Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Chi-Ming Che' 'Pui-Ming Chan' 'Ka-Lai Yip' 'Wing-Yiu Yu' 'Nian-Yong Zhu' _publ_contact_author_name 'Prof Chi-Ming Che' _publ_contact_author_address ; Chemistry Department The University of Hong Kong Open Laboratory of Chemical Biology Pokfulam Road 852 2857-1586 HONG KONG ; _publ_contact_author_email WYYU@HKU.HK _publ_section_title ; Nitrido-ruthenium(VI) and Osmium(VI) Complexes of Multianionic Chelating (N,O) Ligands. Reactions with Nucleophiles, Electrophiles and Oxidizing Agents ; data_ic5819 _database_code_CSD 209727 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C66 H54 F6 N4 O5 P Ru2' _chemical_formula_weight 1330.24 _chemical_melting_point ? _chemical_compound_source ? 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.8677(3) _cell_length_b 19.0282(2) _cell_length_c 18.8130(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.100(1) _cell_angle_gamma 90.00 _cell_volume 6113.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7861 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method ? _exptl_crystal_F_000 2700 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.7831 _exptl_absorpt_correction_T_max 0.8945 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41573 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12505 _reflns_number_observed 8828 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+7.3620P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12505 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_obs 0.0465 _refine_ls_wR_factor_all 0.1288 _refine_ls_wR_factor_obs 0.1115 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.019 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.19554(2) 0.90657(2) 0.35444(2) 0.03381(10) Uani 1 d . . Ru2 Ru 0.24531(2) 1.04288(2) 0.50699(2) 0.03089(10) Uani 1 d . . O1 O 0.2362(2) 0.99874(14) 0.40598(14) 0.0370(6) Uani 1 d . . O2 O 0.1744(2) 0.97100(15) 0.2714(2) 0.0445(7) Uani 1 d . . O3 O 0.1453(2) 0.89844(15) 0.4318(2) 0.0414(7) Uani 1 d . . O4 O 0.3294(2) 0.9760(2) 0.54147(15) 0.0404(7) Uani 1 d . . O5 O 0.2513(2) 1.12496(15) 0.4493(2) 0.0461(8) Uani 1 d . . N1 N 0.2760(2) 0.8638(2) 0.3700(2) 0.0478(9) Uani 1 d . . N2 N 0.1601(2) 1.0247(2) 0.5154(2) 0.0475(9) Uani 1 d . . N3 N 0.1272(2) 0.8273(2) 0.2892(2) 0.0391(8) Uani 1 d . . N4 N 0.2852(2) 1.0970(2) 0.6075(2) 0.0346(8) Uani 1 d . . C1 C 0.1484(3) 0.9533(2) 0.1938(2) 0.0392(10) Uani 1 d . . C2 C 0.1689(3) 0.8762(2) 0.1844(3) 0.0446(11) Uani 1 d . . H2A H 0.1588(3) 0.8667(2) 0.1318(3) 0.054 Uiso 1 calc R . H2B H 0.2246(3) 0.8697(2) 0.2079(3) 0.054 Uiso 1 calc R . C3 C 0.1249(3) 0.8230(2) 0.2163(3) 0.0437(10) Uani 1 d . . C4 C 0.0858(3) 0.7678(3) 0.1729(3) 0.0553(13) Uani 1 d . . H4A H 0.0826(3) 0.7662(3) 0.1227(3) 0.066 Uiso 1 calc R . C5 C 0.0518(3) 0.7155(3) 0.2031(3) 0.067(2) Uani 1 d . . H5A H 0.0262(3) 0.6781(3) 0.1741(3) 0.081 Uiso 1 calc R . C6 C 0.0566(3) 0.7196(3) 0.2777(3) 0.0572(13) Uani 1 d . . H6A H 0.0347(3) 0.6842(3) 0.2993(3) 0.069 Uiso 1 calc R . C7 C 0.0936(3) 0.7756(2) 0.3202(3) 0.0444(11) Uani 1 d . . C8 C 0.0988(3) 0.7796(2) 0.4020(3) 0.0482(11) Uani 1 d . . H8A H 0.1512(3) 0.7656(2) 0.4307(3) 0.058 Uiso 1 calc R . H8B H 0.0626(3) 0.7456(2) 0.4118(3) 0.058 Uiso 1 calc R . C9 C 0.0812(2) 0.8518(2) 0.4306(2) 0.0404(10) Uani 1 d . . C10 C 0.1917(3) 1.0036(2) 0.1550(2) 0.0436(11) Uani 1 d . . C11 C 0.1916(4) 1.0751(3) 0.1696(3) 0.067(2) Uani 1 d . . H11A H 0.1659(4) 1.0915(3) 0.2028(3) 0.080 Uiso 1 calc R . C12 C 0.2291(4) 1.1224(3) 0.1358(4) 0.078(2) Uani 1 d . . H12A H 0.2282(4) 1.1700(3) 0.1467(4) 0.094 Uiso 1 calc R . C13 C 0.2674(4) 1.1003(3) 0.0865(3) 0.071(2) Uani 1 d . . H13A H 0.2918(4) 1.1326(3) 0.0636(3) 0.085 Uiso 1 calc R . C14 C 0.2693(3) 1.0297(3) 0.0716(3) 0.066(2) Uani 1 d . . H14A H 0.2957(3) 1.0139(3) 0.0388(3) 0.079 Uiso 1 calc R . C15 C 0.2313(3) 0.9815(3) 0.1058(3) 0.0565(13) Uani 1 d . . H15A H 0.2328(3) 0.9338(3) 0.0953(3) 0.068 Uiso 1 calc R . C16 C 0.0589(3) 0.9669(2) 0.1622(2) 0.0462(11) Uani 1 d . . C17 C 0.0177(3) 1.0046(3) 0.2007(3) 0.072(2) Uani 1 d . . H17A H 0.0433(3) 1.0211(3) 0.2482(3) 0.087 Uiso 1 calc R . C18 C -0.0621(4) 1.0184(4) 0.1692(4) 0.086(2) Uani 1 d . . H18A H -0.0888(4) 1.0443(4) 0.1959(4) 0.104 Uiso 1 calc R . C19 C -0.1015(4) 0.9944(4) 0.1001(4) 0.086(2) Uani 1 d . . H19A H -0.1547(4) 1.0032(4) 0.0800(4) 0.104 Uiso 1 calc R . C20 C -0.0616(4) 0.9573(4) 0.0609(4) 0.082(2) Uani 1 d . . H20A H -0.0878(4) 0.9410(4) 0.0135(4) 0.099 Uiso 1 calc R . C21 C 0.0187(3) 0.9434(3) 0.0914(3) 0.0648(15) Uani 1 d . . H21A H 0.0452(3) 0.9181(3) 0.0640(3) 0.078 Uiso 1 calc R . C22 C 0.0801(3) 0.8428(2) 0.5117(3) 0.0449(11) Uani 1 d . . C23 C 0.0113(4) 0.8331(4) 0.5290(3) 0.093(2) Uani 1 d . . H23A H -0.0357(4) 0.8332(4) 0.4909(3) 0.112 Uiso 1 calc R . C24 C 0.0100(4) 0.8232(5) 0.6020(4) 0.102(3) Uani 1 d . . H24A H -0.0375(4) 0.8166(5) 0.6120(4) 0.123 Uiso 1 calc R . C25 C 0.0781(4) 0.8231(3) 0.6589(3) 0.069(2) Uani 1 d . . H25A H 0.0773(4) 0.8173(3) 0.7077(3) 0.083 Uiso 1 calc R . C26 C 0.1475(3) 0.8316(3) 0.6433(3) 0.068(2) Uani 1 d . . H26A H 0.1944(3) 0.8311(3) 0.6815(3) 0.081 Uiso 1 calc R . C27 C 0.1481(3) 0.8410(3) 0.5701(3) 0.0571(13) Uani 1 d . . H27A H 0.1959(3) 0.8462(3) 0.5603(3) 0.068 Uiso 1 calc R . C28 C 0.0044(3) 0.8852(3) 0.3838(3) 0.0459(11) Uani 1 d . . C29 C -0.0053(3) 0.9572(3) 0.3899(4) 0.069(2) Uani 1 d . . H29A H 0.0361(3) 0.9836(3) 0.4193(4) 0.083 Uiso 1 calc R . C30 C -0.0742(4) 0.9905(4) 0.3538(4) 0.088(2) Uani 1 d . . H30A H -0.0794(4) 1.0385(4) 0.3604(4) 0.105 Uiso 1 calc R . C31 C -0.1341(4) 0.9541(4) 0.3092(4) 0.085(2) Uani 1 d . . H31A H -0.1796(4) 0.9774(4) 0.2829(4) 0.103 Uiso 1 calc R . C32 C -0.1284(4) 0.8831(5) 0.3023(4) 0.097(3) Uani 1 d . . H32A H -0.1703(4) 0.8580(5) 0.2718(4) 0.116 Uiso 1 calc R . C33 C -0.0583(3) 0.8470(4) 0.3418(4) 0.077(2) Uani 1 d . . H33A H -0.0552(3) 0.7984(4) 0.3390(4) 0.093 Uiso 1 calc R . C34 C 0.3636(2) 0.9511(2) 0.6161(2) 0.0363(9) Uani 1 d . . C35 C 0.3185(3) 0.9819(2) 0.6666(2) 0.0395(10) Uani 1 d . . H35A H 0.2644(3) 0.9668(2) 0.6487(2) 0.047 Uiso 1 calc R . H35B H 0.3404(3) 0.9633(2) 0.7164(2) 0.047 Uiso 1 calc R . C36 C 0.3207(3) 1.0606(2) 0.6702(2) 0.0399(10) Uani 1 d . . C37 C 0.3528(3) 1.0956(3) 0.7365(3) 0.0615(14) Uani 1 d . . H37A H 0.3772(3) 1.0706(3) 0.7795(3) 0.074 Uiso 1 calc R . C38 C 0.3484(4) 1.1684(3) 0.7386(3) 0.076(2) Uani 1 d . . H38A H 0.3723(4) 1.1926(3) 0.7823(3) 0.091 Uiso 1 calc R . C39 C 0.3081(3) 1.2045(3) 0.6748(3) 0.0601(14) Uani 1 d . . H39A H 0.3029(3) 1.2531(3) 0.6760(3) 0.072 Uiso 1 calc R . C40 C 0.2754(3) 1.1679(2) 0.6092(2) 0.0400(10) Uani 1 d . . C41 C 0.2257(3) 1.2044(2) 0.5408(2) 0.0432(10) Uani 1 d . . H41A H 0.2226(3) 1.2540(2) 0.5518(2) 0.052 Uiso 1 calc R . H41B H 0.1731(3) 1.1854(2) 0.5281(2) 0.052 Uiso 1 calc R . C42 C 0.2571(3) 1.1970(2) 0.4727(2) 0.0408(10) Uani 1 d . . C43 C 0.3575(2) 0.8704(2) 0.6136(3) 0.0424(10) Uani 1 d . . C44 C 0.3539(3) 0.8311(3) 0.6743(3) 0.0625(14) Uani 1 d . . H44A H 0.3564(3) 0.8533(3) 0.7190(3) 0.075 Uiso 1 calc R . C45 C 0.3465(4) 0.7586(3) 0.6690(4) 0.088(2) Uani 1 d . . H45A H 0.3428(4) 0.7331(3) 0.7100(4) 0.106 Uiso 1 calc R . C46 C 0.3445(4) 0.7235(4) 0.6050(5) 0.097(2) Uani 1 d . . H46A H 0.3403(4) 0.6748(4) 0.6026(5) 0.116 Uiso 1 calc R . C47 C 0.3488(4) 0.7615(4) 0.5447(5) 0.091(2) Uani 1 d . . H47A H 0.3472(4) 0.7385(4) 0.5007(5) 0.109 Uiso 1 calc R . C48 C 0.3557(3) 0.8355(3) 0.5485(3) 0.0619(14) Uani 1 d . . H48A H 0.3590(3) 0.8608(3) 0.5072(3) 0.074 Uiso 1 calc R . C49 C 0.4509(2) 0.9718(2) 0.6429(2) 0.0388(10) Uani 1 d . . C50 C 0.4939(3) 0.9656(3) 0.7172(3) 0.0529(12) Uani 1 d . . H50A H 0.4688(3) 0.9508(3) 0.7515(3) 0.063 Uiso 1 calc R . C51 C 0.5731(3) 0.9811(3) 0.7418(3) 0.0655(15) Uani 1 d . . H51A H 0.6003(3) 0.9773(3) 0.7920(3) 0.079 Uiso 1 calc R . C52 C 0.6114(3) 1.0020(3) 0.6919(3) 0.069(2) Uani 1 d . . H52A H 0.6647(3) 1.0117(3) 0.7079(3) 0.082 Uiso 1 calc R . C53 C 0.5701(3) 1.0084(4) 0.6181(3) 0.075(2) Uani 1 d . . H53A H 0.5957(3) 1.0226(4) 0.5840(3) 0.090 Uiso 1 calc R . C54 C 0.4903(3) 0.9937(3) 0.5938(3) 0.0644(15) Uani 1 d . . H54A H 0.4630(3) 0.9989(3) 0.5437(3) 0.077 Uiso 1 calc R . C55 C 0.3431(3) 1.2212(2) 0.4965(2) 0.0441(11) Uani 1 d . . C56 C 0.4034(4) 1.1740(3) 0.5007(4) 0.074(2) Uani 1 d . . H56A H 0.3922(4) 1.1280(3) 0.4843(4) 0.089 Uiso 1 calc R . C57 C 0.4821(4) 1.1963(4) 0.5303(5) 0.107(3) Uani 1 d . . H57A H 0.5229(4) 1.1649(4) 0.5337(5) 0.128 Uiso 1 calc R . C58 C 0.4979(4) 1.2643(5) 0.5538(4) 0.098(2) Uani 1 d . . H58A H 0.5496(4) 1.2784(5) 0.5737(4) 0.118 Uiso 1 calc R . C59 C 0.4391(4) 1.3117(4) 0.5485(3) 0.074(2) Uani 1 d . . H59A H 0.4509(4) 1.3579(4) 0.5639(3) 0.089 Uiso 1 calc R . C60 C 0.3617(3) 1.2904(3) 0.5202(3) 0.0548(13) Uani 1 d . . H60A H 0.3217(3) 1.3226(3) 0.5169(3) 0.066 Uiso 1 calc R . C61 C 0.2074(3) 1.2391(2) 0.4050(2) 0.0443(11) Uani 1 d . . C62 C 0.1625(3) 1.2967(3) 0.4106(3) 0.0614(14) Uani 1 d . . H62A H 0.1630(3) 1.3130(3) 0.4574(3) 0.074 Uiso 1 calc R . C63 C 0.1165(4) 1.3308(3) 0.3471(4) 0.076(2) Uani 1 d . . H63A H 0.0863(4) 1.3692(3) 0.3522(4) 0.091 Uiso 1 calc R . C64 C 0.1149(4) 1.3092(3) 0.2786(4) 0.081(2) Uani 1 d . . H64A H 0.0830(4) 1.3315(3) 0.2366(4) 0.098 Uiso 1 calc R . C65 C 0.1614(4) 1.2531(3) 0.2717(3) 0.084(2) Uani 1 d . . H65A H 0.1615(4) 1.2382(3) 0.2247(3) 0.101 Uiso 1 calc R . C66 C 0.2079(4) 1.2190(3) 0.3340(3) 0.067(2) Uani 1 d . . H66A H 0.2398(4) 1.1821(3) 0.3284(3) 0.080 Uiso 1 calc R . P P 0.1622(2) 0.40865(14) 0.61132(12) 0.1173(9) Uani 1 d . . F1 F 0.2282(3) 0.3917(3) 0.5746(3) 0.149(2) Uani 1 d . . F2 F 0.0980(4) 0.4264(4) 0.6495(3) 0.178(3) Uani 1 d . . F3 F 0.1094(5) 0.4313(6) 0.5386(4) 0.252(5) Uani 1 d . . F4 F 0.2168(7) 0.3879(10) 0.6845(5) 0.360(10) Uani 1 d . . F5 F 0.1306(7) 0.3371(4) 0.5938(9) 0.322(8) Uani 1 d . . F6 F 0.1959(6) 0.4807(6) 0.6294(9) 0.351(8) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0328(2) 0.0317(2) 0.0357(2) -0.00305(14) 0.00812(14) -0.00330(14) Ru2 0.0332(2) 0.0285(2) 0.0297(2) -0.00005(13) 0.00720(13) -0.00315(14) O1 0.044(2) 0.033(2) 0.0309(14) -0.0053(12) 0.0072(12) -0.0101(13) O2 0.059(2) 0.038(2) 0.0312(15) -0.0029(12) 0.0058(14) -0.0024(14) O3 0.044(2) 0.037(2) 0.047(2) -0.0078(13) 0.0200(14) -0.0089(13) O4 0.042(2) 0.046(2) 0.0309(15) 0.0007(12) 0.0076(13) 0.0091(13) O5 0.076(2) 0.028(2) 0.037(2) 0.0002(12) 0.021(2) -0.0024(15) N1 0.039(2) 0.045(2) 0.057(2) -0.006(2) 0.010(2) 0.001(2) N2 0.040(2) 0.056(3) 0.045(2) -0.004(2) 0.012(2) -0.006(2) N3 0.035(2) 0.033(2) 0.048(2) -0.009(2) 0.010(2) -0.003(2) N4 0.042(2) 0.035(2) 0.029(2) -0.0009(14) 0.0128(15) -0.003(2) C1 0.043(2) 0.041(2) 0.031(2) -0.008(2) 0.008(2) -0.002(2) C2 0.050(3) 0.040(3) 0.043(2) -0.010(2) 0.014(2) -0.004(2) C3 0.043(3) 0.039(2) 0.048(3) -0.010(2) 0.013(2) -0.002(2) C4 0.062(3) 0.053(3) 0.052(3) -0.020(2) 0.019(2) -0.016(3) C5 0.070(4) 0.055(3) 0.077(4) -0.027(3) 0.023(3) -0.022(3) C6 0.060(3) 0.043(3) 0.074(4) -0.012(3) 0.028(3) -0.014(2) C7 0.042(2) 0.034(2) 0.058(3) -0.007(2) 0.016(2) -0.001(2) C8 0.054(3) 0.035(2) 0.059(3) 0.000(2) 0.020(2) -0.006(2) C9 0.036(2) 0.039(2) 0.049(3) -0.002(2) 0.015(2) -0.007(2) C10 0.039(2) 0.049(3) 0.037(2) 0.000(2) 0.002(2) -0.004(2) C11 0.089(4) 0.055(3) 0.064(3) -0.007(3) 0.033(3) -0.013(3) C12 0.109(5) 0.050(3) 0.083(4) 0.003(3) 0.041(4) -0.013(3) C13 0.073(4) 0.075(4) 0.063(4) 0.010(3) 0.019(3) -0.017(3) C14 0.063(4) 0.089(5) 0.048(3) -0.001(3) 0.021(3) -0.014(3) C15 0.059(3) 0.062(3) 0.047(3) -0.008(2) 0.014(2) -0.007(3) C16 0.049(3) 0.050(3) 0.039(2) 0.002(2) 0.012(2) -0.006(2) C17 0.073(4) 0.092(5) 0.052(3) -0.003(3) 0.020(3) 0.020(3) C18 0.067(4) 0.123(6) 0.076(4) 0.017(4) 0.031(4) 0.033(4) C19 0.052(4) 0.116(6) 0.087(5) 0.031(4) 0.014(3) 0.009(4) C20 0.065(4) 0.091(5) 0.067(4) 0.011(4) -0.018(3) -0.015(4) C21 0.059(3) 0.076(4) 0.053(3) -0.012(3) 0.006(3) -0.004(3) C22 0.046(3) 0.039(3) 0.051(3) 0.000(2) 0.016(2) -0.009(2) C23 0.054(4) 0.176(8) 0.051(3) 0.002(4) 0.018(3) -0.033(4) C24 0.069(4) 0.173(8) 0.076(4) 0.007(5) 0.037(4) -0.038(5) C25 0.082(4) 0.078(4) 0.054(3) 0.016(3) 0.028(3) 0.001(3) C26 0.064(4) 0.083(4) 0.055(3) 0.019(3) 0.015(3) 0.006(3) C27 0.046(3) 0.069(4) 0.058(3) 0.008(3) 0.018(2) 0.000(2) C28 0.039(2) 0.054(3) 0.047(3) -0.004(2) 0.016(2) -0.003(2) C29 0.057(3) 0.056(3) 0.094(4) 0.002(3) 0.022(3) 0.005(3) C30 0.071(4) 0.078(5) 0.113(6) 0.014(4) 0.027(4) 0.019(4) C31 0.064(4) 0.126(6) 0.067(4) -0.001(4) 0.020(3) 0.042(4) C32 0.046(3) 0.150(7) 0.083(5) -0.049(5) 0.000(3) 0.014(4) C33 0.049(3) 0.084(4) 0.094(4) -0.039(4) 0.014(3) 0.007(3) C34 0.038(2) 0.038(2) 0.033(2) 0.003(2) 0.010(2) 0.001(2) C35 0.042(2) 0.043(2) 0.035(2) 0.007(2) 0.013(2) 0.004(2) C36 0.046(3) 0.044(3) 0.033(2) -0.001(2) 0.016(2) 0.001(2) C37 0.086(4) 0.056(3) 0.034(3) 0.002(2) 0.005(2) 0.009(3) C38 0.114(5) 0.059(4) 0.044(3) -0.014(3) 0.007(3) -0.008(3) C39 0.099(4) 0.041(3) 0.040(3) -0.009(2) 0.021(3) -0.004(3) C40 0.051(3) 0.037(2) 0.036(2) -0.004(2) 0.018(2) -0.004(2) C41 0.055(3) 0.034(2) 0.043(2) -0.002(2) 0.018(2) 0.002(2) C42 0.058(3) 0.028(2) 0.036(2) -0.001(2) 0.013(2) -0.001(2) C43 0.033(2) 0.038(2) 0.051(3) 0.001(2) 0.005(2) 0.001(2) C44 0.071(4) 0.045(3) 0.064(3) 0.012(3) 0.008(3) -0.002(3) C45 0.095(5) 0.055(4) 0.104(5) 0.028(4) 0.014(4) -0.004(3) C46 0.089(5) 0.043(4) 0.151(8) 0.004(4) 0.024(5) 0.000(3) C47 0.095(5) 0.062(4) 0.113(6) -0.033(4) 0.027(4) -0.003(4) C48 0.070(4) 0.047(3) 0.069(4) -0.003(3) 0.022(3) 0.004(3) C49 0.038(2) 0.034(2) 0.043(2) 0.002(2) 0.009(2) 0.002(2) C50 0.047(3) 0.062(3) 0.045(3) 0.010(2) 0.008(2) -0.004(2) C51 0.051(3) 0.081(4) 0.054(3) 0.007(3) -0.002(3) -0.008(3) C52 0.043(3) 0.080(4) 0.076(4) -0.002(3) 0.007(3) -0.010(3) C53 0.052(3) 0.113(5) 0.065(4) 0.007(3) 0.023(3) -0.022(3) C54 0.052(3) 0.097(4) 0.043(3) 0.010(3) 0.012(2) -0.012(3) C55 0.054(3) 0.042(3) 0.039(2) 0.007(2) 0.020(2) 0.000(2) C56 0.071(4) 0.050(3) 0.110(5) 0.012(3) 0.041(4) 0.004(3) C57 0.065(5) 0.092(6) 0.170(8) 0.036(6) 0.045(5) 0.015(4) C58 0.056(4) 0.120(7) 0.111(6) 0.022(5) 0.013(4) -0.020(4) C59 0.080(4) 0.080(4) 0.062(4) -0.006(3) 0.019(3) -0.028(4) C60 0.063(3) 0.053(3) 0.050(3) -0.004(2) 0.020(2) -0.008(3) C61 0.054(3) 0.034(2) 0.043(2) 0.000(2) 0.010(2) -0.009(2) C62 0.080(4) 0.046(3) 0.052(3) 0.003(2) 0.010(3) 0.010(3) C63 0.083(4) 0.056(4) 0.081(4) 0.014(3) 0.011(3) 0.017(3) C64 0.093(5) 0.066(4) 0.063(4) 0.021(3) -0.012(3) -0.001(4) C65 0.126(6) 0.071(4) 0.041(3) 0.008(3) 0.004(3) 0.004(4) C66 0.097(4) 0.052(3) 0.049(3) 0.006(2) 0.018(3) 0.011(3) P 0.171(2) 0.122(2) 0.0679(12) -0.0163(12) 0.0491(14) 0.051(2) F1 0.179(5) 0.156(5) 0.144(4) -0.063(4) 0.096(4) -0.003(4) F2 0.172(5) 0.281(8) 0.093(3) -0.025(4) 0.058(3) 0.104(5) F3 0.215(8) 0.431(15) 0.108(5) 0.064(7) 0.043(5) 0.087(9) F4 0.304(12) 0.677(26) 0.131(6) 0.163(11) 0.114(7) 0.290(16) F5 0.392(14) 0.133(6) 0.606(22) -0.134(10) 0.406(16) -0.081(8) F6 0.288(12) 0.286(12) 0.529(21) -0.295(14) 0.197(13) -0.048(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.603(4) . ? Ru1 O3 1.928(3) . ? Ru1 O2 1.934(3) . ? Ru1 O1 2.032(3) . ? Ru1 N3 2.096(3) . ? Ru2 N2 1.613(4) . ? Ru2 O5 1.923(3) . ? Ru2 O4 1.930(3) . ? Ru2 O1 2.040(3) . ? Ru2 N4 2.086(3) . ? O2 C1 1.435(5) . ? O3 C9 1.445(5) . ? O4 C34 1.437(5) . ? O5 C42 1.435(5) . ? N3 C3 1.362(6) . ? N3 C7 1.369(6) . ? N4 C36 1.354(5) . ? N4 C40 1.362(5) . ? C1 C2 1.533(6) . ? C1 C10 1.544(6) . ? C1 C16 1.555(6) . ? C2 C3 1.511(6) . ? C3 C4 1.386(6) . ? C4 C5 1.374(7) . ? C5 C6 1.381(7) . ? C6 C7 1.380(6) . ? C7 C8 1.516(6) . ? C8 C9 1.540(6) . ? C9 C28 1.533(6) . ? C9 C22 1.541(6) . ? C10 C15 1.385(7) . ? C10 C11 1.389(7) . ? C11 C12 1.383(8) . ? C12 C13 1.370(8) . ? C13 C14 1.375(8) . ? C14 C15 1.407(7) . ? C16 C17 1.376(7) . ? C16 C21 1.388(7) . ? C17 C18 1.400(8) . ? C18 C19 1.361(9) . ? C19 C20 1.364(9) . ? C20 C21 1.405(8) . ? C22 C23 1.374(7) . ? C22 C27 1.379(7) . ? C23 C24 1.393(8) . ? C24 C25 1.365(8) . ? C25 C26 1.365(8) . ? C26 C27 1.391(7) . ? C28 C33 1.374(7) . ? C28 C29 1.390(7) . ? C29 C30 1.374(8) . ? C30 C31 1.342(9) . ? C31 C32 1.364(10) . ? C32 C33 1.430(9) . ? C34 C35 1.531(6) . ? C34 C43 1.538(6) . ? C34 C49 1.543(6) . ? C35 C36 1.498(6) . ? C36 C37 1.381(6) . ? C37 C38 1.388(7) . ? C38 C39 1.386(7) . ? C39 C40 1.387(6) . ? C40 C41 1.503(6) . ? C41 C42 1.547(6) . ? C42 C55 1.540(6) . ? C42 C61 1.545(6) . ? C43 C44 1.384(7) . ? C43 C48 1.385(7) . ? C44 C45 1.386(8) . ? C45 C46 1.368(10) . ? C46 C47 1.367(10) . ? C47 C48 1.413(8) . ? C49 C54 1.380(6) . ? C49 C50 1.388(6) . ? C50 C51 1.385(7) . ? C51 C52 1.373(8) . ? C52 C53 1.373(8) . ? C53 C54 1.393(7) . ? C55 C56 1.386(7) . ? C55 C60 1.399(7) . ? C56 C57 1.417(9) . ? C57 C58 1.369(11) . ? C58 C59 1.366(10) . ? C59 C60 1.388(8) . ? C61 C62 1.380(7) . ? C61 C66 1.392(7) . ? C62 C63 1.396(7) . ? C63 C64 1.344(9) . ? C64 C65 1.381(9) . ? C65 C66 1.383(7) . ? P F5 1.474(7) . ? P F3 1.479(7) . ? P F4 1.488(8) . ? P F6 1.496(10) . ? P F2 1.558(5) . ? P F1 1.567(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O3 114.4(2) . . ? N1 Ru1 O2 114.9(2) . . ? O3 Ru1 O2 129.59(13) . . ? N1 Ru1 O1 100.1(2) . . ? O3 Ru1 O1 83.65(11) . . ? O2 Ru1 O1 78.23(11) . . ? N1 Ru1 N3 94.5(2) . . ? O3 Ru1 N3 93.66(13) . . ? O2 Ru1 N3 92.37(13) . . ? O1 Ru1 N3 164.94(12) . . ? N2 Ru2 O5 116.1(2) . . ? N2 Ru2 O4 119.3(2) . . ? O5 Ru2 O4 123.94(14) . . ? N2 Ru2 O1 100.6(2) . . ? O5 Ru2 O1 79.11(11) . . ? O4 Ru2 O1 83.27(11) . . ? N2 Ru2 N4 95.6(2) . . ? O5 Ru2 N4 92.87(12) . . ? O4 Ru2 N4 89.78(13) . . ? O1 Ru2 N4 163.79(12) . . ? Ru1 O1 Ru2 136.01(14) . . ? C1 O2 Ru1 126.9(3) . . ? C9 O3 Ru1 125.5(2) . . ? C34 O4 Ru2 127.7(2) . . ? C42 O5 Ru2 127.9(2) . . ? C3 N3 C7 120.0(4) . . ? C3 N3 Ru1 118.2(3) . . ? C7 N3 Ru1 121.3(3) . . ? C36 N4 C40 121.0(4) . . ? C36 N4 Ru2 119.1(3) . . ? C40 N4 Ru2 119.9(3) . . ? O2 C1 C2 109.0(3) . . ? O2 C1 C10 106.1(3) . . ? C2 C1 C10 111.6(4) . . ? O2 C1 C16 109.8(3) . . ? C2 C1 C16 111.7(4) . . ? C10 C1 C16 108.5(3) . . ? C3 C2 C1 115.1(4) . . ? N3 C3 C4 119.9(4) . . ? N3 C3 C2 119.6(4) . . ? C4 C3 C2 120.3(4) . . ? C5 C4 C3 120.8(5) . . ? C4 C5 C6 118.5(5) . . ? C7 C6 C5 120.6(5) . . ? N3 C7 C6 120.2(4) . . ? N3 C7 C8 119.5(4) . . ? C6 C7 C8 120.3(4) . . ? C7 C8 C9 116.2(4) . . ? O3 C9 C28 109.0(4) . . ? O3 C9 C8 108.1(3) . . ? C28 C9 C8 114.2(4) . . ? O3 C9 C22 107.1(3) . . ? C28 C9 C22 110.2(4) . . ? C8 C9 C22 108.1(4) . . ? C15 C10 C11 117.5(5) . . ? C15 C10 C1 123.6(4) . . ? C11 C10 C1 119.0(4) . . ? C12 C11 C10 121.1(5) . . ? C13 C12 C11 121.2(6) . . ? C12 C13 C14 119.0(5) . . ? C13 C14 C15 120.0(5) . . ? C10 C15 C14 121.2(5) . . ? C17 C16 C21 117.8(5) . . ? C17 C16 C1 122.3(4) . . ? C21 C16 C1 119.8(4) . . ? C16 C17 C18 120.8(6) . . ? C19 C18 C17 121.1(6) . . ? C18 C19 C20 119.0(6) . . ? C19 C20 C21 120.6(6) . . ? C16 C21 C20 120.7(6) . . ? C23 C22 C27 116.6(5) . . ? C23 C22 C9 121.4(4) . . ? C27 C22 C9 121.9(4) . . ? C22 C23 C24 121.8(6) . . ? C25 C24 C23 120.2(6) . . ? C24 C25 C26 119.2(5) . . ? C25 C26 C27 120.0(5) . . ? C22 C27 C26 122.0(5) . . ? C33 C28 C29 117.9(5) . . ? C33 C28 C9 123.5(5) . . ? C29 C28 C9 118.3(4) . . ? C30 C29 C28 121.9(6) . . ? C31 C30 C29 120.4(7) . . ? C30 C31 C32 120.1(6) . . ? C31 C32 C33 120.3(6) . . ? C28 C33 C32 119.2(6) . . ? O4 C34 C35 109.3(3) . . ? O4 C34 C43 107.0(3) . . ? C35 C34 C43 110.9(3) . . ? O4 C34 C49 109.5(3) . . ? C35 C34 C49 111.4(3) . . ? C43 C34 C49 108.7(3) . . ? C36 C35 C34 113.6(3) . . ? N4 C36 C37 120.3(4) . . ? N4 C36 C35 118.1(4) . . ? C37 C36 C35 121.5(4) . . ? C36 C37 C38 119.7(5) . . ? C39 C38 C37 119.3(5) . . ? C38 C39 C40 119.8(5) . . ? N4 C40 C39 119.7(4) . . ? N4 C40 C41 119.1(4) . . ? C39 C40 C41 121.2(4) . . ? C40 C41 C42 113.6(4) . . ? O5 C42 C55 110.5(4) . . ? O5 C42 C61 105.7(3) . . ? C55 C42 C61 111.5(3) . . ? O5 C42 C41 109.3(3) . . ? C55 C42 C41 107.8(3) . . ? C61 C42 C41 112.0(4) . . ? C44 C43 C48 118.4(5) . . ? C44 C43 C34 122.3(4) . . ? C48 C43 C34 119.3(4) . . ? C43 C44 C45 120.4(6) . . ? C46 C45 C44 121.8(7) . . ? C47 C46 C45 118.6(6) . . ? C46 C47 C48 120.7(7) . . ? C43 C48 C47 120.1(6) . . ? C54 C49 C50 117.4(4) . . ? C54 C49 C34 121.6(4) . . ? C50 C49 C34 121.0(4) . . ? C51 C50 C49 121.8(5) . . ? C52 C51 C50 119.9(5) . . ? C51 C52 C53 119.4(5) . . ? C52 C53 C54 120.5(5) . . ? C49 C54 C53 121.1(5) . . ? C56 C55 C60 119.0(5) . . ? C56 C55 C42 121.0(4) . . ? C60 C55 C42 119.8(4) . . ? C55 C56 C57 119.5(6) . . ? C58 C57 C56 119.8(7) . . ? C59 C58 C57 121.3(6) . . ? C58 C59 C60 119.5(6) . . ? C59 C60 C55 120.9(5) . . ? C62 C61 C66 117.4(5) . . ? C62 C61 C42 123.7(4) . . ? C66 C61 C42 119.0(4) . . ? C61 C62 C63 120.8(5) . . ? C64 C63 C62 121.3(6) . . ? C63 C64 C65 118.8(5) . . ? C64 C65 C66 120.8(6) . . ? C65 C66 C61 120.8(6) . . ? F5 P F3 88.0(7) . . ? F5 P F4 93.8(8) . . ? F3 P F4 178.1(9) . . ? F5 P F6 178.9(7) . . ? F3 P F6 92.7(8) . . ? F4 P F6 85.5(8) . . ? F5 P F2 91.0(4) . . ? F3 P F2 90.5(4) . . ? F4 P F2 90.1(4) . . ? F6 P F2 89.9(5) . . ? F5 P F1 90.0(3) . . ? F3 P F1 90.6(4) . . ? F4 P F1 88.8(4) . . ? F6 P F1 89.1(4) . . ? F2 P F1 178.6(4) . . ? _refine_diff_density_max 0.732 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.087 data_mar71 _database_code_CSD 209728 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H41 Cl2 N3 O4 Ru' _chemical_formula_sum 'C39 H41 Cl2 N3 O4 Ru' _chemical_formula_weight 787.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 10.098(2) _cell_length_b 14.093(3) _cell_length_c 14.192(3) _cell_angle_alpha 66.68(2) _cell_angle_beta 79.25(2) _cell_angle_gamma 87.84(2) _cell_volume 1820.