7) -0.001(10) C6A 0.059(11) 0.088(13) 0.031(9) -0.011(8) 0.015(7) -0.033(11) N1B 0.038(7) 0.084(12) 0.027(6) 0.001(6) 0.004(5) 0.023(8) C2B 0.051(11) 0.035(10) 0.051(9) 0.011(7) 0.009(7) 0.006(9) C3B 0.065(11) 0.039(9) 0.034(8) -0.010(7) 0.015(6) -0.014(9) C4B 0.060(10) 0.021(8) 0.033(8) -0.005(6) -0.008(6) 0.001(8) C5B 0.083(13) 0.042(10) 0.028(7) -0.013(7) 0.008(7) -0.009(9) C6B 0.037(9) 0.037(9) 0.061(10) 0.008(7) 0.012(6) 0.015(8) N1 0.047(8) 0.057(9) 0.033(6) -0.003(5) -0.003(5) -0.009(7) N2 0.070(9) 0.058(9) 0.026(6) 0.003(5) -0.003(5) -0.008(8) N3 0.064(9) 0.037(8) 0.044(7) 0.002(5) -0.001(6) -0.002(7) N4 0.067(9) 0.043(8) 0.047(7) -0.011(5) 0.012(6) -0.010(7) N5 0.055(8) 0.031(7) 0.036(6) -0.016(5) 0.005(5) 0.019(6) N6 0.047(8) 0.033(7) 0.031(6) -0.006(5) 0.007(5) -0.008(6) N7 0.049(8) 0.034(7) 0.045(6) 0.001(5) 0.002(5) 0.017(7) N8 0.054(8) 0.036(7) 0.043(6) 0.001(5) 0.002(5) 0.006(6) C1C 0.057(12) 0.032(10) 0.093(13) -0.004(9) 0.004(9) 0.000(9) C2C 0.077(15) 0.049(13) 0.127(17) 0.047(12) 0.012(12) -0.008(12) C3C 0.073(18) 0.057(17) 0.20(3) 0.027(16) 0.035(16) -0.018(14) C4C 0.069(18) 0.033(15) 0.26(4) -0.01(2) 0.025(19) -0.026(14) C5C 0.065(17) 0.049(16) 0.22(3) -0.005(16) 0.074(17) -0.009(14) C6C 0.062(14) 0.053(13) 0.121(16) -0.007(11) 0.024(10) -0.007(12) C1D 0.057(10) 0.022(8) 0.046(9) 0.000(6) -0.009(7) -0.009(8) C2D 0.085(14) 0.047(10) 0.030(8) -0.007(7) -0.005(8) -0.016(10) C3D 0.041(10) 0.087(13) 0.032(8) -0.004(8) 0.018(7) -0.001(10) C4D 0.065(12) 0.073(13) 0.048(10) 0.009(8) -0.004(8) -0.006(11) C5D 0.066(12) 0.074(13) 0.042(9) -0.009(8) 0.007(8) 0.011(11) C6D 0.055(11) 0.063(11) 0.045(8) 0.008(7) 0.007(8) 0.012(10) C1E 0.068(13) 0.049(11) 0.073(12) 0.003(9) 0.024(9) 0.012(10) C2E 0.100(16) 0.062(14) 0.061(12) 0.004(9) 0.018(10) -0.015(12) C3E 0.087(17) 0.079(17) 0.102(16) 0.009(12) 0.018(12) -0.026(14) C4E 0.078(16) 0.056(13) 0.13(2) 0.013(14) 0.034(13) 0.016(12) C5E 0.14(2) 0.062(16) 0.125(19) 0.023(14) 0.063(17) 0.005(16) C6E 0.108(18) 0.063(14) 0.074(12) -0.017(10) 0.015(10) -0.006(13) C1F 0.050(10) 0.065(12) 0.027(7) -0.007(7) 0.003(6) 0.018(9) C2F 0.056(11) 0.047(9) 0.034(7) 0.002(6) 0.005(7) 0.001(9) C3F 0.046(10) 0.064(12) 0.037(8) 0.005(7) 0.012(7) 0.009(10) C4F 0.058(11) 0.049(11) 0.036(8) 0.012(7) 0.000(7) -0.012(10) C5F 0.041(9) 0.039(9) 0.047(8) 0.011(7) 0.023(7) 0.003(9) C6F 0.063(11) 0.027(9) 0.036(7) 0.005(6) 0.012(7) 0.008(8) C1G 0.072(12) 0.021(8) 0.031(7) -0.005(6) -0.005(7) -0.023(8) C2G 0.072(12) 0.047(10) 0.022(7) -0.005(6) 0.006(7) -0.011(9) C3G 0.077(13) 0.049(11) 0.048(9) 0.021(8) -0.001(8) -0.025(11) C4G 0.050(10) 0.035(9) 0.051(8) -0.003(6) 0.008(8) -0.015(9) C5G 0.069(13) 0.043(10) 0.043(8) 0.007(7) 0.024(7) 0.001(10) C6G 0.043(10) 0.042(9) 0.038(8) -0.011(7) 0.010(6) -0.004(8) C1H 0.058(11) 0.036(9) 0.034(8) 0.004(6) -0.004(7) 0.019(8) C2H 0.077(14) 0.064(12) 0.041(9) 0.007(8) 0.028(8) 0.024(11) C3H 0.073(13) 0.052(11) 0.058(10) 0.014(8) 0.008(8) -0.012(11) C4H 0.084(14) 0.040(10) 0.040(8) 0.007(7) -0.015(8) 0.019(10) C5H 0.056(11) 0.035(9) 0.048(8) 0.002(7) 0.012(7) -0.004(9) C6H 0.055(10) 0.048(10) 0.036(8) 0.009(7) -0.001(7) -0.004(9) C50 0.097(18) 0.051(12) 0.125(17) -0.018(11) 0.034(12) 0.007(13) Cl51 0.136(7) 0.241(11) 0.143(6) 0.048(7) 0.015(5) 0.036(7) Cl52 0.180(9) 0.106(5) 0.150(6) -0.039(4) 0.049(5) -0.022(5) Cl53 0.129(6) 0.177(8) 0.100(4) 0.016(4) -0.008(4) 0.004(5) C60 0.096(11) 0.113(11) 0.099(10) -0.013(8) 0.011(8) 0.007(9) Cl61 0.081(4) 0.153(5) 0.064(3) -0.015(3) -0.003(2) 0.029(3) Cl62 0.081(4) 0.143(5) 0.077(3) 0.006(3) -0.010(2) 0.006(3) Cl63 0.194(7) 0.246(8) 0.092(4) -0.007(4) -0.001(4) 0.139(6) Cl71 0.144(9) 0.148(9) 0.115(7) 0.044(6) -0.028(6) -0.052(7) Cl72 0.080(6) 0.103(7) 0.117(6) 0.022(5) 0.002(5) 0.018(6) Cl73 0.176(10) 0.152(10) 0.163(9) -0.040(8) -0.010(8) 0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1X 1.760(15) . ? Ru N1A 2.120(12) . ? Ru N1B 2.133(13) . ? Ru Cl2 2.356(4) . ? Ru Cl3 2.358(5) . ? Ru Cl1 2.374(4) . ? N1X O1X 1.016(13) . ? N1A C2A 1.34(2) . ? N1A C6A 1.344(18) . ? C2A C3A 1.36(2) . ? C3A C4A 1.41(2) . ? C4A C5A 1.41(2) . ? C4A C20 1.50(2) . ? C5A C6A 1.37(2) . ? N1B C2B 1.327(19) . ? N1B C6B 1.411(18) . ? C2B C3B 1.41(2) . ? C3B C4B 1.392(18) . ? C4B C5B 1.36(2) . ? C4B C40 1.50(2) . ? C5B C6B 1.43(2) . ? N1 C1 1.378(19) . ? N1 C4 1.406(19) . ? N2 C9 1.404(19) . ? N2 C6 1.419(19) . ? N3 C14 1.35(2) . ? N3 C11 1.410(19) . ? N4 C16 1.37(2) . ? N4 C19 1.388(19) . ? C1 C20 1.41(2) . ? C1 C2 1.44(2) . ? C2 C3 1.35(2) . ? C3 C4 1.42(2) . ? C4 C5 1.37(2) . ? C5 C6 1.40(2) . ? C5 C1C 1.50(2) . ? C6 C7 1.42(2) . ? C7 C8 1.35(2) . ? C8 C9 1.45(2) . ? C9 C10 1.37(2) . ? C10 C11 1.43(2) . ? C10 C1D 1.50(2) . ? C11 C12 1.42(2) . ? C12 C13 1.33(2) . ? C13 C14 1.40(2) . ? C14 C15 1.45(2) . ? C15 C16 1.34(2) . ? C15 C1E 1.54(2) . ? C16 C17 1.43(2) . ? C17 C18 1.29(2) . ? C18 C19 1.40(2) . ? C19 C20 1.39(2) . ? N5 C21 1.374(18) . ? N5 C24 1.396(18) . ? N6 C26 1.364(18) . ? N6 C29 1.391(17) . ? N7 C31 1.361(18) . ? N7 C34 1.377(19) . ? N8 C39 1.367(18) . ? N8 C36 1.397(19) . ? C21 C22 1.40(2) . ? C21 C40 1.42(2) . ? C22 C23 1.39(2) . ? C23 C24 1.41(2) . ? C24 C25 1.393(18) . ? C25 C26 1.42(2) . ? C25 C1F 1.47(2) . ? C26 C27 1.461(18) . ? C27 C28 1.318(19) . ? C28 C29 1.49(2) . ? C29 C30 1.38(2) . ? C30 C31 1.39(2) . ? C30 C1G 1.52(2) . ? C31 C32 1.43(2) . ? C32 C33 1.349(19) . ? C33 C34 1.40(2) . ? C34 C35 1.41(2) . ? C35 C36 1.41(2) . ? C35 C1H 1.50(2) . ? C36 C37 1.45(2) . ? C37 C38 1.36(2) . ? C38 C39 1.43(2) . ? C39 C40 1.39(2) . ? C1C C2C 1.39(3) . ? C1C C6C 1.39(3) . ? C2C C3C 1.44(3) . ? C3C C4C 1.33(4) . ? C4C C5C 1.39(4) . ? C5C C6C 1.40(3) . ? C1D C2D 1.38(2) . ? C1D C6D 1.42(2) . ? C2D C3D 1.34(2) . ? C3D C4D 1.34(2) . ? C4D C5D 1.38(2) . ? C5D C6D 1.38(2) . ? C1E C2E 1.32(3) . ? C1E C6E 1.43(3) . ? C2E C3E 1.49(3) . ? C3E C4E 1.40(3) . ? C4E C5E 1.30(3) . ? C5E C6E 1.39(3) . ? C1F C2F 1.38(2) . ? C1F C6F 1.41(2) . ? C2F C3F 1.41(2) . ? C3F C4F 1.39(2) . ? C4F C5F 1.35(2) . ? C5F C6F 1.37(2) . ? C1G C6G 1.38(2) . ? C1G C2G 1.39(2) . ? C2G C3G 1.42(2) . ? C3G C4G 1.34(2) . ? C4G C5G 1.41(2) . ? C5G C6G 1.37(2) . ? C1H C6H 1.38(2) . ? C1H C2H 1.40(2) . ? C2H C3H 1.38(2) . ? C3H C4H 1.43(2) . ? C4H C5H 1.38(2) . ? C5H C6H 1.36(2) . ? C50 Cl53 1.71(2) . ? C50 Cl51 1.72(2) . ? C50 Cl52 1.74(2) . ? C60 Cl63 1.54(2) . ? C60 Cl61 1.71(2) . ? C60 Cl62 1.73(2) . ? C70 Cl73 1.56(3) . ? C70 Cl71 1.70(3) . ? C70 Cl72 1.73(3) . ? C41 C42 1.57(2) . ? C42 C43 1.52(2) . ? C43 C44 1.52(2) . ? C44 C45 1.51(2) . ? C45 C46 1.51(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 N1X Ru N1A 90.0(6) . . ? N1X Ru N1B 178.8(6) . . ? N1A Ru N1B 89.0(4) . . ? N1X Ru Cl2 93.4(6) . . ? N1A Ru Cl2 88.2(3) . . ? N1B Ru Cl2 85.9(4) . . ? N1X Ru Cl3 91.2(5) . . ? N1A Ru Cl3 178.4(3) . . ? N1B Ru Cl3 89.7(3) . . ? Cl2 Ru Cl3 90.65(15) . . ? N1X Ru Cl1 92.5(6) . . ? N1A Ru Cl1 89.3(3) . . ? N1B Ru Cl1 88.1(4) . . ? Cl2 Ru Cl1 173.60(15) . . ? Cl3 Ru Cl1 91.63(15) . . ? O1X N1X Ru 167.7(19) . . ? C2A N1A C6A 120.0(12) . . ? C2A N1A Ru 121.4(9) . . ? C6A N1A Ru 118.2(10) . . ? N1A C2A C3A 120.9(13) . . ? C2A C3A C4A 121.2(15) . . ? C5A C4A C3A 115.9(13) . . ? C5A C4A C20 121.8(12) . . ? C3A C4A C20 122.3(14) . . ? C6A C5A C4A 119.8(12) . . ? N1A C6A C5A 121.9(15) . . ? C2B N1B C6B 119.5(13) . . ? C2B N1B Ru 123.4(9) . . ? C6B N1B Ru 116.6(12) . . ? N1B C2B C3B 122.8(13) . . ? C4B C3B C2B 119.6(14) . . ? C5B C4B C3B 117.4(12) . . ? C5B C4B C40 119.9(12) . . ? C3B C4B C40 122.5(13) . . ? C4B C5B C6B 123.4(12) . . ? N1B C6B C5B 116.9(14) . . ? C1 N1 C4 109.5(12) . . ? C9 N2 C6 104.7(12) . . ? C14 N3 C11 107.8(12) . . ? C16 N4 C19 106.7(13) . . ? N1 C1 C20 124.7(13) . . ? N1 C1 C2 106.4(13) . . ? C20 C1 C2 128.9(14) . . ? C3 C2 C1 108.9(15) . . ? C2 C3 C4 108.8(15) . . ? C5 C4 N1 126.6(14) . . ? C5 C4 C3 127.0(15) . . ? N1 C4 C3 106.4(13) . . ? C4 C5 C6 126.3(15) . . ? C4 C5 C1C 118.4(14) . . ? C6 C5 C1C 115.0(14) . . ? C5 C6 C7 125.5(15) . . ? C5 C6 N2 125.9(14) . . ? C7 C6 N2 108.4(14) . . ? C8 C7 C6 111.0(15) . . ? C7 C8 C9 105.0(14) . . ? C10 C9 N2 124.2(14) . . ? C10 C9 C8 124.9(14) . . ? N2 C9 C8 110.9(13) . . ? C9 C10 C11 127.6(14) . . ? C9 C10 C1D 118.7(13) . . ? C11 C10 C1D 113.7(13) . . ? N3 C11 C12 105.2(13) . . ? N3 C11 C10 123.0(13) . . ? C12 C11 C10 131.5(14) . . ? C13 C12 C11 110.0(16) . . ? C12 C13 C14 107.1(16) . . ? N3 C14 C13 109.9(14) . . ? N3 C14 C15 124.1(15) . . ? C13 C14 C15 126.0(16) . . ? C16 C15 C14 128.3(17) . . ? C16 C15 C1E 118.1(15) . . ? C14 C15 C1E 113.4(16) . . ? C15 C16 N4 126.1(15) . . ? C15 C16 C17 127.4(16) . . ? N4 C16 C17 106.4(14) . . ? C18 C17 C16 110.3(16) . . ? C17 C18 C19 107.8(16) . . ? N4 C19 C20 123.5(15) . . ? N4 C19 C18 108.7(14) . . ? C20 C19 C18 127.8(15) . . ? C19 C20 C1 128.1(14) . . ? C19 C20 C4A 115.0(14) . . ? C1 C20 C4A 116.8(13) . . ? C21 N5 C24 109.1(11) . . ? C26 N6 C29 107.8(10) . . ? C31 N7 C34 110.1(12) . . ? C39 N8 C36 105.5(11) . . ? N5 C21 C22 107.3(12) . . ? N5 C21 C40 126.1(14) . . ? C22 C21 C40 126.4(13) . . ? C23 C22 C21 108.9(13) . . ? C22 C23 C24 107.0(13) . . ? C25 C24 N5 125.5(11) . . ? C25 C24 C23 127.0(12) . . ? N5 C24 C23 107.5(11) . . ? C24 C25 C26 124.1(12) . . ? C24 C25 C1F 118.6(12) . . ? C26 C25 C1F 117.2(11) . . ? N6 C26 C25 127.1(11) . . ? N6 C26 C27 108.8(11) . . ? C25 C26 C27 124.1(12) . . ? C28 C27 C26 108.6(12) . . ? C27 C28 C29 107.1(12) . . ? C30 C29 N6 125.9(12) . . ? C30 C29 C28 126.2(12) . . ? N6 C29 C28 107.4(13) . . ? C29 C30 C31 126.1(13) . . ? C29 C30 C1G 118.2(13) . . ? C31 C30 C1G 115.5(14) . . ? N7 C31 C30 125.7(14) . . ? N7 C31 C32 106.7(11) . . ? C30 C31 C32 127.6(13) . . ? C33 C32 C31 107.1(12) . . ? C32 C33 C34 109.6(13) . . ? N7 C34 C33 106.3(12) . . ? N7 C34 C35 126.7(14) . . ? C33 C34 C35 127.0(13) . . ? C36 C35 C34 125.1(13) . . ? C36 C35 C1H 118.2(12) . . ? C34 C35 C1H 116.7(12) . . ? N8 C36 C35 126.1(12) . . ? N8 C36 C37 109.6(12) . . ? C35 C36 C37 124.3(13) . . ? C38 C37 C36 106.5(13) . . ? C37 C38 C39 107.3(14) . . ? N8 C39 C40 125.3(13) . . ? N8 C39 C38 111.0(14) . . ? C40 C39 C38 123.6(14) . . ? C39 C40 C21 124.8(14) . . ? C39 C40 C4B 120.1(13) . . ? C21 C40 C4B 115.0(14) . . ? C2C C1C C6C 121(2) . . ? C2C C1C C5 120.0(17) . . ? C6C C1C C5 119.0(17) . . ? C1C C2C C3C 117(2) . . ? C4C C3C C2C 123(3) . . ? C3C C4C C5C 117(3) . . ? C4C C5C C6C 123(3) . . ? C1C C6C C5C 118(2) . . ? C2D C1D C6D 115.3(14) . . ? C2D C1D C10 124.0(13) . . ? C6D C1D C10 120.5(12) . . ? C3D C2D C1D 124.2(14) . . ? C4D C3D C2D 119.9(14) . . ? C3D C4D C5D 120.2(16) . . ? C6D C5D C4D 120.1(17) . . ? C5D C6D C1D 120.3(14) . . ? C2E C1E C6E 122.0(19) . . ? C2E C1E C15 120.0(16) . . ? C6E C1E C15 117.5(17) . . ? C1E C2E C3E 118.7(18) . . ? C4E C3E C2E 116(2) . . ? C5E C4E C3E 123(2) . . ? C4E C5E C6E 122(2) . . ? C5E C6E C1E 118(2) . . ? C2F C1F C6F 118.0(14) . . ? C2F C1F C25 121.1(15) . . ? C6F C1F C25 121.0(14) . . ? C1F C2F C3F 120.4(15) . . ? C4F C3F C2F 119.9(15) . . ? C5F C4F C3F 119.5(15) . . ? C4F C5F C6F 121.5(14) . . ? C5F C6F C1F 120.7(15) . . ? C6G C1G C2G 118.8(12) . . ? C6G C1G C30 122.1(14) . . ? C2G C1G C30 119.0(14) . . ? C1G C2G C3G 118.0(15) . . ? C4G C3G C2G 123.2(16) . . ? C3G C4G C5G 117.9(14) . . ? C6G C5G C4G 119.6(15) . . ? C5G C6G C1G 122.3(15) . . ? C6H C1H C2H 118.4(13) . . ? C6H C1H C35 120.9(14) . . ? C2H C1H C35 120.7(13) . . ? C3H C2H C1H 121.7(14) . . ? C2H C3H C4H 117.1(17) . . ? C5H C4H C3H 121.3(14) . . ? C6H C5H C4H 119.0(13) . . ? C5H C6H C1H 122.2(15) . . ? Cl53 C50 Cl51 110.9(12) . . ? Cl53 C50 Cl52 113.9(14) . . ? Cl51 C50 Cl52 112.4(13) . . ? Cl63 C60 Cl61 118.6(14) . . ? Cl63 C60 Cl62 122.5(14) . . ? Cl61 C60 Cl62 111.7(11) . . ? Cl73 C70 Cl71 110.4(19) . . ? Cl73 C70 Cl72 116(2) . . ? Cl71 C70 Cl72 109.2(17) . . ? C43 C42 C41 132(3) . . ? C42 C43 C44 124(3) . . ? C45 C44 C43 121(2) . . ? C46 C45 C44 114(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Ru N1X O1X -117(9) . . . . ? N1B Ru N1X O1X -152(29) . . . . ? Cl2 Ru N1X O1X 155(9) . . . . ? Cl3 Ru N1X O1X 64(9) . . . . ? Cl1 Ru N1X O1X -27(9) . . . . ? N1X Ru N1A C2A 136.2(13) . . . . ? N1B Ru N1A C2A -44.5(12) . . . . ? Cl2 Ru N1A C2A -130.5(11) . . . . ? Cl3 Ru N1A C2A -84(13) . . . . ? Cl1 Ru N1A C2A 43.6(11) . . . . ? N1X Ru N1A C6A -50.9(12) . . . . ? N1B Ru N1A C6A 128.5(11) . . . . ? Cl2 Ru N1A C6A 42.5(10) . . . . ? Cl3 Ru N1A C6A 89(13) . . . . ? Cl1 Ru N1A C6A -143.4(10) . . . . ? C6A N1A C2A C3A 5(2) . . . . ? Ru N1A C2A C3A 178.3(12) . . . . ? N1A C2A C3A C4A -5(2) . . . . ? C2A C3A C4A C5A 4(2) . . . . ? C2A C3A C4A C20 -175.8(15) . . . . ? C3A C4A C5A C6A -3(2) . . . . ? C20 C4A C5A C6A 176.5(15) . . . . ? C2A N1A C6A C5A -5(2) . . . . ? Ru N1A C6A C5A -178.0(13) . . . . ? C4A C5A C6A N1A 4(3) . . . . ? N1X Ru N1B C2B -16(35) . . . . ? N1A Ru N1B C2B -51.5(12) . . . . ? Cl2 Ru N1B C2B 36.8(11) . . . . ? Cl3 Ru N1B C2B 127.5(11) . . . . ? Cl1 Ru N1B C2B -140.9(11) . . . . ? N1X Ru N1B C6B 172(100) . . . . ? N1A Ru N1B C6B 136.2(9) . . . . ? Cl2 Ru N1B C6B -135.4(9) . . . . ? Cl3 Ru N1B C6B -44.8(9) . . . . ? Cl1 Ru N1B C6B 46.9(9) . . . . ? C6B N1B C2B C3B 5(2) . . . . ? Ru N1B C2B C3B -167.5(12) . . . . ? N1B C2B C3B C4B 1(2) . . . . ? C2B C3B C4B C5B -5(2) . . . . ? C2B C3B C4B C40 169.3(15) . . . . ? C3B C4B C5B C6B 4(2) . . . . ? C40 C4B C5B C6B -170.4(15) . . . . ? C2B N1B C6B C5B -5.3(19) . . . . ? Ru N1B C6B C5B 167.2(11) . . . . ? C4B C5B C6B N1B 1(2) . . . . ? C4 N1 C1 C20 -178.8(13) . . . . ? C4 N1 C1 C2 -1.2(14) . . . . ? N1 C1 C2 C3 2.4(16) . . . . ? C20 C1 C2 C3 180(100) . . . . ? C1 C2 C3 C4 -2.5(17) . . . . ? C1 N1 C4 C5 -179(100) . . . . ? C1 N1 C4 C3 -0.2(14) . . . . ? C2 C3 C4 C5 -179(100) . . . . ? C2 C3 C4 N1 1.7(16) . . . . ? N1 C4 C5 C6 -3(2) . . . . ? C3 C4 C5 C6 178.6(14) . . . . ? N1 C4 C5 C1C -176.5(13) . . . . ? C3 C4 C5 C1C 5(2) . . . . ? C4 C5 C6 C7 -171.3(14) . . . . ? C1C C5 C6 C7 2(2) . . . . ? C4 C5 C6 N2 3(2) . . . . ? C1C C5 C6 N2 176.5(13) . . . . ? C9 N2 C6 C5 -173.7(14) . . . . ? C9 N2 C6 C7 1.2(14) . . . . ? C5 C6 C7 C8 173.8(14) . . . . ? N2 C6 C7 C8 -1.2(16) . . . . ? C6 C7 C8 C9 0.6(16) . . . . ? C6 N2 C9 C10 177.9(13) . . . . ? C6 N2 C9 C8 -0.9(14) . . . . ? C7 C8 C9 C10 -178.6(13) . . . . ? C7 C8 C9 N2 0.2(15) . . . . ? N2 C9 C10 C11 -2(2) . . . . ? C8 C9 C10 C11 176.5(13) . . . . ? N2 C9 C10 C1D 179.6(12) . . . . ? C8 C9 C10 C1D -2(2) . . . . ? C14 N3 C11 C12 2.0(14) . . . . ? C14 N3 C11 C10 175.9(13) . . . . ? C9 C10 C11 N3 -1(2) . . . . ? C1D C10 C11 N3 177.0(12) . . . . ? C9 C10 C11 C12 170.9(15) . . . . ? C1D C10 C11 C12 -11(2) . . . . ? N3 C11 C12 C13 -1.5(16) . . . . ? C10 C11 C12 C13 -174.8(15) . . . . ? C11 C12 C13 C14 0.5(18) . . . . ? C11 N3 C14 C13 -1.7(16) . . . . ? C11 N3 C14 C15 -179.2(14) . . . . ? C12 C13 C14 N3 0.8(18) . . . . ? C12 C13 C14 C15 178.1(15) . . . . ? N3 C14 C15 C16 -4(3) . . . . ? C13 C14 C15 C16 178.7(16) . . . . ? N3 C14 C15 C1E -178.9(14) . . . . ? C13 C14 C15 C1E 4(2) . . . . ? C14 C15 C16 N4 8(3) . . . . ? C1E C15 C16 N4 -177.8(15) . . . . ? C14 C15 C16 C17 -175.4(16) . . . . ? C1E C15 C16 C17 -1(2) . . . . ? C19 N4 C16 C15 180(100) . . . . ? C19 N4 C16 C17 2.5(15) . . . . ? C15 C16 C17 C18 -178.5(16) . . . . ? N4 C16 C17 C18 -1.1(17) . . . . ? C16 C17 C18 C19 -0.8(18) . . . . ? C16 N4 C19 C20 178.0(14) . . . . ? C16 N4 C19 C18 -3.1(16) . . . . ? C17 C18 C19 N4 2.4(17) . . . . ? C17 C18 C19 C20 -178.7(15) . . . . ? N4 C19 C20 C1 3(2) . . . . ? C18 C19 C20 C1 -176.2(15) . . . . ? N4 C19 C20 C4A -179.2(13) . . . . ? C18 C19 C20 C4A 2(2) . . . . ? N1 C1 C20 C19 -3(2) . . . . ? C2 C1 C20 C19 180.0(15) . . . . ? N1 C1 C20 C4A 178.7(12) . . . . ? C2 C1 C20 C4A 2(2) . . . . ? C5A C4A C20 C19 -67.3(19) . . . . ? C3A C4A C20 C19 112.3(16) . . . . ? C5A C4A C20 C1 111.2(17) . . . . ? C3A C4A C20 C1 -69.3(18) . . . . ? C24 N5 C21 C22 3.7(16) . . . . ? C24 N5 C21 C40 179.6(14) . . . . ? N5 C21 C22 C23 -2.1(17) . . . . ? C40 C21 C22 C23 -178.0(15) . . . . ? C21 C22 C23 C24 -0.3(17) . . . . ? C21 N5 C24 C25 174.0(14) . . . . ? C21 N5 C24 C23 -3.9(16) . . . . ? C22 C23 C24 C25 -175.3(14) . . . . ? C22 C23 C24 N5 2.5(16) . . . . ? N5 C24 C25 C26 4(2) . . . . ? C23 C24 C25 C26 -179.0(14) . . . . ? N5 C24 C25 C1F -176.4(13) . . . . ? C23 C24 C25 C1F 1(2) . . . . ? C29 N6 C26 C25 176.3(14) . . . . ? C29 N6 C26 C27 -3.4(14) . . . . ? C24 C25 C26 N6 11(2) . . . . ? C1F C25 C26 N6 -169.3(13) . . . . ? C24 C25 C26 C27 -169.6(13) . . . . ? C1F C25 C26 C27 10(2) . . . . ? N6 C26 C27 C28 5.2(16) . . . . ? C25 C26 C27 C28 -174.5(14) . . . . ? C26 C27 C28 C29 -4.6(16) . . . . ? C26 N6 C29 C30 -172.3(14) . . . . ? C26 N6 C29 C28 