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20527 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.58 _reflns_number_total 6364 _reflns_number_gt 5419 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0740P)^2^+0.8639P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6364 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Ru2 Ru 0.19003(3) 0.322093(19) 0.26305(2) 0.03211(12) Uani 1 1 d . . . Cl1 Cl -0.01512(9) 0.25826(7) 0.24515(8) 0.0444(2) Uani 1 1 d . . . Cl2 Cl 0.39967(9) 0.36341(8) 0.29418(8) 0.0471(2) Uani 1 1 d . . . C1 C 0.3654(3) 0.2193(3) 0.1197(3) 0.0344(7) Uani 1 1 d . . . C2 C 0.4231(3) 0.3319(3) 0.0703(3) 0.0374(8) Uani 1 1 d . . . H2A H 0.4685 0.3424 0.1201 0.045 Uiso 1 1 calc R . . H2B H 0.4913 0.3391 0.0096 0.045 Uiso 1 1 calc R . . C3 C 0.3274(3) 0.4169(3) 0.0370(3) 0.0334(7) Uani 1 1 d . . . C4 C 0.3480(4) 0.4867(3) -0.0663(3) 0.0407(8) Uani 1 1 d . . . H4 H 0.4183 0.4781 -0.1146 0.049 Uiso 1 1 calc R . . C5 C 0.2650(4) 0.5687(3) -0.0980(3) 0.0419(8) Uani 1 1 d . . . H5 H 0.2781 0.6157 -0.1672 0.050 Uiso 1 1 calc R . . C6 C 0.1626(4) 0.5793(3) -0.0249(3) 0.0429(8) Uani 1 1 d . . . H6 H 0.1054 0.6342 -0.0445 0.052 Uiso 1 1 calc R . . C7 C 0.1438(4) 0.5091(2) 0.0774(3) 0.0357(7) Uani 1 1 d . . . C8 C 0.0275(3) 0.5180(3) 0.1551(3) 0.0374(8) Uani 1 1 d . . . H8A H -0.0372 0.4617 0.1723 0.045 Uiso 1 1 calc R . . H8B H -0.0160 0.5820 0.1217 0.045 Uiso 1 1 calc R . . C9 C 0.0587(3) 0.5162(3) 0.2579(3) 0.0364(8) Uani 1 1 d . . . C10 C 0.4848(3) 0.1469(3) 0.1346(3) 0.0371(8) Uani 1 1 d . . . C11 C 0.4923(4) 0.0622(3) 0.1086(3) 0.0484(9) Uani 1 1 d . . . H11 H 0.4218 0.0464 0.0827 0.058 Uiso 1 1 calc R . . C12 C 0.6026(5) 0.0002(3) 0.1202(4) 0.0574(11) Uani 1 1 d . . . H12 H 0.6059 -0.0563 0.1016 0.069 Uiso 1 1 calc R . . C13 C 0.7071(4) 0.0217(3) 0.1588(4) 0.0569(11) Uani 1 1 d . . . H13 H 0.7809 -0.0203 0.1671 0.068 Uiso 1 1 calc R . . C14 C 0.7020(4) 0.1053(3) 0.1852(4) 0.0602(12) Uani 1 1 d . . . H14 H 0.7734 0.1210 0.2102 0.072 Uiso 1 1 calc R . . C15 C 0.5913(4) 0.1664(3) 0.1747(3) 0.0501(10) Uani 1 1 d . . . H15 H 0.5878 0.2219 0.1948 0.060 Uiso 1 1 calc R . . C16 C 0.2739(4) 0.1984(3) 0.0553(3) 0.0416(8) Uani 1 1 d . . . C17 C 0.1620(5) 0.1333(4) 0.1026(5) 0.0748(16) Uani 1 1 d . . . H17 H 0.1401 0.1015 0.1751 0.090 Uiso 1 1 calc R . . C18 C 0.0811(6) 0.1149(7) 0.0416(7) 0.116(3) Uani 1 1 d . . . H18 H 0.0059 0.0699 0.0739 0.139 Uiso 1 1 calc R . . C19 C 0.1106(7) 0.1622(7) -0.0655(7) 0.109(3) Uani 1 1 d . . . H19 H 0.0553 0.1499 -0.1053 0.130 Uiso 1 1 calc R . . C20 C 0.2196(7) 0.2261(4) -0.1120(5) 0.085(2) Uani 1 1 d . . . H20 H 0.2397 0.2585 -0.1845 0.103 Uiso 1 1 calc R . . C21 C 0.3032(5) 0.2444(3) -0.0528(4) 0.0563(11) Uani 1 1 d . . . H21 H 0.3795 0.2879 -0.0862 0.068 Uiso 1 1 calc R . . C22 C 0.1676(4) 0.5978(3) 0.2385(3) 0.0404(8) Uani 1 1 d . . . C23 C 0.1798(5) 0.6923(3) 0.1547(4) 0.0582(11) Uani 1 1 d . . . H23 H 0.1233 0.7062 0.1064 0.070 Uiso 1 1 calc R . . C24 C 0.2755(7) 0.7669(4) 0.1420(5) 0.0834(18) Uani 1 1 d . . . H24 H 0.2829 0.8304 0.0854 0.100 Uiso 1 1 calc R . . C25 C 0.3591(6) 0.7465(5) 0.2134(6) 0.090(2) Uani 1 1 d . . . H25 H 0.4231 0.7962 0.2054 0.108 Uiso 1 1 calc R . . C26 C 0.3478(6) 0.6535(5) 0.2956(6) 0.093(2) Uani 1 1 d . . . H26 H 0.4044 0.6401 0.3438 0.111 Uiso 1 1 calc R . . C27 C 0.2543(5) 0.5789(4) 0.3087(5) 0.0692(14) Uani 1 1 d . . . H27 H 0.2490 0.5153 0.3649 0.083 Uiso 1 1 calc R . . C28 C -0.0745(3) 0.5342(3) 0.3212(3) 0.0382(8) Uani 1 1 d . . . C29 C -0.0878(4) 0.6070(4) 0.3630(4) 0.0607(12) Uani 1 1 d . . . H29 H -0.0125 0.6473 0.3553 0.073 Uiso 1 1 calc R . . C30 C -0.2119(5) 0.6225(4) 0.4172(4) 0.0720(14) Uani 1 1 d . . . H30 H -0.2187 0.6728 0.4448 0.086 Uiso 1 1 calc R . . C31 C -0.3212(5) 0.5643(4) 0.4291(4) 0.0648(12) Uani 1 1 d . . . H31 H -0.4038 0.5742 0.4651 0.078 Uiso 1 1 calc R . . C32 C -0.3113(5) 0.4915(5) 0.3889(4) 0.0764(16) Uani 1 1 d . . . H32 H -0.3876 0.4525 0.3960 0.092 Uiso 1 1 calc R . . C33 C -0.1891(4) 0.4749(4) 0.3376(4) 0.0653(13) Uani 1 1 d . . . H33 H -0.1833 0.4223 0.3132 0.078 Uiso 1 1 calc R . . C34 C 0.0559(4) 0.2143(3) 0.4825(3) 0.0449(9) Uani 1 1 d . . . H34 H 0.0100 0.2755 0.4651 0.054 Uiso 1 1 calc R . . N2 N 0.0138(4) 0.1405(3) 0.5731(3) 0.0551(9) Uani 1 1 d . . . C35 C 0.0732(6) 0.0397(4) 0.6020(4) 0.0849(18) Uani 1 1 d . . . H35A H 0.0299 -0.0050 0.6711 0.127 Uiso 1 1 calc R . . H35B H 0.1678 0.0471 0.6004 0.127 Uiso 1 1 calc R . . H35C H 0.0612 0.0102 0.5535 0.127 Uiso 1 1 calc R . . C36 C -0.0951(6) 0.1540(4) 0.6498(4) 0.0857(18) Uani 1 1 d . . . H36A H -0.1113 0.0910 0.7113 0.129 Uiso 1 1 calc R . . H36B H -0.1757 0.1710 0.6207 0.129 Uiso 1 1 calc R . . H36C H -0.0701 0.2089 0.6677 0.129 Uiso 1 1 calc R . . C37 C 0.4064(5) -0.0286(4) 0.3842(4) 0.0809(16) Uani 1 1 d . . . H37 H 0.4807 -0.0009 0.3308 0.097 Uiso 1 1 calc R . . N3 N 0.4235(5) -0.1156(3) 0.4593(3) 0.0739(12) Uani 1 1 d . . . C38 C 0.5417(8) -0.1751(7) 0.4544(7) 0.179(5) Uani 1 1 d . . . H38A H 0.5345 -0.2361 0.5179 0.269 Uiso 1 1 calc R . . H38B H 0.6203 -0.1342 0.4460 0.269 Uiso 1 1 calc R . . H38C H 0.5491 -0.1948 0.3962 0.269 Uiso 1 1 calc R . . C39 C 0.3214(9) -0.1625(6) 0.5504(6) 0.150(4) Uani 1 1 d . . . H39A H 0.3532 -0.2255 0.5969 0.224 Uiso 1 1 calc R . . H39B H 0.2415 -0.1774 0.5303 0.224 Uiso 1 1 calc R . . H39C H 0.3009 -0.1159 0.5850 0.224 Uiso 1 1 calc R . . N1 N 0.2256(3) 0.4280(2) 0.1090(2) 0.0325(6) Uani 1 1 d . . . O1 O 0.2883(2) 0.20374(18) 0.22234(18) 0.0380(5) Uani 1 1 d . . . O2 O 0.0977(2) 0.41606(17) 0.31894(19) 0.0383(5) Uani 1 1 d . . . O3 O 0.1529(3) 0.20850(18) 0.41798(19) 0.0419(6) Uani 1 1 d . . . O4 O 0.3053(4) 0.0208(3) 0.3752(3) 0.0802(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru2 0.03379(19) 0.02818(16) 0.02933(17) -0.00646(11) -0.00549(11) 0.00299(10) Cl1 0.0393(5) 0.0390(5) 0.0512(6) -0.0131(4) -0.0098(4) -0.0026(3) Cl2 0.0401(5) 0.0571(6) 0.0461(5) -0.0199(4) -0.0136(4) 0.0018(4) C1 0.0340(19) 0.0335(17) 0.0325(18) -0.0129(14) 0.0008(13) 0.0009(13) C2 0.0341(19) 0.0362(18) 0.0363(19) -0.0110(15) 0.0001(14) -0.0030(13) C3 0.0331(18) 0.0338(17) 0.0324(18) -0.0120(14) -0.0053(13) -0.0039(13) C4 0.046(2) 0.0356(18) 0.0333(19) -0.0086(15) 0.0005(15) -0.0078(14) C5 0.056(2) 0.0327(18) 0.0310(19) -0.0037(15) -0.0118(16) -0.0047(15) C6 0.053(2) 0.0326(18) 0.041(2) -0.0091(16) -0.0155(16) 0.0027(15) C7 0.041(2) 0.0296(16) 0.0340(19) -0.0073(14) -0.0120(14) 0.0005(13) C8 0.0375(19) 0.0315(17) 0.039(2) -0.0087(15) -0.0108(14) 0.0082(13) C9 0.0368(19) 0.0302(17) 0.041(2) -0.0126(15) -0.0082(14) 0.0078(13) C10 0.0362(19) 0.0359(18) 0.0361(19) -0.0120(15) -0.0045(14) 0.0017(13) C11 0.047(2) 0.045(2) 0.059(3) -0.025(2) -0.0143(18) 0.0088(16) C12 0.063(3) 0.045(2) 0.068(3) -0.029(2) -0.011(2) 0.0132(19) C13 0.045(2) 0.052(2) 0.072(3) -0.023(2) -0.010(2) 0.0148(18) C14 0.045(3) 0.053(3) 0.081(3) -0.021(2) -0.022(2) 0.0062(18) C15 0.046(2) 0.043(2) 0.067(3) -0.025(2) -0.0167(19) 0.0074(16) C16 0.036(2) 0.042(2) 0.056(2) -0.0289(18) -0.0095(16) 0.0086(14) C17 0.047(3) 0.103(4) 0.091(4) -0.064(3) 0.010(2) -0.022(2) C18 0.042(3) 0.185(8) 0.189(8) -0.151(7) -0.006(4) -0.016(3) C19 0.075(5) 0.158(7) 0.181(8) -0.141(7) -0.078(5) 0.065(4) C20 0.126(6) 0.075(4) 0.097(4) -0.059(3) -0.074(4) 0.056(4) C21 0.083(3) 0.045(2) 0.051(3) -0.024(2) -0.029(2) 0.017(2) C22 0.036(2) 0.0365(18) 0.050(2) -0.0194(17) -0.0048(15) 0.0035(14) C23 0.077(3) 0.040(2) 0.052(3) -0.0153(19) 0.000(2) -0.0070(19) C24 0.105(5) 0.051(3) 0.076(4) -0.024(3) 0.031(3) -0.034(3) C25 0.050(3) 0.088(4) 0.144(6) -0.066(4) 0.009(3) -0.026(3) C26 0.061(4) 0.077(4) 0.165(7) -0.061(4) -0.052(4) 0.007(3) C27 0.064(3) 0.049(2) 0.109(4) -0.034(3) -0.044(3) 0.011(2) C28 0.0366(19) 0.0366(18) 0.037(2) -0.0118(15) -0.0047(14) 0.0043(14) C29 0.045(3) 0.072(3) 0.076(3) -0.045(3) 0.000(2) -0.003(2) C30 0.060(3) 0.088(4) 0.086(4) -0.061(3) 0.002(2) 0.002(2) C31 0.050(3) 0.075(3) 0.066(3) -0.032(3) 0.007(2) 0.001(2) C32 0.047(3) 0.097(4) 0.088(4) -0.051(3) 0.015(2) -0.016(2) C33 0.050(3) 0.072(3) 0.084(4) -0.050(3) 0.009(2) -0.012(2) C34 0.050(2) 0.0378(19) 0.039(2) -0.0094(17) -0.0041(17) -0.0012(15) N2 0.064(2) 0.0481(19) 0.0391(19) -0.0090(16) 0.0054(15) -0.0027(16) C35 0.092(4) 0.062(3) 0.060(3) 0.008(3) 0.005(3) 0.017(3) C36 0.096(4) 0.074(3) 0.066(3) -0.024(3) 0.029(3) -0.011(3) C37 0.057(3) 0.077(3) 0.072(4) 0.004(3) -0.001(2) 0.010(2) N3 0.079(3) 0.059(2) 0.056(3) 0.0023(19) -0.006(2) 0.015(2) C38 0.119(7) 0.172(8) 0.127(7) 0.043(6) 0.010(5) 0.086(6) C39 0.155(8) 0.111(6) 0.091(5) 0.029(4) 0.029(5) 0.051(5) N1 0.0338(16) 0.0283(14) 0.0320(15) -0.0071(12) -0.0081(11) -0.0010(11) O1 0.0435(14) 0.0307(12) 0.0333(13) -0.0098(10) 0.0018(10) 0.0029(10) O2 0.0448(14) 0.0335(12) 0.0342(13) -0.0106(10) -0.0090(10) 0.0064(10) O3 0.0480(15) 0.0367(13) 0.0287(13) -0.0026(10) -0.0025(10) 0.0075(10) _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 Ru2 O2 1.927(2) . ? Ru2 N1 2.073(3) . ? Ru2 O3 2.119(2) . ? Ru2 O1 2.127(2) . ? Ru2 Cl2 2.3793(10) . ? Ru2 Cl1 2.3839(10) . ? C1 O1 1.453(4) . ? C1 C16 1.525(5) . ? C1 C10 1.540(5) . ? C1 C2 1.544(4) . ? C2 C3 1.492(5) . ? C3 N1 1.360(4) . ? C3 C4 1.386(5) . ? C4 C5 1.377(5) . ? C5 C6 1.371(5) . ? C6 C7 1.377(5) . ? C7 N1 1.361(4) . ? C7 C8 1.492(5) . ? C8 C9 1.540(5) . ? C9 O2 1.420(4) . ? C9 C22 1.530(5) . ? C9 C28 1.544(5) . ? C10 C11 1.378(5) . ? C10 C15 1.389(5) . ? C11 C12 1.383(6) . ? C12 C13 1.370(6) . ? C13 C14 1.366(6) . ? C14 C15 1.380(6) . ? C16 C17 1.370(6) . ? C16 C21 1.385(6) . ? C17 C18 1.393(8) . ? C18 C19 1.373(11) . ? C19 C20 1.339(10) . ? C20 C21 1.392(7) . ? C22 C23 1.381(6) . ? C22 C27 1.387(6) . ? C23 C24 1.390(6) . ? C24 C25 1.376(9) . ? C25 C26 1.358(9) . ? C26 C27 1.374(7) . ? C28 C29 1.365(5) . ? C28 C33 1.383(6) . ? C29 C30 1.401(6) . ? C30 C31 1.345(7) . ? C31 C32 1.349(7) . ? C32 C33 1.374(6) . ? C34 O3 1.234(4) . ? C34 N2 1.298(5) . ? N2 C35 1.454(6) . ? N2 C36 1.460(6) . ? C37 O4 1.212(6) . ? C37 N3 1.299(6) . ? N3 C39 1.431(8) . ? N3 C38 1.440(7) . ? 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 O2 Ru2 N1 95.33(10) . . ? O2 Ru2 O3 86.86(10) . . ? N1 Ru2 O3 177.38(10) . . ? O2 Ru2 O1 172.35(9) . . ? N1 Ru2 O1 92.31(10) . . ? O3 Ru2 O1 85.51(9) . . ? O2 Ru2 Cl2 91.45(8) . . ? N1 Ru2 Cl2 93.34(8) . . ? O3 Ru2 Cl2 88.03(8) . . ? O1 Ru2 Cl2 87.82(7) . . ? O2 Ru2 Cl1 92.63(8) . . ? N1 Ru2 Cl1 92.35(8) . . ? O3 Ru2 Cl1 86.11(8) . . ? O1 Ru2 Cl1 87.32(7) . . ? Cl2 Ru2 Cl1 172.66(3) . . ? O1 C1 C16 109.5(3) . . ? O1 C1 C10 108.1(3) . . ? C16 C1 C10 112.1(3) . . ? O1 C1 C2 106.5(3) . . ? C16 C1 C2 112.4(3) . . ? C10 C1 C2 108.0(3) . . ? C3 C2 C1 118.1(3) . . ? N1 C3 C4 120.9(3) . . ? N1 C3 C2 119.8(3) . . ? C4 C3 C2 119.2(3) . . ? C5 C4 C3 120.4(3) . . ? C6 C5 C4 118.4(3) . . ? C5 C6 C7 120.3(3) . . ? N1 C7 C6 121.5(3) . . ? N1 C7 C8 118.5(3) . . ? C6 C7 C8 119.9(3) . . ? C7 C8 C9 117.1(3) . . ? O2 C9 C22 110.6(3) . . ? O2 C9 C8 109.8(3) . . ? C22 C9 C8 111.9(3) . . ? O2 C9 C28 105.9(3) . . ? C22 C9 C28 111.0(3) . . ? C8 C9 C28 107.4(3) . . ? C11 C10 C15 117.4(3) . . ? C11 C10 C1 122.6(3) . . ? C15 C10 C1 120.0(3) . . ? C10 C11 C12 121.2(4) . . ? C13 C12 C11 120.3(4) . . ? C14 C13 C12 119.6(4) . . ? C13 C14 C15 120.1(4) . . ? C14 C15 C10 121.4(4) . . ? C17 C16 C21 118.5(4) . . ? C17 C16 C1 121.0(4) . . ? C21 C16 C1 120.5(3) . . ? C16 C17 C18 119.7(6) . . ? C19 C18 C17 121.1(6) . . ? C20 C19 C18 119.5(5) . . ? C19 C20 C21 120.5(6) . . ? C16 C21 C20 120.8(5) . . ? C23 C22 C27 118.3(4) . . ? C23 C22 C9 121.9(4) . . ? C27 C22 C9 119.7(4) . . ? C22 C23 C24 120.6(5) . . ? C25 C24 C23 119.8(5) . . ? C26 C25 C24 119.7(5) . . ? C25 C26 C27 121.1(6) . . ? C26 C27 C22 120.4(5) . . ? C29 C28 C33 116.4(4) . . ? C29 C28 C9 123.8(3) . . ? C33 C28 C9 119.7(3) . . ? C28 C29 C30 121.7(4) . . ? C31 C30 C29 119.6(4) . . ? C30 C31 C32 120.2(4) . . ? C31 C32 C33 120.3(4) . . ? C32 C33 C28 121.8(4) . . ? O3 C34 N2 124.4(4) . . ? C34 N2 C35 120.8(4) . . ? C34 N2 C36 122.1(4) . . ? C35 N2 C36 117.1(4) . . ? O4 C37 N3 127.8(5) . . ? C37 N3 C39 121.9(5) . . ? C37 N3 C38 122.9(5) . . ? C39 N3 C38 115.1(5) . . ? C3 N1 C7 118.5(3) . . ? C3 N1 Ru2 121.4(2) . . ? C7 N1 Ru2 120.0(2) . . ? C1 O1 Ru2 124.83(19) . . ? C9 O2 Ru2 124.8(2) . . ? C34 O3 Ru2 120.7(2) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.58 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.194 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.132 data_mar86 _database_code_CSD 209729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51.50 H43 Cl3 N O2 P Ru' _chemical_formula_sum 'C51.50 H43 Cl3 N O2 P Ru' _chemical_formula_weight 946.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.254(2) _cell_length_b 17.659(2) _cell_length_c 19.344(3) _cell_angle_alpha 75.31(2) _cell_angle_beta 70.65(2) _cell_angle_gamma 69.06(2) _cell_volume 4537.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26981 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.41 _reflns_number_total 14665 _reflns_number_gt 10368 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.1094P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14665 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.014 _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 0.02889(3) 0.72467(2) 0.58706(2) 0.04026(13) Uani 1 1 d . . . Ru2 Ru 0.55347(2) 0.08239(2) 0.20258(2) 0.03944(13) Uani 1 1 d . . . Cl1 Cl -0.10865(9) 0.67794(8) 0.62132(7) 0.0525(3) Uani 1 1 d . . . Cl2 Cl 0.17326(9) 0.76639(9) 0.53522(8) 0.0573(3) Uani 1 1 d . . . Cl3 Cl 0.70266(9) 0.02079(8) 0.23779(7) 0.0521(3) Uani 1 1 d . . . Cl4 Cl 0.41408(8) 0.12587(8) 0.15771(7) 0.0511(3) Uani 1 1 d . . . P1 P 0.12448(9) 0.58821(8) 0.61049(8) 0.0472(3) Uani 1 1 d . . . P2 P 0.64593(9) 0.11537(8) 0.08227(7) 0.0439(3) Uani 1 1 d . . . O1 O 0.0214(2) 0.7359(2) 0.68802(18) 0.0481(8) Uani 1 1 d . . . O2 O 0.0444(2) 0.71387(19) 0.47646(17) 0.0423(7) Uani 1 1 d . . . O3 O 0.5397(2) 0.1892(2) 0.22226(17) 0.0439(7) Uani 1 1 d . . . O4 O 0.5696(2) -0.03768(19) 0.18174(17) 0.0446(7) Uani 1 1 d . . . N1 N -0.0588(3) 0.8512(2) 0.5663(2) 0.0405(9) Uani 1 1 d . . . N2 N 0.4703(3) 0.0486(3) 0.3144(2) 0.0456(9) Uani 1 1 d . . . C1 C -0.0548(3) 0.7924(3) 0.7335(3) 0.0437(11) Uani 1 1 d . . . C2 C -0.1419(3) 0.8353(3) 0.7001(3) 0.0457(12) Uani 1 1 d . . . H2A H -0.1668 0.7937 0.6960 0.055 Uiso 1 1 calc R . . H2B H -0.1929 0.8696 0.7346 0.055 Uiso 1 1 calc R . . C3 C -0.1224(3) 0.8867(3) 0.6266(3) 0.0466(12) Uani 1 1 d . . . C4 C -0.1728(4) 0.9699(3) 0.6183(3) 0.0590(14) Uani 1 1 d . . . H4 H -0.2157 0.9936 0.6594 0.071 Uiso 1 1 calc R . . C5 C -0.1596(4) 1.0173(4) 0.5494(3) 0.0623(15) Uani 1 1 d . . . H5 H -0.1919 1.0733 0.5436 0.075 Uiso 1 1 calc R . . C6 C -0.0979(4) 0.9801(3) 0.4897(3) 0.0542(13) Uani 1 1 d . . . H6 H -0.0893 1.0112 0.4427 0.065 Uiso 1 1 calc R . . C7 C -0.0477(3) 0.8965(3) 0.4980(3) 0.0437(11) Uani 1 1 d . . . C8 C 0.0196(4) 0.8588(3) 0.4314(3) 0.0440(11) Uani 1 1 d . . . H8A H 0.0858 0.8474 0.4336 0.053 Uiso 1 1 calc R . . H8B H 0.0109 0.8993 0.3878 0.053 Uiso 1 1 calc R . . C9 C 0.0089(3) 0.7791(3) 0.4204(3) 0.0421(11) Uani 1 1 d . . . C10 C -0.0163(3) 0.8572(3) 0.7440(3) 0.0465(12) Uani 1 1 d . . . C11 C 0.0737(4) 0.8656(3) 0.7035(3) 0.0565(13) Uani 1 1 d . . . H11 H 0.1122 0.8327 0.6672 0.068 Uiso 1 1 calc R . . C12 C 0.1075(4) 0.9229(4) 0.7161(3) 0.0655(15) Uani 1 1 d . . . H12 H 0.1689 0.9274 0.6887 0.079 Uiso 1 1 calc R . . C13 C 0.0520(5) 0.9724(4) 0.7682(4) 0.0692(16) Uani 1 1 d . . . H13 H 0.0749 1.0105 0.7767 0.083 Uiso 1 1 calc R . . C14 C -0.0403(5) 0.9649(4) 0.8087(4) 0.0724(17) Uani 1 1 d . . . H14 H -0.0796 0.9983 0.8444 0.087 Uiso 1 1 calc R . . C15 C -0.0723(4) 0.9079(4) 0.7955(3) 0.0635(15) Uani 1 1 d . . . H15 H -0.1339 0.9036 0.8223 0.076 Uiso 1 1 calc R . . C16 C -0.0836(4) 0.7396(3) 0.8092(3) 0.0492(12) Uani 1 1 d . . . C17 C -0.1736(4) 0.7282(4) 0.8400(3) 0.0644(15) Uani 1 1 d . . . H17 H -0.2223 0.7553 0.8157 0.077 Uiso 1 1 calc R . . C18 C -0.1933(5) 0.6766(4) 0.9071(4) 0.0815(19) Uani 1 1 d . . . H18 H -0.2546 0.6689 0.9267 0.098 Uiso 1 1 calc R . . C19 C -0.1242(7) 0.6376(5) 0.9439(4) 0.093(2) Uani 1 1 d . . . H19 H -0.1382 0.6046 0.9894 0.112 Uiso 1 1 calc R . . C20 C -0.0318(6) 0.6474(5) 0.9129(4) 0.098(2) Uani 1 1 d . . . H20 H 0.0169 0.6199 0.9371 0.117 Uiso 1 1 calc R . . C21 C -0.0130(5) 0.6976(4) 0.8469(3) 0.0758(18) Uani 1 1 d . . . H21 H 0.0489 0.7038 0.8267 0.091 Uiso 1 1 calc R . . C22 C -0.0947(3) 0.7849(3) 0.4253(2) 0.0436(11) Uani 1 1 d . . . C23 C -0.1601(4) 0.8570(3) 0.4023(3) 0.0491(12) Uani 1 1 d . . . H23 H -0.1422 0.9050 0.3866 0.059 Uiso 1 1 calc R . . C24 C -0.2514(4) 0.8592(4) 0.4023(3) 0.0591(14) Uani 1 1 d . . . H24 H -0.2933 0.9079 0.3849 0.071 Uiso 1 1 calc R . . C25 C -0.2807(4) 0.7899(4) 0.4279(3) 0.0635(15) Uani 1 1 d . . . H25 H -0.3427 0.7918 0.4288 0.076 Uiso 1 1 calc R . . C26 C -0.2182(4) 0.7179(4) 0.4522(3) 0.0610(15) Uani 1 1 d . . . H26 H -0.2380 0.6708 0.4699 0.073 Uiso 1 1 calc R . . C27 C -0.1259(4) 0.7148(3) 0.4506(3) 0.0502(12) Uani 1 1 d . . . H27 H -0.0838 0.6654 0.4666 0.060 Uiso 1 1 calc R . . C28 C 0.0760(4) 0.7572(3) 0.3441(3) 0.0485(12) Uani 1 1 d . . . C29 C 0.0462(4) 0.7967(4) 0.2805(3) 0.0669(16) Uani 1 1 d . . . H29 H -0.0143 0.8362 0.2840 0.080 Uiso 1 1 calc R . . C30 C 0.1066(6) 0.7777(5) 0.2111(3) 0.080(2) Uani 1 1 d . . . H30 H 0.0865 0.8053 0.1686 0.096 Uiso 1 1 calc R . . C31 C 0.1945(6) 0.7192(5) 0.2054(4) 0.088(2) Uani 1 1 d . . . H31 H 0.2339 0.7060 0.1591 0.105 Uiso 1 1 calc R . . C32 C 0.2243(5) 0.6800(5) 0.2674(4) 0.087(2) Uani 1 1 d . . . H32 H 0.2842 0.6396 0.2636 0.105 Uiso 1 1 calc R . . C33 C 0.1662(4) 0.6998(4) 0.3360(4) 0.0686(16) Uani 1 1 d . . . H33 H 0.1887 0.6737 0.3778 0.082 Uiso 1 1 calc R . . C34 C 0.1801(4) 0.5441(3) 0.5249(3) 0.0583(14) Uani 1 1 d . . . C35 C 0.1233(5) 0.5274(3) 0.4908(4) 0.0743(18) Uani 1 1 d . . . H35 H 0.0569 0.5365 0.5129 0.089 Uiso 1 1 calc R . . C36 C 0.1655(9) 0.4969(4) 0.4235(5) 0.110(3) Uani 1 1 d . . . H36 H 0.1276 0.4854 0.4008 0.132 Uiso 1 1 calc R . . C37 C 0.2628(11) 0.4842(5) 0.3913(5) 0.140(5) Uani 1 1 d . . . H37 H 0.2917 0.4626 0.3472 0.168 Uiso 1 1 calc R . . C38 C 0.3167(8) 0.5026(7) 0.4230(5) 0.130(4) Uani 1 1 d . . . H38 H 0.3824 0.4955 0.3993 0.156 Uiso 1 1 calc R . . C39 C 0.2780(5) 0.5314(5) 0.4891(4) 0.095(2) Uani 1 1 d . . . H39 H 0.3176 0.5427 0.5102 0.114 Uiso 1 1 calc R . . C40 C 0.0588(4) 0.5193(3) 0.6759(3) 0.0543(13) Uani 1 1 d . . . C41 C 0.0594(6) 0.4463(4) 0.6614(4) 0.0801(19) Uani 1 1 d . . . H41 H 0.0941 0.4301 0.6153 0.096 Uiso 1 1 calc R . . C42 C 0.0082(6) 0.3970(4) 0.7154(5) 0.091(2) Uani 1 1 d . . . H42 H 0.0067 0.3493 0.7042 0.109 Uiso 1 1 calc R . . C43 C -0.0394(5) 0.4177(4) 0.7840(5) 0.084(2) Uani 1 1 d . . . H43 H -0.0720 0.3838 0.8202 0.101 Uiso 1 1 calc R . . C44 C -0.0390(5) 0.4892(4) 0.7994(4) 0.093(2) Uani 1 1 d . . . H44 H -0.0709 0.5037 0.8464 0.111 Uiso 1 1 calc R . . C45 C 0.0091(5) 0.5398(4) 0.7446(4) 0.0805(19) Uani 1 1 d . . . H45 H 0.0074 0.5889 0.7553 0.097 Uiso 1 1 calc R . . C46 C 0.2273(4) 0.5628(4) 0.6495(3) 0.0628(15) Uani 1 1 d . . . C47 C 0.2810(5) 0.4792(5) 0.6643(5) 0.097(2) Uani 1 1 d . . . H47 H 0.2616 0.4389 0.6558 0.116 Uiso 1 1 calc R . . C48 C 0.3613(7) 0.4567(6) 0.6910(6) 0.127(3) Uani 1 1 d . . . H48 H 0.3969 0.4016 0.6988 0.153 Uiso 1 1 calc R . . C49 C 0.3892(7) 0.5149(7) 0.7063(6) 0.135(4) Uani 1 1 d . . . H49 H 0.4449 0.4997 0.7227 0.162 Uiso 1 1 calc R . . C50 C 0.3315(7) 0.6001(6) 0.6969(5) 0.124(3) Uani 1 1 d . . . H50 H 0.3453 0.6400 0.7114 0.148 Uiso 1 1 calc R . . C51 C 0.2552(5) 0.6203(4) 0.6654(4) 0.083(2) Uani 1 1 d . . . H51 H 0.2215 0.6754 0.6547 0.099 Uiso 1 1 calc R . . C52 C 0.4656(3) 0.2320(3) 0.2788(3) 0.0438(11) Uani 1 1 d . . . C53 C 0.3798(3) 0.1955(3) 0.3107(3) 0.0489(12) Uani 1 1 d . . . H53A H 0.3285 0.2303 0.3445 0.059 Uiso 1 1 calc R . . H53B H 0.3545 0.1973 0.2702 0.059 Uiso 1 1 calc R . . C54 C 0.4025(3) 0.1092(3) 0.3507(3) 0.0498(12) Uani 1 1 d . . . C55 C 0.3513(5) 0.0928(4) 0.4231(3) 0.0690(17) Uani 1 1 d . . . H55 H 0.3049 0.1353 0.4476 0.083 Uiso 1 1 calc R . . C56 C 0.3691(5) 0.0137(5) 0.4590(4) 0.087(2) Uani 1 1 d . . . H56 H 0.3358 0.0019 0.5083 0.105 Uiso 1 1 calc R . . C57 C 0.4367(5) -0.0480(4) 0.4212(3) 0.0706(16) Uani 1 1 d . . . H57 H 0.4483 -0.1021 0.4449 0.085 Uiso 1 1 calc R . . C58 C 0.4876(4) -0.0306(3) 0.3483(3) 0.0477(12) Uani 1 1 d . . . C59 C 0.5632(4) -0.0980(3) 0.3101(3) 0.0475(12) Uani 1 1 d . . . H59A H 0.5643 -0.1489 0.3443 0.057 Uiso 1 1 calc R . . H59B H 0.6258 -0.0894 0.2999 0.057 Uiso 1 1 calc R . . C60 C 0.5534(3) -0.1098(3) 0.2371(3) 0.0453(11) Uani 1 1 d . . . C61 C 0.4326(4) 0.3208(3) 0.2399(3) 0.0483(12) Uani 1 1 d . . . C62 C 0.5002(5) 0.3628(4) 0.2092(4) 0.0692(16) Uani 1 1 d . . . H62 H 0.5637 0.3366 0.2128 0.083 Uiso 1 1 calc R . . C63 C 0.4773(6) 0.4425(4) 0.1732(4) 0.086(2) Uani 1 1 d . . . H63 H 0.5248 0.4693 0.1532 0.103 Uiso 1 1 calc R . . C64 C 0.3837(6) 0.4825(4) 0.1667(4) 0.088(2) Uani 1 1 d . . . H64 H 0.3670 0.5364 0.1429 0.105 Uiso 1 1 calc R . . C65 C 0.3175(6) 0.4414(5) 0.1957(5) 0.096(2) Uani 1 1 d . . . H65 H 0.2544 0.4674 0.1910 0.116 Uiso 1 1 calc R . . C66 C 0.3405(4) 0.3615(4) 0.2323(4) 0.0728(17) Uani 1 1 d . . . H66 H 0.2926 0.3351 0.2520 0.087 Uiso 1 1 calc R . . C67 C 0.5072(3) 0.2318(3) 0.3414(3) 0.0443(11) Uani 1 1 d . . . C68 C 0.6008(4) 0.1873(3) 0.3439(3) 0.0544(13) Uani 1 1 d . . . H68 H 0.6403 0.1533 0.3086 0.065 Uiso 1 1 calc R . . C69 C 0.6367(4) 0.1933(4) 0.3994(3) 0.0671(16) Uani 1 1 d . . . H69 H 0.7002 0.1630 0.4007 0.080 Uiso 1 1 calc R . . C70 C 0.5805(4) 0.2425(4) 0.4518(3) 0.0638(15) Uani 1 1 d . . . H70 H 0.6056 0.2467 0.4880 0.077 Uiso 1 1 calc R . . C71 C 0.4873(5) 0.2854(4) 0.4501(3) 0.0698(17) Uani 1 1 d . . . H71 H 0.4481 0.3188 0.4859 0.084 Uiso 1 1 calc R . . C72 C 0.4500(4) 0.2801(4) 0.3960(3) 0.0582(14) Uani 1 1 d . . . H72 H 0.3857 0.3094 0.3963 0.070 Uiso 1 1 calc R . . C73 C 0.4530(3) -0.1154(3) 0.2468(3) 0.0452(11) Uani 1 1 d . . . C74 C 0.4157(4) -0.1688(4) 0.3047(3) 0.0665(16) Uani 1 1 d . . . H74 H 0.4519 -0.2004 0.3380 0.080 Uiso 1 1 calc R . . C75 C 0.3245(5) -0.1763(4) 0.3142(4) 0.0740(18) Uani 1 1 d . . . H75 H 0.2996 -0.2120 0.3540 0.089 Uiso 1 1 calc R . . C76 C 0.2720(4) -0.1314(4) 0.2649(4) 0.0653(16) Uani 1 1 d . . . H76 H 0.2114 -0.1368 0.2709 0.078 Uiso 1 1 calc R . . C77 C 0.3075(4) -0.0788(4) 0.2073(3) 0.0601(14) Uani 1 1 d . . . H77 H 0.2710 -0.0483 0.1739 0.072 Uiso 1 1 calc R . . C78 C 0.3975(4) -0.0700(3) 0.1976(3) 0.0519(13) Uani 1 1 d . . . H78 H 0.4210 -0.0334 0.1580 0.062 Uiso 1 1 calc R . . C79 C 0.6345(4) -0.1842(3) 0.2067(3) 0.0560(13) Uani 1 1 d . . . C80 C 0.6206(5) -0.2254(4) 0.1615(4) 0.084(2) Uani 1 1 d . . . H80 H 0.5602 -0.2092 0.1518 0.101 Uiso 1 1 calc R . . C81 C 0.6937(6) -0.2903(5) 0.1302(5) 0.110(3) Uani 1 1 d . . . H81 H 0.6834 -0.3150 0.0977 0.132 Uiso 1 1 calc R . . C82 C 0.7795(7) -0.3173(5) 0.1468(6) 0.121(3) Uani 1 1 d . . . H82 H 0.8268 -0.3639 0.1295 0.146 Uiso 1 1 calc R . . C83 C 0.7974(6) -0.2758(7) 0.1896(6) 0.154(5) Uani 1 1 d . . . H83 H 0.8590 -0.2907 0.1970 0.185 Uiso 1 1 calc R . . C84 C 0.7231(5) -0.2115(6) 0.2217(5) 0.117(3) Uani 1 1 d . . . H84 H 0.7338 -0.1867 0.2539 0.141 Uiso 1 1 calc R . . C85 C 0.6903(3) 0.0247(3) 0.0373(3) 0.0514(12) Uani 1 1 d . . . C86 C 0.7732(4) -0.0370(4) 0.0467(4) 0.0769(18) Uani 1 1 d . . . H86 H 0.8124 -0.0284 0.0702 0.092 Uiso 1 1 calc R . . C87 C 0.8003(6) -0.1108(5) 0.0226(5) 0.100(2) Uani 1 1 d . . . H87 H 0.8564 -0.1515 0.0307 0.120 Uiso 1 1 calc R . . C88 C 0.7458(7) -0.1247(5) -0.0127(4) 0.101(3) Uani 1 1 d . . . H88 H 0.7659 -0.1737 -0.0312 0.121 Uiso 1 1 calc R . . C89 C 0.6604(6) -0.0657(5) -0.0210(4) 0.084(2) Uani 1 1 d . . . H89 H 0.6213 -0.0757 -0.0436 0.100 Uiso 1 1 calc R . . C90 C 0.6325(4) 0.0085(4) 0.0040(3) 0.0629(15) Uani 1 1 d . . . H90 H 0.5744 0.0479 -0.0017 0.075 Uiso 1 1 calc R . . C91 C 0.7548(4) 0.1429(3) 0.0711(3) 0.0534(13) Uani 1 1 d . . . C92 C 0.8346(4) 0.1305(5) 0.0090(4) 0.085(2) Uani 1 1 d . . . H92 H 0.8345 0.1049 -0.0274 0.103 Uiso 1 1 calc R . . C93 C 0.9128(5) 0.1554(6) 0.0008(4) 0.104(3) Uani 1 1 d . . . H93 H 0.9650 0.1475 -0.0413 0.125 Uiso 1 1 calc R . . C94 C 0.9149(5) 0.1928(5) 0.0555(4) 0.093(2) Uani 1 1 d . . . H94 H 0.9689 0.2088 0.0503 0.111 Uiso 1 1 calc R . . C95 C 0.8377(4) 0.2058(4) 0.1166(4) 0.0729(17) Uani 1 1 d . . . H95 H 0.8385 0.2313 0.1529 0.087 Uiso 1 1 calc R . . C96 C 0.7582(4) 0.1809(4) 0.1242(3) 0.0607(14) Uani 1 1 d . . . H96 H 0.7058 0.1898 0.1661 0.073 Uiso 1 1 calc R . . C97 C 0.5855(3) 0.1997(3) 0.0206(3) 0.0481(12) Uani 1 1 d . . . C98 C 0.6112(4) 0.2013(4) -0.0557(3) 0.0622(15) Uani 1 1 d . . . H98 H 0.6592 0.1570 -0.0764 0.075 Uiso 1 1 calc R . . C99 C 0.5668(5) 0.2674(4) -0.1012(3) 0.0727(17) Uani 1 1 d . . . H99 H 0.5821 0.2665 -0.1518 0.087 Uiso 1 1 calc R . . C100 C 0.4995(5) 0.3345(4) -0.0704(4) 0.0786(19) Uani 1 1 d . . . H100 H 0.4707 0.3802 -0.1007 0.094 Uiso 1 1 calc R . . C101 C 0.4750(5) 0.3347(4) 0.0030(4) 0.0784(18) Uani 1 1 d . . . H101 H 0.4293 0.3804 0.0230 0.094 Uiso 1 1 calc R . . C102 C 0.5173(4) 0.2671(4) 0.0495(3) 0.0642(15) Uani 1 1 d . . . H102 H 0.4993 0.2677 0.1003 0.077 Uiso 1 1 calc R . . Cl6 Cl 0.7391(5) 0.4625(4) 0.0848(4) 0.319(3) Uiso 1 1 d D . . Cl5 Cl 0.7225(9) 0.3936(8) -0.0129(7) 0.492(6) Uiso 1 1 d D . . C103 C 0.776(2) 0.4529(18) -0.0063(13) 0.401(16) Uiso 1 1 d D . . H10A H 0.7578 0.5058 -0.0366 0.481 Uiso 1 1 calc R . . H10B H 0.8464 0.4292 -0.0220 0.481 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0402(2) 0.0419(2) 0.0438(2) -0.01244(18) -0.00981(16) -0.01557(17) Ru2 0.0368(2) 0.0467(2) 0.0395(2) -0.00980(17) -0.01062(16) -0.01526(16) Cl1 0.0488(7) 0.0627(8) 0.0561(8) -0.0125(6) -0.0120(6) -0.0277(6) Cl2 0.0496(7) 0.0687(9) 0.0600(8) -0.0014(7) -0.0148(6) -0.0307(6) Cl3 0.0459(6) 0.0568(8) 0.0601(8) -0.0043(6) -0.0232(6) -0.0177(5) Cl4 0.0441(6) 0.0572(8) 0.0599(8) -0.0147(6) -0.0220(5) -0.0131(5) P1 0.0499(7) 0.0418(7) 0.0527(8) -0.0096(6) -0.0164(6) -0.0130(6) P2 0.0416(6) 0.0557(8) 0.0378(7) -0.0095(6) -0.0084(5) -0.0187(6) O1 0.0476(18) 0.053(2) 0.049(2) -0.0168(16) -0.0150(15) -0.0127(15) O2 0.0520(18) 0.0407(18) 0.0362(18) -0.0048(14) -0.0145(14) -0.0147(14) O3 0.0398(17) 0.051(2) 0.0443(19) -0.0152(15) -0.0046(14) -0.0176(14) O4 0.0482(18) 0.0451(19) 0.0432(19) -0.0060(15) -0.0109(14) -0.0188(15) N1 0.046(2) 0.043(2) 0.042(2) -0.0135(19) -0.0130(17) -0.0182(17) N2 0.049(2) 0.055(3) 0.041(2) -0.011(2) -0.0107(18) -0.0245(19) C1 0.042(3) 0.050(3) 0.042(3) -0.017(2) -0.008(2) -0.013(2) C2 0.038(2) 0.057(3) 0.043(3) -0.025(2) -0.001(2) -0.012(2) C3 0.047(3) 0.049(3) 0.052(3) -0.017(2) -0.016(2) -0.015(2) C4 0.055(3) 0.057(4) 0.064(4) -0.028(3) -0.016(3) -0.003(3) C5 0.071(4) 0.047(3) 0.075(4) -0.015(3) -0.031(3) -0.011(3) C6 0.066(3) 0.044(3) 0.058(3) -0.012(3) -0.023(3) -0.013(2) C7 0.057(3) 0.043(3) 0.041(3) -0.004(2) -0.017(2) -0.023(2) C8 0.057(3) 0.038(3) 0.041(3) -0.001(2) -0.017(2) -0.020(2) C9 0.050(3) 0.042(3) 0.037(3) -0.006(2) -0.012(2) -0.017(2) C10 0.049(3) 0.051(3) 0.046(3) -0.013(2) -0.017(2) -0.016(2) C11 0.061(3) 0.063(4) 0.054(3) -0.012(3) -0.014(3) -0.027(3) C12 0.067(4) 0.068(4) 0.076(4) -0.009(3) -0.025(3) -0.034(3) C13 0.079(4) 0.057(4) 0.090(5) -0.008(3) -0.038(4) -0.031(3) C14 0.078(4) 0.059(4) 0.091(5) -0.033(3) -0.023(3) -0.018(3) C15 0.055(3) 0.063(4) 0.077(4) -0.027(3) -0.009(3) -0.019(3) C16 0.063(3) 0.051(3) 0.043(3) -0.015(2) -0.013(2) -0.023(2) C17 0.054(3) 0.071(4) 0.066(4) -0.020(3) -0.002(3) -0.023(3) C18 0.078(4) 0.090(5) 0.068(4) -0.007(4) 0.008(4) -0.044(4) C19 0.146(7) 0.083(5) 0.054(4) 0.004(4) -0.016(4) -0.059(5) C20 0.135(7) 0.097(6) 0.084(5) 0.025(4) -0.057(5) -0.063(5) C21 0.093(5) 0.090(5) 0.064(4) 0.008(4) -0.035(3) -0.051(4) C22 0.055(3) 0.047(3) 0.035(3) -0.009(2) -0.010(2) -0.022(2) C23 0.060(3) 0.048(3) 0.044(3) -0.003(2) -0.020(2) -0.017(2) C24 0.056(3) 0.070(4) 0.055(3) -0.010(3) -0.024(3) -0.014(3) C25 0.061(3) 0.087(5) 0.053(3) -0.003(3) -0.023(3) -0.032(3) C26 0.061(3) 0.078(4) 0.057(4) -0.003(3) -0.017(3) -0.040(3) C27 0.056(3) 0.053(3) 0.049(3) -0.004(2) -0.020(2) -0.023(2) C28 0.059(3) 0.049(3) 0.043(3) -0.014(2) -0.004(2) -0.028(2) C29 0.074(4) 0.078(4) 0.044(3) -0.009(3) -0.008(3) -0.026(3) C30 0.101(5) 0.111(6) 0.041(3) -0.015(3) -0.002(3) -0.061(5) C31 0.094(5) 0.102(6) 0.073(5) -0.047(5) 0.029(4) -0.061(5) C32 0.083(5) 0.081(5) 0.073(5) -0.025(4) 0.018(4) -0.023(4) C33 0.068(4) 0.058(4) 0.067(4) -0.014(3) 0.003(3) -0.019(3) C34 0.064(3) 0.046(3) 0.055(3) -0.013(3) -0.016(3) -0.003(3) C35 0.113(5) 0.042(3) 0.073(4) -0.012(3) -0.039(4) -0.014(3) C36 0.217(11) 0.044(4) 0.084(6) -0.011(4) -0.076(7) -0.024(5) C37 0.216(13) 0.066(5) 0.064(6) -0.024(4) -0.001(7) 0.022(7) C38 0.128(8) 0.133(9) 0.079(7) -0.031(6) -0.013(6) 0.016(6) C39 0.085(5) 0.100(6) 0.075(5) -0.026(4) -0.012(4) 0.001(4) C40 0.060(3) 0.040(3) 0.068(4) -0.008(3) -0.026(3) -0.013(2) C41 0.131(6) 0.055(4) 0.071(4) -0.002(3) -0.038(4) -0.041(4) C42 0.144(7) 0.064(4) 0.092(6) 0.003(4) -0.049(5) -0.057(5) C43 0.076(4) 0.065(5) 0.119(7) 0.017(4) -0.038(4) -0.038(3) C44 0.099(5) 0.072(5) 0.079(5) -0.005(4) 0.016(4) -0.034(4) C45 0.102(5) 0.062(4) 0.074(5) -0.022(3) 0.003(4) -0.037(4) C46 0.066(3) 0.065(4) 0.064(4) -0.003(3) -0.027(3) -0.024(3) C47 0.099(5) 0.077(5) 0.121(7) -0.005(4) -0.062(5) -0.011(4) C48 0.102(6) 0.107(7) 0.181(10) 0.013(6) -0.093(7) -0.016(5) C49 0.102(7) 0.160(10) 0.153(9) 0.038(8) -0.077(6) -0.053(7) C50 0.137(7) 0.135(8) 0.147(8) 0.034(6) -0.099(7) -0.079(6) C51 0.085(5) 0.084(5) 0.095(5) 0.011(4) -0.049(4) -0.038(4) C52 0.040(2) 0.048(3) 0.045(3) -0.012(2) -0.008(2) -0.015(2) C53 0.046(3) 0.056(3) 0.050(3) -0.024(3) -0.002(2) -0.019(2) C54 0.046(3) 0.062(3) 0.051(3) -0.020(3) -0.002(2) -0.030(2) C55 0.087(4) 0.071(4) 0.050(3) -0.022(3) 0.010(3) -0.042(3) C56 0.119(6) 0.092(5) 0.050(4) -0.018(4) 0.012(4) -0.058(5) C57 0.090(4) 0.069(4) 0.055(4) -0.011(3) -0.001(3) -0.042(3) C58 0.058(3) 0.056(3) 0.038(3) -0.008(2) -0.011(2) -0.028(2) C59 0.057(3) 0.050(3) 0.042(3) 0.004(2) -0.020(2) -0.025(2) C60 0.051(3) 0.040(3) 0.048(3) -0.005(2) -0.015(2) -0.016(2) C61 0.051(3) 0.051(3) 0.047(3) -0.015(2) -0.014(2) -0.014(2) C62 0.072(4) 0.062(4) 0.083(4) -0.001(3) -0.032(3) -0.028(3) C63 0.101(5) 0.059(4) 0.104(6) 0.007(4) -0.039(4) -0.033(4) C64 0.107(6) 0.057(4) 0.090(5) -0.006(4) -0.026(4) -0.017(4) C65 0.087(5) 0.074(5) 0.110(6) -0.011(5) -0.044(5) 0.011(4) C66 0.059(4) 0.068(4) 0.089(5) -0.015(4) -0.025(3) -0.009(3) C67 0.049(3) 0.045(3) 0.043(3) -0.010(2) -0.008(2) -0.021(2) C68 0.052(3) 0.065(4) 0.055(3) -0.018(3) -0.015(2) -0.021(3) C69 0.064(4) 0.084(4) 0.067(4) -0.011(3) -0.029(3) -0.028(3) C70 0.075(4) 0.084(4) 0.052(3) -0.010(3) -0.021(3) -0.042(3) C71 0.078(4) 0.088(5) 0.054(4) -0.030(3) -0.008(3) -0.033(4) C72 0.054(3) 0.068(4) 0.058(3) -0.018(3) -0.011(3) -0.023(3) C73 0.049(3) 0.043(3) 0.050(3) -0.010(2) -0.013(2) -0.019(2) C74 0.078(4) 0.072(4) 0.064(4) 0.003(3) -0.029(3) -0.038(3) C75 0.081(4) 0.086(5) 0.065(4) -0.010(4) -0.001(3) -0.055(4) C76 0.057(3) 0.079(4) 0.072(4) -0.031(4) -0.006(3) -0.032(3) C77 0.055(3) 0.063(4) 0.071(4) -0.026(3) -0.018(3) -0.016(3) C78 0.052(3) 0.055(3) 0.057(3) -0.013(3) -0.015(2) -0.023(2) C79 0.063(3) 0.050(3) 0.050(3) -0.008(3) -0.017(3) -0.010(3) C80 0.070(4) 0.078(5) 0.106(6) -0.045(4) -0.014(4) -0.011(3) C81 0.109(6) 0.083(6) 0.132(8) -0.061(5) -0.009(5) -0.013(5) C82 0.120(7) 0.088(6) 0.118(8) -0.045(5) -0.028(6) 0.030(5) C83 0.097(6) 0.186(11) 0.136(9) -0.077(8) -0.059(6) 0.070(7) C84 0.080(5) 0.149(8) 0.117(7) -0.077(6) -0.048(5) 0.031(5) C85 0.049(3) 0.060(3) 0.042(3) -0.015(2) 0.000(2) -0.018(2) C86 0.056(3) 0.084(5) 0.085(5) -0.041(4) -0.006(3) -0.007(3) C87 0.089(5) 0.085(6) 0.106(6) -0.048(5) 0.000(4) -0.004(4) C88 0.146(8) 0.078(5) 0.072(5) -0.040(4) 0.010(5) -0.041(5) C89 0.125(6) 0.084(5) 0.058(4) -0.017(4) -0.020(4) -0.049(5) C90 0.082(4) 0.064(4) 0.050(3) -0.004(3) -0.022(3) -0.030(3) C91 0.047(3) 0.068(4) 0.046(3) -0.004(3) -0.012(2) -0.023(2) C92 0.067(4) 0.147(7) 0.061(4) -0.030(4) -0.001(3) -0.058(4) C93 0.065(4) 0.190(9) 0.072(5) -0.033(5) 0.007(3) -0.069(5) C94 0.068(4) 0.143(7) 0.084(5) -0.011(5) -0.013(4) -0.062(4) C95 0.074(4) 0.098(5) 0.070(4) -0.009(4) -0.022(3) -0.052(4) C96 0.065(3) 0.070(4) 0.056(3) -0.008(3) -0.016(3) -0.031(3) C97 0.047(3) 0.055(3) 0.047(3) -0.007(2) -0.013(2) -0.022(2) C98 0.071(4) 0.068(4) 0.049(3) -0.008(3) -0.012(3) -0.028(3) C99 0.093(5) 0.081(5) 0.049(4) 0.015(3) -0.029(3) -0.039(4) C100 0.088(5) 0.072(5) 0.072(5) 0.018(4) -0.033(4) -0.030(4) C101 0.082(4) 0.058(4) 0.086(5) -0.004(4) -0.027(4) -0.009(3) C102 0.074(4) 0.064(4) 0.052(3) -0.007(3) -0.015(3) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 1.974(3) . ? Ru1 O2 2.123(3) . ? Ru1 N1 2.170(4) . ? Ru1 P1 2.3475(15) . ? Ru1 Cl1 2.3580(12) . ? Ru1 Cl2 2.3917(13) . ? Ru2 O3 1.943(3) . ? Ru2 O4 2.171(3) . ? Ru2 N2 2.171(4) . ? Ru2 P2 2.3387(14) . ? Ru2 Cl4 2.3625(12) . ? Ru2 Cl3 2.3891(13) . ? P1 C34 1.822(6) . ? P1 C40 1.826(6) . ? P1 C46 1.827(6) . ? P2 C85 1.822(5) . ? P2 C91 1.824(5) . ? P2 C97 1.827(5) . ? O1 C1 1.434(5) . ? O2 C9 1.452(5) . ? O3 C52 1.426(5) . ? O4 C60 1.479(6) . ? N1 C7 1.351(6) . ? N1 C3 1.372(6) . ? N2 C54 1.348(6) . ? N2 C58 1.357(6) . ? C1 C2 1.535(6) . ? C1 C10 1.541(6) . ? C1 C16 1.543(7) . ? C2 C3 1.481(7) . ? C3 C4 1.389(7) . ? C4 C5 1.376(8) . ? C5 C6 1.369(8) . ? C6 C7 1.394(7) . ? C7 C8 1.492(7) . ? C8 C9 1.547(6) . ? C9 C22 1.520(7) . ? C9 C28 1.543(7) . ? C10 C15 1.365(7) . ? C10 C11 1.376(7) . ? C11 C12 1.390(7) . ? C12 C13 1.358(8) . ? C13 C14 1.402(8) . ? C14 C15 1.372(8) . ? C16 C17 1.369(7) . ? C16 C21 1.385(8) . ? C17 C18 1.394(9) . ? C18 C19 1.350(10) . ? C19 C20 1.392(10) . ? C20 C21 1.365(9) . ? C22 C23 1.383(7) . ? C22 C27 1.398(7) . ? C23 C24 1.379(7) . ? C24 C25 1.370(8) . ? C25 C26 1.369(8) . ? C26 C27 1.379(7) . ? C28 C33 1.373(8) . ? C28 C29 1.383(8) . ? C29 C30 1.397(8) . ? C30 C31 1.359(10) . ? C31 C32 1.357(10) . ? C32 C33 1.381(8) . ? C34 C39 1.384(9) . ? C34 C35 1.390(8) . ? C35 C36 1.398(10) . ? C36 C37 1.365(15) . ? C37 C38 1.335(15) . ? C38 C39 1.363(11) . ? C40 C45 1.361(8) . ? C40 C41 1.384(8) . ? C41 C42 1.394(10) . ? C42 C43 1.357(10) . ? C43 C44 1.370(9) . ? C44 C45 1.391(9) . ? C46 C51 1.365(8) . ? C46 C47 1.417(9) . ? C47 C48 1.376(10) . ? C48 C49 1.369(13) . ? C49 C50 1.447(13) . ? C50 C51 1.384(9) . ? C52 C61 1.538(7) . ? C52 C67 1.540(6) . ? C52 C53 1.542(6) . ? C53 C54 1.498(7) . ? C54 C55 1.373(7) . ? C55 C56 1.367(9) . ? C56 C57 1.374(9) . ? C57 C58 1.382(7) . ? C58 C59 1.482(7) . ? C59 C60 1.539(6) . ? C60 C73 1.516(6) . ? C60 C79 1.534(7) . ? C61 C66 1.369(7) . ? C61 C62 1.373(8) . ? C62 C63 1.378(9) . ? C63 C64 1.381(9) . ? C64 C65 1.342(10) . ? C65 C66 1.386(10) . ? C67 C68 1.372(7) . ? C67 C72 1.386(7) . ? C68 C69 1.398(7) . ? C69 C70 1.361(8) . ? C70 C71 1.358(8) . ? C71 C72 1.383(8) . ? C73 C74 1.376(7) . ? C73 C78 1.387(7) . ? C74 C75 1.392(8) . ? C75 C76 1.358(9) . ? C76 C77 1.354(8) . ? C77 C78 1.383(7) . ? C79 C84 1.366(8) . ? C79 C80 1.377(8) . ? C80 C81 1.384(9) . ? C81 C82 1.341(11) . ? C82 C83 1.378(13) . ? C83 C84 1.389(11) . ? C85 C86 1.374(8) . ? C85 C90 1.387(7) . ? C86 C87 1.372(9) . ? C87 C88 1.351(11) . ? C88 C89 1.376(11) . ? C89 C90 1.385(9) . ? C91 C96 1.385(7) . ? C91 C92 1.396(8) . ? C92 C93 1.362(9) . ? C93 C94 1.394(10) . ? C94 C95 1.364(9) . ? C95 C96 1.384(7) . ? C97 C102 1.371(8) . ? C97 C98 1.390(7) . ? C98 C99 1.379(8) . ? C99 C100 1.378(9) . ? C100 C101 1.344(9) . ? C101 C102 1.393(8) . ? Cl6 C103 1.695(19) . ? Cl5 C103 1.591(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O2 176.89(12) . . ? O1 Ru1 N1 91.86(14) . . ? O2 Ru1 N1 88.49(13) . . ? O1 Ru1 P1 87.55(10) . . ? O2 Ru1 P1 92.08(9) . . ? N1 Ru1 P1 179.30(10) . . ? O1 Ru1 Cl1 96.19(10) . . ? O2 Ru1 Cl1 86.90(9) . . ? N1 Ru1 Cl1 91.58(10) . . ? P1 Ru1 Cl1 88.85(5) . . ? O1 Ru1 Cl2 91.96(10) . . ? O2 Ru1 Cl2 84.95(9) . . ? N1 Ru1 Cl2 89.78(10) . . ? P1 Ru1 Cl2 89.87(5) . . ? Cl1 Ru1 Cl2 171.69(5) . . ? O3 Ru2 O4 179.30(12) . . ? O3 Ru2 N2 92.41(14) . . ? O4 Ru2 N2 87.19(14) . . ? O3 Ru2 P2 88.66(10) . . ? O4 Ru2 P2 91.73(9) . . ? N2 Ru2 P2 178.52(12) . . ? O3 Ru2 Cl4 95.93(10) . . ? O4 Ru2 Cl4 84.66(9) . . ? N2 Ru2 Cl4 91.58(11) . . ? P2 Ru2 Cl4 89.32(5) . . ? O3 Ru2 Cl3 92.41(10) . . ? O4 Ru2 Cl3 87.02(9) . . ? N2 Ru2 Cl3 91.22(11) . . ? P2 Ru2 Cl3 87.72(5) . . ? Cl4 Ru2 Cl3 171.08(5) . . ? C34 P1 C40 106.0(3) . . ? C34 P1 C46 103.0(3) . . ? C40 P1 C46 99.7(3) . . ? C34 P1 Ru1 110.21(18) . . ? C40 P1 Ru1 115.12(18) . . ? C46 P1 Ru1 121.0(2) . . ? C85 P2 C91 104.8(2) . . ? C85 P2 C97 106.2(2) . . ? C91 P2 C97 101.2(2) . . ? C85 P2 Ru2 107.30(17) . . ? C91 P2 Ru2 118.25(17) . . ? C97 P2 Ru2 117.92(17) . . ? C1 O1 Ru1 126.3(3) . . ? C9 O2 Ru1 126.5(3) . . ? C52 O3 Ru2 126.3(3) . . ? C60 O4 Ru2 127.6(3) . . ? C7 N1 C3 120.0(4) . . ? C7 N1 Ru1 122.6(3) . . ? C3 N1 Ru1 117.3(3) . . ? C54 N2 C58 120.4(4) . . ? C54 N2 Ru2 118.0(3) . . ? C58 N2 Ru2 121.6(3) . . ? O1 C1 C2 111.6(4) . . ? O1 C1 C10 110.5(4) . . ? C2 C1 C10 109.5(4) . . ? O1 C1 C16 104.9(4) . . ? C2 C1 C16 111.3(4) . . ? C10 C1 C16 108.9(4) . . ? C3 C2 C1 116.1(4) . . ? N1 C3 C4 120.3(5) . . ? N1 C3 C2 119.9(4) . . ? C4 C3 C2 119.7(5) . . ? C5 C4 C3 120.3(5) . . ? C6 C5 C4 118.4(5) . . ? C5 C6 C7 121.3(5) . . ? N1 C7 C6 119.7(5) . . ? N1 C7 C8 120.9(4) . . ? C6 C7 C8 119.4(4) . . ? C7 C8 C9 117.3(4) . . ? O2 C9 C22 109.9(4) . . ? O2 C9 C28 107.4(4) . . ? C22 C9 C28 109.5(4) . . ? O2 C9 C8 107.5(3) . . ? C22 C9 C8 113.9(4) . . ? C28 C9 C8 108.5(4) . . ? C15 C10 C11 118.4(5) . . ? C15 C10 C1 119.5(4) . . ? C11 C10 C1 122.2(4) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C11 120.7(6) . . ? C12 C13 C14 118.8(5) . . ? C15 C14 C13 119.6(6) . . ? C10 C15 C14 121.8(6) . . ? C17 C16 C21 117.6(5) . . ? C17 C16 C1 124.1(5) . . ? C21 C16 C1 118.2(5) . . ? C16 C17 C18 121.1(6) . . ? C19 C18 C17 120.5(6) . . ? C18 C19 C20 119.3(6) . . ? C21 C20 C19 119.7(7) . . ? C20 C21 C16 121.8(6) . . ? C23 C22 C27 117.4(5) . . ? C23 C22 C9 122.4(4) . . ? C27 C22 C9 120.1(5) . . ? C24 C23 C22 121.2(5) . . ? C25 C24 C23 120.3(5) . . ? C26 C25 C24 119.7(5) . . ? C25 C26 C27 120.2(5) . . ? C26 C27 C22 121.1(5) . . ? C33 C28 C29 117.7(5) . . ? C33 C28 C9 122.5(5) . . ? C29 C28 C9 119.8(5) . . ? C28 C29 C30 120.3(6) . . ? C31 C30 C29 120.4(7) . . ? C32 C31 C30 119.7(6) . . ? C31 C32 C33 120.3(7) . . ? C28 C33 C32 121.5(7) . . ? C39 C34 C35 117.8(6) . . ? C39 C34 P1 121.6(5) . . ? C35 C34 P1 120.4(5) . . ? C34 C35 C36 120.2(7) . . ? C37 C36 C35 119.4(9) . . ? C38 C37 C36 120.3(9) . . ? C37 C38 C39 121.7(10) . . ? C38 C39 C34 120.5(8) . . ? C45 C40 C41 117.9(6) . . ? C45 C40 P1 117.5(4) . . ? C41 C40 P1 124.5(5) . . ? C40 C41 C42 120.4(7) . . ? C43 C42 C41 120.8(6) . . ? C42 C43 C44 119.3(6) . . ? C43 C44 C45 119.9(7) . . ? C40 C45 C44 121.7(6) . . ? C51 C46 C47 118.0(6) . . ? C51 C46 P1 123.4(5) . . ? C47 C46 P1 118.7(5) . . ? C48 C47 C46 121.2(8) . . ? C49 C48 C47 120.4(9) . . ? C48 C49 C50 119.6(8) . . ? C51 C50 C49 117.8(8) . . ? C46 C51 C50 122.8(7) . . ? O3 C52 C61 104.6(4) . . ? O3 C52 C67 111.0(4) . . ? C61 C52 C67 108.7(4) . . ? O3 C52 C53 111.5(4) . . ? C61 C52 C53 110.8(4) . . ? C67 C52 C53 110.2(4) . . ? C54 C53 C52 115.9(4) . . ? N2 C54 C55 121.1(5) . . ? N2 C54 C53 119.5(4) . . ? C55 C54 C53 119.3(5) . . ? C56 C55 C54 119.5(6) . . ? C55 C56 C57 119.1(6) . . ? C56 C57 C58 120.7(6) . . ? N2 C58 C57 119.1(5) . . ? N2 C58 C59 121.4(4) . . ? C57 C58 C59 119.4(5) . . ? C58 C59 C60 117.7(4) . . ? O4 C60 C73 110.0(4) . . ? O4 C60 C79 105.6(4) . . ? C73 C60 C79 112.0(4) . . ? O4 C60 C59 106.9(4) . . ? C73 C60 C59 111.0(4) . . ? C79 C60 C59 111.1(4) . . ? C66 C61 C62 116.7(5) . . ? C66 C61 C52 125.0(5) . . ? C62 C61 C52 118.2(4) . . ? C61 C62 C63 122.3(6) . . ? C62 C63 C64 119.9(7) . . ? C65 C64 C63 118.2(7) . . ? C64 C65 C66 121.8(7) . . ? C61 C66 C65 121.0(6) . . ? C68 C67 C72 118.2(5) . . ? C68 C67 C52 122.3(4) . . ? C72 C67 C52 119.5(4) . . ? C67 C68 C69 119.8(5) . . ? C70 C69 C68 121.4(5) . . ? C71 C70 C69 118.8(5) . . ? C70 C71 C72 120.9(6) . . ? C71 C72 C67 120.8(5) . . ? C74 C73 C78 118.0(5) . . ? C74 C73 C60 119.7(5) . . ? C78 C73 C60 122.2(4) . . ? C73 C74 C75 121.0(6) . . ? C76 C75 C74 119.7(6) . . ? C77 C76 C75 120.4(5) . . ? C76 C77 C78 120.6(6) . . ? C77 C78 C73 120.3(5) . . ? C84 C79 C80 117.4(6) . . ? C84 C79 C60 122.2(5) . . ? C80 C79 C60 120.4(5) . . ? C79 C80 C81 122.0(7) . . ? C82 C81 C80 119.8(8) . . ? C81 C82 C83 119.8(7) . . ? C82 C83 C84 119.7(8) . . ? C79 C84 C83 121.0(8) . . ? C86 C85 C90 117.0(5) . . ? C86 C85 P2 121.2(4) . . ? C90 C85 P2 120.7(4) . . ? C87 C86 C85 122.2(7) . . ? C88 C87 C86 120.4(8) . . ? C87 C88 C89 119.3(7) . . ? C88 C89 C90 120.3(7) . . ? C89 C90 C85 120.7(6) . . ? C96 C91 C92 117.7(5) . . ? C96 C91 P2 119.6(4) . . ? C92 C91 P2 122.7(4) . . ? C93 C92 C91 121.0(6) . . ? C92 C93 C94 120.2(6) . . ? C95 C94 C93 119.9(6) . . ? C94 C95 C96 119.5(6) . . ? C95 C96 C91 121.6(6) . . ? C102 C97 C98 118.3(5) . . ? C102 C97 P2 118.8(4) . . ? C98 C97 P2 122.7(4) . . ? C99 C98 C97 121.4(6) . . ? C100 C99 C98 118.8(6) . . ? C101 C100 C99 120.6(6) . . ? C100 C101 C102 120.7(6) . . ? C97 C102 C101 120.1(6) . . ? Cl5 C103 Cl6 105.1(18) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 1.392 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.135 #------------------------------------------------------------------------------ data_mar116 _database_code_CSD 209730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H53 Cl N O3 P2 Ru' _chemical_formula_sum 'C59 H53 Cl N O3 P2 Ru' _chemical_formula_weight 1022.