0.6(15) . . . . ? C27 C28 C29 C30 175.6(14) . . . . ? C27 C28 C29 N6 2.7(16) . . . . ? N6 C29 C30 C31 -8(2) . . . . ? C28 C29 C30 C31 -180.0(14) . . . . ? N6 C29 C30 C1G 166.4(13) . . . . ? C28 C29 C30 C1G -5(2) . . . . ? C34 N7 C31 C30 -178.9(14) . . . . ? C34 N7 C31 C32 3.8(16) . . . . ? C29 C30 C31 N7 -6(2) . . . . ? C1G C30 C31 N7 178.7(14) . . . . ? C29 C30 C31 C32 170.2(15) . . . . ? C1G C30 C31 C32 -5(2) . . . . ? N7 C31 C32 C33 -4.7(16) . . . . ? C30 C31 C32 C33 178.1(14) . . . . ? C31 C32 C33 C34 3.8(17) . . . . ? C31 N7 C34 C33 -1.6(16) . . . . ? C31 N7 C34 C35 177.7(14) . . . . ? C32 C33 C34 N7 -1.5(16) . . . . ? C32 C33 C34 C35 179.2(15) . . . . ? N7 C34 C35 C36 4(2) . . . . ? C33 C34 C35 C36 -176.6(15) . . . . ? N7 C34 C35 C1H -177.4(13) . . . . ? C33 C34 C35 C1H 2(2) . . . . ? C39 N8 C36 C35 176.6(15) . . . . ? C39 N8 C36 C37 -2.3(16) . . . . ? C34 C35 C36 N8 7(2) . . . . ? C1H C35 C36 N8 -171.4(14) . . . . ? C34 C35 C36 C37 -174.5(15) . . . . ? C1H C35 C36 C37 7(2) . . . . ? N8 C36 C37 C38 0.1(17) . . . . ? C35 C36 C37 C38 -178.8(14) . . . . ? C36 C37 C38 C39 2.1(17) . . . . ? C36 N8 C39 C40 -179.6(14) . . . . ? C36 N8 C39 C38 3.6(16) . . . . ? C37 C38 C39 N8 -3.7(18) . . . . ? C37 C38 C39 C40 179.5(14) . . . . ? N8 C39 C40 C21 4(2) . . . . ? C38 C39 C40 C21 -179.4(15) . . . . ? N8 C39 C40 C4B -178.0(14) . . . . ? C38 C39 C40 C4B -2(2) . . . . ? N5 C21 C40 C39 -11(3) . . . . ? C22 C21 C40 C39 164.2(15) . . . . ? N5 C21 C40 C4B 171.1(14) . . . . ? C22 C21 C40 C4B -14(2) . . . . ? C5B C4B C40 C39 117.9(17) . . . . ? C3B C4B C40 C39 -57(2) . . . . ? C5B C4B C40 C21 -64(2) . . . . ? C3B C4B C40 C21 121.3(16) . . . . ? C4 C5 C1C C2C 62(2) . . . . ? C6 C5 C1C C2C -112.4(18) . . . . ? C4 C5 C1C C6C -117.3(18) . . . . ? C6 C5 C1C C6C 68(2) . . . . ? C6C C1C C2C C3C -4(3) . . . . ? C5 C1C C2C C3C 176.7(17) . . . . ? C1C C2C C3C C4C 9(3) . . . . ? C2C C3C C4C C5C -11(4) . . . . ? C3C C4C C5C C6C 10(4) . . . . ? C2C C1C C6C C5C 3(3) . . . . ? C5 C1C C6C C5C -178.0(17) . . . . ? C4C C5C C6C C1C -6(3) . . . . ? C9 C10 C1D C2D -58.6(19) . . . . ? C11 C10 C1D C2D 122.9(16) . . . . ? C9 C10 C1D C6D 116.3(15) . . . . ? C11 C10 C1D C6D -62.2(17) . . . . ? C6D C1D C2D C3D 1(2) . . . . ? C10 C1D C2D C3D 176.6(15) . . . . ? C1D C2D C3D C4D -1(3) . . . . ? C2D C3D C4D C5D 2(3) . . . . ? C3D C4D C5D C6D -2(3) . . . . ? C4D C5D C6D C1D 2(3) . . . . ? C2D C1D C6D C5D -2(2) . . . . ? C10 C1D C6D C5D -176.9(15) . . . . ? C16 C15 C1E C2E 105(2) . . . . ? C14 C15 C1E C2E -80(2) . . . . ? C16 C15 C1E C6E -67(2) . . . . ? C14 C15 C1E C6E 107.9(19) . . . . ? C6E C1E C2E C3E -2(3) . . . . ? C15 C1E C2E C3E -173.6(17) . . . . ? C1E C2E C3E C4E 4(3) . . . . ? C2E C3E C4E C5E -4(3) . . . . ? C3E C4E C5E C6E 1(4) . . . . ? C4E C5E C6E C1E 1(4) . . . . ? C2E C1E C6E C5E -1(3) . . . . ? C15 C1E C6E C5E 171(2) . . . . ? C24 C25 C1F C2F -126.5(14) . . . . ? C26 C25 C1F C2F 53.5(18) . . . . ? C24 C25 C1F C6F 53.6(18) . . . . ? C26 C25 C1F C6F -126.4(14) . . . . ? C6F C1F C2F C3F -0.8(18) . . . . ? C25 C1F C2F C3F 179.3(11) . . . . ? C1F C2F C3F C4F 1.3(19) . . . . ? C2F C3F C4F C5F -2.1(19) . . . . ? C3F C4F C5F C6F 2.5(19) . . . . ? C4F C5F C6F C1F -2.0(19) . . . . ? C2F C1F C6F C5F 1.2(18) . . . . ? C25 C1F C6F C5F -178.9(11) . . . . ? C29 C30 C1G C6G 124.6(16) . . . . ? C31 C30 C1G C6G -60.1(18) . . . . ? C29 C30 C1G C2G -52.6(19) . . . . ? C31 C30 C1G C2G 122.6(15) . . . . ? C6G C1G C2G C3G 3(2) . . . . ? C30 C1G C2G C3G -179.3(13) . . . . ? C1G C2G C3G C4G -3(2) . . . . ? C2G C3G C4G C5G 3(2) . . . . ? C3G C4G C5G C6G -3(2) . . . . ? C4G C5G C6G C1G 3(2) . . . . ? C2G C1G C6G C5G -3(2) . . . . ? C30 C1G C6G C5G 179.3(14) . . . . ? C36 C35 C1H C6H 65(2) . . . . ? C34 C35 C1H C6H -113.0(16) . . . . ? C36 C35 C1H C2H -111.7(17) . . . . ? C34 C35 C1H C2H 70(2) . . . . ? C6H C1H C2H C3H 1(2) . . . . ? C35 C1H C2H C3H 178.2(15) . . . . ? C1H C2H C3H C4H 4(3) . . . . ? C2H C3H C4H C5H -5(2) . . . . ? C3H C4H C5H C6H 1(2) . . . . ? C4H C5H C6H C1H 4(2) . . . . ? C2H C1H C6H C5H -5(2) . . . . ? C35 C1H C6H C5H 177.8(13) . . . . ? C41 C42 C43 C44 -172(4) . . . . ? C42 C43 C44 C45 178(4) . . . . ? C43 C44 C45 C46 -179(3) . . . . ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 31.96 _diffrn_measured_fraction_theta_full 0.837 _refine_diff_density_max 1.432 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.210 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 265965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5,10,15,20-(4'pyridyl)-porphyrin)-tetra-(tetrachloro-nitrosyl-ruthenate(III)) tetra(tetrabutylamonium) bis(nitromethane) diethylether solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H26 Cl16 N12 O4 Ru4, 4(C16 H36 N1) 2(C1 H3 N1 O2) 0.5(C4 H10 O1)' _chemical_formula_sum 'C108 H181 Cl16 N18 O8.50 Ru4' _chemical_formula_weight 2839.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.2413 0.3112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.5010 1.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 38.252(6) _cell_length_b 8.936(3) _cell_length_c 40.475(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.49(3) _cell_angle_gamma 90.00 _cell_volume 13453(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5884 _exptl_absorpt_coefficient_mu 2.203 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.0000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'CCD MarResearch' _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 32476 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.78 _reflns_number_total 11985 _reflns_number_gt 11713 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Scala (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.04 (Farrugia, 1999)' _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^)+(0.0646P)^2^+82.8504P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11985 _refine_ls_number_parameters 823 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1522 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.93808(2) 0.31857(11) 0.36868(2) 0.0388(3) Uani 1 1 d D . . Ru2 Ru 0.81683(2) 1.18499(9) 0.629298(17) 0.0300(2) Uani 1 1 d D . . Ru3 Ru 0.56425(2) 0.15378(12) 0.63121(2) 0.0453(3) Uani 1 1 d D . . Ru4 Ru 0.68311(2) -0.66991(9) 0.370569(17) 0.0285(2) Uani 1 1 d D . . Cl10 Cl 0.93612(10) 0.5804(4) 0.36893(9) 0.0648(9) Uani 1 1 d D . . Cl11 Cl 0.88769(8) 0.3193(3) 0.32128(7) 0.0403(7) Uani 1 1 d D . . Cl12 Cl 0.93639(8) 0.0527(4) 0.37039(8) 0.0531(8) Uani 1 1 d D . . Cl13 Cl 0.98479(9) 0.3190(4) 0.41889(8) 0.0536(9) Uani 1 1 d D . . Cl20 Cl 0.79839(7) 1.0576(3) 0.67412(6) 0.0364(6) Uani 1 1 d D . . Cl21 Cl 0.87554(7) 1.0967(3) 0.65123(6) 0.0360(6) Uani 1 1 d D . . Cl22 Cl 0.83590(8) 1.3051(3) 0.58441(6) 0.0392(7) Uani 1 1 d D . . Cl23 Cl 0.82900(11) 1.4085(4) 0.66122(9) 0.0750(11) Uani 1 1 d D . . Cl30 Cl 0.56866(12) -0.1093(5) 0.62529(10) 0.0870(13) Uani 1 1 d D . . Cl31 Cl 0.51611(11) 0.1687(5) 0.58218(10) 0.0734(12) Uani 1 1 d D . . Cl32 Cl 0.56256(8) 0.4167(4) 0.63616(7) 0.0557(8) Uani 1 1 d D . . Cl33 Cl 0.61337(10) 0.1484(4) 0.67824(8) 0.0577(9) Uani 1 1 d D . . Cl40 Cl 0.69934(7) -0.5410(3) 0.32468(6) 0.0366(6) Uani 1 1 d D . . Cl41 Cl 0.62344(7) -0.5944(3) 0.34871(6) 0.0328(6) Uani 1 1 d D . . Cl42 Cl 0.66574(7) -0.7905(3) 0.41632(6) 0.0355(6) Uani 1 1 d D . . Cl43 Cl 0.67188(10) -0.8951(4) 0.33892(7) 0.0603(9) Uani 1 1 d D . . O4 O 0.7582(2) -0.7227(10) 0.39076(19) 0.056(2) Uiso 1 1 d D . . N4 N 0.7292(2) -0.7116(9) 0.38513(19) 0.0309(19) Uiso 1 1 d D . . O2 O 0.7451(2) 1.2618(10) 0.6068(2) 0.057(2) Uiso 1 1 d D . . N2 N 0.7703(2) 1.2420(11) 0.6135(2) 0.043(2) Uiso 1 1 d D . . O1 O 0.9849(3) 0.3062(12) 0.3240(2) 0.080(3) Uiso 1 1 d D . . N1 N 0.9694(3) 0.3179(11) 0.3416(3) 0.052(3) Uiso 1 1 d D . . O3 O 0.5131(6) 0.102(3) 0.6723(5) 0.099(7) Uiso 0.59(3) 1 d PD . . N3 N 0.5315(6) 0.149(3) 0.6579(5) 0.072(8) Uiso 0.59(3) 1 d PD . . Cl34 Cl 0.5261(3) 0.0954(11) 0.6660(2) 0.055(5) Uiso 0.41(3) 1 d PD . . N10 N 0.7901(2) 0.4127(10) 0.49889(18) 0.029(2) Uani 1 1 d . . . H10 H 0.7728 0.3474 0.4987 0.035 Uiso 1 1 calc R . . N20 N 0.7293(2) 0.3926(10) 0.5302(2) 0.033(2) Uani 1 1 d . . . N30 N 0.7080(2) 0.1052(9) 0.49884(19) 0.0279(19) Uani 1 1 d . . . H30 H 0.7252 0.1707 0.4992 0.033 Uiso 1 1 calc R . . N40 N 0.7698(2) 0.1292(10) 0.46723(19) 0.032(2) Uani 1 1 d . . . C1 C 0.8157(3) 0.4039(11) 