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.377(10) _cell_length_b 9.4650(19) _cell_length_c 21.639(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.48(3) _cell_angle_gamma 90.00 _cell_volume 9792(3) _cell_formula_units_Z 8 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4232 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'Marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21135 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.47 _reflns_number_total 7761 _reflns_number_gt 5230 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution Shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0907P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7761 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.878710(7) 0.09414(4) 0.02026(2) 0.03159(15) Uani 1 1 d . . . Cl1 Cl 0.88815(3) -0.08339(14) -0.05389(7) 0.0511(4) Uani 1 1 d . . . P1 P 0.86992(3) 0.29078(12) 0.07849(7) 0.0353(3) Uani 1 1 d . . . P2 P 0.88083(3) 0.26874(12) -0.05481(7) 0.0353(3) Uani 1 1 d . . . O1 O 0.83700(6) 0.0601(3) -0.00482(17) 0.0357(8) Uani 1 1 d . . . O2 O 0.91886(6) 0.1503(3) 0.05580(16) 0.0355(8) Uani 1 1 d . . . N1 N 0.88211(8) -0.0671(4) 0.0940(2) 0.0337(9) Uani 1 1 d . . . C1 C 0.82245(9) -0.0691(5) -0.0035(3) 0.0388(12) Uani 1 1 d . . . C2 C 0.84323(10) -0.1925(4) 0.0217(3) 0.0411(13) Uani 1 1 d . . . H2A H 0.8326 -0.2785 0.0224 0.049 Uiso 1 1 calc R . . H2B H 0.8549 -0.2070 -0.0077 0.049 Uiso 1 1 calc R . . C3 C 0.86150(10) -0.1665(5) 0.0868(3) 0.0385(13) Uani 1 1 d . . . C4 C 0.85858(11) -0.2461(5) 0.1381(3) 0.0504(15) Uani 1 1 d . . . H4 H 0.8436 -0.3081 0.1333 0.061 Uiso 1 1 calc R . . C5 C 0.87751(12) -0.2347(6) 0.1958(3) 0.0569(16) Uani 1 1 d . . . H5 H 0.8753 -0.2844 0.2313 0.068 Uiso 1 1 calc R . . C6 C 0.90002(11) -0.1466(6) 0.1994(3) 0.0506(15) Uani 1 1 d . . . H6 H 0.9141 -0.1435 0.2370 0.061 Uiso 1 1 calc R . . C7 C 0.90224(10) -0.0625(5) 0.1487(3) 0.0360(12) Uani 1 1 d . . . C8 C 0.92742(9) 0.0296(5) 0.1560(3) 0.0400(12) Uani 1 1 d . . . H8A H 0.9425 -0.0143 0.1876 0.048 Uiso 1 1 calc R . . H8B H 0.9233 0.1186 0.1740 0.048 Uiso 1 1 calc R . . C9 C 0.93851(9) 0.0639(5) 0.0983(3) 0.0347(11) Uani 1 1 d . . . C10 C 0.80497(10) -0.0971(5) -0.0717(3) 0.0444(13) Uani 1 1 d . . . C11 C 0.80779(13) -0.2126(7) -0.1077(3) 0.0693(19) Uani 1 1 d . . . H11 H 0.8212 -0.2805 -0.0906 0.083 Uiso 1 1 calc R . . C12 C 0.79103(16) -0.2307(8) -0.1693(4) 0.086(2) Uani 1 1 d . . . H12 H 0.7933 -0.3095 -0.1932 0.103 Uiso 1 1 calc R . . C13 C 0.77130(15) -0.1320(9) -0.1944(4) 0.082(2) Uani 1 1 d . . . H13 H 0.7598 -0.1447 -0.2352 0.099 Uiso 1 1 calc R . . C14 C 0.76822(12) -0.0143(8) -0.1600(3) 0.0704(19) Uani 1 1 d . . . H14 H 0.7548 0.0534 -0.1775 0.085 Uiso 1 1 calc R . . C15 C 0.78500(11) 0.0027(6) -0.1000(3) 0.0532(15) Uani 1 1 d . . . H15 H 0.7830 0.0837 -0.0772 0.064 Uiso 1 1 calc R . . C16 C 0.80300(9) -0.0608(5) 0.0416(3) 0.0385(12) Uani 1 1 d . . . C17 C 0.78499(11) -0.1737(5) 0.0446(3) 0.0469(14) Uani 1 1 d . . . H17 H 0.7840 -0.2501 0.0171 0.056 Uiso 1 1 calc R . . C18 C 0.76878(11) -0.1727(6) 0.0876(3) 0.0535(15) Uani 1 1 d . . . H18 H 0.7570 -0.2487 0.0891 0.064 Uiso 1 1 calc R . . C19 C 0.76970(11) -0.0596(6) 0.1291(3) 0.0524(15) Uani 1 1 d . . . H19 H 0.7587 -0.0595 0.1582 0.063 Uiso 1 1 calc R . . C20 C 0.78726(12) 0.0527(6) 0.1263(3) 0.0585(16) Uani 1 1 d . . . H20 H 0.7880 0.1293 0.1536 0.070 Uiso 1 1 calc R . . C21 C 0.80364(11) 0.0514(5) 0.0832(3) 0.0486(14) Uani 1 1 d . . . H21 H 0.8154 0.1275 0.0820 0.058 Uiso 1 1 calc R . . C22 C 0.94638(9) -0.0629(5) 0.0646(3) 0.0391(13) Uani 1 1 d . . . C23 C 0.94398(10) -0.2015(5) 0.0825(3) 0.0486(14) Uani 1 1 d . . . H23 H 0.9370 -0.2217 0.1176 0.058 Uiso 1 1 calc R . . C24 C 0.95208(12) -0.3115(6) 0.0477(4) 0.0622(18) Uani 1 1 d . . . H24 H 0.9502 -0.4047 0.0594 0.075 Uiso 1 1 calc R . . C25 C 0.96272(12) -0.2833(6) -0.0031(4) 0.068(2) Uani 1 1 d . . . H25 H 0.9678 -0.3578 -0.0260 0.082 Uiso 1 1 calc R . . C26 C 0.96619(12) -0.1464(6) -0.0214(3) 0.0611(17) Uani 1 1 d . . . H26 H 0.9740 -0.1273 -0.0554 0.073 Uiso 1 1 calc R . . C27 C 0.95760(11) -0.0372(6) 0.0127(3) 0.0497(14) Uani 1 1 d . . . H27 H 0.9594 0.0557 0.0004 0.060 Uiso 1 1 calc R . . C28 C 0.96529(10) 0.1516(5) 0.1238(3) 0.0413(13) Uani 1 1 d . . . C29 C 0.98914(11) 0.0911(6) 0.1602(3) 0.0533(15) Uani 1 1 d . . . H29 H 0.9891 -0.0039 0.1711 0.064 Uiso 1 1 calc R . . C30 C 1.01362(11) 0.1701(8) 0.1813(3) 0.0677(19) Uani 1 1 d . . . H30 H 1.0295 0.1267 0.2062 0.081 Uiso 1 1 calc R . . C31 C 1.01467(13) 0.3056(7) 0.1665(4) 0.079(2) Uani 1 1 d . . . H31 H 1.0311 0.3573 0.1805 0.095 Uiso 1 1 calc R . . C32 C 0.99168(14) 0.3653(7) 0.1313(5) 0.128(4) Uani 1 1 d . . . H32 H 0.9920 0.4607 0.1212 0.154 Uiso 1 1 calc R . . C33 C 0.96726(13) 0.2905(7) 0.1092(4) 0.094(3) Uani 1 1 d . . . H33 H 0.9517 0.3359 0.0837 0.113 Uiso 1 1 calc R . . C34 C 0.88858(10) 0.4394(5) 0.0526(3) 0.0431(13) Uani 1 1 d . . . H34A H 0.8839 0.5270 0.0707 0.052 Uiso 1 1 calc R . . H34B H 0.9086 0.4252 0.0672 0.052 Uiso 1 1 calc R . . C35 C 0.88005(11) 0.4473(5) -0.0195(3) 0.0441(13) Uani 1 1 d . . . H35A H 0.8927 0.5095 -0.0343 0.053 Uiso 1 1 calc R . . H35B H 0.8613 0.4862 -0.0333 0.053 Uiso 1 1 calc R . . C36 C 0.87996(10) 0.2912(5) 0.1654(3) 0.0431(13) Uani 1 1 d . . . C37 C 0.86870(11) 0.1886(6) 0.1990(3) 0.0527(15) Uani 1 1 d . . . H37 H 0.8562 0.1223 0.1764 0.063 Uiso 1 1 calc R . . C38 C 0.87599(15) 0.1848(8) 0.2652(3) 0.0704(19) Uani 1 1 d . . . H38 H 0.8682 0.1169 0.2865 0.085 Uiso 1 1 calc R . . C39 C 0.89438(17) 0.2791(9) 0.2986(4) 0.085(2) Uani 1 1 d . . . H39 H 0.8995 0.2738 0.3429 0.102 Uiso 1 1 calc R . . C40 C 0.90552(14) 0.3819(8) 0.2685(4) 0.073(2) Uani 1 1 d . . . H40 H 0.9177 0.4480 0.2923 0.088 Uiso 1 1 calc R . . C41 C 0.89851(11) 0.3884(6) 0.2006(3) 0.0547(15) Uani 1 1 d . . . H41 H 0.9064 0.4576 0.1799 0.066 Uiso 1 1 calc R . . C42 C 0.83385(9) 0.3566(5) 0.0600(3) 0.0389(13) Uani 1 1 d . . . C43 C 0.82232(10) 0.4144(5) 0.1070(3) 0.0466(14) Uani 1 1 d . . . H43 H 0.8332 0.4238 0.1486 0.056 Uiso 1 1 calc R . . C44 C 0.79474(12) 0.4577(6) 0.0914(3) 0.0575(17) Uani 1 1 d . . . H44 H 0.7871 0.4950 0.1230 0.069 Uiso 1 1 calc R . . C45 C 0.77847(12) 0.4466(6) 0.0304(4) 0.0626(18) Uani 1 1 d . . . H45 H 0.7598 0.4744 0.0207 0.075 Uiso 1 1 calc R . . C46 C 0.78993(11) 0.3943(6) -0.0164(3) 0.0575(16) Uani 1 1 d . . . H46 H 0.7792 0.3904 -0.0583 0.069 Uiso 1 1 calc R . . C47 C 0.81743(10) 0.3469(5) -0.0020(3) 0.0461(14) Uani 1 1 d . . . H47 H 0.8248 0.3087 -0.0338 0.055 Uiso 1 1 calc R . . C48 C 0.85458(10) 0.2809(5) -0.1305(3) 0.0413(13) Uani 1 1 d . . . C49 C 0.83952(12) 0.1622(6) -0.1576(3) 0.0583(16) Uani 1 1 d . . . H49 H 0.8426 0.0769 -0.1356 0.070 Uiso 1 1 calc R . . C50 C 0.82059(13) 0.1665(8) -0.2148(3) 0.077(2) Uani 1 1 d . . . H50 H 0.8113 0.0847 -0.2323 0.092 Uiso 1 1 calc R . . C51 C 0.81516(14) 0.2921(9) -0.2469(4) 0.080(2) Uani 1 1 d . . . H51 H 0.8020 0.2967 -0.2859 0.096 Uiso 1 1 calc R . . C52 C 0.82977(15) 0.4146(8) -0.2199(3) 0.072(2) Uani 1 1 d . . . H52 H 0.8260 0.5010 -0.2408 0.087 Uiso 1 1 calc R . . C53 C 0.84950(12) 0.4059(6) -0.1632(3) 0.0569(15) Uani 1 1 d . . . H53 H 0.8596 0.4860 -0.1466 0.068 Uiso 1 1 calc R . . C54 C 0.91344(10) 0.2646(5) -0.0797(3) 0.0425(13) Uani 1 1 d . . . C55 C 0.91759(12) 0.1615(6) -0.1209(3) 0.0566(15) Uani 1 1 d . . . H55 H 0.9029 0.1021 -0.1401 0.068 Uiso 1 1 calc R . . C56 C 0.94356(14) 0.1443(7) -0.1344(3) 0.0698(19) Uani 1 1 d . . . H56 H 0.9461 0.0729 -0.1620 0.084 Uiso 1 1 calc R . . C57 C 0.96538(14) 0.2318(8) -0.1073(4) 0.082(2) Uani 1 1 d . . . H57 H 0.9828 0.2204 -0.1158 0.098 Uiso 1 1 calc R . . C58 C 0.96093(14) 0.3349(8) -0.0681(5) 0.094(3) Uani 1 1 d . . . H58 H 0.9755 0.3960 -0.0499 0.113 Uiso 1 1 calc R . . C59 C 0.93533(12) 0.3525(6) -0.0540(4) 0.0659(19) Uani 1 1 d . . . H59 H 0.9330 0.4249 -0.0267 0.079 Uiso 1 1 calc R . . O3 O 0.97064(16) -0.3277(7) 0.2408(3) 0.169(3) 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 Ru1 0.0267(2) 0.0330(2) 0.0350(3) -0.00014(17) 0.00757(16) 0.00057(15) Cl1 0.0479(8) 0.0559(8) 0.0514(10) -0.0125(7) 0.0158(7) 0.0023(6) P1 0.0305(7) 0.0344(7) 0.0416(9) -0.0026(6) 0.0101(6) 0.0014(5) P2 0.0340(7) 0.0360(7) 0.0366(9) 0.0041(5) 0.0101(6) 0.0009(5) O1 0.0261(17) 0.0361(17) 0.045(2) -0.0012(15) 0.0099(15) -0.0005(12) O2 0.0280(17) 0.0350(17) 0.041(2) 0.0035(15) 0.0043(15) 0.0004(13) N1 0.032(2) 0.035(2) 0.035(3) 0.0036(17) 0.0110(19) 0.0042(16) C1 0.030(3) 0.041(3) 0.044(4) 0.002(2) 0.008(2) -0.007(2) C2 0.035(3) 0.029(3) 0.058(4) -0.007(2) 0.012(3) -0.0028(19) C3 0.035(3) 0.032(3) 0.050(4) 0.000(2) 0.013(3) 0.005(2) C4 0.045(3) 0.047(3) 0.063(5) 0.014(3) 0.020(3) -0.006(2) C5 0.054(4) 0.062(4) 0.059(5) 0.020(3) 0.023(3) -0.001(3) C6 0.044(3) 0.056(3) 0.049(4) 0.011(3) 0.006(3) 0.005(2) C7 0.034(3) 0.037(3) 0.037(3) 0.005(2) 0.008(2) 0.0030(19) C8 0.033(3) 0.045(3) 0.038(4) -0.001(2) 0.003(2) 0.002(2) C9 0.027(2) 0.039(3) 0.036(3) 0.002(2) 0.006(2) 0.0019(19) C10 0.031(3) 0.057(3) 0.044(4) -0.008(3) 0.007(2) -0.014(2) C11 0.064(4) 0.076(4) 0.064(5) -0.022(4) 0.010(4) 0.000(3) C12 0.081(5) 0.106(6) 0.065(6) -0.032(4) 0.007(4) -0.008(4) C13 0.064(5) 0.132(7) 0.048(5) -0.007(5) 0.006(4) -0.032(5) C14 0.047(4) 0.101(5) 0.056(5) 0.011(4) 0.001(3) -0.011(3) C15 0.046(3) 0.073(4) 0.040(4) 0.000(3) 0.011(3) -0.004(3) C16 0.027(3) 0.044(3) 0.043(4) 0.001(2) 0.006(2) 0.0034(19) C17 0.044(3) 0.051(3) 0.046(4) -0.002(3) 0.012(3) -0.008(2) C18 0.035(3) 0.064(4) 0.060(5) 0.008(3) 0.009(3) -0.012(2) C19 0.043(3) 0.069(4) 0.048(4) 0.006(3) 0.017(3) 0.003(3) C20 0.063(4) 0.056(3) 0.065(5) -0.008(3) 0.032(3) -0.005(3) C21 0.048(3) 0.043(3) 0.057(4) -0.003(3) 0.018(3) -0.011(2) C22 0.028(3) 0.044(3) 0.043(4) -0.003(2) 0.004(2) -0.001(2) C23 0.043(3) 0.042(3) 0.062(4) 0.006(3) 0.016(3) 0.001(2) C24 0.055(4) 0.046(3) 0.090(6) -0.004(3) 0.025(4) 0.002(3) C25 0.053(4) 0.062(4) 0.093(6) -0.029(4) 0.024(4) 0.004(3) C26 0.065(4) 0.064(4) 0.061(5) -0.014(3) 0.028(3) 0.003(3) C27 0.047(3) 0.047(3) 0.054(4) 0.002(3) 0.011(3) -0.001(2) C28 0.032(3) 0.044(3) 0.049(4) -0.001(2) 0.012(3) 0.001(2) C29 0.039(3) 0.059(3) 0.057(4) -0.004(3) 0.003(3) 0.003(2) C30 0.030(3) 0.108(5) 0.060(5) -0.014(4) 0.000(3) 0.007(3) C31 0.044(4) 0.075(5) 0.109(7) -0.010(4) 0.003(4) -0.017(3) C32 0.051(4) 0.057(4) 0.246(13) 0.032(6) -0.019(6) -0.015(3) C33 0.041(4) 0.061(4) 0.159(9) 0.027(4) -0.013(4) -0.008(3) C34 0.043(3) 0.038(3) 0.049(4) -0.004(2) 0.013(3) -0.004(2) C35 0.051(3) 0.038(3) 0.048(4) 0.005(2) 0.021(3) 0.001(2) C36 0.036(3) 0.050(3) 0.042(4) -0.004(3) 0.008(3) 0.010(2) C37 0.052(4) 0.062(4) 0.047(4) 0.005(3) 0.018(3) 0.004(3) C38 0.078(5) 0.089(5) 0.048(5) 0.006(4) 0.021(4) 0.017(4) C39 0.095(6) 0.109(6) 0.054(5) 0.016(5) 0.023(5) 0.037(5) C40 0.065(4) 0.090(5) 0.053(5) -0.022(4) -0.009(4) 0.016(4) C41 0.051(3) 0.059(4) 0.053(4) -0.004(3) 0.010(3) 0.004(3) C42 0.032(3) 0.032(3) 0.051(4) -0.002(2) 0.007(3) 0.0013(19) C43 0.041(3) 0.045(3) 0.057(4) -0.008(3) 0.018(3) 0.004(2) C44 0.046(3) 0.055(3) 0.080(6) -0.006(3) 0.031(3) 0.014(3) C45 0.038(3) 0.062(4) 0.090(6) 0.003(3) 0.019(4) 0.017(3) C46 0.038(3) 0.060(4) 0.067(5) 0.007(3) -0.002(3) 0.009(3) C47 0.042(3) 0.043(3) 0.054(4) 0.002(3) 0.012(3) 0.006(2) C48 0.037(3) 0.053(3) 0.037(4) 0.005(2) 0.015(2) 0.002(2) C49 0.054(4) 0.071(4) 0.045(4) 0.013(3) 0.004(3) -0.010(3) C50 0.057(4) 0.116(6) 0.050(5) 0.012(4) -0.001(3) -0.027(4) C51 0.051(4) 0.135(7) 0.049(5) 0.016(5) 0.002(3) 0.010(4) C52 0.083(5) 0.094(5) 0.043(4) 0.025(4) 0.019(4) 0.035(4) C53 0.065(4) 0.060(4) 0.045(4) 0.009(3) 0.013(3) 0.006(3) C54 0.043(3) 0.048(3) 0.040(4) 0.005(2) 0.017(3) 0.000(2) C55 0.049(4) 0.075(4) 0.047(4) -0.003(3) 0.015(3) 0.003(3) C56 0.066(4) 0.096(5) 0.055(5) 0.002(4) 0.029(4) 0.023(4) C57 0.051(4) 0.101(5) 0.105(7) 0.001(5) 0.043(4) -0.002(4) C58 0.052(4) 0.093(5) 0.150(9) -0.028(5) 0.048(5) -0.022(4) C59 0.052(4) 0.056(3) 0.098(6) -0.010(3) 0.035(4) -0.007(3) O3 0.254(8) 0.182(6) 0.060(4) 0.025(4) 0.019(4) 0.179(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O2 2.010(3) . ? Ru1 O1 2.020(3) . ? Ru1 N1 2.183(4) . ? Ru1 P2 2.3379(14) . ? Ru1 P1 2.3480(13) . ? Ru1 Cl1 2.4472(14) . ? P1 C36 1.821(6) . ? P1 C42 1.834(5) . ? P1 C34 1.844(5) . ? P2 C48 1.820(5) . ? P2 C54 1.822(5) . ? P2 C35 1.859(5) . ? O1 C1 1.422(5) . ? O2 C9 1.417(5) . ? N1 C7 1.343(6) . ? N1 C3 1.366(6) . ? C1 C10 1.535(7) . ? C1 C16 1.533(7) . ? C1 C2 1.561(6) . ? C2 C3 1.491(7) . ? C3 C4 1.379(7) . ? C4 C5 1.364(8) . ? C5 C6 1.376(7) . ? C6 C7 1.382(7) . ? C7 C8 1.494(6) . ? C8 C9 1.520(7) . ? C9 C22 1.504(7) . ? C9 C28 1.542(6) . ? C10 C11 1.369(8) . ? C10 C15 1.391(7) . ? C11 C12 1.394(10) . ? C12 C13 1.360(10) . ? C13 C14 1.368(10) . ? C14 C15 1.366(8) . ? C16 C21 1.388(7) . ? C16 C17 1.402(7) . ? C17 C18 1.372(8) . ? C18 C19 1.390(8) . ? C19 C20 1.382(7) . ? C20 C21 1.379(8) . ? C22 C23 1.381(7) . ? C22 C27 1.392(8) . ? C23 C24 1.401(8) . ? C24 C25 1.357(9) . ? C25 C26 1.379(9) . ? C26 C27 1.396(8) . ? C28 C33 1.361(8) . ? C28 C29 1.368(7) . ? C29 C30 1.397(8) . ? C30 C31 1.326(9) . ? C31 C32 1.325(9) . ? C32 C33 1.377(8) . ? C34 C35 1.512(7) . ? C36 C41 1.384(7) . ? C36 C37 1.407(7) . ? C37 C38 1.387(9) . ? C38 C39 1.348(10) . ? C39 C40 1.361(10) . ? C40 C41 1.426(9) . ? C42 C47 1.385(7) . ? C42 C43 1.396(7) . ? C43 C44 1.381(7) . ? C44 C45 1.368(9) . ? C45 C46 1.370(9) . ? C46 C47 1.390(7) . ? C48 C53 1.369(7) . ? C48 C49 1.393(7) . ? C49 C50 1.352(8) . ? C50 C51 1.368(9) . ? C51 C52 1.412(9) . ? C52 C53 1.366(9) . ? C54 C59 1.367(7) . ? C54 C55 1.372(8) . ? C55 C56 1.394(8) . ? C56 C57 1.369(9) . ? C57 C58 1.347(10) . ? C58 C59 1.382(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 O2 Ru1 O1 170.58(13) . . ? O2 Ru1 N1 90.97(13) . . ? O1 Ru1 N1 88.38(14) . . ? O2 Ru1 P2 82.40(10) . . ? O1 Ru1 P2 98.39(10) . . ? N1 Ru1 P2 173.23(10) . . ? O2 Ru1 P1 83.22(10) . . ? O1 Ru1 P1 87.59(9) . . ? N1 Ru1 P1 98.79(11) . . ? P2 Ru1 P1 81.89(5) . . ? O2 Ru1 Cl1 95.81(10) . . ? O1 Ru1 Cl1 93.60(10) . . ? N1 Ru1 Cl1 90.37(11) . . ? P2 Ru1 Cl1 88.91(5) . . ? P1 Ru1 Cl1 170.80(5) . . ? C36 P1 C42 102.9(2) . . ? C36 P1 C34 106.5(2) . . ? C42 P1 C34 101.9(2) . . ? C36 P1 Ru1 121.11(16) . . ? C42 P1 Ru1 116.85(17) . . ? C34 P1 Ru1 105.55(18) . . ? C48 P2 C54 102.6(2) . . ? C48 P2 C35 103.2(2) . . ? C54 P2 C35 104.6(2) . . ? C48 P2 Ru1 121.63(16) . . ? C54 P2 Ru1 112.75(17) . . ? C35 P2 Ru1 110.36(18) . . ? C1 O1 Ru1 128.2(3) . . ? C9 O2 Ru1 123.0(3) . . ? C7 N1 C3 119.2(4) . . ? C7 N1 Ru1 121.8(3) . . ? C3 N1 Ru1 118.7(3) . . ? O1 C1 C10 107.1(4) . . ? O1 C1 C16 111.6(4) . . ? C10 C1 C16 109.2(4) . . ? O1 C1 C2 111.1(4) . . ? C10 C1 C2 111.7(4) . . ? C16 C1 C2 106.1(4) . . ? C3 C2 C1 113.4(4) . . ? N1 C3 C4 120.7(5) . . ? N1 C3 C2 118.6(5) . . ? C4 C3 C2 120.7(5) . . ? C5 C4 C3 120.5(5) . . ? C4 C5 C6 117.3(5) . . ? C5 C6 C7 121.8(5) . . ? N1 C7 C6 119.6(4) . . ? N1 C7 C8 121.7(4) . . ? C6 C7 C8 118.7(5) . . ? C7 C8 C9 119.9(4) . . ? O2 C9 C22 111.3(4) . . ? O2 C9 C8 109.1(4) . . ? C22 C9 C8 114.7(4) . . ? O2 C9 C28 108.0(4) . . ? C22 C9 C28 107.5(4) . . ? C8 C9 C28 105.9(4) . . ? C11 C10 C15 117.0(5) . . ? C11 C10 C1 124.8(5) . . ? C15 C10 C1 118.2(5) . . ? C10 C11 C12 121.5(6) . . ? C13 C12 C11 119.4(7) . . ? C12 C13 C14 120.6(7) . . ? C15 C14 C13 119.3(7) . . ? C14 C15 C10 122.2(6) . . ? C21 C16 C17 117.7(5) . . ? C21 C16 C1 122.4(4) . . ? C17 C16 C1 119.7(4) . . ? C18 C17 C16 120.7(5) . . ? C17 C18 C19 120.9(5) . . ? C20 C19 C18 119.0(5) . . ? C21 C20 C19 120.2(5) . . ? C20 C21 C16 121.6(5) . . ? C23 C22 C27 118.1(5) . . ? C23 C22 C9 124.8(5) . . ? C27 C22 C9 117.0(4) . . ? C22 C23 C24 119.9(6) . . ? C25 C24 C23 120.7(5) . . ? C24 C25 C26 121.2(6) . . ? C25 C26 C27 117.9(6) . . ? C22 C27 C26 122.1(5) . . ? C33 C28 C29 115.9(5) . . ? C33 C28 C9 122.8(5) . . ? C29 C28 C9 121.2(5) . . ? C28 C29 C30 120.9(6) . . ? C31 C30 C29 121.5(6) . . ? C30 C31 C32 118.1(6) . . ? C31 C32 C33 122.0(7) . . ? C28 C33 C32 121.6(6) . . ? C35 C34 P1 108.6(3) . . ? C34 C35 P2 110.5(3) . . ? C41 C36 C37 117.9(6) . . ? C41 C36 P1 122.7(5) . . ? C37 C36 P1 119.4(4) . . ? C38 C37 C36 121.1(6) . . ? C39 C38 C37 120.2(7) . . ? C38 C39 C40 121.0(8) . . ? C39 C40 C41 120.1(7) . . ? C36 C41 C40 119.7(6) . . ? C47 C42 C43 119.0(5) . . ? C47 C42 P1 119.4(4) . . ? C43 C42 P1 121.6(4) . . ? C44 C43 C42 119.7(6) . . ? C45 C44 C43 121.2(6) . . ? C44 C45 C46 119.4(5) . . ? C45 C46 C47 120.8(6) . . ? C42 C47 C46 119.9(5) . . ? C53 C48 C49 118.0(5) . . ? C53 C48 P2 121.1(4) . . ? C49 C48 P2 120.8(4) . . ? C50 C49 C48 122.3(6) . . ? C49 C50 C51 119.5(7) . . ? C50 C51 C52 119.3(6) . . ? C53 C52 C51 119.8(6) . . ? C52 C53 C48 120.9(6) . . ? C59 C54 C55 117.8(5) . . ? C59 C54 P2 122.3(5) . . ? C55 C54 P2 119.6(4) . . ? C54 C55 C56 120.9(6) . . ? C57 C56 C55 120.4(7) . . ? C58 C57 C56 118.2(6) . . ? C57 C58 C59 121.9(6) . . ? C54 C59 C58 120.7(6) . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 1.361 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.135 data_mar131 _database_code_CSD 209731 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C79 H77 Cl4 N4 O5 Ru2' _chemical_formula_sum 'C79 H77 Cl4 N4 O5 Ru2' _chemical_formula_weight 1506.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _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 13.498(3) _cell_length_b 16.684(3) _cell_length_c 17.009(3) _cell_angle_alpha 84.49(3) _cell_angle_beta 74.35(3) _cell_angle_gamma 77.09(3) _cell_volume 3592.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1550 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11824 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8687 _reflns_number_gt 5448 _reflns_threshold_expression >2sigma(I) _computing_data_collection marControl _computing_cell_refinement denzo _computing_data_reduction denzo _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8687 _refine_ls_number_parameters 822 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.004 _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 0.40246(5) 0.24797(3) 0.71819(3) 0.03958(18) Uani 1 1 d . . . Ru2 Ru 0.19314(4) 0.14824(3) 0.79520(3) 0.04116(18) Uani 1 1 d . . . Cl1 Cl 0.26172(15) 0.10010(9) 0.91164(9) 0.0509(4) Uani 1 1 d . . . Cl2 Cl 0.14204(16) 0.19769(10) 0.67243(9) 0.0588(5) Uani 1 1 d . . . Cl3 Cl 0.3237(5) 0.3978(3) 0.1687(2) 0.218(3) Uani 1 1 d . . . Cl4 Cl 0.2768(5) 0.5694(3) 0.1826(4) 0.236(3) Uani 1 1 d . . . N1 N 0.3100(4) 0.1930(3) 0.7530(3) 0.0459(14) Uani 1 1 d . . . O2 O 0.4937(4) 0.2449(2) 0.7872(2) 0.0518(12) Uani 1 1 d . . . O3 O 0.3951(4) 0.3209(2) 0.6246(2) 0.0480(12) Uani 1 1 d . . . O4 O 0.2583(4) 0.0441(2) 0.7430(2) 0.0459(12) Uani 1 1 d . . . O5 O 0.1270(4) 0.2545(2) 0.8515(2) 0.0468(11) Uani 1 1 d . . . O6 O 0.7805(10) 0.8278(6) 0.7151(6) 0.171(3) Uiso 1 1 d . . . N2 N 0.2975(5) 0.3523(3) 0.7847(3) 0.0477(14) Uani 1 1 d . . . H2A H 0.2677 0.3857 0.7489 0.057 Uiso 1 1 calc R . . H2B H 0.2456 0.3331 0.8214 0.057 Uiso 1 1 calc R . . N3 N 0.5026(5) 0.1517(3) 0.6493(3) 0.0427(14) Uani 1 1 d . . . N4 N 0.0507(5) 0.1044(3) 0.8503(2) 0.0420(14) Uani 1 1 d . . . C79 C 0.3386(6) 0.4020(4) 0.8274(3) 0.0448(17) Uani 1 1 d . . . C1 C 0.3454(7) 0.3786(4) 0.9077(4) 0.058(2) Uani 1 1 d . . . C2 C 0.3894(8) 0.4245(5) 0.9476(5) 0.079(3) Uani 1 1 d . . . H2 H 0.3930 0.4103 1.0011 0.095 Uiso 1 1 calc R . . C3 C 0.4293(9) 0.4937(6) 0.9060(6) 0.091(3) Uani 1 1 d . . . H3 H 0.4632 0.5228 0.9308 0.109 Uiso 1 1 calc R . . C4 C 0.4171(9) 0.5162(5) 0.8306(6) 0.084(3) Uani 1 1 d . . . H4 H 0.4402 0.5631 0.8055 0.101 Uiso 1 1 calc R . . C5 C 0.3726(7) 0.4738(4) 0.7885(4) 0.061(2) Uani 1 1 d . . . C6 C 0.3019(7) 0.3057(4) 0.9521(4) 0.075(3) Uani 1 1 d . . . H6A H 0.2749 0.2803 0.9162 0.113 Uiso 1 1 calc R . . H6B H 0.2463 0.3241 0.9993 0.113 Uiso 1 1 calc R . . H6C H 0.3568 0.2664 0.9688 0.113 Uiso 1 1 calc R . . C7 C 0.3533(9) 0.5033(5) 0.7064(4) 0.099(4) Uani 1 1 d . . . H7A H 0.3213 0.4653 0.6880 0.148 Uiso 1 1 calc R . . H7B H 0.4189 0.5070 0.6679 0.148 Uiso 1 1 calc R . . H7C H 0.3073 0.5566 0.7111 0.148 Uiso 1 1 calc R . . C8 C 0.5796(6) 0.1776(4) 0.7949(3) 0.0486(18) Uani 1 1 d . . . C9 C 0.5569(6) 0.0973(4) 0.7735(3) 0.0479(18) Uani 1 1 d . . . H9A H 0.6068 0.0513 0.7891 0.057 Uiso 1 1 calc R . . H9B H 0.4871 0.0919 0.8054 0.057 Uiso 1 1 calc R . . C10 C 0.5630(6) 0.0926(4) 0.6854(4) 0.0491(18) Uani 1 1 d . . . C11 C 0.6260(6) 0.0238(4) 0.6416(4) 0.056(2) Uani 1 1 d . . . H11 H 0.6704 -0.0156 0.6658 0.067 Uiso 1 1 calc R . . C12 C 0.6218(7) 0.0151(4) 0.5636(4) 0.061(2) Uani 1 1 d . . . H12 H 0.6619 -0.0307 0.5345 0.073 Uiso 1 1 calc R . . C13 C 0.5563(7) 0.0759(4) 0.5285(4) 0.060(2) Uani 1 1 d . . . H13 H 0.5523 0.0708 0.4756 0.072 Uiso 1 1 calc R . . C14 C 0.4981(6) 0.1428(4) 0.5713(4) 0.051(2) Uani 1 1 d . . . C15 C 0.4234(7) 0.2087(4) 0.5349(3) 0.054(2) Uani 1 1 d . . . H15A H 0.3519 0.2038 0.5623 0.065 Uiso 1 1 calc R . . H15B H 0.4351 0.1977 0.4778 0.065 Uiso 1 1 calc R . . C16 C 0.4330(6) 0.2978(4) 0.5405(3) 0.0482(18) Uani 1 1 d . . . C17 C 0.5805(7) 0.1778(4) 0.8857(4) 0.055(2) Uani 1 1 d . . . C18 C 0.5744(8) 0.1081(5) 0.9380(4) 0.077(3) Uani 1 1 d . . . H18 H 0.5660 0.0596 0.9203 0.092 Uiso 1 1 calc R . . C19 C 0.5814(9) 0.1139(7) 1.0197(4) 0.099(4) Uani 1 1 d . . . H19 H 0.5802 0.0674 1.0546 0.119 Uiso 1 1 calc R . . C20 C 0.5896(9) 0.1832(8) 1.0472(5) 0.095(3) Uani 1 1 d . . . H20 H 0.5923 0.1856 1.1010 0.114 Uiso 1 1 calc R . . C21 C 0.5938(8) 0.2504(6) 0.9962(5) 0.088(3) Uani 1 1 d . . . H21 H 0.5984 0.2992 1.0159 0.105 Uiso 1 1 calc R . . C22 C 0.5915(7) 0.2488(5) 0.9139(4) 0.067(2) Uani 1 1 d . . . H22 H 0.5974 0.2951 0.8793 0.081 Uiso 1 1 calc R . . C23 C 0.6822(6) 0.1942(4) 0.7402(3) 0.0518(18) Uani 1 1 d . . . C24 C 0.7729(8) 0.1354(5) 0.7372(4) 0.072(2) Uani 1 1 d . . . H24 H 0.7703 0.0869 0.7689 0.087 Uiso 1 1 calc R . . C25 C 0.8690(8) 0.1486(7) 0.6865(6) 0.099(3) Uani 1 1 d . . . H25 H 0.9303 0.1091 0.6843 0.119 Uiso 1 1 calc R . . C26 C 0.8718(10) 0.2199(9) 0.6406(5) 0.114(4) Uani 1 1 d . . . H26 H 0.9352 0.2281 0.6057 0.137 Uiso 1 1 calc R . . C27 C 0.7842(10) 0.2791(8) 0.6445(6) 0.117(4) Uani 1 1 d . . . H27 H 0.7874 0.3288 0.6150 0.140 Uiso 1 1 calc R . . C28 C 0.6902(8) 0.2643(6) 0.6931(5) 0.087(3) Uani 1 1 d . . . H28 H 0.6294 0.3040 0.6937 0.105 Uiso 1 1 calc R . . C29 C 0.3545(8) 0.3530(4) 0.4960(4) 0.059(2) Uani 1 1 d . . . C30 C 0.2486(9) 0.3713(5) 0.5330(5) 0.082(3) Uani 1 1 d . . . H30 H 0.2237 0.3503 0.5856 0.099 Uiso 1 1 calc R . . C31 C 0.1794(9) 0.4196(6) 0.4941(6) 0.094(3) Uani 1 1 d . . . H31 H 0.1079 0.4308 0.5198 0.113 Uiso 1 1 calc R . . C32 C 0.2151(11) 0.4519(6) 0.4165(6) 0.096(3) Uani 1 1 d . . . H32 H 0.1679 0.4857 0.3904 0.115 Uiso 1 1 calc R . . C33 C 0.3182(11) 0.4346(6) 0.3784(5) 0.092(3) Uani 1 1 d . . . H33 H 0.3413 0.4556 0.3255 0.111 Uiso 1 1 calc R . . C34 C 0.3911(8) 0.3858(4) 0.4167(4) 0.076(3) Uani 1 1 d . . . H34 H 0.4625 0.3751 0.3904 0.092 Uiso 1 1 calc R . . C35 C 0.5447(6) 0.3135(4) 0.5058(4) 0.0536(19) Uani 1 1 d . . . C36 C 0.6214(8) 0.2615(5) 0.4544(4) 0.075(3) Uani 1 1 d . . . H36 H 0.6076 0.2139 0.4392 0.090 Uiso 1 1 calc R . . C37 C 0.7223(8) 0.2802(6) 0.4241(5) 0.090(3) Uani 1 1 d . . . H37 H 0.7750 0.2428 0.3911 0.108 Uiso 1 1 calc R . . C38 C 0.7448(9) 0.3499(6) 0.4413(5) 0.085(3) Uani 1 1 d . . . H38 H 0.8113 0.3617 0.4204 0.102 Uiso 1 1 calc R . . C39 C 0.6647(9) 0.4034(6) 0.4913(5) 0.081(3) Uani 1 1 d . . . H39 H 0.6769 0.4532 0.5026 0.098 Uiso 1 1 calc R . . C40 C 0.5689(8) 0.3853(5) 0.5243(4) 0.070(2) Uani 1 1 d . . . H40 H 0.5181 0.4215 0.5601 0.084 Uiso 1 1 calc R . . C41 C 0.2216(6) -0.0298(4) 0.7602(3) 0.0452(17) Uani 1 1 d . . . C42 C 0.1569(6) -0.0350(4) 0.8501(3) 0.0458(18) Uani 1 1 d . . . H42A H 0.1439 -0.0903 0.8620 0.055 Uiso 1 1 calc R . . H42B H 0.1993 -0.0265 0.8851 0.055 Uiso 1 1 calc R . . C43 C 0.0558(6) 