0.4802(2) 0.030(2) Uiso 1 1 d . . . C2 C 0.8377(3) 0.5333(12) 0.4873(2) 0.038(3) Uiso 1 1 d . . . H2 H 0.8574 0.5565 0.4776 0.045 Uiso 1 1 calc R . . C3 C 0.8257(3) 0.6185(12) 0.5102(2) 0.033(2) Uiso 1 1 d . . . H3 H 0.8353 0.7119 0.5192 0.039 Uiso 1 1 calc R . . C4 C 0.7962(3) 0.5413(12) 0.5180(2) 0.034(3) Uiso 1 1 d . . . C5 C 0.7742(3) 0.5936(11) 0.5390(2) 0.030(2) Uiso 1 1 d . . . C6 C 0.7432(3) 0.5293(10) 0.5436(2) 0.024(2) Uiso 1 1 d . . . C7 C 0.7210(3) 0.5923(13) 0.5639(2) 0.040(3) Uiso 1 1 d . . . H7 H 0.7249 0.6848 0.5758 0.048 Uiso 1 1 calc R . . C8 C 0.6930(3) 0.4956(11) 0.5633(2) 0.035(3) Uiso 1 1 d . . . H8 H 0.6740 0.5086 0.5745 0.042 Uiso 1 1 calc R . . C9 C 0.6982(3) 0.3686(12) 0.5421(2) 0.032(2) Uiso 1 1 d . . . C10 C 0.6771(3) 0.2394(12) 0.5376(2) 0.030(2) Uiso 1 1 d . . . C11 C 0.6821(3) 0.1180(11) 0.5175(2) 0.031(2) Uiso 1 1 d . . . C12 C 0.6599(3) -0.0092(12) 0.5098(3) 0.040(3) Uiso 1 1 d . . . H12 H 0.6399 -0.0322 0.5190 0.048 Uiso 1 1 calc R . . C13 C 0.6723(3) -0.0945(13) 0.4866(2) 0.038(3) Uiso 1 1 d . . . H13 H 0.6621 -0.1857 0.4768 0.045 Uiso 1 1 calc R . . C14 C 0.7031(3) -0.0222(11) 0.4799(2) 0.027(2) Uiso 1 1 d . . . C15 C 0.7236(3) -0.0700(11) 0.4583(2) 0.028(2) Uiso 1 1 d . . . C16 C 0.7549(3) -0.0055(11) 0.4530(2) 0.030(2) Uiso 1 1 d . . . C17 C 0.7785(3) -0.0668(12) 0.4332(2) 0.031(2) Uiso 1 1 d . . . H17 H 0.7756 -0.1606 0.4218 0.037 Uiso 1 1 calc R . . C18 C 0.8049(3) 0.0294(12) 0.4335(2) 0.035(3) Uiso 1 1 d . . . H18 H 0.8237 0.0192 0.4219 0.042 Uiso 1 1 calc R . . C19 C 0.7997(3) 0.1516(11) 0.4546(2) 0.031(2) Uiso 1 1 d . . . C20 C 0.8205(3) 0.2832(11) 0.4593(2) 0.026(2) Uiso 1 1 d . . . N1A N 0.9004(3) 0.3164(9) 0.4002(2) 0.034(2) Uani 1 1 d . . . N1B N 0.8063(2) 0.9862(9) 0.59910(18) 0.031(2) Uani 1 1 d D . . N1C N 0.6013(3) 0.1834(10) 0.5994(2) 0.037(2) Uani 1 1 d . . . N1D N 0.6914(2) -0.4712(9) 0.39935(19) 0.030(2) Uani 1 1 d D . . C2A C 0.8710(3) 0.3983(12) 0.3938(2) 0.035(3) Uiso 1 1 d . . . H2A H 0.8673 0.4647 0.3750 0.042 Uiso 1 1 calc R . . C2B C 0.8165(3) 0.8524(12) 0.6123(3) 0.031(3) Uiso 1 1 d . . . H2B H 0.8309 0.8466 0.6348 0.037 Uiso 1 1 calc R . . C2C C 0.5964(3) 0.2879(14) 0.5743(3) 0.046(3) Uiso 1 1 d . . . H2C H 0.5753 0.3480 0.5704 0.055 Uiso 1 1 calc R . . C2D C 0.6822(3) -0.3384(11) 0.3864(3) 0.031(3) Uiso 1 1 d . . . H2D H 0.6690 -0.3317 0.3635 0.037 Uiso 1 1 calc R . . C3A C 0.8449(3) 0.3944(12) 0.4128(2) 0.035(3) Uiso 1 1 d . . . H3A H 0.8243 0.4571 0.4071 0.042 Uiso 1 1 calc R . . C3B C 0.8067(3) 0.7182(13) 0.5938(2) 0.033(2) Uiso 1 1 d . . . H3B H 0.8130 0.6225 0.6036 0.039 Uiso 1 1 calc R . . C3C C 0.6199(3) 0.3100(11) 0.5548(2) 0.030(2) Uiso 1 1 d . . . H3C H 0.6158 0.3881 0.5385 0.036 Uiso 1 1 calc R . . C3D C 0.6911(3) -0.2038(12) 0.4054(2) 0.031(2) Uiso 1 1 d . . . H3D H 0.6828 -0.1105 0.3953 0.037 Uiso 1 1 calc R . . C4A C 0.8496(3) 0.2981(13) 0.4399(3) 0.039(3) Uiso 1 1 d . . . C4B C 0.7866(3) 0.7353(12) 0.5594(2) 0.028(2) Uiso 1 1 d . . . C4C C 0.6499(3) 0.2202(12) 0.5584(2) 0.029(2) Uiso 1 1 d . . . C4D C 0.7117(3) -0.2069(11) 0.4385(2) 0.026(2) Uiso 1 1 d . . . C5A C 0.8808(3) 0.2148(13) 0.4472(3) 0.043(3) Uiso 1 1 d . . . H5A H 0.8857 0.1508 0.4665 0.051 Uiso 1 1 calc R . . C5B C 0.7785(3) 0.8724(12) 0.5471(2) 0.029(2) Uiso 1 1 d . . . H5B H 0.7657 0.8838 0.5241 0.034 Uiso 1 1 calc R . . C5C C 0.6548(3) 0.1084(13) 0.5838(3) 0.042(3) Uiso 1 1 d . . . H5C H 0.6748 0.0424 0.5868 0.050 Uiso 1 1 calc R . . C5D C 0.7208(3) -0.3484(13) 0.4525(3) 0.040(3) Uiso 1 1 d . . . H5D H 0.7340 -0.3572 0.4754 0.048 Uiso 1 1 calc R . . C6A C 0.9051(3) 0.2238(13) 0.4266(2) 0.035(3) Uiso 1 1 d . . . H6A H 0.9258 0.1616 0.4315 0.042 Uiso 1 1 calc R . . C6B C 0.7882(3) 0.9979(13) 0.5668(3) 0.038(3) Uiso 1 1 d . . . H6B H 0.7819 1.0941 0.5572 0.046 Uiso 1 1 calc R . . C6C C 0.6308(3) 0.0953(12) 0.6040(3) 0.036(3) Uiso 1 1 d . . . H6C H 0.6350 0.0228 0.6216 0.044 Uiso 1 1 calc R . . C6D C 0.7104(3) -0.4782(13) 0.4328(3) 0.038(3) Uiso 1 1 d . . . H6D H 0.7167 -0.5734 0.4429 0.045 Uiso 1 1 calc R . . N11 N 0.6338(3) 0.6862(10) 0.7324(2) 0.035(2) Uiso 1 1 d . . . C31 C 0.6669(3) 0.7688(12) 0.7505(2) 0.029(2) Uiso 1 1 d . . . H31A H 0.6630 0.8036 0.7726 0.035 Uiso 1 1 calc R . . H31B H 0.6871 0.6966 0.7555 0.035 Uiso 1 1 calc R . . C32 C 0.6781(3) 0.8974(13) 0.7332(3) 0.042(3) Uiso 1 1 d . . . H32A H 0.6574 0.9663 0.7259 0.051 Uiso 1 1 calc R . . H32B H 0.6855 0.8628 0.7127 0.051 Uiso 1 1 calc R . . C33 C 0.7094(3) 0.9815(13) 0.7565(3) 0.039(3) Uiso 1 1 d . . . H33A H 0.7015 1.0171 0.7767 0.047 Uiso 1 1 calc R . . H33B H 0.7294 0.9101 0.7644 0.047 Uiso 1 1 calc R . . C34 C 0.7235(4) 1.1133(15) 0.7403(3) 0.059(3) Uiso 1 1 d . . . H34A H 0.7312 1.0800 0.7200 0.089 Uiso 1 1 calc R . . H34B H 0.7441 1.1570 0.7566 0.089 Uiso 1 1 calc R . . H34C H 0.7045 1.1886 0.7339 0.089 Uiso 1 1 calc R . . C35 C 0.6004(3) 0.7878(12) 0.7275(2) 0.032(2) Uiso 1 1 d . . . H35A H 0.6048 0.8796 0.7154 0.038 Uiso 1 1 calc R . . H35B H 0.5798 0.7351 0.7127 0.038 Uiso 1 1 calc R . . C36 C 0.5902(3) 0.8322(13) 0.7593(3) 0.045(3) Uiso 1 1 d . . . H36A H 0.6109 0.8814 0.7746 0.054 Uiso 1 1 calc R . . H36B H 0.5842 0.7414 0.7708 0.054 Uiso 1 1 calc R . . C37 C 0.5587(3) 0.9368(14) 0.7528(3) 0.046(3) Uiso 1 1 d . . . H37A H 0.5381 0.8884 0.7370 0.056 Uiso 1 1 calc R . . H37B H 0.5649 1.0284 0.7417 0.056 Uiso 1 1 calc R . . C38 C 0.5474(3) 0.9802(14) 0.7847(3) 0.053(3) Uiso 1 1 d . . . H38A H 0.5352 0.8956 0.7926 0.079 Uiso 1 1 calc R . . H38B H 0.5310 1.0659 0.7800 0.079 Uiso 1 1 calc R . . H38C H 0.5687 1.0074 0.8023 0.079 Uiso 1 1 calc R . . C39 C 0.6288(3) 0.5525(12) 0.7538(2) 0.036(3) Uiso 1 1 d . . . H39A H 0.6276 0.5903 0.7765 0.043 Uiso 1 1 calc R . . H39B H 0.6506 0.4899 0.7569 0.043 Uiso 1 1 calc R . . C40 C 0.5965(3) 0.4507(12) 0.7415(2) 0.035(3) Uiso 1 1 d . . . H40A H 0.5742 0.5112 0.7360 0.042 Uiso 1 1 calc R . . H40B H 0.5988 0.3980 0.7206 0.042 Uiso 1 1 calc R . . C41 C 0.5943(3) 0.3372(13) 0.7688(3) 0.044(3) Uiso 1 1 d . . . H41A H 0.5913 0.3911 0.7894 0.053 Uiso 1 1 calc R . . H41B H 0.5727 0.2741 0.7608 0.053 Uiso 1 1 calc R . . C42 C 0.6267(3) 0.2381(15) 0.7782(3) 0.055(3) Uiso 1 1 d . . . H42A H 0.6331 0.2024 0.7575 0.083 Uiso 1 1 calc R . . H42B H 0.6213 0.1524 0.7913 0.083 Uiso 1 1 calc R . . H42C H 0.6468 0.2948 0.7920 0.083 Uiso 1 1 calc R . . C43 C 0.6369(3) 0.6343(13) 0.6968(3) 0.036(3) Uiso 1 1 d . . . H43A H 0.6137 0.5886 0.6851 0.043 Uiso 1 1 calc R . . H43B H 0.6405 0.7238 0.6835 0.043 Uiso 1 1 calc R . . C44 C 0.6663(3) 0.5248(13) 0.6957(3) 0.040(3) Uiso 1 1 d . . . H44A H 0.6624 0.4315 0.7075 0.047 Uiso 1 1 calc R . . H44B H 0.6898 0.5674 0.7076 0.047 Uiso 1 1 calc R . . C45 C 0.6669(3) 0.4897(13) 0.6593(3) 0.044(3) Uiso 1 1 d . . . H45A H 0.6731 0.5814 0.6482 0.053 Uiso 1 1 calc R . . H45B H 0.6426 0.4574 0.6469 0.053 Uiso 1 1 calc R . . C46 C 0.6939(4) 0.3675(15) 0.6572(3) 0.055(3) Uiso 1 1 d . . . H46A H 0.7181 0.4020 0.6680 0.083 Uiso 1 1 calc R . . H46B H 0.6926 0.3438 0.6333 0.083 Uiso 1 1 calc R . . H46C H 0.6882 0.2777 0.6689 0.083 Uiso 1 1 calc R . . N12 N 0.5491(2) 0.7391(10) 0.91069(19) 0.042(2) Uiso 1 1 d . . . C47 C 0.5183(3) 0.7017(13) 0.8807(2) 0.044(3) Uiso 1 1 d . . . H47A H 0.5018 0.6316 0.8885 0.053 Uiso 1 1 calc R . . H47B H 0.5047 0.7945 0.8730 0.053 Uiso 1 1 calc R . . C48 C 0.5298(3) 0.6326(15) 0.8508(3) 0.052(3) Uiso 1 1 d . . . H48A H 0.5397 0.5314 0.8571 0.063 Uiso 1 1 calc R . . H48B H 0.5489 0.6944 0.8449 0.063 Uiso 1 1 calc R . . C49 C 0.4977(3) 0.6214(15) 0.8198(3) 0.056(3) Uiso 1 1 d . . . H49A H 0.4781 0.5634 0.8260 0.067 Uiso 1 1 calc R . . H49B H 0.4885 0.7230 0.8130 0.067 Uiso 1 1 calc R . . C50 C 0.5083(4) 0.5475(17) 0.7907(3) 0.068(3) Uiso 1 1 d . . . H50A H 0.5288 0.6009 0.7856 0.102 Uiso 1 1 calc R . . H50B H 0.4881 0.5496 0.7708 0.102 Uiso 1 1 calc R . . H50C H 0.5151 0.4435 0.7967 0.102 Uiso 1 1 calc R . . C51 C 0.5707(3) 0.5984(13) 0.9234(3) 0.047(3) Uiso 1 1 d . . . H51A H 0.5808 0.5599 0.9046 0.057 Uiso 1 1 calc R . . H51B H 0.5913 0.6282 0.9420 0.057 Uiso 1 1 calc R . . C52 C 0.5523(5) 0.475(2) 0.9356(4) 0.106(5) Uiso 1 1 d D . . H52A H 0.5348 0.4302 0.9163 0.128 Uiso 1 1 calc R . . H52B H 0.5387 0.5148 0.9518 0.128 Uiso 1 1 calc R . . C53 C 0.5797(5) 0.349(2) 0.9542(4) 0.100(5) Uiso 1 1 d D . . H53A H 0.5657 0.2602 0.9584 0.120 