0.0233(4) 0.8717(3) 0.0439(17) Uani 1 1 d . . . C44 C -0.0355(6) -0.0031(4) 0.9140(3) 0.0510(18) Uani 1 1 d . . . H44 H -0.0323 -0.0585 0.9288 0.061 Uiso 1 1 calc R . . C45 C -0.1284(6) 0.0504(4) 0.9340(4) 0.0556(19) Uani 1 1 d . . . H45 H -0.1891 0.0324 0.9627 0.067 Uiso 1 1 calc R . . C46 C -0.1317(6) 0.1328(4) 0.9110(4) 0.0555(19) Uani 1 1 d . . . H46 H -0.1950 0.1708 0.9244 0.067 Uiso 1 1 calc R . . C47 C -0.0428(6) 0.1579(4) 0.8689(3) 0.0431(16) Uani 1 1 d . . . C48 C -0.0478(6) 0.2465(4) 0.8398(4) 0.0513(18) Uani 1 1 d . . . H48A H -0.1204 0.2758 0.8546 0.062 Uiso 1 1 calc R . . H48B H -0.0235 0.2488 0.7806 0.062 Uiso 1 1 calc R . . C49 C 0.0184(6) 0.2903(4) 0.8752(4) 0.0491(18) Uani 1 1 d . . . C50 C 0.3207(6) -0.0995(4) 0.7470(3) 0.0445(17) Uani 1 1 d . . . C51 C 0.3112(8) -0.1817(5) 0.7546(5) 0.079(3) Uani 1 1 d . . . H51 H 0.2451 -0.1949 0.7673 0.095 Uiso 1 1 calc R . . C52 C 0.4031(9) -0.2448(5) 0.7430(5) 0.089(3) Uani 1 1 d . . . H52 H 0.3972 -0.2997 0.7482 0.107 Uiso 1 1 calc R . . C53 C 0.4973(8) -0.2262(5) 0.7246(4) 0.069(2) Uani 1 1 d . . . H53 H 0.5573 -0.2679 0.7162 0.083 Uiso 1 1 calc R . . C54 C 0.5061(8) -0.1475(5) 0.7183(5) 0.082(3) Uani 1 1 d . . . H54 H 0.5723 -0.1348 0.7068 0.098 Uiso 1 1 calc R . . C55 C 0.4187(7) -0.0853(5) 0.7286(4) 0.070(2) Uani 1 1 d . . . H55 H 0.4275 -0.0311 0.7226 0.084 Uiso 1 1 calc R . . C56 C 0.1578(6) -0.0390(4) 0.7001(3) 0.0469(18) Uani 1 1 d . . . C57 C 0.0788(7) -0.0842(4) 0.7204(4) 0.060(2) Uani 1 1 d . . . H57 H 0.0611 -0.1074 0.7730 0.072 Uiso 1 1 calc R . . C58 C 0.0252(8) -0.0957(5) 0.6638(5) 0.080(3) Uani 1 1 d . . . H58 H -0.0295 -0.1240 0.6787 0.096 Uiso 1 1 calc R . . C59 C 0.0558(9) -0.0638(6) 0.5851(5) 0.092(3) Uani 1 1 d . . . H59 H 0.0253 -0.0747 0.5454 0.111 Uiso 1 1 calc R . . C60 C 0.1281(9) -0.0177(6) 0.5653(5) 0.088(3) Uani 1 1 d . . . H60 H 0.1424 0.0077 0.5136 0.105 Uiso 1 1 calc R . . C61 C 0.1842(7) -0.0066(5) 0.6220(4) 0.066(2) Uani 1 1 d . . . H61 H 0.2382 0.0224 0.6062 0.079 Uiso 1 1 calc R . . C62 C 0.0154(7) 0.3799(4) 0.8401(4) 0.056(2) Uani 1 1 d . . . C63 C 0.0243(9) 0.4394(5) 0.8857(5) 0.085(3) Uani 1 1 d . . . H63 H 0.0258 0.4264 0.9398 0.102 Uiso 1 1 calc R . . C64 C 0.0310(11) 0.5180(5) 0.8554(6) 0.109(4) Uani 1 1 d . . . H64 H 0.0354 0.5573 0.8889 0.131 Uiso 1 1 calc R . . C65 C 0.0311(10) 0.5374(5) 0.7771(6) 0.102(4) Uani 1 1 d . . . H65 H 0.0358 0.5903 0.7560 0.122 Uiso 1 1 calc R . . C66 C 0.0243(9) 0.4800(5) 0.7289(5) 0.100(4) Uani 1 1 d . . . H66 H 0.0226 0.4941 0.6749 0.120 Uiso 1 1 calc R . . C67 C 0.0200(9) 0.3989(5) 0.7597(5) 0.084(3) Uani 1 1 d . . . H67 H 0.0203 0.3587 0.7253 0.100 Uiso 1 1 calc R . . C68 C -0.0237(7) 0.2875(4) 0.9690(4) 0.051(2) Uani 1 1 d . . . C69 C 0.0376(7) 0.2473(4) 1.0189(4) 0.057(2) Uani 1 1 d . . . H69 H 0.1063 0.2204 0.9959 0.068 Uiso 1 1 calc R . . C70 C -0.0014(9) 0.2462(5) 1.1033(5) 0.072(3) Uani 1 1 d . . . H70 H 0.0413 0.2175 1.1359 0.087 Uiso 1 1 calc R . . C71 C -0.0983(10) 0.2851(5) 1.1387(5) 0.079(3) Uani 1 1 d . . . H71 H -0.1231 0.2858 1.1952 0.095 Uiso 1 1 calc R . . C72 C -0.1596(10) 0.3236(6) 1.0898(6) 0.096(3) Uani 1 1 d . . . H72 H -0.2283 0.3497 1.1137 0.116 Uiso 1 1 calc R . . C73 C -0.1239(8) 0.3257(5) 1.0050(5) 0.072(2) Uani 1 1 d . . . H73 H -0.1682 0.3530 0.9731 0.087 Uiso 1 1 calc R . . C74 C 0.256(2) 0.4907(8) 0.1483(11) 0.266(12) Uani 1 1 d . . . H74A H 0.2700 0.4984 0.0894 0.319 Uiso 1 1 calc R . . H74B H 0.1821 0.4901 0.1690 0.319 Uiso 1 1 calc R . . C75 C 0.8188(17) 0.7643(10) 0.6530(9) 0.197(7) Uiso 1 1 d . . . H75A H 0.8883 0.7340 0.6551 0.236 Uiso 1 1 calc R . . H75B H 0.7720 0.7258 0.6638 0.236 Uiso 1 1 calc R . . C76 C 0.8225(13) 0.8025(8) 0.5760(7) 0.157(5) Uiso 1 1 d . . . H76A H 0.8453 0.7614 0.5354 0.235 Uiso 1 1 calc R . . H76B H 0.8710 0.8389 0.5648 0.235 Uiso 1 1 calc R . . H76C H 0.7538 0.8334 0.5747 0.235 Uiso 1 1 calc R . . C77 C 0.7588(16) 0.7936(9) 0.7993(8) 0.180(6) Uiso 1 1 d . . . H77A H 0.8192 0.7549 0.8102 0.216 Uiso 1 1 calc R . . H77B H 0.6984 0.7678 0.8126 0.216 Uiso 1 1 calc R . . C78 C 0.7347(14) 0.8788(8) 0.8464(7) 0.171(5) Uiso 1 1 d . . . H78A H 0.7130 0.8680 0.9043 0.256 Uiso 1 1 calc R . . H78B H 0.6798 0.9176 0.8292 0.256 Uiso 1 1 calc R . . H78C H 0.7972 0.9011 0.8336 0.256 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0385(4) 0.0427(3) 0.0384(3) 0.0025(2) -0.0079(2) -0.0143(3) Ru2 0.0358(4) 0.0417(3) 0.0468(3) 0.0036(2) -0.0086(2) -0.0144(3) Cl1 0.0523(13) 0.0501(9) 0.0546(9) 0.0040(7) -0.0210(8) -0.0135(8) Cl2 0.0597(15) 0.0655(11) 0.0523(9) 0.0132(7) -0.0182(8) -0.0170(10) Cl3 0.349(9) 0.169(4) 0.141(3) 0.025(2) -0.078(4) -0.061(4) Cl4 0.170(6) 0.150(4) 0.411(7) 0.085(4) -0.142(5) -0.038(4) N1 0.045(4) 0.041(3) 0.050(3) 0.000(2) -0.002(2) -0.018(3) O2 0.060(4) 0.049(3) 0.050(2) -0.0027(18) -0.019(2) -0.012(2) O3 0.059(4) 0.048(3) 0.040(2) 0.0024(17) -0.011(2) -0.020(2) O4 0.049(4) 0.038(2) 0.049(2) 0.0015(17) -0.003(2) -0.020(2) O5 0.040(4) 0.040(2) 0.059(3) -0.0022(18) -0.010(2) -0.009(2) N2 0.046(4) 0.047(3) 0.045(3) 0.001(2) -0.006(2) -0.007(3) N3 0.046(4) 0.046(3) 0.037(3) 0.000(2) -0.006(2) -0.019(3) N4 0.043(4) 0.050(3) 0.035(3) 0.003(2) -0.007(2) -0.020(3) C79 0.041(5) 0.041(4) 0.053(4) -0.012(3) -0.007(3) -0.009(3) C1 0.062(7) 0.048(4) 0.060(4) -0.007(3) -0.011(4) -0.009(4) C2 0.089(9) 0.079(6) 0.081(5) -0.021(4) -0.040(5) -0.011(5) C3 0.111(11) 0.083(7) 0.102(7) -0.019(5) -0.054(6) -0.027(6) C4 0.088(9) 0.046(5) 0.115(7) -0.012(4) -0.009(6) -0.023(5) C5 0.059(7) 0.048(4) 0.070(5) -0.009(3) -0.005(4) -0.008(4) C6 0.088(8) 0.082(6) 0.053(4) 0.001(4) -0.008(4) -0.027(5) C7 0.166(13) 0.059(5) 0.069(5) 0.011(4) -0.013(6) -0.043(6) C8 0.048(6) 0.052(4) 0.050(4) -0.001(3) -0.025(3) -0.004(4) C9 0.049(6) 0.048(4) 0.045(4) -0.001(3) -0.011(3) -0.010(3) C10 0.048(6) 0.048(4) 0.051(4) 0.001(3) -0.008(3) -0.017(4) C11 0.049(6) 0.047(4) 0.061(4) 0.000(3) -0.002(3) -0.003(4) C12 0.066(7) 0.051(4) 0.060(4) -0.011(3) -0.003(4) -0.011(4) C13 0.082(7) 0.053(4) 0.044(4) -0.010(3) -0.004(4) -0.023(4) C14 0.061(6) 0.049(4) 0.046(4) 0.001(3) -0.009(3) -0.025(4) C15 0.069(6) 0.060(4) 0.037(3) -0.002(3) -0.011(3) -0.021(4) C16 0.058(6) 0.050(4) 0.040(4) 0.001(3) -0.016(3) -0.015(4) C17 0.046(6) 0.069(5) 0.047(4) 0.001(3) -0.016(3) 0.001(4) C18 0.084(8) 0.089(6) 0.055(5) 0.006(4) -0.016(4) -0.018(5) C19 0.116(11) 0.119(8) 0.042(5) 0.019(5) -0.014(5) 0.000(7) C20 0.080(9) 0.144(10) 0.048(5) -0.016(6) -0.014(4) 0.002(7) C21 0.067(8) 0.118(8) 0.077(6) -0.038(5) -0.030(5) 0.011(6) C22 0.057(7) 0.077(5) 0.070(5) -0.020(4) -0.025(4) -0.001(4) C23 0.041(6) 0.075(5) 0.040(4) -0.001(3) -0.010(3) -0.014(4) C24 0.054(7) 0.090(6) 0.075(5) -0.010(4) -0.017(4) -0.017(5) C25 0.042(8) 0.155(10) 0.096(7) -0.031(7) -0.010(5) -0.009(7) C26 0.071(10) 0.193(12) 0.075(6) 0.031(7) -0.004(6) -0.053(9) C27 0.065(9) 0.176(11) 0.105(8) 0.064(7) -0.021(6) -0.043(9) C28 0.069(8) 0.116(7) 0.082(6) 0.036(5) -0.027(5) -0.038(6) C29 0.072(8) 0.049(4) 0.057(4) -0.001(3) -0.025(4) -0.006(4) C30 0.078(9) 0.095(6) 0.071(5) 0.021(4) -0.023(5) -0.016(6) C31 0.062(8) 0.124(8) 0.099(7) 0.013(6) -0.034(5) -0.015(6) C32 0.118(12) 0.091(7) 0.090(7) 0.003(5) -0.065(7) -0.002(7) C33 0.111(11) 0.098(7) 0.058(5) 0.010(4) -0.031(6) 0.004(7) C34 0.097(9) 0.073(5) 0.048(4) 0.003(4) -0.021(4) 0.006(5) C35 0.057(6) 0.062(5) 0.041(4) 0.008(3) -0.008(3) -0.019(4) C36 0.091(8) 0.063(5) 0.063(5) -0.003(4) 0.005(5) -0.030(5) C37 0.072(8) 0.087(7) 0.084(6) 0.008(5) 0.014(5) -0.006(6) C38 0.082(9) 0.094(7) 0.079(6) 0.020(5) -0.013(5) -0.037(6) C39 0.095(9) 0.087(6) 0.074(5) -0.001(4) -0.016(5) -0.051(6) C40 0.076(7) 0.078(5) 0.056(4) -0.002(4) 0.000(4) -0.036(5) C41 0.044(5) 0.044(4) 0.047(4) -0.002(3) -0.006(3) -0.015(3) C42 0.054(6) 0.042(4) 0.040(3) 0.004(3) -0.007(3) -0.017(3) C43 0.049(5) 0.052(4) 0.033(3) 0.007(3) -0.010(3) -0.020(4) C44 0.056(6) 0.050(4) 0.049(4) 0.005(3) -0.008(3) -0.025(4) C45 0.045(6) 0.072(5) 0.050(4) 0.003(3) -0.005(3) -0.023(4) C46 0.037(5) 0.073(5) 0.055(4) -0.002(3) -0.010(3) -0.013(4) C47 0.032(5) 0.049(4) 0.051(4) -0.007(3) -0.008(3) -0.014(3) C48 0.034(5) 0.052(4) 0.064(4) 0.003(3) -0.013(3) -0.003(3) C49 0.042(6) 0.039(4) 0.065(4) 0.003(3) -0.013(3) -0.009(3) C50 0.054(6) 0.043(4) 0.038(3) -0.004(2) -0.011(3) -0.014(3) C51 0.063(8) 0.057(5) 0.115(7) -0.007(4) -0.013(5) -0.018(5) C52 0.085(10) 0.043(5) 0.136(8) -0.014(4) -0.031(6) 0.001(5) C53 0.058(7) 0.068(6) 0.071(5) -0.004(4) -0.014(4) 0.004(5) C54 0.039(7) 0.077(6) 0.119(7) 0.007(5) -0.015(5) -0.002(5) C55 0.057(7) 0.053(5) 0.098(6) 0.004(4) -0.013(4) -0.018(4) C56 0.050(6) 0.049(4) 0.044(4) -0.001(3) -0.012(3) -0.015(4) C57 0.061(7) 0.068(5) 0.055(4) 0.005(3) -0.017(4) -0.022(4) C58 0.082(9) 0.096(6) 0.084(6) -0.006(4) -0.030(5) -0.050(6) C59 0.099(10) 0.130(8) 0.069(6) -0.013(5) -0.032(5) -0.052(7) C60 0.090(9) 0.125(8) 0.065(5) 0.017(5) -0.034(5) -0.046(7) C61 0.062(7) 0.090(6) 0.052(4) 0.006(4) -0.014(4) -0.035(5) C62 0.051(6) 0.039(4) 0.076(5) 0.001(3) -0.012(4) -0.011(4) C63 0.112(10) 0.066(6) 0.087(6) 0.018(4) -0.036(5) -0.035(5) C64 0.181(15) 0.059(6) 0.103(7) 0.003(5) -0.037(7) -0.057(7) C65 0.136(12) 0.052(6) 0.115(8) 0.019(5) -0.021(7) -0.037(6) C66 0.144(12) 0.064(6) 0.088(6) 0.027(5) -0.024(6) -0.033(6) C67 0.117(11) 0.054(5) 0.073(5) 0.006(4) -0.025(5) -0.007(5) C68 0.049(6) 0.037(4) 0.060(4) -0.006(3) 0.000(4) -0.012(4) C69 0.054(6) 0.051(4) 0.056(4) -0.002(3) -0.001(4) -0.006(4) C70 0.082(9) 0.060(5) 0.072(5) 0.007(4) -0.013(5) -0.018(5) C71 0.088(9) 0.081(6) 0.067(5) -0.009(4) 0.000(5) -0.035(6) C72 0.067(9) 0.103(7) 0.095(7) -0.018(5) 0.022(6) -0.014(6) C73 0.047(7) 0.077(5) 0.082(6) -0.007(4) -0.005(4) -0.001(5) C74 0.33(4) 0.066(10) 0.38(3) 0.014(12) -0.09(2) -0.001(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.661(5) . ? Ru1 O2 1.906(5) . ? Ru1 O3 1.919(4) . ? Ru1 N3 2.077(5) . ? Ru1 N2 2.175(5) . ? Ru2 N1 1.837(5) . ? Ru2 O4 1.943(4) . ? Ru2 O5 2.003(4) . ? Ru2 N4 2.153(5) . ? Ru2 Cl2 2.3893(17) . ? Ru2 Cl1 2.4033(17) . ? Cl3 C74 1.670(16) . ? Cl4 C74 1.592(19) . ? O2 C8 1.448(8) . ? O3 C16 1.442(7) . ? O4 C41 1.405(7) . ? O5 C49 1.416(9) . ? O6 C77 1.468(12) . ? O6 C75 1.477(15) . ? N2 C79 1.436(8) . ? N3 C10 1.345(9) . ? N3 C14 1.368(7) . ? N4 C47 1.351(8) . ? N4 C43 1.359(7) . ? C79 C1 1.405(8) . ? C79 C5 1.418(9) . ? C1 C2 1.386(11) . ? C1 C6 1.517(10) . ? C2 C3 1.427(12) . ? C3 C4 1.343(11) . ? C4 C5 1.378(12) . ? C5 C7 1.504(10) . ? C8 C23 1.512(10) . ? C8 C9 1.535(9) . ? C8 C17 1.549(8) . ? C9 C10 1.488(8) . ? C10 C11 1.407(9) . ? C11 C12 1.367(9) . ? C12 C13 1.390(11) . ? C13 C14 1.359(9) . ? C14 C15 1.524(10) . ? C15 C16 1.535(8) . ? C16 C35 1.536(11) . ? C16 C29 1.550(11) . ? C17 C22 1.370(10) . ? C17 C18 1.398(9) . ? C18 C19 1.431(10) . ? C19 C20 1.326(12) . ? C20 C21 1.352(12) . ? C21 C22 1.412(10) . ? C23 C28 1.361(10) . ? C23 C24 1.381(11) . ? C24 C25 1.401(13) . ? C25 C26 1.361(13) . ? C26 C27 1.351(15) . ? C27 C28 1.373(14) . ? C29 C30 1.375(13) . ? C29 C34 1.408(9) . ? C30 C31 1.362(13) . ? C31 C32 1.379(11) . ? C32 C33 1.345(15) . ? C33 C34 1.394(13) . ? C35 C36 1.358(10) . ? C35 C40 1.393(9) . ? C36 C37 1.414(13) . ? C37 C38 1.342(12) . ? C38 C39 1.381(12) . ? C39 C40 1.352(12) . ? C41 C56 1.540(10) . ? C41 C50 1.545(10) . ? C41 C42 1.548(7) . ? C42 C43 1.466(9) . ? C43 C44 1.390(10) . ? C44 C45 1.346(10) . ? C45 C46 1.388(9) . ? C46 C47 1.353(9) . ? C47 C48 1.505(8) . ? C48 C49 1.537(10) . ? C49 C68 1.543(8) . ? C49 C62 1.550(9) . ? C50 C55 1.345(11) . ? C50 C51 1.395(9) . ? C51 C52 1.419(13) . ? C52 C53 1.325(13) . ? C53 C54 1.337(10) . ? C54 C55 1.369(11) . ? C56 C61 1.370(8) . ? C56 C57 1.391(10) . ? C57 C58 1.401(11) . ? C58 C59 1.381(10) . ? C59 C60 1.330(12) . ? C60 C61 1.424(12) . ? C62 C63 1.361(10) . ? C62 C67 1.363(9) . ? C63 C64 1.375(10) . ? C64 C65 1.339(11) . ? C65 C66 1.352(12) . ? C66 C67 1.412(10) . ? C68 C73 1.361(12) . ? C68 C69 1.370(11) . ? C69 C70 1.390(9) . ? C70 C71 1.329(13) . ? C71 C72 1.347(14) . ? C72 C73 1.393(10) . ? C75 C76 1.394(14) . ? C77 C78 1.624(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O2 114.9(2) . . ? N1 Ru1 O3 118.6(2) . . ? O2 Ru1 O3 125.66(19) . . ? N1 Ru1 N3 91.9(2) . . ? O2 Ru1 N3 93.2(2) . . ? O3 Ru1 N3 93.72(18) . . ? N1 Ru1 N2 89.4(2) . . ? O2 Ru1 N2 88.5(2) . . ? O3 Ru1 N2 83.43(17) . . ? N3 Ru1 N2 177.15(17) . . ? N1 Ru2 O4 93.69(19) . . ? N1 Ru2 O5 86.4(2) . . ? O4 Ru2 O5 178.59(16) . . ? N1 Ru2 N4 175.4(2) . . ? O4 Ru2 N4 90.87(18) . . ? O5 Ru2 N4 89.03(19) . . ? N1 Ru2 Cl2 86.88(16) . . ? O4 Ru2 Cl2 87.64(13) . . ? O5 Ru2 Cl2 93.77(12) . . ? N4 Ru2 Cl2 93.87(14) . . ? N1 Ru2 Cl1 87.75(16) . . ? O4 Ru2 Cl1 90.98(13) . . ? O5 Ru2 Cl1 87.62(13) . . ? N4 Ru2 Cl1 91.62(13) . . ? Cl2 Ru2 Cl1 174.36(7) . . ? Ru1 N1 Ru2 170.7(3) . . ? C8 O2 Ru1 125.5(3) . . ? C16 O3 Ru1 125.8(4) . . ? C41 O4 Ru2 126.9(4) . . ? C49 O5 Ru2 126.9(4) . . ? C77 O6 C75 113.4(10) . . ? C79 N2 Ru1 119.4(5) . . ? C10 N3 C14 119.8(6) . . ? C10 N3 Ru1 119.1(4) . . ? C14 N3 Ru1 120.6(5) . . ? C47 N4 C43 119.8(6) . . ? C47 N4 Ru2 120.3(4) . . ? C43 N4 Ru2 119.7(5) . . ? C1 C79 C5 120.5(6) . . ? C1 C79 N2 119.4(5) . . ? C5 C79 N2 120.1(6) . . ? C2 C1 C79 119.5(7) . . ? C2 C1 C6 119.6(7) . . ? C79 C1 C6 120.9(6) . . ? C1 C2 C3 119.6(7) . . ? C4 C3 C2 119.1(8) . . ? C3 C4 C5 123.8(7) . . ? C4 C5 C79 117.4(7) . . ? C4 C5 C7 122.7(7) . . ? C79 C5 C7 119.7(7) . . ? O2 C8 C23 110.3(5) . . ? O2 C8 C9 109.1(6) . . ? C23 C8 C9 111.2(5) . . ? O2 C8 C17 103.6(5) . . ? C23 C8 C17 110.0(6) . . ? C9 C8 C17 112.3(5) . . ? C10 C9 C8 113.7(5) . . ? N3 C10 C11 120.3(6) . . ? N3 C10 C9 119.5(6) . . ? C11 C10 C9 120.1(6) . . ? C12 C11 C10 119.8(7) . . ? C11 C12 C13 118.8(7) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 N3 121.0(7) . . ? C13 C14 C15 121.1(6) . . ? N3 C14 C15 117.9(6) . . ? C14 C15 C16 115.8(6) . . ? O3 C16 C15 109.2(5) . . ? O3 C16 C35 109.4(5) . . ? C15 C16 C35 114.4(6) . . ? O3 C16 C29 105.3(6) . . ? C15 C16 C29 106.6(6) . . ? C35 C16 C29 111.5(5) . . ? C22 C17 C18 119.8(6) . . ? C22 C17 C8 117.8(6) . . ? C18 C17 C8 122.4(7) . . ? C17 C18 C19 117.8(8) . . ? C20 C19 C18 122.2(8) . . ? C19 C20 C21 119.2(8) . . ? C20 C21 C22 122.0(9) . . ? C17 C22 C21 119.0(8) . . ? C28 C23 C24 117.8(8) . . ? C28 C23 C8 123.5(8) . . ? C24 C23 C8 118.7(6) . . ? C23 C24 C25 120.1(8) . . ? C26 C25 C24 119.4(11) . . ? C27 C26 C25 121.2(10) . . ? C26 C27 C28 118.6(10) . . ? C23 C28 C27 122.9(10) . . ? C30 C29 C34 118.8(7) . . ? C30 C29 C16 121.0(7) . . ? C34 C29 C16 120.2(8) . . ? C31 C30 C29 121.1(8) . . ? C30 C31 C32 120.1(10) . . ? C33 C32 C31 120.1(9) . . ? C32 C33 C34 121.2(9) . . ? C33 C34 C29 118.6(9) . . ? C36 C35 C40 117.7(8) . . ? C36 C35 C16 122.6(7) . . ? C40 C35 C16 119.6(7) . . ? C35 C36 C37 119.6(8) . . ? C38 C37 C36 122.4(9) . . ? C37 C38 C39 117.0(9) . . ? C40 C39 C38 121.8(8) . . ? C39 C40 C35 121.3(8) . . ? O4 C41 C56 110.5(5) . . ? O4 C41 C50 105.9(6) . . ? C56 C41 C50 108.8(5) . . ? O4 C41 C42 111.0(4) . . ? C56 C41 C42 111.6(6) . . ? C50 C41 C42 108.9(5) . . ? C43 C42 C41 116.1(5) . . ? N4 C43 C44 119.2(7) . . ? N4 C43 C42 119.8(6) . . ? C44 C43 C42 121.0(6) . . ? C45 C44 C43 121.1(6) . . ? C44 C45 C46 118.6(7) . . ? C47 C46 C45 120.0(7) . . ? N4 C47 C46 121.2(6) . . ? N4 C47 C48 118.9(6) . . ? C46 C47 C48 119.9(7) . . ? C47 C48 C49 113.6(6) . . ? O5 C49 C48 112.3(5) . . ? O5 C49 C68 111.0(5) . . ? C48 C49 C68 107.6(5) . . ? O5 C49 C62 102.5(6) . . ? C48 C49 C62 111.8(6) . . ? C68 C49 C62 111.7(5) . . ? C55 C50 C51 116.8(7) . . ? C55 C50 C41 122.8(6) . . ? C51 C50 C41 120.3(7) . . ? C50 C51 C52 119.4(9) . . ? C53 C52 C51 120.5(8) . . ? C52 C53 C54 119.9(9) . . ? C53 C54 C55 120.8(9) . . ? C50 C55 C54 122.5(8) . . ? C61 C56 C57 118.4(6) . . ? C61 C56 C41 119.2(6) . . ? C57 C56 C41 122.3(5) . . ? C56 C57 C58 121.7(7) . . ? C59 C58 C57 118.2(8) . . ? C60 C59 C58 120.9(8) . . ? C59 C60 C61 121.1(8) . . ? C56 C61 C60 119.4(8) . . ? C63 C62 C67 117.4(6) . . ? C63 C62 C49 120.6(6) . . ? C67 C62 C49 121.2(6) . . ? C62 C63 C64 123.0(8) . . ? C65 C64 C63 119.3(8) . . ? C64 C65 C66 120.0(7) . . ? C65 C66 C67 120.5(8) . . ? C62 C67 C66 119.5(7) . . ? C73 C68 C69 117.7(7) . . ? C73 C68 C49 120.6(7) . . ? C69 C68 C49 121.7(7) . . ? C68 C69 C70 120.9(8) . . ? C71 C70 C69 121.5(9) . . ? C70 C71 C72 117.8(9) . . ? C71 C72 C73 122.5(10) . . ? C68 C73 C72 119.5(8) . . ? Cl4 C74 Cl3 118.9(15) . . ? C76 C75 O6 108.9(13) . . ? O6 C77 C78 98.3(10) . . ? _diffrn_measured_fraction_theta_max 0.649 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.649 _refine_diff_density_max 0.731 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.092 data_mar141a _database_code_CSD 209732 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H35 Cl N3 O3 Os' _chemical_formula_sum 'C37 H35 Cl N3 O3 Os' _chemical_formula_weight 795.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.2165 7.6030 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.468(3) _cell_length_b 20.539(4) _cell_length_c 12.319(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.03(3) _cell_angle_gamma 90.00 _cell_volume 3319.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 3.962 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14506 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3972 _reflns_number_gt 2358 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0815P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3972 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 Os1 Os 0.93113(5) 0.13062(2) 0.78817(4) 0.0528(3) Uani 1 1 d . . . Cl1 Cl 0.9298(3) 0.00117(15) 0.8110(3) 0.0731(12) Uani 1 1 d . . . O1 O 0.7867(7) 0.1115(4) 0.7176(7) 0.059(3) Uani 1 1 d . . . O2 O 1.0736(7) 0.1181(4) 0.8741(6) 0.053(2) Uani 1 1 d . . . O3 O 0.8291(11) 0.1536(5) 1.1475(9) 0.088(4) Uani 1 1 d . . . N1 N 0.9249(9) 0.2109(5) 0.7908(9) 0.069(4) Uani 1 1 d . . . N2 N 0.9697(10) 0.1155(5) 0.6323(9) 0.049(3) Uani 1 1 d . . . N3 N 0.9001(10) 0.1191(5) 0.9492(9) 0.060(3) Uani 1 1 d . . . C1 C 0.7936(15) 0.1189(9) 0.9552(13) 0.111(7) Uani 1 1 d . . . H1A H 0.7578 0.0858 0.9051 0.133 Uiso 1 1 calc R . . H1B H 0.7637 0.1607 0.9297 0.133 Uiso 1 1 calc R . . C2 C 0.7779(16) 0.1058(11) 1.0733(13) 0.130(8) Uani 1 1 d . . . H2A H 0.7057 0.1066 1.0725 0.157 Uiso 1 1 calc R . . H2B H 0.8041 0.0630 1.0981 0.157 Uiso 1 1 calc R . . C3 C 0.9338(15) 0.1527(7) 1.1470(12) 0.080(5) Uani 1 1 d . . . H3A H 0.9617 0.1104 1.1729 0.096 Uiso 1 1 calc R . . H3B H 0.9688 0.1852 1.1990 0.096 Uiso 1 1 calc R . . C4 C 0.9549(12) 0.1658(7) 1.0328(10) 0.064(4) Uani 1 1 d . . . H4A H 0.9336 0.2098 1.0097 0.077 Uiso 1 1 calc R . . H4B H 1.0275 0.1625 1.0372 0.077 Uiso 1 1 calc R . . C5 C 0.7331(11) 0.1297(7) 0.6070(12) 0.064(4) Uani 1 1 d . . . C6 C 0.8071(12) 0.1683(7) 0.5504(11) 0.070(5) Uani 1 1 d . . . H6A H 0.7712 0.1798 0.4754 0.084 Uiso 1 1 calc R . . H6B H 0.8257 0.2085 0.5912 0.084 Uiso 1 1 calc R . . C7 C 0.9052(10) 0.1320(6) 0.5437(10) 0.041(3) Uani 1 1 d . . . C8 C 0.9168(14) 0.1174(8) 0.4368(11) 0.073(5) Uani 1 1 d . . . H8 H 0.8668 0.1284 0.3742 0.087 Uiso 1 1 calc R . . C9 C 1.0052(15) 0.0859(7) 0.4267(13) 0.070(5) Uani 1 1 d . . . H9 H 1.0170 0.0758 0.3571 0.084 Uiso 1 1 calc R . . C10 C 1.0743(12) 0.0703(6) 0.5216(11) 0.062(4) Uani 1 1 d . . . H10 H 1.1331 0.0477 0.5174 0.075 Uiso 1 1 calc R . . C11 C 1.0580(12) 0.0877(6) 0.6233(11) 0.052(4) Uani 1 1 d . . . C12 C 1.1390(11) 0.0702(7) 0.7252(10) 0.062(4) Uani 1 1 d . . . H12A H 1.2026 0.0639 0.7021 0.074 Uiso 1 1 calc R . . H12B H 1.1208 0.0287 0.7529 0.074 Uiso 1 1 calc R . . C13 C 1.1587(10) 0.1199(6) 0.8242(10) 0.048(4) Uani 1 1 d . . . C14' C 0.6367(17) 0.1719(11) 0.599(2) 0.051(8) Uiso 0.50 1 d PG . . C15' C 0.645(2) 0.2125(15) 0.691(2) 0.19(2) Uiso 0.50 1 d PG . . H15' H 0.7030 0.2109 0.7485 0.225 Uiso 0.50 1 calc PR . . C16' C 0.567(3) 0.2554(14) 0.697(2) 0.44(8) Uiso 0.50 1 d PG . . H16' H 0.5722 0.2826 0.7582 0.529 Uiso 0.50 1 calc PR . . C17' C 0.480(2) 0.2578(11) 0.611(2) 0.102(11) Uiso 0.50 1 d PG . . H17' H 0.4276 0.2866 0.6144 0.123 Uiso 0.50 1 calc PR . . C18' C 0.4717(17) 0.2173(13) 0.519(2) 0.130(15) Uiso 0.50 1 d PG . . H18' H 0.4137 0.2189 0.4610 0.156 Uiso 0.50 1 calc PR . . C19' C 0.550(2) 0.1743(11) 0.5128(18) 0.130(14) Uiso 0.50 1 d PG . . H19' H 0.5445 0.1471 0.4513 0.156 Uiso 0.50 1 calc PR . . C14 C 0.652(2) 0.1758(17) 0.652(3) 0.108(14) Uiso 0.50 1 d PG . . C15 C 0.645(2) 0.2428(18) 0.636(3) 0.20(3) Uiso 0.50 1 d PG . . H15 H 0.6894 0.2639 0.5997 0.245 Uiso 0.50 1 calc PR . . C16 C 0.573(3) 0.2783(13) 0.675(2) 0.135(17) Uiso 0.50 1 d PG . . H16 H 0.5682 0.3231 0.6650 0.162 Uiso 0.50 1 calc PR . . C17 C 0.507(2) 0.247(2) 0.730(3) 0.167(19) Uiso 0.50 1 d PG . . H17 H 0.4581 0.2704 0.7563 0.200 Uiso 0.50 1 calc PR . . C18 C 0.513(3) 0.180(2) 0.746(3) 0.28(3) Uiso 0.50 1 d PG . . H18 H 0.4693 0.1586 0.7823 0.338 Uiso 0.50 1 calc PR . . C19 C 0.586(3) 0.1442(13) 0.707(3) 0.18(2) Uiso 0.50 1 d PG . . H19 H 0.5905 0.0994 0.7170 0.220 Uiso 0.50 1 calc PR . . C20 C 0.6947(11) 0.0687(9) 0.5425(11) 0.070(5) Uani 1 1 d . . . C21 C 0.659(2) 0.0680(12) 0.4252(17) 0.165(11) Uani 1 1 d . . . H21 H 0.6642 0.1051 0.3834 0.197 Uiso 1 1 calc R . . C22 C 0.617(2) 0.0101(15) 0.373(2) 0.172(13) Uani 1 1 d . . . H22 H 0.5872 0.0114 0.2967 0.206 Uiso 1 1 calc R . . C23 C 0.6172(17) -0.0434(12) 0.423(2) 0.120(8) Uani 1 1 d . . . H23 H 0.5945 -0.0811 0.3836 0.145 Uiso 1 1 calc R . . C24 C 0.6496(15) -0.0455(9) 0.5314(17) 0.105(6) Uani 1 1 d . . . H24 H 0.6433 -0.0838 0.5696 0.126 Uiso 1 1 calc R . . C25 C 0.6930(14) 0.0085(8) 0.5891(14) 0.090(6) Uani 1 1 d . . . H25 H 0.7230 0.0037 0.6645 0.108 Uiso 1 1 calc R . . C26 C 1.1743(11) 0.1893(7) 0.7880(10) 0.057(4) Uani 1 1 d . . . C27 C 1.2079(12) 0.2038(8) 0.6929(12) 0.074(5) Uani 1 1 d . . . H27 H 1.2168 0.1711 0.6438 0.089 Uiso 1 1 