Uiso 1 1 calc R . . H53B H 0.5950 0.3173 0.9388 0.120 Uiso 1 1 calc R . . C54 C 0.6022(5) 0.396(2) 0.9855(4) 0.111(6) Uiso 1 1 d . . . H54A H 0.6186 0.4739 0.9812 0.166 Uiso 1 1 calc R . . H54B H 0.6161 0.3106 0.9967 0.166 Uiso 1 1 calc R . . H54C H 0.5873 0.4360 1.0001 0.166 Uiso 1 1 calc R . . C55 C 0.5328(3) 0.8102(13) 0.9372(3) 0.048(3) Uiso 1 1 d . . . H55A H 0.5194 0.7320 0.9465 0.058 Uiso 1 1 calc R . . H55B H 0.5151 0.8855 0.9259 0.058 Uiso 1 1 calc R . . C56 C 0.5587(3) 0.8868(15) 0.9672(3) 0.059(3) Uiso 1 1 d . . . H56A H 0.5696 0.9754 0.9589 0.071 Uiso 1 1 calc R . . H56B H 0.5783 0.8167 0.9775 0.071 Uiso 1 1 calc R . . C57 C 0.5387(3) 0.9361(16) 0.9945(3) 0.065(3) Uiso 1 1 d . . . H57A H 0.5168 0.9920 0.9832 0.078 Uiso 1 1 calc R . . H57B H 0.5310 0.8458 1.0050 0.078 Uiso 1 1 calc R . . C58 C 0.5610(3) 1.0323(15) 1.0219(3) 0.059(3) Uiso 1 1 d . . . H58A H 0.5837 0.9814 1.0318 0.089 Uiso 1 1 calc R . . H58B H 0.5478 1.0502 1.0395 0.089 Uiso 1 1 calc R . . H58C H 0.5660 1.1281 1.0121 0.089 Uiso 1 1 calc R . . C59 C 0.5757(3) 0.8496(13) 0.9005(3) 0.047(3) Uiso 1 1 d . . . H59A H 0.5942 0.8759 0.9212 0.057 Uiso 1 1 calc R . . H59B H 0.5881 0.7974 0.8849 0.057 Uiso 1 1 calc R . . C60 C 0.5598(3) 0.9939(13) 0.8835(3) 0.048(3) Uiso 1 1 d . . . H60A H 0.5456 1.0444 0.8978 0.057 Uiso 1 1 calc R . . H60B H 0.5436 0.9715 0.8612 0.057 Uiso 1 1 calc R . . C61 C 0.5905(3) 1.0964(14) 0.8788(3) 0.051(3) Uiso 1 1 d . . . H61A H 0.6066 1.1183 0.9012 0.062 Uiso 1 1 calc R . . H61B H 0.6047 1.0452 0.8647 0.062 Uiso 1 1 calc R . . C62 C 0.5756(4) 1.2384(16) 0.8622(3) 0.067(3) Uiso 1 1 d . . . H62A H 0.5597 1.2164 0.8401 0.100 Uiso 1 1 calc R . . H62B H 0.5954 1.3024 0.8591 0.100 Uiso 1 1 calc R . . H62C H 0.5621 1.2901 0.8766 0.100 Uiso 1 1 calc R . . N13 N 0.8667(2) 0.2002(9) 0.76903(19) 0.0256(19) Uiso 1 1 d . . . C63 C 0.8620(3) 0.1468(13) 0.8024(3) 0.039(3) Uiso 1 1 d . . . H63A H 0.8576 0.2352 0.8157 0.046 Uiso 1 1 calc R . . H63B H 0.8849 0.1015 0.8148 0.046 Uiso 1 1 calc R . . C64 C 0.8326(3) 0.0359(12) 0.8022(3) 0.037(3) Uiso 1 1 d . . . H64A H 0.8365 -0.0539 0.7892 0.044 Uiso 1 1 calc R . . H64B H 0.8092 0.0804 0.7907 0.044 Uiso 1 1 calc R . . C65 C 0.8314(3) -0.0106(12) 0.8387(3) 0.036(3) Uiso 1 1 d . . . H65A H 0.8556 -0.0437 0.8510 0.044 Uiso 1 1 calc R . . H65B H 0.8248 0.0774 0.8508 0.044 Uiso 1 1 calc R . . C66 C 0.8048(3) -0.1352(14) 0.8393(3) 0.049(3) Uiso 1 1 d . . . H66A H 0.7821 -0.1127 0.8231 0.074 Uiso 1 1 calc R . . H66B H 0.8006 -0.1439 0.8622 0.074 Uiso 1 1 calc R . . H66C H 0.8145 -0.2297 0.8330 0.074 Uiso 1 1 calc R . . C67 C 0.8323(3) 0.2825(13) 0.7487(3) 0.035(2) Uiso 1 1 d . . . H67A H 0.8367 0.3160 0.7268 0.042 Uiso 1 1 calc R . . H67B H 0.8123 0.2095 0.7436 0.042 Uiso 1 1 calc R . . C68 C 0.8203(3) 0.4176(12) 0.7664(2) 0.036(2) Uiso 1 1 d . . . H68A H 0.8402 0.4904 0.7727 0.043 Uiso 1 1 calc R . . H68B H 0.8133 0.3854 0.7874 0.043 Uiso 1 1 calc R . . C69 C 0.7880(3) 0.4904(13) 0.7418(3) 0.042(3) Uiso 1 1 d . . . H69A H 0.7955 0.5219 0.7210 0.050 Uiso 1 1 calc R . . H69B H 0.7687 0.4148 0.7350 0.050 Uiso 1 1 calc R . . C70 C 0.7728(4) 0.6260(15) 0.7567(3) 0.056(3) Uiso 1 1 d . . . H70A H 0.7693 0.6006 0.7793 0.084 Uiso 1 1 calc R . . H70B H 0.7497 0.6546 0.7418 0.084 Uiso 1 1 calc R . . H70C H 0.7897 0.7098 0.7587 0.084 Uiso 1 1 calc R . . C71 C 0.8711(3) 0.0713(12) 0.7457(2) 0.034(2) Uiso 1 1 d . . . H71A H 0.8491 0.0088 0.7414 0.041 Uiso 1 1 calc R . . H71B H 0.8735 0.1126 0.7237 0.041 Uiso 1 1 calc R . . C72 C 0.9030(3) -0.0258(12) 0.7599(3) 0.038(3) Uiso 1 1 d . . . H72A H 0.8997 -0.0768 0.7807 0.046 Uiso 1 1 calc R . . H72B H 0.9250 0.0367 0.7662 0.046 Uiso 1 1 calc R . . C73 C 0.9077(3) -0.1450(13) 0.7330(3) 0.045(3) Uiso 1 1 d . . . H73A H 0.9126 -0.0926 0.7130 0.054 Uiso 1 1 calc R . . H73B H 0.9288 -0.2079 0.7428 0.054 Uiso 1 1 calc R . . C74 C 0.8751(3) -0.2460(15) 0.7212(3) 0.054(3) Uiso 1 1 d . . . H74A H 0.8724 -0.3105 0.7400 0.081 Uiso 1 1 calc R . . H74B H 0.8785 -0.3082 0.7022 0.081 Uiso 1 1 calc R . . H74C H 0.8535 -0.1845 0.7137 0.081 Uiso 1 1 calc R . . C75 C 0.8987(3) 0.3048(13) 0.7760(3) 0.043(3) Uiso 1 1 d . . . H75A H 0.9188 0.2552 0.7922 0.052 Uiso 1 1 calc R . . H75B H 0.8923 0.3957 0.7873 0.052 Uiso 1 1 calc R . . C76 C 0.9122(3) 0.3536(14) 0.7446(3) 0.048(3) Uiso 1 1 d . . . H76A H 0.9207 0.2649 0.7340 0.057 Uiso 1 1 calc R . . H76B H 0.8922 0.3999 0.7276 0.057 Uiso 1 1 calc R . . C77 C 0.9427(3) 0.4648(13) 0.7549(3) 0.046(3) Uiso 1 1 d . . . H77A H 0.9621 0.4191 0.7725 0.055 Uiso 1 1 calc R . . H77B H 0.9339 0.5541 0.7649 0.055 Uiso 1 1 calc R . . C78 C 0.9580(3) 0.5134(14) 0.7252(3) 0.053(3) Uiso 1 1 d . . . H78A H 0.9784 0.5806 0.7333 0.080 Uiso 1 1 calc R . . H78B H 0.9394 0.5658 0.7084 0.080 Uiso 1 1 calc R . . H78C H 0.9660 0.4252 0.7146 0.080 Uiso 1 1 calc R . . N14 N 0.4609(3) 0.3077(11) 0.1032(2) 0.047(2) Uiso 1 1 d . . . C79 C 0.4249(3) 0.3661(13) 0.0814(3) 0.049(3) Uiso 1 1 d . . . H79A H 0.4191 0.3078 0.0600 0.059 Uiso 1 1 calc R . . H79B H 0.4059 0.3446 0.0937 0.059 Uiso 1 1 calc R . . C80 C 0.4228(3) 0.5263(15) 0.0724(3) 0.063(3) Uiso 1 1 d . . . H80A H 0.4379 0.5469 0.0561 0.076 Uiso 1 1 calc R . . H80B H 0.4321 0.5872 0.0931 0.076 Uiso 1 1 calc R . . C81 C 0.3831(3) 0.5695(15) 0.0564(3) 0.055(3) Uiso 1 1 d . . . H81A H 0.3684 0.5440 0.0727 0.066 Uiso 1 1 calc R . . H81B H 0.3818 0.6792 0.0530 0.066 Uiso 1 1 calc R . . C82 C 0.3675(4) 0.4976(16) 0.0242(3) 0.069(3) Uiso 1 1 d . . . H82A H 0.3809 0.5270 0.0073 0.103 Uiso 1 1 calc R . . H82B H 0.3423 0.5286 0.0163 0.103 Uiso 1 1 calc R . . H82C H 0.3687 0.3887 0.0271 0.103 Uiso 1 1 calc R . . C83 C 0.4911(3) 0.3624(15) 0.0885(3) 0.057(3) Uiso 1 1 d . . . H83A H 0.5141 0.3250 0.1029 0.069 Uiso 1 1 calc R . . H83B H 0.4918 0.4731 0.0897 0.069 Uiso 1 1 calc R . . C84 C 0.4888(4) 0.3156(16) 0.0523(3) 0.070(4) Uiso 1 1 d . B . H84A H 0.4644 0.3373 0.0384 0.083 Uiso 1 1 calc R . . H84B H 0.4928 0.2063 0.0515 0.083 Uiso 1 1 calc R . . C85 C 0.5165(5) 0.397(2) 0.0370(4) 0.096(5) Uiso 1 1 d D . . H85A H 0.5388 0.4065 0.0551 0.115 Uiso 1 1 calc R A 1 H85B H 0.5223 0.3303 0.0194 0.115 Uiso 1 1 calc R A 1 C86 C 0.5086(9) 0.541(3) 0.0219(8) 0.096(10) Uiso 0.50 1 d PD B 1 H86A H 0.5305 0.5851 0.0176 0.144 Uiso 0.50 1 calc PR B 1 H86B H 0.4993 0.6057 0.0375 0.144 Uiso 0.50 1 calc PR B 1 H86C H 0.4905 0.5313 0.0005 0.144 Uiso 0.50 1 calc PR B 1 C86A C 0.5046(9) 0.409(4) 0.0004(6) 0.088(8) Uiso 0.50 1 d PD B 2 H86D H 0.4826 0.4695 -0.0054 0.131 Uiso 0.50 1 calc PR B 2 H86E H 0.4996 0.3088 -0.0095 0.131 Uiso 0.50 1 calc PR B 2 H86F H 0.5234 0.4567 -0.0088 0.131 Uiso 0.50 1 calc PR B 2 C87 C 0.4607(3) 0.1417(14) 0.1041(3) 0.055(3) Uiso 1 1 d . . . H87A H 0.4853 0.1072 0.1146 0.066 Uiso 1 1 calc R . . H87B H 0.4547 0.1049 0.0803 0.066 Uiso 1 1 calc R . . C88 C 0.4351(3) 0.0691(15) 0.1227(3) 0.056(3) Uiso 1 1 d . . . H88A H 0.4125 0.1271 0.1180 0.067 Uiso 1 1 calc R . . H88B H 0.4458 0.0747 0.1474 0.067 Uiso 1 1 calc R . . C89 C 0.4262(4) -0.0952(17) 0.1131(3) 0.072(4) Uiso 1 1 d . . . H89A H 0.4126 -0.0993 0.0891 0.086 Uiso 1 1 calc R . . H89B H 0.4490 -0.1504 0.1147 0.086 Uiso 1 1 calc R . . C90 C 0.4055(4) -0.1709(15) 0.1341(3) 0.061(3) Uiso 1 1 d . . . H90A H 0.4182 -0.1627 0.1580 0.092 Uiso 1 1 calc R . . H90B H 0.4027 -0.2767 0.1276 0.092 Uiso 1 1 calc R . . H90C H 0.3818 -0.1242 0.1307 0.092 Uiso 1 1 calc R . . C91 C 0.4666(3) 0.3738(15) 0.1393(3) 0.056(3) Uiso 1 1 d . . . H91A H 0.4678 0.4840 0.1372 0.067 Uiso 1 1 calc R . . H91B H 0.4448 0.3511 0.1476 0.067 Uiso 1 1 calc R . . C92 C 0.4982(3) 0.3260(13) 0.1660(3) 0.051(3) Uiso 1 1 d . . . H92A H 0.5206 0.3591 0.1598 0.061 Uiso 1 1 calc R . . H92B H 0.4987 0.2155 0.1676 0.061 Uiso 1 1 calc R . . C93 C 0.4966(4) 0.3919(15) 0.1998(3) 0.060(3) Uiso 1 1 d . . . H93A H 0.5170 0.3526 0.2174 0.073 Uiso 1 1 calc R . . H93B H 0.4741 0.3577 0.2057 0.073 Uiso 1 1 calc R . . C94 C 0.4977(3) 0.5650(15) 0.2012(3) 0.063(3) Uiso 1 1 d . . . H94A H 0.5179 0.6009 0.1923 0.095 Uiso 1 1 calc R . . H94B H 0.5007 0.5983 0.2247 0.095 Uiso 1 1 calc R . . H94C H 0.4752 0.6052 0.1873 0.095 Uiso 1 1 calc R . . N5 N 0.7732(3) 0.3312(11) 0.8582(3) 0.047(3) Uani 1 1 d . . . O51 O 0.7964(3) 0.3756(14) 0.8436(3) 0.086(3) Uani 1 1 d . . . O52 O 0.7694(2) 0.3723(9) 0.8851(2) 0.0430(19) Uani 1 1 d . . . C25 C 0.7474(4) 0.2100(14) 0.8408(3) 0.053(3) Uani 1 1 d . . . H25A H 0.7576 0.1594 0.8237 0.080 Uiso 1 1 calc R . . H25B H 0.7243 0.2554 0.8297 0.080 Uiso 1 1 calc R . . H25C H 0.7437 0.1370 0.8577 0.080 Uiso 1 1 calc R . . N6 N 0.2246(3) 0.6634(12) 0.1411(3) 0.053(3) Uani 1 1 d . . . O61 O 0.2290(3) 0.6124(11) 0.1141(2) 0.059(2) Uani 1 1 d . . . O62 O 0.2014(3) 0.6230(14) 0.1539(3) 0.081(3) Uani 1 1 d . . . C26 C 0.2499(4) 0.7792(16) 0.1582(3) 0.057(4) Uani 1 1 d . . . H26A H 0.2742 0.7371 0.1647 0.085 Uiso 1 1 calc R . . H26B H 0.2426 0.8140 0.1785 0.085 Uiso 1 1 calc R . . H26C H 0.2496 0.8636 0.1427 0.085 Uiso 1 1 calc R . . C21 C 0.3825(4) 0.3010(19) 0.4167(4) 0.023(4) Uiso 0.50 1 d PD . . H21A H 0.3615 0.2848 0.4263 0.035 Uiso 0.50 1 calc PR . . H21B H 0.3798 0.2421 0.3959 0.035 Uiso 0.50 1 calc PR . . H21C H 0.3842 0.4074 0.4115 0.035 Uiso 0.50 1 calc PR . . C22 C 0.4142(5) 0.256(3) 0.4407(4) 0.044(5) Uiso 0.50 1 d PD . . H22A H 0.4238 0.1655 0.4317 0.053 Uiso 0.50 1 calc PR . . H22B H 0.4323 0.3358 0.4423 0.053 Uiso 0.50 1 calc PR . . O9 O 0.4108(4) 0.225(2) 0.4714(4) 0.074(5) Uani 0.50 1 d PDU . . C23 C 0.4386(9) 0.175(3) 0.4946(9) 0.117(13) Uiso 0.50 1 d PD . . H23A H 0.4398 0.2357 0.5152 0.140 Uiso 0.50 1 calc PR . . H23B H 0.4603 0.1997 0.4863 0.140 Uiso 0.50 1 calc PR . . C24 C 0.4426(5) 0.022(2) 0.5055(4) 0.034(4) Uiso 0.50 1 d PD . . H24A H 0.4225 -0.0057 0.5154 0.052 Uiso 0.50 1 calc PR . . H24B H 0.4652 0.0106 0.5226 0.052 Uiso 0.50 1 calc PR . . H24C H 0.4428 -0.0424 0.4860 0.052 Uiso 0.50 1 calc PR . . 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 0.0272(6) 0.0547(6) 0.0369(5) 0.0004(4) 0.0125(4) -0.0077(4) Ru2 0.0275(5) 0.0323(5) 0.0296(5) -0.0014(3) 0.0058(4) 0.0013(4) Ru3 0.0340(6) 0.0663(7) 0.0373(5) -0.0015(4) 0.0116(4) -0.0120(5) Ru4 0.0256(5) 0.0317(5) 0.0281(4) -0.0021(3) 0.0063(4) 0.0000(4) Cl10 0.057(2) 0.078(2) 0.0612(18) 0.0011(16) 0.0176(15) -0.0189(18) Cl11 0.0361(17) 0.0506(19) 0.0349(14) 0.0001(10) 0.0100(12) -0.0039(12) Cl12 0.0399(17) 0.064(2) 0.0590(17) -0.0044(15) 0.0197(13) 0.0051(16) Cl13 0.0354(19) 0.079(3) 0.0439(17) 0.0073(13) 0.0052(14) -0.0120(15) Cl20 0.0367(15) 0.0435(17) 0.0299(13) -0.0038(10) 0.0097(11) -0.0051(13) Cl21 0.0302(15) 0.0412(17) 0.0351(13) 0.0012(11) 0.0047(10) -0.0019(13) Cl22 0.0452(18) 0.0376(17) 0.0349(14) 0.0030(11) 0.0094(12) -0.0012(13) Cl23 0.091(3) 0.075(3) 0.063(2) 0.0103(18) 0.0268(19) 0.004(2) Cl30 0.074(3) 0.117(4) 0.074(2) -0.005(2) 0.0242(19) -0.032(3) Cl31 0.055(3) 0.101(3) 0.069(2) -0.0014(18) 0.0231(19) -0.0171(19) Cl32 0.0388(17) 0.074(2) 0.0544(16) -0.0091(15) 0.0110(12) 0.0128(16) Cl33 0.059(2) 0.068(2) 0.0498(18) 0.0021(14) 0.0192(15) -0.0075(17) Cl40 0.0341(15) 0.0461(17) 0.0294(13) -0.0041(10) 0.0068(10) -0.0062(13) Cl41 0.0241(14) 0.0387(16) 0.0339(13) -0.0001(10) 0.0032(10) -0.0003(12) Cl42 0.0335(16) 0.0372(15) 0.0363(15) 0.0035(11) 0.0090(11) 0.0005(13) Cl43 0.067(2) 0.066(2) 0.0470(17) 0.0046(15) 0.0128(14) 0.0053(18) N10 0.021(4) 0.039(6) 0.030(4) -0.005(4) 0.008(3) -0.010(4) N20 0.030(5) 0.042(6) 0.033(5) -0.002(4) 0.017(4) -0.005(4) N30 0.031(5) 0.018(5) 0.033(4) -0.006(3) 0.005(4) -0.008(4) N40 0.023(5) 0.040(5) 0.028(4) -0.007(4) -0.001(3) -0.008(4) N1A 0.036(6) 0.031(6) 0.030(5) -0.006(3) 0.003(4) -0.002(4) N1B 0.027(5) 0.045(6) 0.020(4) 0.002(3) 0.003(4) 0.004(4) N1C 0.029(6) 0.041(6) 0.041(6) -0.003(4) 0.009(4) -0.012(4) N1D 0.013(4) 0.046(6) 0.026(4) 0.003(4) -0.004(3) 0.006(4) N5 0.041(7) 0.046(7) 0.061(8) 0.010(5) 0.025(6) 0.011(5) O51 0.092(9) 0.097(9) 0.085(7) 0.004(6) 0.051(7) -0.003(7) O52 0.041(5) 0.045(5) 0.043(5) 0.003(4) 0.010(4) -0.001(4) C25 0.061(9) 0.047(8) 0.046(7) -0.009(6) 0.002(6) 0.013(7) N6 0.050(8) 0.056(8) 0.056(8) 0.011(5) 0.020(6) 0.006(6) O61 0.066(6) 0.067(6) 0.044(5) 0.009(4) 0.010(4) -0.007(5) O62 0.071(8) 0.096(8) 0.091(8) -0.008(6) 0.047(6) -0.022(7) C26 0.065(10) 0.056(9) 0.049(8) -0.002(6) 0.014(7) 0.020(8) O9 0.050(8) 0.096(9) 0.075(8) 0.045(7) 0.015(6) 0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. The nitrosyl N3-O3 ligand was found disorder in the coordination sphere of Ru3. A satisfactory refinement of occupancies was obtained only with the ligand in trans to the pyridine that provided a NO:Cl (Cl34) ratio of 0.59:0.41, being the remaining 41% of NO spread over the other cis located chlorides. ; 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 1.802(9) . ? Ru1 N1A 2.136(10) . ? Ru1 Cl10 2.341(4) . ? Ru1 Cl13 2.372(3) . ? Ru1 Cl12 2.378(4) . ? Ru1 Cl11 2.381(3) . ? Ru2 N2 1.816(9) . ? Ru2 N1B 2.140(8) . ? Ru2 Cl21 2.350(3) . ? Ru2 Cl23 2.365(4) . ? Ru2 Cl22 2.367(3) . ? Ru2 Cl20 2.384(3) . ? Ru3 N3 1.834(15) . ? Ru3 N1C 2.140(10) . ? Ru3 Cl34 2.313(11) . ? Ru3 Cl33 2.343(4) . ? Ru3 Cl32 2.360(4) . ? Ru3 Cl30 2.373(5) . ? Ru3 Cl31 2.375(4) . ? Ru4 N4 1.764(8) . ? Ru4 N1D 2.107(8) . ? Ru4 Cl41 2.347(3) . ? Ru4 Cl42 2.368(3) . ? Ru4 Cl43 2.371(4) . ? Ru4 Cl40 2.388(3) . ? O4 N4 1.082(9) . ? O2 N2 0.956(9) . ? O1 N1 1.032(10) . ? O3 Cl34 0.61(2) . ? O3 N3 1.093(19) . ? N3 Cl34 0.64(2) . ? N10 C1 1.372(13) . ? N10 C4 1.375(14) . ? N20 C6 1.390(13) . ? N20 C9 1.403(14) . ? N30 C14 1.360(13) . ? N30 C11 1.383(13) . ? N40 C19 1.369(14) . ? N40 C16 1.397(13) . ? C1 C20 1.408(14) . ? C1 C2 1.419(15) . ? C2 C3 1.358(15) . ? C3 C4 1.421(15) . ? C4 C5 1.409(15) . ? C5 C6 1.369(14) . ? C5 C4B 1.525(14) . ? C6 C7 1.428(15) . ? C7 C8 1.372(15) . ? C8 C9 1.463(15) . ? C9 C10 1.395(15) . ? C10 C11 1.394(15) . ? C10 C4C 1.495(14) . ? C11 C12 1.409(15) . ? C12 C13 1.377(15) . ? C13 C14 1.424(15) . ? C14 C15 1.371(14) . ? C15 C16 1.389(14) . ? C15 C4D 1.477(14) . ? C16 C17 1.450(14) . ? C17 C18 1.323(15) . ? C18 C19 1.430(15) . ? C19 C20 1.409(14) . ? C20 C4A 1.510(15) . ? N1A C2A 1.314(14) . ? N1A C6A 1.331(14) . ? N1B C2B 1.331(13) . ? N1B C6B 1.334(13) . ? N1C C6C 1.355(14) . ? N1C C2C 1.360(15) . ? N1D C2D 1.311(13) . ? N1D C6D 1.381(13) . ? C2A C3A 1.397(15) . ? C2B C3B 1.418(16) . ? C2C C3C 1.341(16) . ? C2D C3D 1.426(15) . ? C3A C4A 1.372(16) . ? C3B C4B 1.431(14) . ? C3C C4C 1.381(15) . ? C3D C4D 1.384(14) . ? C4A C5A 1.378(16) . ? C4B C5B 1.332(15) . ? C4C C5C 1.414(16) . ? C4D C5D 1.397(15) . ? C5A C6A 1.390(16) . ? C5B C6B 1.375(15) . ? C5C C6C 1.370(16) . ? C5D C6D 1.411(16) . ? N11 C31 1.500(14) . ? N11 C39 1.514(14) . ? N11 C35 1.544(14) . ? N11 C43 1.546(14) . ? C31 C32 1.460(16) . ? C32 C33 1.537(15) . ? C33 C34 1.506(17) . ? C35 C36 1.483(16) . ? C36 C37 1.499(17) . ? C37 C38 1.503(16) . ? C39 C40 1.522(15) . ? C40 C41 1.519(15) . ? C41 C42 1.498(17) . ? C43 C44 1.500(16) . ? C44 C45 1.511(15) . ? C45 C46 1.519(17) . ? N12 C55 1.503(14) . ? N12 C47 1.519(13) . ? N12 C51 1.527(15) . ? N12 C59 1.542(14) . ? C47 C48 1.511(16) . ? C48 C49 1.540(16) . ? C49 C50 1.486(18) . ? C51 C52 1.46(2) . ? C52 C53 1.606(16) . ? C53 C54 1.42(2) . ? C55 C56 1.537(15) . ? C56 C57 1.544(17) . ? C57 C58 1.501(17) . ? C59 C60 1.519(15) . ? C60 C61 1.534(16) . ? C61 C62 1.485(18) . ? N13 C63 1.484(14) . ? N13 C75 1.513(15) . ? N13 C71 1.523(13) . ? N13 C67 1.563(13) . ? C63 C64 1.497(16) . ? C64 C65 1.544(15) . ? C65 C66 1.512(16) . ? C67 C68 1.528(15) . ? C68 C69 1.539(15) . ? C69 C70 1.528(17) . ? C71 C72 1.499(15) . ? C72 C73 1.564(15) . ? C73 C74 1.521(17) . ? C75 C76 1.545(17) . ? C76 C77 1.515(17) . ? C77 C78 1.517(17) . ? N14 C87 1.484(16) . ? N14 C83 1.500(15) . ? N14 C79 1.543(15) . ? N14 C91 1.543(15) . ? C79 C80 1.474(17) . ? C80 C81 1.555(16) . ? C81 C82 1.450(16) . ? C83 C84 1.510(17) . ? C84 C85 1.53(2) . ? C85 C86 1.43(3) . ? C85 C86A 1.45(2) . ? C87 C88 1.512(16) . ? C88 C89 1.536(19) . ? C89 C90 1.458(19) . ? C91 C92 1.486(16) . ? C92 C93 1.506(17) . ? C93 C94 1.547(19) . ? N5 O52 1.187(13) . ? N5 O51 1.241(15) . ? N5 C25 1.522(17) . ? N6 O62 1.182(14) . ? N6 O61 1.232(14) . ? N6 C26 1.473(18) . ? C21 C22 1.43(2) . ? C22 O9 1.30(2) . ? O9 C23 1.32(2) . ? C23 C24 1.43(3) . ? 