calc R . . C28 C 1.2288(13) 0.2703(9) 0.6714(14) 0.089(6) Uani 1 1 d . . . H28 H 1.2488 0.2809 0.6061 0.107 Uiso 1 1 calc R . . C29 C 1.2201(13) 0.3178(9) 0.7434(15) 0.088(5) Uani 1 1 d . . . H29 H 1.2400 0.3600 0.7309 0.105 Uiso 1 1 calc R . . C30 C 1.1819(12) 0.3044(7) 0.8359(14) 0.078(5) Uani 1 1 d . . . H30 H 1.1705 0.3375 0.8831 0.094 Uiso 1 1 calc R . . C31 C 1.1611(10) 0.2400(7) 0.8562(11) 0.061(4) Uani 1 1 d . . . H31 H 1.1369 0.2306 0.9194 0.074 Uiso 1 1 calc R . . C32 C 1.2504(16) 0.0984(7) 0.9088(11) 0.068(5) Uani 1 1 d . . . C33 C 1.3448(16) 0.1062(9) 0.8858(15) 0.091(6) Uani 1 1 d . . . H33 H 1.3512 0.1256 0.8195 0.109 Uiso 1 1 calc R . . C34 C 1.4309(18) 0.0846(11) 0.963(2) 0.127(7) Uani 1 1 d . . . H34 H 1.4956 0.0887 0.9487 0.152 Uiso 1 1 calc R . . C35 C 1.416(2) 0.0556(11) 1.0656(19) 0.127(10) Uani 1 1 d . . . H35 H 1.4718 0.0398 1.1175 0.152 Uiso 1 1 calc R . . C36 C 1.326(2) 0.0514(11) 1.0858(19) 0.125(9) Uani 1 1 d . . . H36 H 1.3182 0.0359 1.1543 0.150 Uiso 1 1 calc R . . C37 C 1.2403(15) 0.0701(8) 1.0053(13) 0.083(5) Uani 1 1 d . . . H37 H 1.1756 0.0631 1.0179 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0708(5) 0.0466(4) 0.0450(4) -0.0001(3) 0.0213(3) -0.0002(4) Cl1 0.112(4) 0.037(2) 0.080(3) -0.0041(16) 0.042(2) 0.000(2) O1 0.055(7) 0.067(6) 0.055(6) -0.009(4) 0.015(5) -0.023(5) O2 0.062(7) 0.054(6) 0.040(5) 0.008(4) 0.003(5) 0.015(5) O3 0.118(12) 0.094(9) 0.063(7) -0.009(6) 0.041(7) 0.001(7) N1 0.098(11) 0.022(6) 0.085(8) 0.014(5) 0.020(7) 0.005(6) N2 0.050(9) 0.049(8) 0.044(7) 0.007(5) 0.001(7) 0.000(6) N3 0.086(10) 0.051(8) 0.056(8) -0.009(5) 0.040(7) -0.009(7) C1 0.117(19) 0.16(2) 0.059(12) -0.032(10) 0.030(11) -0.045(14) C2 0.16(2) 0.19(2) 0.059(12) -0.028(12) 0.057(12) -0.069(17) C3 0.115(18) 0.073(11) 0.057(11) -0.004(7) 0.032(10) 0.015(10) C4 0.085(13) 0.066(10) 0.045(9) -0.007(7) 0.021(8) 0.001(9) C5 0.061(11) 0.057(9) 0.070(10) 0.012(8) 0.004(8) -0.007(9) C6 0.083(14) 0.071(10) 0.049(9) 0.013(7) 0.001(8) -0.028(10) C7 0.048(10) 0.046(8) 0.032(8) 0.005(6) 0.017(7) 0.006(8) C8 0.078(14) 0.098(13) 0.038(9) 0.001(7) 0.005(8) -0.040(11) C9 0.093(15) 0.070(11) 0.061(12) -0.003(8) 0.043(11) -0.019(10) C10 0.085(13) 0.072(10) 0.035(9) 0.003(7) 0.021(9) -0.007(9) C11 0.053(12) 0.053(9) 0.049(10) 0.007(7) 0.007(8) -0.007(8) C12 0.057(11) 0.070(10) 0.064(10) -0.003(7) 0.027(8) 0.008(8) C13 0.050(10) 0.055(10) 0.044(8) -0.009(6) 0.020(7) 0.007(7) C20 0.053(12) 0.103(14) 0.048(10) 0.003(9) -0.003(8) -0.017(10) C21 0.21(3) 0.15(2) 0.094(16) 0.041(14) -0.043(17) -0.07(2) C22 0.22(3) 0.15(2) 0.110(19) 0.006(19) -0.043(19) -0.06(2) C23 0.108(19) 0.12(2) 0.12(2) -0.057(15) -0.001(16) -0.001(16) C24 0.120(19) 0.084(14) 0.098(15) -0.021(11) -0.002(13) -0.014(12) C25 0.116(17) 0.062(11) 0.081(12) -0.004(9) -0.002(11) -0.004(11) C26 0.069(12) 0.067(10) 0.035(8) 0.006(7) 0.012(7) 0.003(8) C27 0.067(13) 0.087(12) 0.067(11) -0.004(8) 0.013(9) -0.019(9) C28 0.075(14) 0.120(16) 0.070(12) 0.012(11) 0.009(10) -0.037(12) C29 0.096(16) 0.081(13) 0.085(13) 0.002(10) 0.019(11) -0.029(11) C30 0.073(14) 0.056(11) 0.106(13) -0.006(9) 0.019(11) 0.008(9) C31 0.050(11) 0.073(11) 0.067(10) -0.004(8) 0.025(8) 0.003(8) C32 0.093(17) 0.073(10) 0.031(9) 0.002(7) -0.003(9) 0.027(10) C33 0.055(14) 0.110(15) 0.093(14) 0.007(10) -0.017(13) 0.018(11) C34 0.10(2) 0.129(19) 0.14(2) -0.009(15) 0.001(17) 0.012(15) C35 0.17(3) 0.108(17) 0.076(16) -0.011(12) -0.028(17) 0.065(19) C36 0.15(3) 0.14(2) 0.083(16) 0.004(12) 0.008(19) 0.06(2) C37 0.097(15) 0.086(12) 0.059(10) -0.006(9) 0.001(10) 0.042(11) _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 Os1 N1 1.652(9) . ? Os1 O1 1.983(9) . ? Os1 O2 1.988(9) . ? Os1 N2 2.122(11) . ? Os1 N3 2.130(10) . ? Os1 Cl1 2.674(3) . ? O1 C5 1.440(15) . ? O2 C13 1.417(15) . ? O3 C2 1.411(18) . ? O3 C3 1.412(19) . ? N2 C7 1.278(15) . ? N2 C11 1.346(16) . ? N3 C1 1.45(2) . ? N3 C4 1.478(16) . ? C1 C2 1.54(2) . ? C3 C4 1.521(18) . ? C5 C20 1.511(19) . ? C5 C14' 1.55(2) . ? C5 C6 1.556(18) . ? C5 C14 1.63(3) . ? C6 C7 1.535(19) . ? C7 C8 1.394(18) . ? C8 C9 1.38(2) . ? C9 C10 1.358(19) . ? C10 C11 1.367(17) . ? C11 C12 1.510(17) . ? C12 C13 1.567(16) . ? C13 C32 1.493(19) . ? C13 C26 1.523(17) . ? C14' C15' 1.3900 . ? C14' C19' 1.3900 . ? C15' C16' 1.3900 . ? C16' C17' 1.3900 . ? C17' C18' 1.3900 . ? C18' C19' 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C20 C25 1.367(19) . ? C20 C21 1.42(2) . ? C21 C22 1.41(3) . ? C22 C23 1.26(3) . ? C23 C24 1.31(2) . ? C24 C25 1.37(2) . ? C26 C31 1.375(17) . ? C26 C27 1.380(17) . ? C27 C28 1.43(2) . ? C28 C29 1.34(2) . ? C29 C30 1.38(2) . ? C30 C31 1.385(18) . ? C32 C37 1.36(2) . ? C32 C33 1.37(2) . ? C33 C34 1.39(2) . ? C34 C35 1.46(3) . ? C35 C36 1.30(3) . ? C36 C37 1.39(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 Os1 O1 99.0(5) . . ? N1 Os1 O2 99.5(5) . . ? O1 Os1 O2 160.3(3) . . ? N1 Os1 N2 100.8(5) . . ? O1 Os1 N2 89.5(4) . . ? O2 Os1 N2 93.4(4) . . ? N1 Os1 N3 94.0(4) . . ? O1 Os1 N3 90.4(4) . . ? O2 Os1 N3 81.9(4) . . ? N2 Os1 N3 165.0(4) . . ? N1 Os1 Cl1 171.4(4) . . ? O1 Os1 Cl1 79.6(3) . . ? O2 Os1 Cl1 81.1(2) . . ? N2 Os1 Cl1 87.6(3) . . ? N3 Os1 Cl1 77.6(3) . . ? C5 O1 Os1 126.6(8) . . ? C13 O2 Os1 122.9(7) . . ? C2 O3 C3 109.3(13) . . ? C7 N2 C11 119.0(11) . . ? C7 N2 Os1 118.5(9) . . ? C11 N2 Os1 122.5(9) . . ? C1 N3 C4 108.0(11) . . ? C1 N3 Os1 116.8(10) . . ? C4 N3 Os1 113.9(8) . . ? N3 C1 C2 113.3(16) . . ? O3 C2 C1 109.8(15) . . ? O3 C3 C4 113.3(14) . . ? N3 C4 C3 111.2(12) . . ? O1 C5 C20 108.7(11) . . ? O1 C5 C14' 116.1(14) . . ? C20 C5 C14' 104.4(15) . . ? O1 C5 C6 108.8(11) . . ? C20 C5 C6 111.4(12) . . ? C14' C5 C6 107.4(13) . . ? O1 C5 C14 93.4(15) . . ? C20 C5 C14 118.8(17) . . ? C14' C5 C14 23.1(14) . . ? C6 C5 C14 113.7(18) . . ? C7 C6 C5 115.0(11) . . ? N2 C7 C8 123.4(14) . . ? N2 C7 C6 120.7(11) . . ? C8 C7 C6 115.9(13) . . ? C9 C8 C7 117.8(14) . . ? C10 C9 C8 118.0(14) . . ? C9 C10 C11 120.4(15) . . ? N2 C11 C10 120.9(13) . . ? N2 C11 C12 121.3(12) . . ? C10 C11 C12 117.6(14) . . ? C11 C12 C13 117.1(11) . . ? O2 C13 C32 108.2(12) . . ? O2 C13 C26 109.3(10) . . ? C32 C13 C26 109.5(12) . . ? O2 C13 C12 108.1(11) . . ? C32 C13 C12 108.6(11) . . ? C26 C13 C12 113.1(10) . . ? C15' C14' C19' 120.0 . . ? C15' C14' C5 111.8(19) . . ? C19' C14' C5 128.2(19) . . ? C16' C15' C14' 120.0 . . ? C17' C16' C15' 120.0 . . ? C16' C17' C18' 120.0 . . ? C19' C18' C17' 120.0 . . ? C18' C19' C14' 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 C5 124(3) . . ? C19 C14 C5 116(3) . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C14 120.0 . . ? C25 C20 C21 112.7(16) . . ? C25 C20 C5 124.5(13) . . ? C21 C20 C5 122.8(16) . . ? C22 C21 C20 119.1(19) . . ? C23 C22 C21 123(2) . . ? C22 C23 C24 120(2) . . ? C23 C24 C25 120(2) . . ? C20 C25 C24 124.0(17) . . ? C31 C26 C27 117.9(14) . . ? C31 C26 C13 119.0(12) . . ? C27 C26 C13 123.0(13) . . ? C26 C27 C28 118.6(15) . . ? C29 C28 C27 121.5(16) . . ? C28 C29 C30 120.3(16) . . ? C29 C30 C31 118.0(15) . . ? C26 C31 C30 123.5(14) . . ? C37 C32 C33 120.8(17) . . ? C37 C32 C13 120.6(18) . . ? C33 C32 C13 118.7(15) . . ? C32 C33 C34 119(2) . . ? C33 C34 C35 118(2) . . ? C36 C35 C34 121(2) . . ? C35 C36 C37 120(2) . . ? C32 C37 C36 121(2) . . ? _diffrn_measured_fraction_theta_max 0.659 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.659 _refine_diff_density_max 0.877 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.228 data_mar156 _database_code_CSD 209733 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39.25 H40 Cl1.50 N3 O2.25 Os' _chemical_formula_sum 'C39.25 H40 Cl1.50 N3 O2.25 Os' _chemical_formula_weight 833.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.2165 7.6030 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.177(3) _cell_length_b 20.538(4) _cell_length_c 27.433(6) _cell_angle_alpha 101.49(3) _cell_angle_beta 103.64(3) _cell_angle_gamma 109.64(3) _cell_volume 7455(3) _cell_formula_units_Z 8 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 3.565 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16416 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.49 _reflns_number_total 12904 _reflns_number_gt 8060 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.1143P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12904 _refine_ls_number_parameters 909 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.002 _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 Os1 Os 0.59909(4) 0.17906(4) 0.64798(3) 0.0595(2) Uani 1 1 d . . . Os2 Os 0.23873(4) 0.31206(4) 0.86201(3) 0.0573(2) Uani 1 1 d . . . Os3 Os 0.82854(4) 0.55438(4) 0.61006(3) 0.0549(2) Uani 1 1 d . . . Os4 Os 0.16784(4) 0.92792(4) 0.89425(2) 0.0533(2) Uani 1 1 d . . . Cl1 Cl 0.6317(3) 0.1263(2) 0.72841(18) 0.0747(13) Uani 1 1 d . . . Cl2 Cl 0.2237(3) 0.3867(2) 0.79153(18) 0.0741(13) Uani 1 1 d . . . Cl3 Cl 0.8555(3) 0.6224(2) 0.53531(18) 0.0723(13) Uani 1 1 d . . . Cl4 Cl 0.1529(3) 0.8826(2) 0.97742(17) 0.0689(12) Uani 1 1 d . . . Cl5 Cl 0.5892(10) 0.3923(7) 0.2279(6) 0.303(6) Uiso 1 1 d . . . Cl6 Cl 0.5562(19) 0.4024(13) 0.1217(11) 0.474(13) Uiso 1 1 d . . . O1 O 0.6067(7) 0.0875(6) 0.6127(4) 0.069(3) Uani 1 1 d . . . O2 O 0.5882(7) 0.2508(6) 0.7037(4) 0.062(3) Uani 1 1 d . . . O3 O 0.2501(7) 0.2516(6) 0.8007(4) 0.061(3) Uani 1 1 d . . . O4 O 0.2318(7) 0.3982(6) 0.9050(4) 0.063(3) Uani 1 1 d . . . O5 O 0.7089(7) 0.4938(6) 0.5493(4) 0.058(3) Uani 1 1 d . . . O6 O 0.9531(7) 0.6404(6) 0.6500(4) 0.064(3) Uani 1 1 d . . . O7 O 0.0456(6) 0.8400(5) 0.8601(4) 0.057(3) Uani 1 1 d . . . O8 O 0.2931(7) 1.0021(6) 0.9497(4) 0.055(3) Uani 1 1 d . . . N1 N 0.5632(9) 0.2012(7) 0.5952(5) 0.065(4) Uani 1 1 d . . . N2 N 0.7542(9) 0.2403(8) 0.6712(5) 0.061(4) Uani 1 1 d . . . N3 N 0.4517(8) 0.1175(7) 0.6437(5) 0.059(4) Uani 1 1 d . . . N4 N 0.2642(9) 0.2740(7) 0.9068(5) 0.069(4) Uani 1 1 d . . . N5 N 0.0834(8) 0.2532(7) 0.8314(5) 0.058(3) Uani 1 1 d . . . N6 N 0.3899(9) 0.3810(9) 0.8785(6) 0.081(4) Uani 1 1 d . . . N7 N 0.8081(8) 0.5218(7) 0.6573(5) 0.064(4) Uani 1 1 d . . . N8 N 0.9005(8) 0.4907(7) 0.5808(5) 0.058(3) Uani 1 1 d . . . N9 N 0.7469(8) 0.6204(7) 0.6168(5) 0.062(4) Uani 1 1 d . . . N10 N 0.1864(8) 0.9484(6) 0.8421(5) 0.054(3) Uani 1 1 d . . . N11 N 0.0940(8) 0.9932(8) 0.9145(5) 0.061(4) Uani 1 1 d . . . N12 N 0.2532(9) 0.8643(7) 0.8946(5) 0.065(4) Uani 1 1 d . . . C1 C 0.6930(11) 0.0905(9) 0.6004(6) 0.063(4) Uiso 1 1 d . . . C2 C 0.7846(12) 0.1317(10) 0.6530(7) 0.080(5) Uiso 1 1 d . . . H2A H 0.7672 0.1130 0.6807 0.096 Uiso 1 1 calc R . . H2B H 0.8393 0.1201 0.6478 0.096 Uiso 1 1 calc R . . C3 C 0.8195(12) 0.2114(10) 0.6712(6) 0.064(4) Uiso 1 1 d . . . C4 C 0.9207(12) 0.2525(10) 0.6906(7) 0.074(5) Uiso 1 1 d . . . H4 H 0.9659 0.2310 0.6912 0.089 Uiso 1 1 calc R . . C5 C 0.9505(15) 0.3246(12) 0.7085(8) 0.091(6) Uiso 1 1 d . . . H5 H 1.0180 0.3539 0.7219 0.109 Uiso 1 1 calc R . . C6 C 0.8838(13) 0.3567(11) 0.7074(7) 0.088(6) Uiso 1 1 d . . . H6 H 0.9062 0.4070 0.7195 0.106 Uiso 1 1 calc R . . C7 C 0.7861(12) 0.3148(10) 0.6886(6) 0.063(4) Uiso 1 1 d . . . C8 C 0.7109(11) 0.3480(9) 0.6835(6) 0.066(4) Uiso 1 1 d . . . H8A H 0.6712 0.3328 0.6467 0.080 Uiso 1 1 calc R . . H8B H 0.7454 0.4004 0.6948 0.080 Uiso 1 1 calc R . . C9 C 0.6375(12) 0.3252(10) 0.7178(6) 0.063(4) Uiso 1 1 d . . . C10 C 0.7039(12) 0.1171(9) 0.5555(6) 0.068(5) Uiso 1 1 d . . . C11 C 0.7920(13) 0.1531(9) 0.5509(7) 0.079(5) Uiso 1 1 d . . . H11 H 0.8497 0.1615 0.5771 0.095 Uiso 1 1 calc R . . C12 C 0.7994(14) 0.1790(11) 0.5064(8) 0.098(6) Uiso 1 1 d . . . H12 H 0.8604 0.2033 0.5030 0.118 Uiso 1 1 calc R . . C13 C 0.7161(15) 0.1668(11) 0.4710(8) 0.101(6) Uiso 1 1 d . . . H13 H 0.7193 0.1826 0.4417 0.122 Uiso 1 1 calc R . . C14 C 0.6324(14) 0.1351(10) 0.4743(8) 0.090(6) Uiso 1 1 d . . . H14 H 0.5762 0.1295 0.4482 0.108 Uiso 1 1 calc R . . C15 C 0.6221(13) 0.1088(10) 0.5154(7) 0.086(5) Uiso 1 1 d . . . H15 H 0.5590 0.0847 0.5165 0.103 Uiso 1 1 calc R . . C16 C 0.6786(13) 0.0072(10) 0.5898(7) 0.080(5) Uiso 1 1 d . . . C17 C 0.6469(14) -0.0290(12) 0.6201(9) 0.105(7) Uiso 1 1 d . . . H17 H 0.6336 -0.0073 0.6490 0.126 Uiso 1 1 calc R . . C18 C 0.6327(16) -0.1043(13) 0.6077(10) 0.121(7) Uiso 1 1 d . . . H18 H 0.6025 -0.1331 0.6262 0.146 Uiso 1 1 calc R . . C19 C 0.6613(17) -0.1319(15) 0.5715(10) 0.138(9) Uiso 1 1 d . . . H19 H 0.6563 -0.1793 0.5667 0.166 Uiso 1 1 calc R . . C20 C 0.6981(19) -0.0958(16) 0.5401(12) 0.165(10) Uiso 1 1 d . . . H20 H 0.7153 -0.1176 0.5128 0.198 Uiso 1 1 calc R . . C21 C 0.7099(16) -0.0173(14) 0.5517(10) 0.127(8) Uiso 1 1 d . . . H21 H 0.7378 0.0121 0.5329 0.153 Uiso 1 1 calc R . . C22 C 0.7043(11) 0.3544(10) 0.7773(7) 0.067(5) Uiso 1 1 d . . . C23 C 0.7026(13) 0.3083(12) 0.8070(8) 0.090(6) Uiso 1 1 d . . . H23 H 0.6661 0.2587 0.7911 0.108 Uiso 1 1 calc R . . C24 C 0.7549(14) 0.3348(12) 0.8609(8) 0.093(6) Uiso 1 1 d . . . H24 H 0.7514 0.3018 0.8799 0.112 Uiso 1 1 calc R . . C25 C 0.8125(14) 0.4085(11) 0.8878(8) 0.093(6) Uiso 1 1 d . . . H25 H 0.8465 0.4251 0.9238 0.111 Uiso 1 1 calc R . . C26 C 0.8155(15) 0.4529(14) 0.8589(9) 0.115(7) Uiso 1 1 d . . . H26 H 0.8545 0.5021 0.8752 0.138 Uiso 1 1 calc R . . C27 C 0.7631(15) 0.4299(13) 0.8054(9) 0.105(6) Uiso 1 1 d . . . H27 H 0.7662 0.4640 0.7874 0.126 Uiso 1 1 calc R . . C28 C 0.5662(11) 0.3589(9) 0.7092(6) 0.058(4) Uiso 1 1 d . . . C29 C 0.4876(14) 0.3337(11) 0.7240(7) 0.089(6) Uiso 1 1 d . . . H29 H 0.4797 0.2948 0.7375 0.107 Uiso 1 1 calc R . . C30 C 0.4188(15) 0.3616(11) 0.7206(8) 0.101(6) Uiso 1 1 d . . . H30 H 0.3686 0.3438 0.7345 0.121 Uiso 1 1 calc R . . C31 C 0.4190(15) 0.4122(12) 0.6987(8) 0.113(7) Uiso 1 1 d . . . H31 H 0.3671 0.4272 0.6935 0.135 Uiso 1 1 calc R . . C32 C 0.5040(15) 0.4442(12) 0.6827(8) 0.110(7) Uiso 1 1 d . . . H32 H 0.5107 0.4820 0.6681 0.132 Uiso 1 1 calc R . . C33 C 0.5752(14) 0.4152(11) 0.6905(7) 0.090(6) Uiso 1 1 d . . . H33 H 0.6320 0.4362 0.6821 0.109 Uiso 1 1 calc R . . C34 C 0.4096(13) 0.0375(10) 0.6182(8) 0.083(5) Uiso 1 1 d . . . H34A H 0.4555 0.0178 0.6333 0.100 Uiso 1 1 calc R . . H34B H 0.4006 0.0274 0.5808 0.100 Uiso 1 1 calc R . . C35 C 0.3117(15) 0.0013(12) 0.6257(9) 0.124(8) Uiso 1 1 d . . . H35A H 0.3206 0.0108 0.6630 0.149 Uiso 1 1 calc R . . H35B H 0.2860 -0.0508 0.6096 0.149 Uiso 1 1 calc R . . C36 C 0.2384(15) 0.0308(12) 0.6005(9) 0.112(7) Uiso 1 1 d . . . H36A H 0.2274 0.0195 0.5629 0.134 Uiso 1 1 calc R . . H36B H 0.1755 0.0081 0.6056 0.134 Uiso 1 1 calc R . . C37 C 0.2779(13) 0.1088(10) 0.6242(8) 0.094(6) Uiso 1 1 d . . . H37A H 0.2817 0.1194 0.6610 0.113 Uiso 1 1 calc R . . H37B H 0.2333 0.1278 0.6066 0.113 Uiso 1 1 calc R . . C38 C 0.3842(13) 0.1478(10) 0.6205(7) 0.089(6) Uiso 1 1 d . . . H38A H 0.3794 0.1419 0.5838 0.107 Uiso 1 1 calc R . . H38B H 0.4101 0.1993 0.6387 0.107 Uiso 1 1 calc R . . C39 C 0.1931(11) 0.1771(9) 0.7778(6) 0.051(4) Uiso 1 1 d . . . C40 C 0.1232(11) 0.1458(9) 0.8077(6) 0.067(5) Uiso 1 1 d . . . H40A H 0.0872 0.0940 0.7908 0.080 Uiso 1 1 calc R . . H40B H 0.1624 0.1532 0.8434 0.080 Uiso 1 1 calc R . . C41 C 0.0515(12) 0.1797(11) 0.8097(7) 0.066(5) Uiso 1 1 d . . . C42 C -0.0485(12) 0.1392(10) 0.7898(6) 0.073(5) Uiso 1 1 d . . . H42 H -0.0724 0.0892 0.7748 0.087 Uiso 1 1 calc R . . C43 C -0.1149(13) 0.1721(10) 0.7920(7) 0.078(5) Uiso 1 1 d . . . H43 H -0.1827 0.1441 0.7783 0.094 Uiso 1 1 calc R . . C44 C -0.0812(12) 0.2440(10) 0.8137(6) 0.068(5) Uiso 1 1 d . . . H44 H -0.1250 0.2664 0.8150 0.081 Uiso 1 1 calc R . . C45 C 0.0177(12) 0.2833(9) 0.8339(6) 0.065(4) Uiso 1 1 d . . . C46 C 0.0590(11) 0.3664(9) 0.8603(6) 0.069(5) Uiso 1 1 d . . . H46A H 0.0813 0.3902 0.8356 0.083 Uiso 1 1 calc R . . H46B H 0.0045 0.3782 0.8656 0.083 Uiso 1 1 calc R . . C47 C 0.1420(12) 0.3991(10) 0.9117(7) 0.071(5) Uiso 1 1 d . . . C48 C 0.2693(11) 0.1407(9) 0.7796(6) 0.056(4) Uiso 1 1 d . . . C49 C 0.3601(11) 0.1795(9) 0.7752(6) 0.059(4) Uiso 1 1 d . . . H49 H 0.3747 0.2256 0.7715 0.071 Uiso 1 1 calc R . . C50 C 0.4269(12) 0.1494(10) 0.7764(7) 0.075(5) Uiso 1 1 d . . . H50 H 0.4886 0.1774 0.7753 0.090 Uiso 1 1 calc R . . C51 C 0.4109(13) 0.0817(10) 0.7790(7) 0.080(5) Uiso 1 1 d . . . H51 H 0.4586 0.0630 0.7779 0.096 Uiso 1 1 calc R . . C52 C 0.3258(14) 0.0428(11) 0.7833(7) 0.098(6) Uiso 1 1 d . . . H52 H 0.3154 -0.0028 0.7874 0.117 Uiso 1 1 calc R . . C53 C 0.2488(13) 0.0686(10) 0.7818(7) 0.085(5) Uiso 1 1 d . . . H53 H 0.1873 0.0393 0.7822 0.102 Uiso 1 1 calc R . . C54 C 0.1327(12) 0.1585(11) 0.7201(7) 0.073(5) Uiso 1 1 d . . . C55 C 0.1463(13) 0.2144(11) 0.6977(7) 0.085(5) Uiso 1 1 d . . . H55 H 0.1867 0.2627 0.7166 0.102 Uiso 1 1 calc R . . C56 C 0.0844(16) 0.1868(13) 0.6350(9) 0.113(7) Uiso 1 1 d . . . H56 H 0.0918 0.2184 0.6148 0.136 Uiso 1 1 calc R . . C57 C 0.0276(14) 0.1228(12) 0.6157(8) 0.095(6) Uiso 1 1 d . . . H57 H -0.0144 0.1099 0.5815 0.114 Uiso 1 1 calc R . . C58 C 0.0183(15) 0.0718(14) 0.6358(9) 0.116(7) Uiso 1 1 d . . . H58 H -0.0224 0.0244 0.6148 0.139 Uiso 1 1 calc R . . C59 C 0.0675(15) 0.0848(13) 0.6885(9) 0.103(6) Uiso 1 1 d . . . H59 H 0.0587 0.0470 0.7032 0.124 Uiso 1 1 calc R . . C60 C 0.1593(11) 0.4776(9) 0.9346(6) 0.060(4) Uiso 1 1 d . . . C61 C 0.2408(15) 0.5281(12) 0.9347(8) 0.097(6) Uiso 1 1 d . . . H61 H 0.2894 0.5170 0.9242 0.117 Uiso 1 1 calc R . . C62 C 0.2489(17) 0.5972(13) 0.9511(9) 0.113(7) Uiso 1 1 d . . . H62 H 0.3060 0.6354 0.9535 0.135 Uiso 1 1 calc R . . C63 C 0.1724(19) 0.6121(14) 0.9645(10) 0.134(9) Uiso 1 1 d . . . H63 H 0.1803 0.6602 0.9750 0.161 Uiso 1 1 calc R . . C64 C 0.0937(15) 0.5637(12) 0.9631(8) 0.099(6) Uiso 1 1 d . . . H64 H 0.0426 0.5747 0.9705 0.119 Uiso 1 1 calc R . . C65 C 0.0875(14) 0.4961(12) 0.9506(8) 0.094(6) Uiso 1 1 d . . . H65 H 0.0332 0.4595 0.9524 0.113 Uiso 1 1 calc R . . C66 C 0.1162(12) 0.3579(9) 0.9519(6) 0.067(5) Uiso 1 1 d . . . C67 C 0.1925(13) 0.3591(10) 0.9910(7) 0.084(5) Uiso 1 1 d . . . H67 H 0.2565 0.3833 0.9911 0.101 Uiso 1 1 calc R . . C68 C 0.1823(17) 0.3272(12) 1.0305(10) 0.128(8) Uiso 1 1 d . . . H68 H 0.2349 0.3308 1.0579 0.154 Uiso 1 1 calc R . . C69 C 0.0725(15) 0.2849(11) 1.0231(9) 0.107(7) Uiso 1 1 d . . . H69 H 0.0603 0.2603 1.0474 0.129 Uiso 1 1 calc R . . C70 C -0.0045(18) 0.2793(13) 0.9876(10) 0.131(8) Uiso 1 1 d . . . H70 H -0.0693 0.2522 0.9850 0.157 Uiso 1 1 calc R . . C71 C 0.0236(13) 0.3222(9) 0.9507(7) 0.082(5) Uiso 1 1 d . . . H71 H -0.0275 0.3239 0.9252 0.098 Uiso 1 1 calc R . . C72 C 0.449(2) 0.354(2) 0.8501(14) 0.074(10) Uiso 0.50 1 d P . . C72' C 0.432(4) 0.453(3) 0.914(2) 0.147(19) Uiso 0.50 1 d P . . C73' C 0.551(5) 0.491(3) 0.903(3) 0.18(2) Uiso 0.50 1 d P . . C73 C 0.553(3) 0.417(2) 0.8611(15) 0.087(11) Uiso 0.50 1 d P . . C74 C 0.609(2) 0.4448(18) 0.9242(12) 0.162(10) Uiso 1 1 d . . . C75' C 0.562(3) 0.371(3) 0.8909(19) 0.111(14) Uiso 0.50 1 d P . . C75 C 0.560(3) 0.466(2) 0.9590(16) 0.101(13) Uiso 0.50 1 d P . . C76 C 0.444(3) 0.402(2) 0.9410(15) 0.086(11) Uiso 0.50 1 d P . . C76' C 0.459(3) 0.335(2) 0.8890(17) 0.094(12) Uiso 0.50 1 d P . . C77 C 0.6722(10) 0.4168(9) 0.5277(6) 0.051(4) Uiso 1 1 d . . . C78 C 0.7383(11) 0.3859(9) 0.5589(6) 0.068(5) Uiso 1 1 d . . . H78A H 0.7387 0.3967 0.5951 0.082 Uiso 1 1 calc R . . H78B H 0.7109 0.3336 0.5438 0.082 Uiso 1 1 calc R . . C79 C 0.8423(13) 0.4173(11) 0.5583(7) 0.071(5) Uiso 1 1 d . . . C80 C 0.8829(14) 0.3740(11) 0.5333(7) 0.089(6) Uiso 1 1 d . . . H80 H 0.8465 0.3243 0.5177 0.106 Uiso 1 1 calc R . . C81 C 0.9757(14) 0.4059(11) 0.5324(7) 0.088(6) Uiso 1 1 d . . . H81 H 1.0013 0.3782 0.5136 0.106 Uiso 1 1 calc R . . C82 C 1.0328(13) 0.4772(10) 0.5582(7) 0.078(5) Uiso 1 1 d . . . H82 H 1.0986 0.4967 0.5597 0.094 Uiso 1 1 calc R . . C83 C 0.9939(12) 0.5206(9) 0.5822(6) 0.063(4) Uiso 1 1 d . . . C84 C 1.0577(11) 0.5991(8) 0.6086(6) 0.059(4) Uiso 1 1 d . . . H84A H 1.0446 0.6249 0.5836 0.071 Uiso 1 1 calc R . . H84B H 1.1261 0.6049 0.6154 0.071 Uiso 1 1 calc R . . C85 C 1.0488(10) 0.6369(9) 0.6601(6) 0.054(4) Uiso 1 1 d . . . C86 C 0.5657(10) 0.3846(9) 0.5313(6) 0.055(4) Uiso 1 1 d . . . C87 C 0.5248(13) 0.3203(10) 0.5424(7) 0.082(5) Uiso 1 1 d . . . H87 H 0.5615 0.2927 0.5483 0.099 Uiso 1 1 calc R . . C88 C 0.4336(15) 0.2979(11) 0.5447(8) 0.101(6) Uiso 1 1 d . . . H88 H 0.4082 0.2549 0.5528 0.121 Uiso 1 1 calc R . . C89 C 0.3766(15) 0.3344(11) 0.5359(8) 0.098(6) Uiso 1 1 d . . . H89 H 0.3135 0.3174 0.5386 0.118 Uiso 1 1 calc R . . C90 C 0.4122(14) 0.3987(11) 0.5225(8) 0.094(6) Uiso 1 1 d . . . H90 H 0.3725 0.4236 0.5141 0.113 Uiso 1 1 calc R . . C91 C 0.5104(12) 0.4238(10) 0.5225(7) 0.080(5) Uiso 1 1 d . . . H91 H 0.5381 0.4678 0.5162 0.096 Uiso 1 1 calc R . . C92 C 0.6655(11) 0.3976(10) 0.4699(6) 0.062(4) Uiso 1 1 d . . . C93 C 0.6280(14) 0.3250(12) 0.4400(8) 0.100(6) Uiso 1 1 d . . . H93 H 0.6066 0.2890 0.4556 0.120 Uiso 1 1 calc R . . C94 C 0.6216(16) 0.3042(14) 0.3851(10) 0.127(8) Uiso 1 1 d . . . H94 H 0.5957 0.2558 0.3650 0.152 Uiso 1 1 calc R . . C95 C 0.6546(15) 0.3579(13) 0.3646(10) 0.112(7) Uiso 1 1 d . . . H95 H 0.6583 0.3470 0.3307 0.134 Uiso 1 1 calc R . . C96 C 0.6811(12) 0.4239(11) 0.3908(7) 0.087(6) Uiso 1 1 d . . . H96 H 0.6938 0.4586 0.3733 0.105 Uiso 1 1 calc R . . C97 C 0.6926(11) 0.4481(10) 0.4459(6) 0.069(5) Uiso 1 1 d . . . H97 H 0.7180 0.4973 0.4642 0.083 Uiso 1 1 calc R . . C98 C 1.1277(12) 0.7145(10) 0.6813(6) 0.065(4) Uiso 1 1 d . . . C99 C 1.106(2) 0.7693(16) 0.6685(11) 0.168(11) Uiso 1 1 d . . . H99 H 1.0408 0.7636 0.6569 0.202 Uiso 1 1 calc R . . C100 C 1.184(2) 0.8363(15) 0.6725(11) 0.150(9) Uiso 1 1 d . . . H100 H 1.1710 0.8664 0.6533 0.181 Uiso 1 1 calc R . . C101 C 1.2786(17) 0.8545(13) 0.7058(9) 0.120(8) Uiso 1 1 d . . . H101 H 1.3275 0.9013 0.7165 0.144 Uiso 1 1 calc R . . C102 C 1.2961(15) 0.8005(12) 0.7220(8) 0.102(6) Uiso 1 1 d . . . H102 H 1.3600 0.8108 0.7429 0.122 Uiso 1 1 calc R . . C103 C 1.2238(13) 0.7299(11) 0.7093(7) 0.081(5) Uiso 1 1 d . . . H103 H 1.2408 0.6942 0.7198 0.098 Uiso 1 1 calc R . . C104 C 1.0633(11) 0.6000(9) 0.7040(6) 0.069(5) Uiso 1 1 d . . . C105 C 1.1124(12) 0.5522(10) 0.7030(7) 0.084(5) Uiso 1 1 d . . . H105 H 1.1355 0.5410 0.6752 0.101 Uiso 1 1 calc R . . C106 C 1.1260(14) 0.5215(11) 0.7449(8) 0.098(6) Uiso 1 1 d . . . H106 H 1.1587 0.4904 0.7444 0.117 Uiso 1 1 calc R . . C107 C 1.0919(14) 0.5370(11) 0.7860(8) 0.103(6) Uiso 1 1 d . . . H107 H 1.1039 0.5182 0.8138 0.124 Uiso 1 1 calc R . . C108 C 1.0418(13) 0.5789(11) 0.7857(8) 0.100(6) Uiso 1 1 d . . . H108 H 1.0166 0.5878 0.8130 0.119 Uiso 1 1 calc R . . C109 C 1.0255(12) 0.6113(9) 0.7433(7) 0.076(5) Uiso 1 1 d . . . H109 H 0.9890 0.6397 0.7434 0.092 Uiso 1 1 calc R . . C110 C 0.6650(12) 0.5869(10) 0.6387(7) 0.085(5) Uiso 1 1 d . . . H11A H 0.6939 0.5892 0.6748 0.101 Uiso 1 1 calc R . . H11B H 0.6268 0.5363 0.6182 0.101 Uiso 1 1 calc R . . C111 C 0.5942(15) 0.6293(11) 0.6363(9) 0.111(7) Uiso 1 1 d . . . H11C H 0.5536 0.6177 0.6001 0.134 Uiso 1 1 calc R . . H11D H 0.5508 0.6146 0.6565 0.134 Uiso 1 1 calc R . . C112 C 0.6563(17) 0.7094(13) 0.6584(10) 0.126(8) Uiso 1 1 d . . . H11E H 0.6124 0.7345 0.6536 0.151 Uiso 1 1 calc R . . H11F H 0.6871 0.7207 0.6959 0.151 Uiso 1 1 calc R . . C113 C 0.7353(15) 0.7396(12) 0.6357(9) 0.123(8) Uiso 1 1 d . . . H11G H 0.7721 0.7913 0.6528 0.148 Uiso 1 1 calc R . . H11H H 0.7074 0.7310 0.5982 0.148 Uiso 1 1 calc R . . C114 C 0.8036(14) 0.6972(11) 0.6468(8) 0.098(6) Uiso 1 1 d . . . H11I H 0.8613 0.7167 0.6363 0.117 Uiso 1 1 calc R . . H11J H 0.8259 0.7026 0.6841 0.117 Uiso 1 1 calc R . . C115 C -0.0504(11) 0.8419(9) 0.8476(6) 0.057(4) Uiso 1 1 d . . . C116 C -0.0579(11) 0.8835(8) 0.8998(6) 0.062(4) Uiso 1 1 d . . . H11K H -0.1271 0.8731 0.8953 0.074 Uiso 1 1 calc R . . H11L H -0.0337 0.8650 0.9277 0.074 Uiso 1 1 calc R . . C117 C -0.0009(12) 0.9647(9) 0.9169(6) 0.064(4) Uiso 1 1 d . . . C118 C -0.0390(12) 1.0123(10) 0.9377(7) 0.069(5) Uiso 1 1 d . . . H118 H -0.1012 0.9934 0.9413 0.083 Uiso 1 1 calc R . . C119 C 0.0114(12) 1.0855(10) 0.9529(6) 0.068(5) Uiso 1 1 d . . . H119 H -0.0161 1.1163 0.9663 0.082 Uiso 1 1 calc R . . C120 C 0.1049(11) 1.1133(9) 0.9480(6) 0.065(4) Uiso 1 1 d . . . H120 H 0.1392 1.1633 0.9570 0.078 Uiso 1 1 calc R . . C121 C 0.1469(11) 1.0689(10) 0.9305(6) 0.056(4) Uiso 1 1 d . . . C122 C 0.2432(10) 1.0959(9) 0.9239(6) 0.060(4) Uiso 1 1 d . . . H12A H 0.2679 1.1482 0.9319 0.072 Uiso 1 1 calc R . . H12B H 0.2364 1.0758 0.8874 0.072 Uiso 1 1 calc R . . C123 C 0.3194(11) 1.0762(10) 0.9596(6) 0.055(4) Uiso 1 1 d . . . C124 C -0.1264(12) 0.7618(10) 0.8308(6) 0.067(5) Uiso 1 1 d . . . C125 C -0.0946(17) 0.7064(13) 0.8275(9) 0.117(7) Uiso 1 1 d . . . H125 H -0.0282 0.7141 0.8351 0.141 Uiso 1 1 calc R . . C126 C -0.169(2) 0.6389(16) 0.8120(11) 0.151(9) Uiso 1 1 d . . . H126 H -0.1490 0.6008 0.8101 0.181 Uiso 1 1 calc R . . C127 C -0.2678(16) 0.6193(13) 0.7991(8) 0.103(6) Uiso 1 1 d . . . H127 H -0.3122 0.5711 0.7889 0.124 Uiso 1 1 calc R . . C128 C -0.296(2) 0.6719(15) 0.8019(10) 0.141(9) Uiso 1 1 d . . . H128 H -0.3629 0.6626 0.7967 0.170 Uiso 1 1 calc R . . C129 C -0.2291(19) 0.7419(15) 0.8126(10) 0.133(8) Uiso 1 1 d . . . H129 H -0.2527 0.7772 0.8076 0.160 Uiso 1 1 calc R . . C130 C -0.0699(11) 0.8729(9) 0.8019(6) 0.066(4) Uiso 1 1 d . . . C131 C -0.1330(12) 0.9128(9) 0.7965(7) 0.076(5) Uiso 1 1 d . . . H131 H -0.1612 0.9218 0.8223 0.092 Uiso 1 1 calc R . . C132 C -0.1512(13) 0.9371(10) 0.7544(7) 0.088(6) Uiso 1 1 d . . . H132 H -0.1953 0.9596 0.7505 0.106 Uiso 1 1 calc R . . C133 C -0.1070(14) 0.9292(11) 0.7185(8) 0.105(7) Uiso 1 1 d . . . H133 H -0.1222 0.9459 0.6898 0.126 Uiso 1 1 calc R . . C134 C -0.0397(14) 0.8974(10) 0.7214(8) 0.100(6) Uiso 1 1 d . . . H134 H -0.0071 0.8949 0.6968 0.120 Uiso 1 1 calc R . . C135 C -0.0227(12) 0.8681(10) 0.7653(7) 0.082(5) Uiso 1 1 d . . . H135 H 0.0213 0.8456 0.7685 0.098 Uiso 1 1 calc R . . C136 C 0.4233(12) 1.1082(10) 0.9502(7) 0.069(5) Uiso 1 1 d . . . C137 C 0.4870(12) 1.0739(10) 0.9651(7) 0.077(5) Uiso 1 1 d . . . H137 H 0.4658 1.0329 0.9759 0.093 Uiso 1 1 calc R . . C138 C 0.5869(14) 1.1048(11) 0.9629(8) 0.093(6) Uiso 1 1 d . . . H138 H 0.6344 1.0879 0.9759 0.111 Uiso 1 1 calc R . . C139 C 0.6076(15) 1.1598(11) 0.9409(8) 0.102(6) Uiso 1 1 d . . . H139 H 0.6697 1.1776 0.9371 0.122 Uiso 1 1 calc R . . C140 C 0.5432(16) 1.1913(12) 0.9238(9) 0.119(7) Uiso 1 1 d . . . H140 H 0.5618 1.2283 0.9087 0.143 Uiso 1 1 calc R . . C141 C 0.4510(15) 1.1669(11) 0.9297(8) 0.103(6) Uiso 1 1 d . . . H141 H 0.4078 1.1888 0.9203 0.123 Uiso 1 1 calc R . . C142 C 0.3376(12) 1.1158(10) 1.0175(7) 0.068(5) Uiso 1 1 d . . . C143 C 0.3151(11) 1.0727(10) 1.0495(7) 0.075(5) Uiso 1 1 d . . . H143 H 0.2915 1.0224 1.0367 0.090 Uiso 1 1 calc R . . C144 C 0.3299(14) 1.1094(13) 1.1051(9) 0.103(6) Uiso 1 1 d . . . H144 H 0.3143 1.0841 1.1287 0.124 Uiso 1 1 calc R . . C145 C 0.3682(14) 1.1832(13) 1.1187(9) 0.108(7) Uiso 1 1 d . . . H145 H 0.3828 1.2072 1.1540 0.129 Uiso 1 1 calc R . . C146 C 0.3871(17) 1.2249(15) 1.0891(10) 0.138(9) Uiso 1 1 d . . . H146 H 0.4078 1.2749 1.1024 0.165 Uiso 1 1 calc R . . C147 C 0.3753(14) 1.1921(12) 1.0361(9) 0.100(6) Uiso 1 1 d . . . H147 H 0.3920 1.2200 1.0142 0.120 Uiso 1 1 calc R . . C148 C 0.3310(12) 0.8866(10) 0.8691(7) 0.077(5) Uiso 1 1 d . . . H14A H 0.3692 0.9386 0.8833 0.092 Uiso 1 1 calc R . . H14B H 0.2997 0.8748 0.8315 0.092 Uiso 1 1 calc R . . C149 C 0.4004(14) 0.8468(10) 0.8792(8) 0.099(6) Uiso 1 1 d . . . H14C H 0.4489 0.8606 0.8615 0.119 Uiso 1 1 calc R . . H14D H 0.4358 0.8622 0.9167 0.119 Uiso 1 1 calc R . . C150 C 0.3474(13) 0.7679(10) 0.8609(8) 0.091(6) Uiso 1 1 d . . . H15A H 0.3933 0.7453 0.8695 0.109 Uiso 1 1 calc R . . H15B H 0.3162 0.7513 0.8229 0.109 Uiso 1 1 calc R . . C151 C 0.2684(14) 0.7465(11) 0.8876(8) 0.106(7) Uiso 1 1 d . . . H15C H 0.2297 0.6945 0.8743 0.127 Uiso 1 1 calc R . . H15D H 0.2997 0.7598 0.9253 0.127 Uiso 1 1 calc R . . C152 C 0.2019(13) 0.7866(11) 0.8753(8) 0.086(6) Uiso 1 1 d . . . H15E H 0.1707 0.7721 0.8375 0.103 Uiso 1 1 calc R . . H15F H 0.1498 0.7721 0.8907 0.103 Uiso 1 1 calc R . . C153 C 0.612(5) 0.445(3) 0.179(3) 0.42(4) Uiso 1 1 d . . . H15G H 0.5944 0.4859 0.1873 0.510 Uiso 1 1 calc R . . H15H H 0.6821 0.4636 0.1837 0.510 Uiso 1 1 calc R . . O9 O 0.311(2) 0.0104(15) 0.1919(12) 0.254(11) Uiso 1 1 d . . . C154 C 0.419(2) 0.0612(15) 0.2330(12) 0.168(11) Uiso 1 1 d . . . H15I H 0.4352 0.0395 0.2603 0.201 Uiso 1 1 calc R . . H15J H 0.4681 0.0663 0.2151 0.201 Uiso 1 1 calc R . . C155 C 0.421(3) 0.135(2) 0.2570(16) 0.277(19) Uiso 1 1 d . . . H15K H 0.4849 0.1656 0.2822 0.416 Uiso 1 1 calc R . . H15L H 0.3716 0.1292 0.2743 0.416 Uiso 1 1 calc R . . H15M H 0.4062 0.1564 0.2297 0.416 Uiso 1 1 calc R . . C156 C 0.331(2) -0.0415(18) 0.1630(14) 0.213(14) Uiso 1 1 d . . . H15N H 0.3531 -0.0699 0.1834 0.256 Uiso 1 1 calc R . . H15O H 0.3773 -0.0222 0.1453 0.256 Uiso 1 1 calc R . . C157 C 0.2234(17) -0.0830(13) 0.1254(10) 0.139(8) Uiso 1 1 d . . . H15P H 0.2192 -0.1241 0.0995 0.209 Uiso 1 1 calc R . . H15Q H 0.2037 -0.0514 0.1080 0.209 Uiso 1 1 calc R . . H15R H 0.1804 -0.0993 0.1451 0.209 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0508(4) 0.0494(5) 0.0724(5) 0.0113(4) 0.0181(3) 0.0188(4) Os2 0.0501(4) 0.0554(5) 0.0622(5) 0.0152(4) 0.0146(3) 0.0202(4) Os3 0.0491(4) 0.0503(5) 0.0643(5) 0.0144(4) 0.0169(3) 0.0216(4) Os4 0.0464(4) 0.0466(5) 0.0632(5) 0.0126(4) 0.0162(3) 0.0181(3) Cl1 0.070(3) 0.068(3) 0.092(3) 0.031(3) 0.025(2) 0.033(3) Cl2 0.075(3) 0.074(4) 0.089(3) 0.039(3) 0.034(2) 0.035(3) Cl3 0.065(3) 0.064(3) 0.095(3) 0.036(3) 0.032(2) 0.025(2) Cl4 0.063(2) 0.071(3) 0.077(3) 0.030(3) 0.029(2) 0.023(2) O1 0.058(6) 0.047(8) 0.086(8) 0.003(6) 0.014(6) 0.019(6) O2 0.049(6) 0.040(8) 0.090(8) 0.013(6) 0.023(6) 0.013(6) O3 0.048(6) 0.061(8) 0.070(8) 0.023(7) 0.018(5) 0.015(6) O4 0.049(6) 0.059(8) 0.079(8) 0.012(6) 0.020(5) 0.025(6) O5 0.054(6) 0.054(8) 0.073(7) 0.025(6) 0.019(5) 0.030(6) O6 0.043(6) 0.061(8) 0.068(7) 0.012(6) 0.012(5) 0.007(6) O7 0.040(5) 0.038(7) 0.080(8) 0.007(6) 0.024(5) 0.004(5) O8 0.056(6) 0.040(8) 0.077(8) 0.026(6) 0.022(5) 0.022(6) N1 0.066(8) 0.049(9) 0.058(9) 0.004(7) 0.005(7) 0.013(7) N2 0.062(8) 0.064(11) 0.088(10) 0.034(9) 0.042(7) 0.046(8) N3 0.054(7) 0.031(9) 0.087(10) 0.018(8) 0.019(7) 0.015(7) N4 0.070(8) 0.071(11) 0.062(9) 0.033(8) 0.010(7) 0.024(8) N5 0.049(7) 0.058(10) 0.063(9) 0.017(8) 0.018(6) 0.017(7) N6 0.051(8) 0.089(13) 0.085(12) 0.012(10) 0.011(8) 0.022(9) N7 0.042(7) 0.078(11) 0.061(9) 0.016(8) 0.015(6) 0.014(7) N8 0.045(7) 0.044(9) 0.068(9) 0.011(7) 0.009(6) 0.008(7) N9 0.046(7) 0.039(9) 0.089(10) 0.007(8) 0.023(7) 0.009(7) N10 0.055(7) 0.037(9) 0.086(10) 0.036(8) 0.037(7) 0.018(7) N11 0.043(7) 0.079(12) 0.061(9) 0.017(8) 0.013(6) 0.031(8) N12 0.052(7) 0.052(10) 0.093(11) 0.015(8) 0.030(7) 0.023(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. ; 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 Os1 N1 1.631(12) . ? Os1 O2 1.979(10) . ? Os1 O1 1.990(10) . ? Os1 N2 2.124(12) . ? Os1 N3 2.129(11) . ? Os1 Cl1 2.661(4) . ? Os2 N4 1.623(11) . ? Os2 O3 1.961(11) . ? Os2 O4 1.972(10) . ? Os2 N5 2.114(12) . ? Os2 N6 2.131(13) . ? Os2 Cl2 2.711(4) . ? Os3 N7 1.618(11) . ? Os3 O5 1.962(10) . ? Os3 O6 1.975(10) . ? Os3 N8 2.123(12) . ? Os3 N9 2.133(12) . ? Os3 Cl3 2.734(4) . ? Os4 N10 1.630(11) . ? Os4 O7 1.958(10) . ? Os4 O8 2.003(11) . ? Os4 N11 2.090(11) . ? Os4 N12 2.127(11) . ? Os4 Cl4 2.660(4) . ? Cl5 C153 1.90(5) . ? Cl6 C153 1.51(7) . ? O1 C1 1.413(16) . ? O2 C9 1.380(18) . ? O3 C39 1.398(17) . ? O4 C47 1.423(16) . ? O5 C77 1.429(17) . ? O6 C85 1.443(15) . ? O7 C115 1.432(15) . ? O8 C123 1.387(17) . ? N2 C3 1.314(17) . ? N2 C7 1.381(19) . ? N3 C38 1.456(18) . ? N3 C34 1.49(2) . ? N5 C45 1.347(17) . ? N5 C41 1.372(19) . ? N6 C72' 1.42(6) . ? N6 C72 1.48(3) . ? N6 C76 1.61(4) . ? N6 C76' 1.63(4) . ? N8 C83 1.329(17) . ? N8 C79 1.38(2) . ? N9 C114 1.46(2) . ? N9 C110 1.523(18) . ? N11 C117 1.384(17) . ? N11 C121 1.406(18) . ? N12 C152 1.44(2) . ? N12 C148 1.499(17) . ? C1 C10 1.463(19) . ? C1 C2 1.58(2) . ? C1 C16 1.61(2) . ? C2 C3 1.48(2) . ? C3 C4 1.39(2) . ? C4 C5 1.34(2) . ? C5 C6 1.38(2) . ? C6 C7 1.34(2) . ? C7 C8 1.507(19) . ? C8 C9 1.634(19) . ? C9 C28 1.467(19) . ? C9 C22 1.57(2) . ? C10 C11 1.344(19) . ? C10 C15 1.39(2) . ? C11 C12 1.44(2) . ? C12 C13 1.31(2) . ? C13 C14 1.25(2) . ? C14 C15 1.36(2) . ? C16 C17 1.29(2) . ? C16 C21 1.33(3) . ? C17 C18 1.44(3) . ? C18 C19 1.28(3) . ? C19 C20 1.34(3) . ? C20 C21 1.52(3) . ? C22 C23 1.36(2) . ? C22 C27 1.44(3) . ? C23 C24 1.40(3) . ? C24 C25 1.40(3) . ? C25 C26 1.32(2) . ? C26 C27 1.39(3) . ? C28 C29 1.325(19) . ? C28 C33 1.335(19) . ? C29 C30 1.34(2) . ? C30 C31 1.30(2) . ? C31 C32 1.45(2) . ? C32 C33 1.39(2) . ? C34 C35 1.51(2) . ? C35 C36 1.53(2) . ? C36 C37 1.45(2) . ? C37 C38 1.58(2) . ? C39 C54 1.53(2) . ? C39 C40 1.542(18) . ? C39 C48 1.573(18) . ? C40 C41 1.480(19) . ? C41 C42 1.37(2) . ? C42 C43 1.395(19) . ? C43 C44 1.34(2) . ? C44 C45 1.35(2) . ? C45 C46 1.55(2) . ? C46 C47 1.50(2) . ? C47 C60 1.52(2) . ? C47 C66 1.56(2) . ? C48 C49 1.388(18) . ? C48 C53 1.422(19) . ? C49 C50 1.352(19) . ? C50 C51 1.35(2) . ? C51 C52 1.32(2) . ? C52 C53 1.43(2) . ? C54 C55 1.386(19) . ? C54 C59 1.44(3) . ? C55 C56 1.63(3) . ? C56 C57 1.22(3) . ? C57 C58 1.26(2) . ? C58 C59 1.39(3) . ? C60 C61 1.32(2) . ? C60 C65 1.40(2) . ? C61 C62 1.35(2) . ? C62 C63 1.40(3) . ? C63 C64 1.26(2) . ? C64 C65 1.33(2) . ? C66 C71 1.339(19) . ? C66 C67 1.37(2) . ? C67 C68 1.38(2) . ? C68 C69 1.54(3) . ? C69 C70 1.29(3) . ? C70 C71 1.51(2) . ? C72 C76' 1.20(4) . ? C72 C73 1.58(5) . ? C72 C75' 1.69(5) . ? C72' C76 1.44(5) . ? C72' C73' 1.83(7) . ? C72' C75 1.94(7) . ? C73' C74 1.61(6) . ? C73' C75 1.71(7) . ? C73' C73 1.74(7) . ? C73 C75' 1.39(5) . ? C73 C74 1.62(5) . ? C74 C75 1.42(4) . ? C74 C75' 1.43(5) . ? C75' C76' 1.47(5) . ? C75 C76 1.69(5) . ? C76 C76' 1.87(5) . ? C77 C92 1.52(2) . ? C77 C78 1.543(18) . ? C77 C86 1.563(18) . ? C78 C79 1.50(2) . ? C79 C80 1.40(2) . ? C80 C81 1.35(2) . ? C81 C82 1.36(2) . ? C82 C83 1.37(2) . ? C83 C84 1.49(2) . ? C84 C85 1.530(19) . ? C85 C98 1.53(2) . ? C85 C104 1.556(18) . ? C86 C91 1.357(18) . ? C86 C87 1.387(19) . ? C87 C88 1.33(2) . ? C88 C89 1.33(2) . ? C89 C90 1.41(2) . ? C90 C91 1.41(2) . ? C92 C97 1.338(18) . ? C92 C93 1.39(2) . ? C93 C94 1.45(3) . ? C94 C95 1.34(2) . ? C95 C96 1.27(3) . ? C96 C97 1.44(2) . ? C98 C99 1.36(3) . ? C98 C103 1.37(2) . ? C99 C100 1.44(3) . ? C100 C101 1.38(3) . ? C101 C102 1.36(2) . ? C102 C103 1.41(2) . ? C104 C109 1.35(2) . ? C104 C105 1.418(19) . ? C105 C106 1.42(2) . ? C106 C107 1.37(2) . ? C107 C108 1.33(2) . ? C108 C109 1.46(2) . ? C110 C111 1.59(2) . ? C111 C112 1.50(3) . ? C112 C113 1.49(2) . ? C113 C114 1.58(2) . ? C115 C130 1.526(19) . ? C115 C124 1.56(2) . ? C115 C116 1.56(2) . ? C116 C117 1.51(2) . ? C117 C118 1.39(2) . ? C118 C119 1.36(2) . ? C119 C120 1.391(18) . ? C120 C121 1.352(19) . ? C121 C122 1.449(18) . ? C122 C123 1.548(18) . ? C123 C142 1.55(2) . ? C123 C136 1.60(2) . ? C124 C125 1.37(2) . ? C124 C129 1.40(2) . ? C125 C126 1.37(3) . ? C126 C127 1.35(3) . ? C127 C128 1.29(3) . ? C128 C129 1.38(3) . ? C130 C135 1.37(2) . ? C130 C131 1.457(19) . ? C131 C132 1.35(2) . ? C132 C133 1.33(2) . ? C133 C134 1.38(2) . ? C134 C135 1.46(2) . ? C136 C137 1.41(2) . ? C136 C141 1.41(2) . ? C137 C138 1.46(2) . ? C138 C139 1.36(2) . ? C139 C140 1.39(2) . ? C140 C141 1.38(2) . ? C142 C143 1.385(19) . ? C142 C147 1.41(2) . ? C143 C144 1.49(3) . ? C144 C145 1.36(2) . ? C145 C146 1.30(2) . ? C146 C147 1.42(3) . ? C148 C149 1.54(2) . ? C149 C150 1.46(2) . ? C150 C151 1.53(2) . ? C151 C152 1.52(2) . ? O9 C156 1.36(4) . ? O9 C154 1.60(3) . ? C154 C155 1.52(4) . ? C156 C157 1.54(4) . ? 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 Os1 O2 103.1(5) . . ? N1 Os1 O1 97.3(5) . . ? O2 Os1 O1 158.1(4) . . ? N1 Os1 N2 99.5(5) . . ? O2 Os1 N2 90.7(4) . . ? O1 Os1 N2 93.6(5) . . ? N1 Os1 N3 93.5(5) . . ? O2 Os1 N3 82.0(4) . . ? O1 Os1 N3 89.1(4) . . ? N2 Os1 N3 166.3(5) . . ? N1 Os1 Cl1 171.5(4) . . ? O2 Os1 Cl1 79.3(3) . . ? O1 Os1 Cl1 79.3(3) . . ? N2 Os1 Cl1 88.6(3) . . ? N3 Os1 Cl1 78.7(3) . . ? N4 Os2 O3 102.3(6) . . ? N4 Os2 O4 100.0(6) . . ? O3 Os2 O4 156.7(4) . . ? N4 Os2 N5 99.0(5) . . ? O3 Os2 N5 88.9(4) . . ? O4 Os2 N5 94.2(5) . . ? N4 Os2 N6 93.8(6) . . ? O3 Os2 N6 86.9(5) . . ? O4 Os2 N6 85.0(5) . . ? N5 Os2 N6 167.2(5) . . ? N4 Os2 Cl2 172.0(5) . . ? O3 Os2 Cl2 77.5(3) . . ? O4 Os2 Cl2 79.4(3) . . ? N5 Os2 Cl2 89.0(3) . . ? N6 Os2 Cl2 78.3(4) . . ? N7 Os3 O5 104.0(5) . . ? N7 Os3 O6 99.9(5) . . ? O5 Os3 O6 155.2(4) . . ? N7 Os3 N8 99.3(5) . . ? O5 Os3 N8 88.7(4) . . ? O6 Os3 N8 94.1(4) . . ? N7 Os3 N9 95.9(5) . . ? O5 Os3 N9 81.1(4) . . ? O6 Os3 N9 89.9(4) . . ? N8 Os3 N9 163.4(5) . . ? N7 Os3 Cl3 172.9(5) . . ? O5 Os3 Cl3 77.1(3) . . ? O6 Os3 Cl3 78.4(3) . . ? N8 Os3 Cl3 87.7(3) . . ? N9 Os3 Cl3 77.3(3) . . ? N10 Os4 O7 99.1(5) . . ? N10 Os4 O8 100.0(5) . . ? O7 Os4 O8 159.9(4) . . ? N10 Os4 N11 100.1(5) . . ? O7 Os4 N11 93.6(5) . . ? O8 Os4 N11 89.3(4) . . ? N10 Os4 N12 93.2(5) . . ? O7 Os4 N12 90.5(5) . . ? O8 Os4 N12 82.2(5) . . ? N11 Os4 N12 165.3(5) . . ? N10 Os4 Cl4 171.4(4) . . ? O7 Os4 Cl4 80.7(3) . . ? O8 Os4 Cl4 79.4(3) . . ? N11 Os4 Cl4 88.4(3) . . ? N12 Os4 Cl4 78.3(4) . . ? C1 O1 Os1 119.5(10) . . ? C9 O2 Os1 126.0(9) . . ? C39 O3 Os2 124.4(8) . . ? C47 O4 Os2 122.7(10) . . ? C77 O5 Os3 125.4(8) . . ? C85 O6 Os3 122.3(9) . . ? C115 O7 Os4 122.5(9) . . ? C123 O8 Os4 122.9(8) . . ? C3 N2 C7 119.5(14) . . ? C3 N2 Os1 124.0(12) . . ? C7 N2 Os1 116.4(9) . . ? C38 N3 C34 109.9(14) . . ? C38 N3 Os1 110.8(10) . . ? C34 N3 Os1 117.7(9) . . ? C45 N5 C41 120.4(13) . . ? C45 N5 Os2 124.0(11) . . ? C41 N5 Os2 115.6(10) . . ? C72' N6 C72 120(3) . . ? C72' N6 C76 56(2) . . ? C72 N6 C76 108.6(19) . . ? C72' N6 C76' 114(3) . . ? C72 N6 C76' 45.0(16) . . ? C76 N6 C76' 70(2) . . ? C72' N6 Os2 121(2) . . ? C72 N6 Os2 118.7(17) . . ? C76 N6 Os2 107.0(15) . . ? C76' N6 Os2 109.4(16) . . ? C83 N8 C79 123.0(14) . . ? C83 N8 Os3 121.6(11) . . ? C79 N8 Os3 115.3(10) . . ? C114 N9 C110 110.0(14) . . ? C114 N9 Os3 116.9(10) . . ? C110 N9 Os3 109.6(9) . . ? C117 N11 C121 119.5(13) . . ? C117 N11 Os4 122.4(11) . . ? C121 N11 Os4 117.8(9) . . ? C152 N12 C148 108.5(13) . . ? C152 N12 Os4 118.4(10) . . ? C148 N12 Os4 113.6(9) . . ? O1 C1 C10 114.8(13) . . ? O1 C1 C2 108.0(13) . . ? C10 C1 C2 115.2(14) . . ? O1 C1 C16 100.8(12) . . ? C10 C1 C16 113.0(15) . . ? C2 C1 C16 103.6(13) . . ? C3 C2 C1 116.1(14) . . ? N2 C3 C4 122.8(17) . . ? N2 C3 C2 119.1(15) . . ? C4 C3 C2 117.9(15) . . ? C5 C4 C3 116.8(17) . . ? C4 C5 C6 122(2) . . ? C7 C6 C5 119.5(19) . . ? C6 C7 N2 119.5(15) . . ? C6 C7 C8 121.1(17) . . ? N2 C7 C8 119.3(14) . . ? C7 C8 C9 113.3(12) . . ? O2 C9 C28 110.2(14) . . ? O2 C9 C22 109.2(14) . . ? C28 C9 C22 110.7(14) . . ? O2 C9 C8 110.9(13) . . ? C28 C9 C8 108.8(13) . . ? C22 C9 C8 107.1(13) . . ? C11 C10 C15 115.2(16) . . ? C11 C10 C1 123.5(15) . . ? C15 C10 C1 121.3(16) . . ? C10 C11 C12 121.7(17) . . ? C13 C12 C11 116.9(19) . . ? C14 C13 C12 124(2) . . ? C13 C14 C15 121(2) . . ? C14 C15 C10 121.3(18) . . ? C17 C16 C21 124(2) . . ? C17 C16 C1 120.6(19) . . ? C21 C16 C1 114.7(18) . . ? C16 C17 C18 118(2) . . ? C19 C18 C17 121(2) . . ? C18 C19 C20 123(3) . . ? C19 C20 C21 116(3) . . ? C16 C21 C20 117(2) . . ? C23 C22 C27 115.4(18) . . ? C23 C22 C9 120.5(18) . . ? C27 C22 C9 123.8(17) . . ? C22 C23 C24 121(2) . . ? C23 C24 C25 123(2) . . ? C26 C25 C24 116(2) . . ? C25 C26 C27 123(3) . . ? C26 C27 C22 121(2) . . ? C29 C28 C33 116.5(16) . . ? C29 C28 C9 116.9(16) . . ? C33 C28 C9 126.5(15) . . ? C28 C29 C30 123.2(19) . . ? C31 C30 C29 123(2) . . ? C30 C31 C32 117(2) . . ? C33 C32 C31 116.4(19) . . ? C28 C33 C32 123.6(17) . . ? N3 C34 C35 110.7(15) . . ? C34 C35 C36 109.5(17) . . ? C37 C36 C35 109(2) . . ? C36 C37 C38 111.7(16) . . ? N3 C38 C37 110.8(13) . . ? O3 C39 C54 112.1(14) . . ? O3 C39 C40 112.7(13) . . ? C54 C39 C40 109.3(13) . . ? O3 C39 C48 105.7(12) . . ? C54 C39 C48 107.5(12) . . ? C40 C39 C48 109.4(12) . . ? C41 C40 C39 112.7(12) . . ? C42 C41 N5 117.7(15) . . ? C42 C41 C40 121.5(17) . . ? N5 C41 C40 120.8(15) . . ? C41 C42 C43 120.6(17) . . ? C44 C43 C42 120.2(17) . . ? C43 C44 C45 118.7(16) . . ? N5 C45 C44 122.4(16) . . ? N5 C45 C46 117.7(14) . . ? C44 C45 C46 119.9(15) . . ? C47 C46 C45 118.0(14) . . ? O4 C47 C46 111.4(14) . . ? O4 C47 C60 107.5(13) . . ? C46 C47 C60 109.1(14) . . ? O4 C47 C66 109.3(13) . . ? C46 C47 C66 111.0(14) . . ? C60 C47 C66 108.4(14) . . ? C49 C48 C53 117.9(14) . . ? C49 C48 C39 117.8(14) . . ? C53 C48 C39 124.2(13) . . ? C50 C49 C48 119.1(15) . . ? C51 C50 C49 124.8(17) . . ? C52 C51 C50 118.1(17) . . ? C51 C52 C53 122.0(19) . . ? C48 C53 C52 117.9(16) . . ? C55 C54 C59 120.3(17) . . ? C55 C54 C39 117.7(17) . . ? C59 C54 C39 122.0(17) . . ? C54 C55 C56 113.1(18) . . ? C57 C56 C55 117(2) . . ? C56 C57 C58 129(3) . . ? C57 C58 C59 121(3) . . ? C58 C59 C54 119(2) . . ? C61 C60 C65 120.9(18) . . ? C61 C60 C47 117.5(16) . . ? C65 C60 C47 121.3(16) . . ? C60 C61 C62 115(2) . . ? C61 C62 C63 121(2) . . ? C64 C63 C62 124(3) . . ? C63 C64 C65 116(2) . . ? C64 C65 C60 123(2) . . ? C71 C66 C67 117.9(16) . . ? C71 C66 C47 123.7(15) . . ? C67 C66 C47 118.4(15) . . ? C66 C67 C68 125.5(19) . . ? C67 C68 C69 111(2) . . ? C70 C69 C68 128(2) . . ? C69 C70 C71 111(2) . . ? C66 C71 C70 125.3(17) . . ? C76' C72 N6 74(3) . . ? C76' C72 C73 104(3) . . ? N6 C72 C73 111(3) . . ? C76' C72 C75' 58(3) . . ? N6 C72 C75' 112(3) . . ? C73 C72 C75' 50(2) . . ? N6 C72' C76 69(3) . . ? N6 C72' C73' 102(4) . . ? C76 C72' C73' 104(4) . . ? N6 C72' C75 106(3) . . ? C76 C72' C75 58(3) . . ? C73' C72' C75 54(3) . . ? C74 C73' C75 51(2) . . ? C74 C73' C73 58(3) . . ? C75 C73' C73 100(4) . . ? C74 C73' C72' 103(4) . . ? C75 C73' C72' 66(3) . . ? C73 C73' C72' 103(4) . . ? C75' C73 C72 69(3) . . ? C75' C73 C74 56(2) . . ? C72 C73 C74 107(3) . . ? C75' C73 C73' 106(3) . . ? C72 C73 C73' 103(3) . . ? C74 C73 C73' 57(3) . . ? C75 C74 C75' 116(3) . . ? C75 C74 C73' 68(3) . . ? C75' C74 C73' 110(4) . . ? C75 C74 C73 120(3) . . ? C75' C74 C73 54(2) . . ? C73' C74 C73 65(3) . . ? C73 C75' C74 70(3) . . ? C73 C75' C76' 101(3) . . ? C74 C75' C76' 112(4) . . ? C73 C75' C72 61(2) . . ? C74 C75' C72 110(3) . . ? C76' C75' C72 44(2) . . ? C74 C75 C76 109(3) . . ? C74 C75 C73' 61(3) . . ? C76 C75 C73' 99(3) . . ? C74 C75 C72' 105(3) . . ? C76 C75 C72' 46(2) . . ? C73' C75 C72' 60(3) . . ? C72' C76 N6 55(3) . . ? C72' C76 C75 76(3) . . ? N6 C76 C75 110(2) . . ? C72' C76 C76' 101(3) . . ? N6 C76 C76' 55.3(18) . . ? C75 C76 C76' 96(2) . . ? C72 C76' C75' 78(3) . . ? C72 C76' N6 61(2) . . ? C75' C76' N6 116(3) . . ? C72 C76' C76 108(3) . . ? C75' C76' C76 104(3) . . ? N6 C76' C76 54.3(17) . . ? O5 C77 C92 109.3(13) . . ? O5 C77 C78 111.2(13) . . ? C92 C77 C78 110.9(13) . . ? O5 C77 C86 106.7(11) . . ? C92 C77 C86 108.9(12) . . ? C78 C77 C86 109.7(12) . . ? C79 C78 C77 111.6(13) . . ? N8 C79 C80 117.6(15) . . ? N8 C79 C78 121.0(15) . . ? C80 C79 C78 121.3(17) . . ? C81 C80 C79 118.6(19) . . ? C80 C81 C82 121.7(19) . . ? C81 C82 C83 120.2(17) . . ? N8 C83 C82 118.5(17) . . ? N8 C83 C84 122.8(14) . . ? C82 C83 C84 118.7(15) . . ? C83 C84 C85 118.8(13) . . ? O6 C85 C98 107.9(12) . . ? O6 C85 C84 109.7(12) . . ? C98 C85 C84 108.4(12) . . ? O6 C85 C104 108.5(11) . . ? C98 C85 C104 107.7(13) . . ? C84 C85 C104 114.4(12) . . ? C91 C86 C87 118.9(15) . . ? C91 C86 C77 116.0(14) . . ? C87 C86 C77 125.1(14) . . ? C88 C87 C86 120.3(18) . . ? C87 C88 C89 123(2) . . ? C88 C89 C90 120(2) . . ? C91 C90 C89 117.0(18) . . ? C86 C91 C90 121.0(17) . . ? C97 C92 C93 117.8(16) . . ? C97 C92 C77 122.6(16) . . ? C93 C92 C77 119.6(16) . . ? C92 C93 C94 121(2) . . ? C95 C94 C93 117(2) . . ? C96 C95 C94 121(2) . . ? C95 C96 C97 124(2) . . ? C92 C97 C96 118.0(18) . . ? C99 C98 C103 118(2) . . ? C99 C98 C85 120.4(19) . . ? C103 C98 C85 121.4(16) . . ? C98 C99 C100 121(3) . . ? C101 C100 C99 118(3) . . ? C102 C101 C100 116(2) . . ? C101 C102 C103 124(2) . . ? C98 C103 C102 119.1(18) . . ? C109 C104 C105 118.4(15) . . ? C109 C104 C85 119.9(14) . . ? C105 C104 C85 121.7(14) . . ? C104 C105 C106 119.3(16) . . ? C107 C106 C105 121.2(18) . . ? C108 C107 C106 120(2) . . ? C107 C108 C109 121.1(18) . . ? C104 C109 C108 120.2(16) . . ? N9 C110 C111 110.0(13) . . ? C112 C111 C110 109.2(17) . . ? C113 C112 C111 117(2) . . ? C112 C113 C114 104.1(17) . . ? N9 C114 C113 108.8(16) . . ? O7 C115 C130 111.4(11) . . ? O7 C115 C124 106.3(12) . . ? C130 C115 C124 108.9(14) . . ? O7 C115 C116 107.0(12) . . ? C130 C115 C116 115.0(12) . . ? C124 C115 C116 107.7(12) . . ? C117 C116 C115 114.5(12) . . ? N11 C117 C118 118.4(16) . . ? N11 C117 C116 119.6(14) . . ? C118 C117 C116 121.9(14) . . ? C119 C118 C117 122.3(16) . . ? C118 C119 C120 118.5(16) . . ? C121 C120 C119 121.1(17) . . ? C120 C121 N11 120.0(14) . . ? C120 C121 C122 122.6(16) . . ? N11 C121 C122 117.3(14) . . ? C121 C122 C123 112.6(12) . . ? O8 C123 C142 113.0(13) . . ? O8 C123 C122 113.7(13) . . ? C142 C123 C122 108.0(12) . . ? O8 C123 C136 106.6(12) . . ? C142 C123 C136 105.8(14) . . ? C122 C123 C136 109.4(12) . . ? C125 C124 C129 117(2) . . ? C125 C124 C115 120.3(17) . . ? C129 C124 C115 122.5(18) . . ? C126 C125 C124 114(2) . . ? C127 C126 C125 130(3) . . ? C128 C127 C126 115(3) . . ? C127 C128 C129 120(3) . . ? C128 C129 C124 123(2) . . ? C135 C130 C131 116.3(15) . . ? C135 C130 C115 120.7(14) . . ? C131 C130 C115 123.0(13) . . ? C132 C131 C130 121.1(15) . . ? C133 C132 C131 120.8(18) . . ? C132 C133 C134 124(2) . . ? C133 C134 C135 116.2(18) . . ? C130 C135 C134 121.8(16) . . ? C137 C136 C141 122.0(16) . . ? C137 C136 C123 114.5(15) . . ? C141 C136 C123 123.4(15) . . ? C136 C137 C138 117.8(17) . . ? C139 C138 C137 116.8(17) . . ? C138 C139 C140 125(2) . . ? C141 C140 C139 119(2) . . ? C140 C141 C136 119.0(19) . . ? C143 C142 C147 122.5(18) . . ? C143 C142 C123 116.8(16) . . ? C147 C142 C123 120.7(17) . . ? C142 C143 C144 117.8(18) . . ? C145 C144 C143 114(2) . . ? C146 C145 C144 129(3) . . ? C145 C146 C147 118(3) . . ? C142 C147 C146 118(2) . . ? N12 C148 C149 110.1(13) . . ? C150 C149 C148 112.8(16) . . ? C149 C150 C151 108.8(17) . . ? C152 C151 C150 107.8(15) . . ? N12 C152 C151 113.8(16) . . ? Cl6 C153 Cl5 116(4) . . ? C156 O9 C154 100(2) . . ? C155 C154 O9 108(2) . . ? O9 C156 C157 94(2) . . ? _diffrn_measured_fraction_theta_max 0.465 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.465 _refine_diff_density_max 1.366 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.155 data_mar341 _database_code_CSD 209734 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H46 Cl2 N4 O7 Os' _chemical_formula_sum 'C36 H46 Cl2 N4 O7 Os' _chemical_formula_weight 907.