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 N1A 179.0(4) . . ? N1 Ru1 Cl10 91.9(3) . . ? N1A Ru1 Cl10 88.8(2) . . ? N1 Ru1 Cl13 92.6(3) . . ? N1A Ru1 Cl13 88.1(3) . . ? Cl10 Ru1 Cl13 90.75(12) . . ? N1 Ru1 Cl12 92.3(3) . . ? N1A Ru1 Cl12 87.0(2) . . ? Cl10 Ru1 Cl12 175.72(13) . . ? Cl13 Ru1 Cl12 89.82(11) . . ? N1 Ru1 Cl11 92.2(3) . . ? N1A Ru1 Cl11 87.1(3) . . ? Cl10 Ru1 Cl11 88.85(12) . . ? Cl13 Ru1 Cl11 175.15(12) . . ? Cl12 Ru1 Cl11 90.22(11) . . ? N2 Ru2 N1B 89.7(4) . . ? N2 Ru2 Cl21 176.1(3) . . ? N1B Ru2 Cl21 88.4(2) . . ? N2 Ru2 Cl23 90.4(3) . . ? N1B Ru2 Cl23 178.2(2) . . ? Cl21 Ru2 Cl23 91.61(13) . . ? N2 Ru2 Cl22 93.1(3) . . ? N1B Ru2 Cl22 89.3(2) . . ? Cl21 Ru2 Cl22 90.21(10) . . ? Cl23 Ru2 Cl22 88.85(11) . . ? N2 Ru2 Cl20 87.8(3) . . ? N1B Ru2 Cl20 89.4(2) . . ? Cl21 Ru2 Cl20 88.79(9) . . ? Cl23 Ru2 Cl20 92.45(11) . . ? Cl22 Ru2 Cl20 178.38(10) . . ? N3 Ru3 N1C 174.2(9) . . ? N3 Ru3 Cl34 11.8(9) . . ? N1C Ru3 Cl34 173.9(4) . . ? N3 Ru3 Cl33 92.8(8) . . ? N1C Ru3 Cl33 88.5(3) . . ? Cl34 Ru3 Cl33 90.1(2) . . ? N3 Ru3 Cl32 86.5(8) . . ? N1C Ru3 Cl32 87.9(3) . . ? Cl34 Ru3 Cl32 98.0(3) . . ? Cl33 Ru3 Cl32 89.10(12) . . ? N3 Ru3 Cl30 96.2(8) . . ? N1C Ru3 Cl30 89.4(3) . . ? Cl34 Ru3 Cl30 84.7(3) . . ? Cl33 Ru3 Cl30 89.95(14) . . ? Cl32 Ru3 Cl30 177.12(14) . . ? N3 Ru3 Cl31 89.5(8) . . ? N1C Ru3 Cl31 89.1(3) . . ? Cl34 Ru3 Cl31 92.6(2) . . ? Cl33 Ru3 Cl31 176.98(13) . . ? Cl32 Ru3 Cl31 89.08(13) . . ? Cl30 Ru3 Cl31 91.76(15) . . ? N4 Ru4 N1D 89.1(3) . . ? N4 Ru4 Cl41 174.6(3) . . ? N1D Ru4 Cl41 88.5(2) . . ? N4 Ru4 Cl42 94.8(3) . . ? N1D Ru4 Cl42 89.1(2) . . ? Cl41 Ru4 Cl42 90.00(10) . . ? N4 Ru4 Cl43 92.4(3) . . ? N1D Ru4 Cl43 177.9(3) . . ? Cl41 Ru4 Cl43 90.16(11) . . ? Cl42 Ru4 Cl43 89.29(11) . . ? N4 Ru4 Cl40 86.6(3) . . ? N1D Ru4 Cl40 89.5(2) . . ? Cl41 Ru4 Cl40 88.54(10) . . ? Cl42 Ru4 Cl40 177.99(11) . . ? Cl43 Ru4 Cl40 92.09(11) . . ? O4 N4 Ru4 169.8(9) . . ? O2 N2 Ru2 172.9(11) . . ? O1 N1 Ru1 171.7(11) . . ? Cl34 O3 N3 30(2) . . ? Cl34 N3 O3 28.1(19) . . ? Cl34 N3 Ru3 132(3) . . ? O3 N3 Ru3 159(3) . . ? O3 Cl34 N3 122(4) . . ? O3 Cl34 Ru3 157(3) . . ? N3 Cl34 Ru3 36(2) . . ? C1 N10 C4 108.1(8) . . ? C6 N20 C9 106.1(8) . . ? C14 N30 C11 110.9(8) . . ? C19 N40 C16 105.7(8) . . ? N10 C1 C20 125.8(9) . . ? N10 C1 C2 107.8(9) . . ? C20 C1 C2 126.2(10) . . ? C3 C2 C1 108.5(10) . . ? C2 C3 C4 107.0(9) . . ? N10 C4 C5 124.8(9) . . ? N10 C4 C3 108.6(9) . . ? C5 C4 C3 126.3(10) . . ? C6 C5 C4 126.9(9) . . ? C6 C5 C4B 116.5(8) . . ? C4 C5 C4B 116.5(9) . . ? C5 C6 N20 125.5(9) . . ? C5 C6 C7 124.2(9) . . ? N20 C6 C7 110.3(9) . . ? C8 C7 C6 107.9(10) . . ? C7 C8 C9 106.7(10) . . ? C10 C9 N20 126.3(10) . . ? C10 C9 C8 124.6(10) . . ? N20 C9 C8 108.9(9) . . ? C11 C10 C9 124.6(10) . . ? C11 C10 C4C 116.5(9) . . ? C9 C10 C4C 118.5(9) . . ? N30 C11 C10 126.5(10) . . ? N30 C11 C12 106.4(9) . . ? C10 C11 C12 126.9(10) . . ? C13 C12 C11 108.2(10) . . ? C12 C13 C14 108.1(10) . . ? N30 C14 C15 126.7(9) . . ? N30 C14 C13 106.4(8) . . ? C15 C14 C13 126.9(9) . . ? C14 C15 C16 127.5(9) . . ? C14 C15 C4D 117.1(9) . . ? C16 C15 C4D 115.4(8) . . ? C15 C16 N40 125.4(9) . . ? C15 C16 C17 126.9(9) . . ? N40 C16 C17 107.7(9) . . ? C18 C17 C16 108.8(9) . . ? C17 C18 C19 106.8(10) . . ? N40 C19 C20 124.6(9) . . ? N40 C19 C18 110.8(9) . . ? C20 C19 C18 124.3(10) . . ? C1 C20 C19 124.8(10) . . ? C1 C20 C4A 117.5(9) . . ? C19 C20 C4A 117.7(9) . . ? C2A N1A C6A 116.9(10) . . ? C2A N1A Ru1 122.9(7) . . ? C6A N1A Ru1 120.1(8) . . ? C2B N1B C6B 120.0(9) . . ? C2B N1B Ru2 121.2(6) . . ? C6B N1B Ru2 118.7(7) . . ? C6C N1C C2C 117.8(10) . . ? C6C N1C Ru3 119.6(7) . . ? C2C N1C Ru3 122.6(8) . . ? C2D N1D C6D 117.6(8) . . ? C2D N1D Ru4 123.4(6) . . ? C6D N1D Ru4 118.7(7) . . ? N1A C2A C3A 124.6(10) . . ? N1B C2B C3B 122.1(9) . . ? C3C C2C N1C 123.1(12) . . ? N1D C2D C3D 122.7(9) . . ? C4A C3A C2A 118.5(11) . . ? C2B C3B C4B 116.1(10) . . ? C2C C3C C4C 120.6(10) . . ? C4D C3D C2D 120.9(10) . . ? C3A C4A C5A 117.2(11) . . ? C3A C4A C20 119.8(10) . . ? C5A C4A C20 123.0(10) . . ? C5B C4B C3B 119.1(9) . . ? C5B C4B C5 123.1(9) . . ? C3B C4B C5 117.8(9) . . ? C3C C4C C5C 116.9(10) . . ? C3C C4C C10 123.2(9) . . ? C5C C4C C10 119.9(10) . . ? C3D C4D C5D 116.3(9) . . ? C3D C4D C15 122.8(9) . . ? C5D C4D C15 120.8(8) . . ? C4A C5A C6A 120.4(11) . . ? C4B C5B C6B 121.7(9) . . ? C6C C5C C4C 120.0(11) . . ? C4D C5D C6D 120.2(10) . . ? N1A C6A C5A 122.3(11) . . ? N1B C6B C5B 120.8(10) . . ? N1C C6C C5C 121.5(10) . . ? N1D C6D C5D 122.1(10) . . ? C31 N11 C39 108.3(8) . . ? C31 N11 C35 110.7(8) . . ? C39 N11 C35 109.0(9) . . ? C31 N11 C43 111.4(9) . . ? C39 N11 C43 110.2(8) . . ? C35 N11 C43 107.3(8) . . ? C32 C31 N11 117.4(8) . . ? C31 C32 C33 111.4(9) . . ? C34 C33 C32 115.1(9) . . ? C36 C35 N11 115.0(9) . . ? C35 C36 C37 112.3(9) . . ? C36 C37 C38 113.0(9) . . ? N11 C39 C40 119.1(8) . . ? C41 C40 C39 109.8(9) . . ? C42 C41 C40 113.3(11) . . ? C44 C43 N11 116.3(9) . . ? C43 C44 C45 110.2(9) . . ? C44 C45 C46 111.6(10) . . ? C55 N12 C47 106.8(8) . . ? C55 N12 C51 113.0(8) . . ? C47 N12 C51 110.2(8) . . ? C55 N12 C59 109.3(8) . . ? C47 N12 C59 111.4(8) . . ? C51 N12 C59 106.1(8) . . ? C48 C47 N12 114.4(9) . . ? C47 C48 C49 110.8(10) . . ? C50 C49 C48 111.2(10) . . ? C52 C51 N12 117.9(11) . . ? C51 C52 C53 112.1(14) . . ? C54 C53 C52 113.6(16) . . ? N12 C55 C56 117.0(9) . . ? C55 C56 C57 110.9(10) . . ? C58 C57 C56 113.7(11) . . ? C60 C59 N12 116.4(9) . . ? C59 C60 C61 109.0(9) . . ? C62 C61 C60 110.2(10) . . ? C63 N13 C75 107.0(8) . . ? C63 N13 C71 112.0(8) . . ? C75 N13 C71 112.4(8) . . ? C63 N13 C67 111.3(8) . . ? C75 N13 C67 110.7(8) . . ? C71 N13 C67 103.4(7) . . ? N13 C63 C64 117.3(9) . . ? C63 C64 C65 111.3(9) . . ? C66 C65 C64 112.6(9) . . ? C68 C67 N13 115.7(8) . . ? C67 C68 C69 108.4(8) . . ? C70 C69 C68 113.6(9) . . ? C72 C71 N13 113.5(8) . . ? C71 C72 C73 110.0(9) . . ? C74 C73 C72 113.9(10) . . ? N13 C75 C76 115.6(9) . . ? C77 C76 C75 110.0(9) . . ? C76 C77 C78 112.5(9) . . ? C87 N14 C83 110.2(9) . . ? C87 N14 C79 110.0(9) . . ? C83 N14 C79 109.4(8) . . ? C87 N14 C91 111.1(9) . . ? C83 N14 C91 107.4(9) . . ? C79 N14 C91 108.8(9) . . ? C80 C79 N14 117.3(10) . . ? C79 C80 C81 109.5(10) . . ? C82 C81 C80 115.1(11) . . ? N14 C83 C84 114.8(10) . . ? C83 C84 C85 112.0(12) . . ? C86 C85 C86A 60.8(18) . . ? C86 C85 C84 120(2) . . ? C86A C85 C84 111.5(17) . . ? N14 C87 C88 116.7(10) . . ? C87 C88 C89 114.5(11) . . ? C90 C89 C88 114.5(11) . . ? C92 C91 N14 119.4(10) . . ? C91 C92 C93 110.5(11) . . ? C92 C93 C94 114.6(10) . . ? O52 N5 O51 126.2(12) . . ? O52 N5 C25 116.1(10) . . ? O51 N5 C25 117.7(12) . . ? O62 N6 O61 123.1(12) . . ? O62 N6 C26 119.1(12) . . ? O61 N6 C26 117.8(11) . . ? O9 C22 C21 116.7(18) . . ? C22 O9 C23 120(3) . . ? O9 C23 C24 124(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1D Ru4 N4 O4 -78(5) . . . . ? Cl41 Ru4 N4 O4 -14(7) . . . . ? Cl42 Ru4 N4 O4 -167(5) . . . . ? Cl43 Ru4 N4 O4 104(5) . . . . ? Cl40 Ru4 N4 O4 12(5) . . . . ? N1B Ru2 N2 O2 68(9) . . . . ? Cl21 Ru2 N2 O2 7(12) . . . . ? Cl23 Ru2 N2 O2 -114(9) . . . . ? Cl22 Ru2 N2 O2 157(9) . . . . ? Cl20 Ru2 N2 O2 -22(9) . . . . ? N1A Ru1 N1 O1 0(30) . . . . ? Cl10 Ru1 N1 O1 -132(8) . . . . ? Cl13 Ru1 N1 O1 137(8) . . . . ? Cl12 Ru1 N1 O1 47(8) . . . . ? Cl11 Ru1 N1 O1 -43(8) . . . . ? Cl34 O3 N3 Ru3 23(6) . . . . ? N1C Ru3 N3 Cl34 -180(100) . . . . ? Cl33 Ru3 N3 Cl34 -77(4) . . . . ? Cl32 Ru3 N3 Cl34 -166(4) . . . . ? Cl30 Ru3 N3 Cl34 13(4) . . . . ? Cl31 Ru3 N3 Cl34 105(4) . . . . ? N1C Ru3 N3 O3 166(5) . . . . ? Cl34 Ru3 N3 O3 -14(4) . . . . ? Cl33 Ru3 N3 O3 -91(6) . . . . ? Cl32 Ru3 N3 O3 180(100) . . . . ? Cl30 Ru3 N3 O3 -1(6) . . . . ? Cl31 Ru3 N3 O3 91(6) . . . . ? N3 O3 Cl34 Ru3 -16(5) . . . . ? Ru3 N3 Cl34 O3 -169(3) . . . . ? O3 N3 Cl34 Ru3 169(3) . . . . ? N3 Ru3 Cl34 O3 24(7) . . . . ? N1C Ru3 Cl34 O3 -157(6) . . . . ? Cl33 Ru3 Cl34 O3 127(7) . . . . ? Cl32 Ru3 Cl34 O3 38(7) . . . . ? Cl30 Ru3 Cl34 O3 -143(7) . . . . ? Cl31 Ru3 Cl34 O3 -51(7) . . . . ? N1C Ru3 Cl34 N3 180(100) . . . . ? Cl33 Ru3 Cl34 N3 103(4) . . . . ? Cl32 Ru3 Cl34 N3 14(4) . . . . ? Cl30 Ru3 Cl34 N3 -167(4) . . . . ? Cl31 Ru3 Cl34 N3 -75(4) . . . . ? C4 N10 C1 C20 174.7(9) . . . . ? C4 N10 C1 C2 -1.6(11) . . . . ? N10 C1 C2 C3 0.5(11) . . . . ? C20 C1 C2 C3 -175.8(9) . . . . ? C1 C2 C3 C4 0.8(11) . . . . ? C1 N10 C4 C5 176.1(9) . . . . ? C1 N10 C4 C3 2.1(11) . . . . ? C2 C3 C4 N10 -1.8(12) . . . . ? C2 C3 C4 C5 -175.6(9) . . . . ? N10 C4 C5 C6 -1.5(16) . . . . ? C3 C4 C5 C6 171.4(10) . . . . ? N10 C4 C5 C4B 177.3(9) . . . . ? C3 C4 C5 C4B -9.8(15) . . . . ? C4 C5 C6 N20 5.7(16) . . . . ? C4B C5 C6 N20 -173.0(8) . . . . ? C4 C5 C6 C7 -176.5(9) . . . . ? C4B C5 C6 C7 4.7(14) . . . . ? C9 N20 C6 C5 178.0(9) . . . . ? C9 N20 C6 C7 0.0(10) . . . . ? C5 C6 C7 C8 -178.3(9) . . . . ? N20 C6 C7 C8 -0.2(11) . . . . ? C6 C7 C8 C9 0.4(11) . . . . ? C6 N20 C9 C10 -174.1(9) . . . . ? C6 N20 C9 C8 0.2(10) . . . . ? C7 C8 C9 C10 174.0(9) . . . . ? C7 C8 C9 N20 -0.4(11) . . . . ? N20 C9 C10 C11 -6.3(16) . . . . ? C8 C9 C10 C11 -179.8(10) . . . . ? N20 C9 C10 C4C 166.6(9) . . . . ? C8 C9 C10 C4C -6.9(14) . . . . ? C14 N30 C11 C10 -174.7(9) . . . . ? C14 N30 C11 C12 0.2(11) . . . . ? C9 C10 C11 N30 -0.4(16) . . . . ? C4C C10 C11 N30 -173.5(9) . . . . ? C9 C10 C11 C12 -174.4(10) . . . . ? C4C C10 C11 C12 12.6(15) . . . . ? N30 C11 C12 C13 -0.8(11) . . . . ? C10 C11 C12 C13 174.1(10) . . . . ? C11 C12 C13 C14 1.0(12) . . . . ? C11 N30 C14 C15 179.5(9) . . . . ? C11 N30 C14 C13 0.4(11) . . . . ? C12 C13 C14 N30 -0.9(11) . . . . ? C12 C13 C14 C15 -180.0(9) . . . . ? N30 C14 C15 C16 5.3(17) . . . . ? C13 C14 C15 C16 -175.9(10) . . . . ? N30 C14 C15 C4D -175.7(9) . . . . ? C13 C14 C15 C4D 3.2(15) . . . . ? C14 C15 C16 N40 -5.3(16) . . . . ? C4D C15 C16 N40 175.6(8) . . . . ? C14 C15 C16 C17 172.1(9) . . . . ? C4D C15 C16 C17 -7.0(14) . . . . ? C19 N40 C16 C15 -178.5(9) . . . . ? C19 N40 C16 C17 3.7(10) . . . . ? C15 C16 C17 C18 178.4(10) . . . . ? N40 C16 C17 C18 -3.9(11) . . . . ? C16 C17 C18 C19 2.3(11) . . . . ? C16 N40 C19 C20 172.3(9) . . . . ? C16 N40 C19 C18 -2.4(11) . . . . ? C17 C18 C19 N40 0.0(12) . . . . ? C17 C18 C19 C20 -174.7(9) . . . . ? N10 C1 C20 C19 -0.2(15) . . . . ? C2 C1 C20 C19 175.5(9) . . . . ? N10 C1 C20 C4A 178.0(9) . . . . ? C2 C1 C20 C4A -6.3(14) . . . . ? N40 C19 C20 C1 6.3(15) . . . . ? C18 C19 C20 C1 -179.8(9) . . . . ? N40 C19 C20 C4A -171.9(9) . . . . ? C18 C19 C20 C4A 2.0(14) . . . . ? N1 Ru1 N1A C2A -85(24) . . . . ? Cl10 Ru1 N1A C2A 47.2(8) . . . . ? Cl13 Ru1 N1A C2A 137.9(8) . . . . ? Cl12 Ru1 N1A C2A -132.1(8) . . . . ? Cl11 Ru1 N1A C2A -41.8(8) . . . . ? N1 Ru1 N1A C6A 91(24) . . . . ? Cl10 Ru1 N1A C6A -136.5(8) . . . . ? Cl13 Ru1 N1A C6A -45.7(8) . . . . ? Cl12 Ru1 N1A C6A 44.3(8) . . . . ? Cl11 Ru1 N1A C6A 134.6(8) . . . . ? N2 Ru2 N1B C2B -131.6(9) . . . . ? Cl21 Ru2 N1B C2B 45.0(8) . . . . ? Cl23 Ru2 N1B C2B 137(8) . . . . ? Cl22 Ru2 N1B C2B 135.3(8) . . . . ? Cl20 Ru2 N1B C2B -43.8(8) . . . . ? N2 Ru2 N1B C6B 46.3(8) . . . . ? Cl21 Ru2 N1B C6B -137.1(8) . . . . ? Cl23 Ru2 N1B C6B -45(9) . . . . ? Cl22 Ru2 N1B C6B -46.9(8) . . . . ? Cl20 Ru2 N1B C6B 134.1(8) . . . . ? N3 Ru3 N1C C6C 150(8) . . . . ? Cl34 Ru3 N1C C6C -29(3) . . . . ? Cl33 Ru3 N1C C6C 46.7(7) . . . . ? Cl32 Ru3 N1C C6C 135.9(8) . . . . ? Cl30 Ru3 N1C C6C -43.2(8) . . . . ? Cl31 Ru3 N1C C6C -135.0(8) . . . . ? N3 Ru3 N1C C2C -31(8) . . . . ? Cl34 Ru3 N1C C2C 150(3) . . . . ? Cl33 Ru3 N1C C2C -133.6(9) . . . . ? Cl32 Ru3 N1C C2C -44.4(8) . . . . ? Cl30 Ru3 N1C C2C 136.5(9) . . . . ? Cl31 Ru3 N1C C2C 44.7(9) . . . . ? N4 Ru4 N1D C2D 125.8(9) . . . . ? Cl41 Ru4 N1D C2D -49.4(9) . . . . ? Cl42 Ru4 N1D C2D -139.4(9) . . . . ? Cl43 Ru4 N1D C2D -99(7) . . . . ? Cl40 Ru4 N1D C2D 39.2(9) . . . . ? N4 Ru4 N1D C6D -48.0(8) . . . . ? Cl41 Ru4 N1D C6D 136.8(8) . . . . ? Cl42 Ru4 N1D C6D 46.8(8) . . . . ? Cl43 Ru4 N1D C6D 87(7) . . . . ? Cl40 Ru4 N1D C6D -134.6(8) . . . . ? C6A N1A C2A C3A 0.1(15) . . . . ? Ru1 N1A C2A C3A 176.6(8) . . . . ? C6B N1B C2B C3B -4.4(16) . . . . ? Ru2 N1B C2B C3B 173.4(8) . . . . ? C6C N1C C2C C3C -2.1(16) . . . . ? Ru3 N1C C2C C3C 178.2(8) . . . . ? C6D N1D C2D C3D 0.2(17) . . . . ? Ru4 N1D C2D C3D -173.6(8) . . . . ? N1A C2A C3A C4A -0.6(16) . . . . ? N1B C2B C3B C4B 3.1(16) . . . . ? N1C C2C C3C C4C 3.4(17) . . . . ? N1D C2D C3D C4D 3.0(17) . . . . ? C2A C3A C4A C5A 2.2(16) . . . . ? C2A C3A C4A C20 -175.6(9) . . . . ? C1 C20 C4A C3A -71.7(13) . . . . ? C19 C20 C4A C3A 106.7(12) . . . . ? C1 C20 C4A C5A 110.6(12) . . . . ? C19 C20 C4A C5A -71.1(13) . . . . ? C2B C3B C4B C5B -0.2(15) . . . . ? C2B C3B C4B C5 -177.6(9) . . . . ? C6 C5 C4B C5B -94.5(12) . . . . ? C4 C5 C4B C5B 86.6(12) . . . . ? C6 C5 C4B C3B 82.8(12) . . . . ? C4 C5 C4B C3B -96.1(11) . . . . ? C2C C3C C4C C5C -1.6(15) . . . . ? C2C C3C C4C C10 -179.7(10) . . . . ? C11 C10 C4C C3C -119.6(11) . . . . ? C9 C10 C4C C3C 66.9(13) . . . . ? C11 C10 C4C C5C 62.3(12) . . . . ? C9 C10 C4C C5C -111.2(12) . . . . ? C2D C3D C4D C5D -4.2(15) . . . . ? C2D C3D C4D C15 175.8(10) . . . . ? C14 C15 C4D C3D 96.4(12) . . . . ? C16 C15 C4D C3D -84.4(12) . . . . ? C14 C15 C4D C5D -83.5(12) . . . . ? C16 C15 C4D C5D 95.6(11) . . . . ? C3A C4A C5A C6A -3.4(17) . . . . ? C20 C4A C5A C6A 174.4(10) . . . . ? C3B C4B C5B C6B -1.4(15) . . . . ? C5 C4B C5B C6B 175.8(10) . . . . ? C3C C4C C5C C6C -1.4(15) . . . . ? C10 C4C C5C C6C 176.8(9) . . . . ? C3D C4D C5D C6D 2.6(15) . . . . ? C15 C4D C5D C6D -177.5(10) . . . . ? C2A N1A C6A C5A -1.4(16) . . . . ? Ru1 N1A C6A C5A -178.0(8) . . . . ? C4A C5A C6A N1A 3.1(17) . . . . ? C2B N1B C6B C5B 2.7(16) . . . . ? Ru2 N1B C6B C5B -175.2(8) . . . . ? C4B C5B C6B N1B 0.3(17) . . . . ? C2C N1C C6C C5C -1.1(15) . . . . ? Ru3 N1C C6C C5C 178.6(8) . . . . ? C4C C5C C6C N1C 2.8(16) . . . . ? C2D N1D C6D C5D -1.9(16) . . . . ? Ru4 N1D C6D C5D 172.3(8) . . . . ? C4D C5D C6D N1D 0.5(17) . . . . ? C39 N11 C31 C32 176.4(10) . . . . ? C35 N11 C31 C32 -64.2(12) . . . . ? C43 N11 C31 C32 55.0(12) . . . . ? N11 C31 C32 C33 173.1(9) . . . . ? C31 C32 C33 C34 178.1(10) . . . . ? C31 N11 C35 C36 -66.2(11) . . . . ? C39 N11 C35 C36 52.9(12) . . . . ? C43 N11 C35 C36 172.1(9) . . . . ? N11 C35 C36 C37 177.1(9) . . . . ? C35 C36 C37 C38 178.7(10) . . . . ? C31 N11 C39 C40 178.8(9) . . . . ? C35 N11 C39 C40 58.3(11) . . . . ? C43 N11 C39 C40 -59.1(13) . . . . ? N11 C39 C40 C41 -172.8(9) . . . . ? C39 C40 C41 C42 -60.6(13) . . . . ? C31 N11 C43 C44 62.9(12) . . . . ? C39 N11 C43 C44 -57.3(13) . . . . ? C35 N11 C43 C44 -175.8(9) . . . . ? N11 C43 C44 C45 -177.7(9) . . . . ? C43 C44 C45 C46 -174.3(10) . . . . ? C55 N12 C47 C48 178.3(10) . . . . ? C51 N12 C47 C48 -58.5(12) . . . . ? C59 N12 C47 C48 59.0(12) . . . . ? N12 C47 C48 C49 -171.1(10) . . . . ? C47 C48 C49 C50 -177.5(11) . . . . ? C55 N12 C51 C52 58.6(14) . . . . ? C47 N12 C51 C52 -60.9(13) . . . . ? C59 N12 C51 C52 178.4(11) . . . . ? N12 C51 C52 C53 -169.7(11) . . . . ? C51 C52 C53 C54 68(2) . . . . ? C47 N12 C55 C56 -168.2(10) . . . . ? C51 N12 C55 C56 70.4(13) . . . . ? C59 N12 C55 C56 -47.5(12) . . . . ? N12 C55 C56 C57 -172.7(10) . . . . ? C55 C56 C57 C58 -171.1(11) . . . . ? C55 N12 C59 C60 -63.9(11) . . . . ? C47 N12 C59 C60 54.0(12) . . . . ? C51 N12 C59 C60 173.9(9) . . . . ? N12 C59 C60 C61 173.9(9) . . . . ? C59 C60 C61 C62 179.9(9) . . . . ? C75 N13 C63 C64 -177.6(10) . . . . ? C71 N13 C63 C64 -53.9(13) . . . . ? C67 N13 C63 C64 61.3(12) . . . . ? N13 C63 C64 C65 179.1(9) . . . . ? C63 C64 C65 C66 -173.6(10) . . . . ? C63 N13 C67 C68 58.0(12) . . . . ? C75 N13 C67 C68 -60.9(11) . . . . ? C71 N13 C67 C68 178.5(9) . . . . ? N13 C67 C68 C69 175.9(9) . . . . ? C67 C68 C69 C70 178.9(10) . . . . ? C63 N13 C71 C72 -60.1(12) . . . . ? C75 N13 C71 C72 60.5(11) . . . . ? C67 N13 C71 C72 179.9(9) . . . . ? N13 C71 C72 C73 -174.4(9) . . . . ? C71 C72 C73 C74 -58.5(13) . . . . ? C63 N13 C75 C76 170.5(10) . . . . ? C71 N13 C75 C76 47.1(12) . . . . ? C67 N13 C75 C76 -68.0(12) . . . . ? N13 C75 C76 C77 176.6(9) . . . . ? C75 C76 C77 C78 178.2(10) . . . . ? C87 N14 C79 C80 -168.9(10) . . . . ? C83 N14 C79 C80 -47.7(13) . . . . ? C91 N14 C79 C80 69.2(13) . . . . ? N14 C79 C80 C81 -169.8(9) . . . . ? C79 C80 C81 C82 -64.8(14) . . . . ? C87 N14 C83 C84 62.2(13) . . . . ? C79 N14 C83 C84 -58.8(14) . . . . ? C91 N14 C83 C84 -176.7(11) . . . . ? N14 C83 C84 C85 170.0(11) . . . . ? C83 C84 C85 C86 -85(2) . . . . ? C83 C84 C85 C86A -153.1(18) . . . . ? C83 N14 C87 C88 171.6(9) . . . . ? C79 N14 C87 C88 -67.8(12) . . . . ? C91 N14 C87 C88 52.7(13) . . . . ? N14 C87 C88 C89 160.2(10) . . . . ? C87 C88 C89 C90 172.3(11) . . . . ? C87 N14 C91 C92 54.5(14) . . . . ? C83 N14 C91 C92 -66.1(14) . . . . ? C79 N14 C91 C92 175.7(11) . . . . ? N14 C91 C92 C93 -174.4(11) . . . . ? C91 C92 C93 C94 -62.3(14) . . . . ? C21 C22 O9 C23 176(2) . . . . ? C22 O9 C23 C24 -105(4) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 30.78 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.939 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.095