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.2165 7.6030 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.732(3) _cell_length_b 18.256(4) _cell_length_c 15.546(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.81(3) _cell_angle_gamma 90.00 _cell_volume 3840.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.511 _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 301(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12707 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.74 _reflns_number_total 4308 _reflns_number_gt 2536 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4308 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 Os1 Os 0.54121(4) 0.09388(3) 0.14584(3) 0.0880(3) Uani 1 1 d . . . Cl1 Cl 0.5596(3) 0.46709(19) 0.1108(3) 0.1252(12) Uani 1 1 d . . . Cl2 Cl 0.7821(3) 0.42002(18) 0.1361(3) 0.1296(14) Uani 1 1 d . . . O1 O 0.4181(6) 0.0369(4) 0.1007(5) 0.093(2) Uani 1 1 d . . . O2 O 0.6031(6) -0.0014(4) 0.1181(5) 0.092(2) Uani 1 1 d . . . O3 O 0.3402(7) 0.2637(5) 0.1259(7) 0.136(4) Uani 1 1 d . . . O4 O 0.8088(8) 0.1608(5) 0.0846(7) 0.132(4) Uani 1 1 d . . . O5 O 0.9378(8) 0.0653(6) 0.1741(6) 0.132(3) Uani 1 1 d . . . O6 O 0.6593(8) -0.1366(5) 0.1215(6) 0.132(3) Uani 1 1 d . . . O7 O 0.5353(5) 0.0990(3) 0.9777(4) 0.085(2) Uani 1 1 d . . . N1 N 0.5502(8) 0.0887(5) 0.2513(6) 0.107(3) Uani 1 1 d . . . N2 N 0.4753(9) 0.1893(5) 0.1195(5) 0.082(3) Uani 1 1 d . . . N3 N 0.6510(10) 0.1502(5) 0.1358(5) 0.098(4) Uani 1 1 d . . . N4 N 0.6228(8) 0.2904(6) 0.8351(7) 0.100(3) Uani 1 1 d . . . C1 C 0.3241(10) 0.0660(10) 0.0937(7) 0.098(4) Uani 1 1 d . . . C2 C 0.3004(13) 0.1398(8) 0.0983(7) 0.091(4) Uani 1 1 d . . . C3 C 0.2002(12) 0.1601(10) 0.0830(8) 0.115(5) Uani 1 1 d . . . H3 H 0.1848 0.2097 0.0809 0.138 Uiso 1 1 calc R . . C4 C 0.1227(15) 0.1101(9) 0.0708(10) 0.126(6) Uani 1 1 d . . . H4 H 0.0570 0.1249 0.0637 0.151 Uiso 1 1 calc R . . C5 C 0.1494(11) 0.0357(12) 0.0700(8) 0.127(6) Uani 1 1 d . . . H5 H 0.0992 0.0009 0.0623 0.152 Uiso 1 1 calc R . . C6 C 0.2482(12) 0.0110(8) 0.0800(7) 0.104(4) Uani 1 1 d . . . H6 H 0.2634 -0.0385 0.0779 0.125 Uiso 1 1 calc R . . C7 C 0.3731(13) 0.2028(9) 0.1164(8) 0.103(4) Uani 1 1 d . . . C8 C 0.5422(11) 0.2486(7) 0.1233(7) 0.086(4) Uani 1 1 d . . . C9 C 0.6412(10) 0.2269(7) 0.1281(6) 0.074(3) Uani 1 1 d . . . C10 C 0.7129(9) 0.2802(8) 0.1326(7) 0.090(3) Uani 1 1 d . . . H10 H 0.7788 0.2662 0.1380 0.108 Uiso 1 1 calc R . . C11 C 0.6892(11) 0.3547(8) 0.1295(7) 0.095(4) Uani 1 1 d . . . C12 C 0.5902(13) 0.3752(7) 0.1203(8) 0.098(4) Uani 1 1 d . . . C13 C 0.5183(9) 0.3226(8) 0.1194(7) 0.091(4) Uani 1 1 d . . . H13 H 0.4527 0.3367 0.1161 0.109 Uiso 1 1 calc R . . C14 C 0.7016(10) -0.0093(7) 0.1315(7) 0.083(3) Uani 1 1 d . . . C15 C 0.7691(10) 0.0450(8) 0.1368(7) 0.091(4) Uani 1 1 d . . . C16 C 0.8708(11) 0.0208(9) 0.1562(8) 0.096(4) Uani 1 1 d . . . C17 C 0.8994(12) -0.0565(9) 0.1631(8) 0.112(4) Uani 1 1 d . . . H17 H 0.9660 -0.0690 0.1738 0.134 Uiso 1 1 calc R . . C18 C 0.8304(12) -0.1099(8) 0.1540(8) 0.104(4) Uani 1 1 d . . . H18 H 0.8493 -0.1588 0.1594 0.125 Uiso 1 1 calc R . . C19 C 0.7275(12) -0.0904(8) 0.1359(8) 0.099(4) Uani 1 1 d . . . C20 C 0.7444(16) 0.1260(7) 0.1175(9) 0.110(6) Uani 1 1 d . . . C24 C 0.7158(11) 0.2582(8) 0.8910(9) 0.125(5) Uani 1 1 d . . . H24A H 0.7028 0.2077 0.9044 0.151 Uiso 1 1 calc R . . H24B H 0.7292 0.2849 0.9457 0.151 Uiso 1 1 calc R . . C25 C 0.8087(12) 0.2608(11) 0.8476(12) 0.187(8) Uani 1 1 d . . . H25A H 0.8164 0.3092 0.8237 0.224 Uiso 1 1 calc R . . H25B H 0.8035 0.2253 0.8006 0.224 Uiso 1 1 calc R . . C26 C 0.8979(16) 0.2426(18) 0.9193(18) 0.291(18) Uani 1 1 d . . . H26A H 0.8968 0.2738 0.9697 0.349 Uiso 1 1 calc R . . H26B H 0.8936 0.1921 0.9376 0.349 Uiso 1 1 calc R . . C27 C 0.981(2) 0.253(2) 0.8894(19) 0.37(2) Uani 1 1 d . . . H27A H 1.0358 0.2436 0.9352 0.551 Uiso 1 1 calc R . . H27B H 0.9837 0.3023 0.8694 0.551 Uiso 1 1 calc R . . H27C H 0.9835 0.2196 0.8419 0.551 Uiso 1 1 calc R . . C28 C 0.6424(9) 0.3679(8) 0.8099(9) 0.106(4) Uani 1 1 d . . . H28A H 0.5829 0.3864 0.7736 0.127 Uiso 1 1 calc R . . H28B H 0.6937 0.3667 0.7741 0.127 Uiso 1 1 calc R . . C29 C 0.6731(11) 0.4224(8) 0.8829(9) 0.118(5) Uani 1 1 d . . . H29A H 0.7316 0.4041 0.9208 0.141 Uiso 1 1 calc R . . H29B H 0.6207 0.4264 0.9174 0.141 Uiso 1 1 calc R . . C30 C 0.6950(11) 0.4979(9) 0.8501(10) 0.143(6) Uani 1 1 d . . . H30A H 0.7458 0.4936 0.8140 0.171 Uiso 1 1 calc R . . H30B H 0.6359 0.5167 0.8137 0.171 Uiso 1 1 calc R . . C31 C 0.7280(13) 0.5507(10) 0.9207(11) 0.176(7) Uani 1 1 d . . . H31A H 0.7407 0.5972 0.8960 0.264 Uiso 1 1 calc R . . H31B H 0.7875 0.5330 0.9563 0.264 Uiso 1 1 calc R . . H31C H 0.6775 0.5562 0.9559 0.264 Uiso 1 1 calc R . . C32 C 0.5435(10) 0.2871(7) 0.8893(8) 0.103(4) Uani 1 1 d . . . H32A H 0.5627 0.3177 0.9404 0.123 Uiso 1 1 calc R . . H32B H 0.5387 0.2371 0.9095 0.123 Uiso 1 1 calc R . . C33 C 0.4419(10) 0.3112(8) 0.8434(7) 0.106(4) Uani 1 1 d . . . H33A H 0.4482 0.3571 0.8133 0.128 Uiso 1 1 calc R . . H33B H 0.4160 0.2749 0.7999 0.128 Uiso 1 1 calc R . . C34 C 0.3694(10) 0.3212(7) 0.9060(8) 0.106(4) Uani 1 1 d . . . H34A H 0.3672 0.2762 0.9389 0.127 Uiso 1 1 calc R . . H34B H 0.3939 0.3596 0.9472 0.127 Uiso 1 1 calc R . . C35 C 0.2675(10) 0.3401(9) 0.8641(9) 0.136(5) Uani 1 1 d . . . H35A H 0.2266 0.3454 0.9081 0.204 Uiso 1 1 calc R . . H35B H 0.2415 0.3019 0.8244 0.204 Uiso 1 1 calc R . . H35C H 0.2682 0.3853 0.8327 0.204 Uiso 1 1 calc R . . C36 C 0.5964(11) 0.2505(8) 0.7506(9) 0.115(4) Uani 1 1 d . . . H36A H 0.5399 0.2746 0.7162 0.138 Uiso 1 1 calc R . . H36B H 0.6512 0.2548 0.7189 0.138 Uiso 1 1 calc R . . C37 C 0.5730(12) 0.1726(10) 0.7580(10) 0.142(6) Uani 1 1 d . . . H37A H 0.5162 0.1670 0.7869 0.170 Uiso 1 1 calc R . . H37B H 0.6285 0.1473 0.7922 0.170 Uiso 1 1 calc R . . C38 C 0.5499(15) 0.1393(9) 0.6637(16) 0.195(10) Uani 1 1 d . . . H38A H 0.4907 0.1616 0.6314 0.234 Uiso 1 1 calc R . . H38B H 0.6043 0.1493 0.6328 0.234 Uiso 1 1 calc R . . C39 C 0.5365(13) 0.0640(15) 0.6693(13) 0.223(10) Uani 1 1 d . . . H39A H 0.5215 0.0436 0.6117 0.334 Uiso 1 1 calc R . . H39B H 0.4829 0.0544 0.7001 0.334 Uiso 1 1 calc R . . H39C H 0.5959 0.0420 0.7001 0.334 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0948(4) 0.0884(4) 0.0758(4) 0.0025(3) 0.0004(3) -0.0046(3) Cl1 0.144(3) 0.086(2) 0.143(3) 0.008(2) 0.017(2) 0.002(2) Cl2 0.126(3) 0.098(3) 0.158(3) 0.008(2) 0.003(3) -0.028(2) O1 0.104(7) 0.081(5) 0.092(6) 0.004(4) 0.014(5) -0.020(5) O2 0.095(6) 0.082(5) 0.094(5) 0.008(4) 0.001(5) -0.003(5) O3 0.116(8) 0.090(7) 0.211(11) -0.001(7) 0.052(7) 0.000(6) O4 0.144(9) 0.088(7) 0.176(10) 0.018(6) 0.062(7) -0.005(6) O5 0.108(8) 0.145(8) 0.137(8) -0.010(7) 0.008(6) -0.004(7) O6 0.140(8) 0.097(7) 0.147(9) -0.004(6) -0.010(7) 0.007(6) O7 0.092(5) 0.086(5) 0.075(5) -0.002(4) 0.008(4) -0.003(4) N1 0.139(9) 0.112(8) 0.065(6) 0.001(5) 0.004(6) -0.007(6) N2 0.099(8) 0.077(7) 0.072(6) -0.003(5) 0.018(6) -0.011(7) N3 0.165(11) 0.069(8) 0.051(6) -0.005(5) -0.005(6) 0.053(8) N4 0.112(9) 0.121(9) 0.068(7) 0.014(7) 0.022(7) 0.008(7) C1 0.065(10) 0.174(16) 0.054(7) 0.001(8) 0.007(7) 0.001(11) C2 0.128(14) 0.082(10) 0.068(8) -0.008(7) 0.030(8) 0.000(10) C3 0.087(11) 0.166(15) 0.094(10) -0.012(10) 0.024(8) -0.001(12) C4 0.159(17) 0.122(13) 0.102(12) -0.024(10) 0.036(11) -0.002(13) C5 0.065(10) 0.24(2) 0.071(9) -0.018(11) 0.013(7) -0.030(12) C6 0.109(12) 0.136(11) 0.069(8) -0.024(8) 0.018(8) -0.050(11) C7 0.118(14) 0.100(12) 0.095(10) 0.023(9) 0.027(9) -0.003(11) C8 0.108(12) 0.077(10) 0.069(8) -0.001(6) 0.002(7) -0.004(9) C9 0.065(9) 0.084(10) 0.066(7) 0.008(6) -0.006(6) -0.022(8) C10 0.088(10) 0.098(10) 0.078(8) 0.003(7) 0.000(7) -0.001(9) C11 0.100(11) 0.093(11) 0.085(9) 0.004(7) -0.001(8) -0.016(9) C12 0.121(12) 0.090(10) 0.076(8) -0.005(7) -0.002(8) 0.005(10) C13 0.096(10) 0.094(10) 0.078(8) -0.003(7) 0.000(7) -0.018(9) C14 0.067(9) 0.108(11) 0.070(8) -0.003(7) 0.001(7) 0.017(9) C15 0.075(10) 0.130(13) 0.066(8) -0.004(8) 0.011(7) -0.035(10) C16 0.081(12) 0.113(13) 0.094(9) -0.016(8) 0.017(8) -0.014(10) C17 0.136(14) 0.107(12) 0.089(9) -0.013(9) 0.008(9) 0.015(11) C18 0.108(12) 0.116(13) 0.084(9) -0.005(8) 0.003(8) 0.037(10) C19 0.127(13) 0.091(11) 0.074(8) -0.008(8) 0.002(8) -0.012(10) C20 0.186(18) 0.043(8) 0.085(10) -0.003(7) -0.021(11) -0.015(10) C24 0.132(13) 0.135(12) 0.104(10) 0.024(9) 0.003(10) 0.041(10) C25 0.114(14) 0.29(2) 0.172(16) 0.070(16) 0.070(13) 0.095(15) C26 0.14(2) 0.47(4) 0.30(3) 0.19(3) 0.14(2) 0.14(2) C27 0.27(4) 0.52(6) 0.33(4) 0.24(4) 0.11(3) 0.15(4) C28 0.097(10) 0.120(11) 0.101(10) 0.015(10) 0.016(8) -0.009(9) C29 0.113(11) 0.135(13) 0.105(11) -0.004(10) 0.016(9) 0.009(9) C30 0.152(15) 0.119(13) 0.163(16) -0.009(12) 0.045(12) -0.014(11) C31 0.190(18) 0.139(14) 0.21(2) -0.031(15) 0.053(15) -0.014(13) C32 0.108(11) 0.119(10) 0.081(9) 0.012(8) 0.015(9) 0.007(8) C33 0.117(12) 0.136(11) 0.064(8) -0.004(7) 0.010(9) -0.021(9) C34 0.102(10) 0.125(11) 0.087(9) 0.001(8) 0.003(9) 0.003(9) C35 0.111(12) 0.178(15) 0.111(11) -0.008(10) -0.003(9) 0.009(10) C36 0.150(13) 0.103(11) 0.104(12) 0.018(9) 0.052(10) 0.000(9) C37 0.168(15) 0.148(16) 0.112(13) -0.010(11) 0.030(11) 0.018(12) C38 0.23(2) 0.084(12) 0.30(3) -0.016(15) 0.12(2) -0.042(13) C39 0.17(2) 0.29(3) 0.22(2) 0.00(2) 0.081(18) 0.04(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 N1 1.625(9) . ? Os1 N3 1.854(13) . ? Os1 N2 1.974(9) . ? Os1 O1 2.007(7) . ? Os1 O2 2.014(8) . ? Cl1 C12 1.730(14) . ? Cl2 C11 1.737(12) . ? O1 C1 1.384(14) . ? O2 C14 1.341(12) . ? O3 C7 1.218(15) . ? O4 C20 1.266(17) . ? O5 C16 1.223(13) . ? O6 C19 1.252(14) . ? N2 C8 1.415(14) . ? N2 C7 1.417(16) . ? N3 C9 1.409(14) . ? N3 C20 1.430(19) . ? N4 C32 1.488(14) . ? N4 C36 1.490(14) . ? N4 C28 1.505(14) . ? N4 C24 1.534(15) . ? C1 C2 1.390(18) . ? C1 C6 1.437(16) . ? C2 C3 1.406(16) . ? C2 C7 1.518(18) . ? C3 C4 1.390(18) . ? C4 C5 1.41(2) . ? C5 C6 1.413(17) . ? C8 C13 1.389(15) . ? C8 C9 1.405(15) . ? C9 C10 1.378(15) . ? C10 C11 1.398(15) . ? C11 C12 1.394(16) . ? C12 C13 1.375(16) . ? C14 C15 1.350(15) . ? C14 C19 1.522(16) . ? C15 C16 1.446(16) . ? C15 C20 1.535(19) . ? C16 C17 1.463(17) . ? C17 C18 1.350(17) . ? C18 C19 1.438(18) . ? C24 C25 1.542(19) . ? C25 C26 1.55(3) . ? C26 C27 1.31(2) . ? C28 C29 1.514(17) . ? C29 C30 1.518(17) . ? C30 C31 1.473(18) . ? C32 C33 1.520(15) . ? C33 C34 1.518(14) . ? C34 C35 1.480(15) . ? C36 C37 1.467(17) . ? C37 C38 1.57(2) . ? C38 C39 1.39(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 Os1 N3 101.2(4) . . ? N1 Os1 N2 102.3(4) . . ? N3 Os1 N2 81.0(5) . . ? N1 Os1 O1 103.7(4) . . ? N3 Os1 O1 155.1(3) . . ? N2 Os1 O1 93.2(4) . . ? N1 Os1 O2 101.7(4) . . ? N3 Os1 O2 94.7(4) . . ? N2 Os1 O2 155.9(3) . . ? O1 Os1 O2 80.7(3) . . ? C1 O1 Os1 123.1(8) . . ? C14 O2 Os1 120.7(7) . . ? C8 N2 C7 120.1(11) . . ? C8 N2 Os1 113.3(9) . . ? C7 N2 Os1 125.2(9) . . ? C9 N3 C20 111.6(11) . . ? C9 N3 Os1 119.4(9) . . ? C20 N3 Os1 127.9(9) . . ? C32 N4 C36 112.9(10) . . ? C32 N4 C28 111.5(10) . . ? C36 N4 C28 105.0(10) . . ? C32 N4 C24 106.4(10) . . ? C36 N4 C24 111.4(11) . . ? C28 N4 C24 109.8(11) . . ? O1 C1 C2 126.3(14) . . ? O1 C1 C6 112.7(15) . . ? C2 C1 C6 121.0(13) . . ? C1 C2 C3 118.5(13) . . ? C1 C2 C7 126.2(15) . . ? C3 C2 C7 115.2(14) . . ? C4 C3 C2 123.7(16) . . ? C3 C4 C5 116.1(17) . . ? C4 C5 C6 123.6(16) . . ? C5 C6 C1 116.9(14) . . ? O3 C7 N2 122.7(13) . . ? O3 C7 C2 117.9(15) . . ? N2 C7 C2 119.4(14) . . ? C13 C8 C9 119.8(13) . . ? C13 C8 N2 126.5(13) . . ? C9 C8 N2 113.7(11) . . ? C10 C9 C8 118.7(12) . . ? C10 C9 N3 129.8(13) . . ? C8 C9 N3 111.3(11) . . ? C9 C10 C11 121.7(12) . . ? C12 C11 C10 118.8(12) . . ? C12 C11 Cl2 121.1(12) . . ? C10 C11 Cl2 120.1(12) . . ? C13 C12 C11 120.0(12) . . ? C13 C12 Cl1 120.9(13) . . ? C11 C12 Cl1 119.1(13) . . ? C12 C13 C8 120.9(13) . . ? O2 C14 C15 126.5(12) . . ? O2 C14 C19 109.5(12) . . ? C15 C14 C19 124.0(12) . . ? C14 C15 C16 114.7(13) . . ? C14 C15 C20 124.6(13) . . ? C16 C15 C20 120.6(13) . . ? O5 C16 C15 120.4(14) . . ? O5 C16 C17 116.3(14) . . ? C15 C16 C17 123.2(14) . . ? C18 C17 C16 120.9(14) . . ? C17 C18 C19 119.4(13) . . ? O6 C19 C18 123.2(14) . . ? O6 C19 C14 119.1(14) . . ? C18 C19 C14 117.6(13) . . ? O4 C20 N3 129.5(13) . . ? O4 C20 C15 114.6(17) . . ? N3 C20 C15 115.8(14) . . ? N4 C24 C25 114.3(12) . . ? C24 C25 C26 106.9(14) . . ? C27 C26 C25 110(2) . . ? N4 C28 C29 117.6(11) . . ? C28 C29 C30 113.0(12) . . ? C31 C30 C29 113.4(15) . . ? N4 C32 C33 115.1(10) . . ? C34 C33 C32 112.5(10) . . ? C35 C34 C33 114.9(11) . . ? C37 C36 N4 115.4(12) . . ? C36 C37 C38 108.4(13) . . ? C39 C38 C37 109.4(19) . . ? _diffrn_measured_fraction_theta_max 0.735 _diffrn_reflns_theta_full 23.74 _diffrn_measured_fraction_theta_full 0.735 _refine_diff_density_max 0.654 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.243 data_mar342 _database_code_CSD 209735 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H49 Cl N3 O4 Ru' _chemical_formula_sum 'C47 H49 Cl N3 O4 Ru' _chemical_formula_weight 856.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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' _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 10.239(2) _cell_length_b 13.922(3) _cell_length_c 16.454(3) _cell_angle_alpha 100.42(3) _cell_angle_beta 106.97(3) _cell_angle_gamma 107.30(3) _cell_volume 2047.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 0.496 _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 301(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9853 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.43 _reflns_number_total 5588 _reflns_number_gt 3929 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5588 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.26190(4) 0.35916(3) 0.67361(3) 0.04183(18) Uani 1 1 d . . . Cl1 Cl 0.44215(13) 0.29618(10) 0.64440(9) 0.0514(4) Uani 1 1 d . . . O1 O 0.1030(3) 0.2456(2) 0.5678(2) 0.0441(8) Uani 1 1 d . . . O2 O 0.4056(3) 0.4661(3) 0.7869(2) 0.0481(9) Uani 1 1 d . . . O4 O 0.2239(8) 0.8928(6) 0.2101(5) 0.176(3) Uani 1 1 d . . . N1 N 0.3010(4) 0.4645(3) 0.6002(3) 0.0405(10) Uani 1 1 d . . . N2 N 0.2356(4) 0.2502(3) 0.7467(3) 0.0446(10) Uani 1 1 d . . . N3 N 0.0925(4) 0.3979(4) 0.7042(3) 0.0504(11) Uani 1 1 d . . . C1 C 0.0245(5) 0.2585(4) 0.4871(3) 0.0412(12) Uani 1 1 d . . . C2 C 0.0426(5) 0.3736(4) 0.4976(3) 0.0438(13) Uani 1 1 d . . . H2A H -0.0206 0.3778 0.4426 0.053 Uiso 1 1 calc R . . H2B H 0.0080 0.3961 0.5439 0.053 Uiso 1 1 calc R . . C3 C 0.1966(5) 0.4501(4) 0.5200(4) 0.0443(13) Uani 1 1 d . . . C4 C 0.2293(6) 0.5047(4) 0.4630(4) 0.0515(14) Uani 1 1 d . . . H4 H 0.1573 0.4918 0.4081 0.062 Uiso 1 1 calc R . . C5 C 0.3681(6) 0.5787(4) 0.4859(4) 0.0568(15) Uani 1 1 d . . . H5 H 0.3913 0.6157 0.4471 0.068 Uiso 1 1 calc R . . C6 C 0.4715(6) 0.5964(4) 0.5682(4) 0.0518(14) Uani 1 1 d . . . H6 H 0.5653 0.6471 0.5860 0.062 Uiso 1 1 calc R . . C7 C 0.4362(5) 0.5390(4) 0.6243(3) 0.0420(12) Uani 1 1 d . . . C8 C 0.5547(5) 0.5550(4) 0.7111(3) 0.0454(13) Uani 1 1 d . . . H8A H 0.6354 0.6201 0.7227 0.054 Uiso 1 1 calc R . . H8B H 0.5911 0.4985 0.7028 0.054 Uiso 1 1 calc R . . C9 C 0.5169(5) 0.5596(4) 0.7953(3) 0.0461(13) Uani 1 1 d . . . C10 C -0.1376(5) 0.1865(4) 0.4621(3) 0.0420(12) Uani 1 1 d . . . C11 C -0.1699(6) 0.0845(5) 0.4633(4) 0.0646(17) Uani 1 1 d . . . H11 H -0.0937 0.0597 0.4775 0.078 Uiso 1 1 calc R . . C12 C -0.3105(6) 0.0173(5) 0.4445(4) 0.0689(17) Uani 1 1 d . . . H12 H -0.3284 -0.0515 0.4466 0.083 Uiso 1 1 calc R . . C13 C -0.4246(6) 0.0519(5) 0.4226(5) 0.0742(19) Uani 1 1 d . . . H13 H -0.5206 0.0072 0.4098 0.089 Uiso 1 1 calc R . . C14 C -0.3947(7) 0.1520(6) 0.4200(6) 0.102(3) Uani 1 1 d . . . H14 H -0.4710 0.1766 0.4055 0.122 Uiso 1 1 calc R . . C15 C -0.2516(6) 0.2193(5) 0.4387(5) 0.079(2) Uani 1 1 d . . . H15 H -0.2340 0.2876 0.4351 0.095 Uiso 1 1 calc R . . C16 C 0.0751(5) 0.2195(4) 0.4126(4) 0.0445(13) Uani 1 1 d . . . C17 C 0.0208(7) 0.2326(5) 0.3291(4) 0.0634(16) Uani 1 1 d . . . H17 H -0.0444 0.2674 0.3191 0.076 Uiso 1 1 calc R . . C18 C 0.0618(8) 0.1951(5) 0.2610(5) 0.080(2) Uani 1 1 d . . . H18 H 0.0236 0.2043 0.2056 0.096 Uiso 1 1 calc R . . C19 C 0.1572(8) 0.1449(6) 0.2741(5) 0.084(2) Uani 1 1 d . . . H19 H 0.1859 0.1204 0.2284 0.100 Uiso 1 1 calc R . . C20 C 0.2117(6) 0.1304(5) 0.3561(5) 0.080(2) Uani 1 1 d . . . H20 H 0.2754 0.0943 0.3650 0.096 Uiso 1 1 calc R . . C21 C 0.1729(6) 0.1687(4) 0.4257(4) 0.0567(15) Uani 1 1 d . . . H21 H 0.2128 0.1601 0.4811 0.068 Uiso 1 1 calc R . . C22 C 0.6592(5) 0.5736(4) 0.8706(4) 0.0508(14) Uani 1 1 d . . . C23 C 0.6648(6) 0.4972(5) 0.9130(4) 0.0699(18) Uani 1 1 d . . . H23 H 0.5830 0.4354 0.8957 0.084 Uiso 1 1 calc R . . C24 C 0.7938(8) 0.5131(6) 0.9819(5) 0.086(2) Uani 1 1 d . . . H24 H 0.7959 0.4619 1.0111 0.103 Uiso 1 1 calc R . . C25 C 0.9158(8) 0.6005(7) 1.0077(5) 0.087(2) Uani 1 1 d . . . H25 H 1.0007 0.6092 1.0538 0.105 Uiso 1 1 calc R . . C26 C 0.9129(7) 0.6767(6) 0.9649(5) 0.084(2) Uani 1 1 d . . . H26 H 0.9969 0.7366 0.9813 0.101 Uiso 1 1 calc R . . C27 C 0.7841(6) 0.6641(5) 0.8970(4) 0.0709(18) Uani 1 1 d . . . H27 H 0.7819 0.7165 0.8693 0.085 Uiso 1 1 calc R . . C28 C 0.4709(6) 0.6518(4) 0.8227(4) 0.0560(15) Uani 1 1 d . . . C29 C 0.4355(7) 0.6622(5) 0.8983(4) 0.080(2) Uani 1 1 d . . . H29 H 0.4454 0.6159 0.9318 0.097 Uiso 1 1 calc R . . C30 C 0.3864(9) 0.7395(7) 0.9244(6) 0.105(3) Uani 1 1 d . . . H30 H 0.3623 0.7444 0.9750 0.126 Uiso 1 1 calc R . . C31 C 0.3723(11) 0.8089(7) 0.8776(7) 0.126(4) Uani 1 1 d . . . H31 H 0.3395 0.8614 0.8962 0.151 Uiso 1 1 calc R . . C32 C 0.4066(10) 0.8014(6) 0.8027(6) 0.116(3) Uani 1 1 d . . . H32 H 0.3954 0.8478 0.7694 0.139 Uiso 1 1 calc R . . C33 C 0.4582(8) 0.7235(5) 0.7771(5) 0.085(2) Uani 1 1 d . . . H33 H 0.4849 0.7201 0.7275 0.102 Uiso 1 1 calc R . . C34 C 0.2529(8) 0.2811(5) 0.8357(4) 0.082(2) Uani 1 1 d . . . H34 H 0.2697 0.3501 0.8646 0.098 Uiso 1 1 calc R . . C35 C 0.2432(10) 0.1997(7) 0.8818(5) 0.108(3) Uani 1 1 d . . . H35 H 0.2739 0.2201 0.9435 0.130 Uiso 1 1 calc R . . C36 C 0.1942(11) 0.1024(5) 0.8401(5) 0.122(4) Uani 1 1 d . . . H36 H 0.1680 0.0527 0.8693 0.146 Uiso 1 1 calc R . . C37 C 0.1799(8) 0.0710(5) 0.7581(6) 0.095(2) Uani 1 1 d . . . H37 H 0.1684 0.0020 0.7332 0.114 Uiso 1 1 calc R . . C38 C 0.1821(7) 0.1444(5) 0.7043(4) 0.0688(17) Uani 1 1 d . . . H38 H 0.1479 0.1197 0.6426 0.083 Uiso 1 1 calc R . . C39 C -0.0353(6) 0.3213(5) 0.6869(4) 0.0651(17) Uani 1 1 d . . . H39 H -0.0505 0.2529 0.6576 0.078 Uiso 1 1 calc R . . C40 C -0.1458(7) 0.3398(7) 0.7110(5) 0.082(2) Uani 1 1 d . . . H40 H -0.2354 0.2850 0.6956 0.099 Uiso 1 1 calc R . . C41 C -0.1236(9) 0.4380(8) 0.7570(5) 0.087(2) Uani 1 1 d . . . H41 H -0.1947 0.4513 0.7767 0.104 Uiso 1 1 calc R . . C42 C 0.0073(8) 0.5171(6) 0.7738(4) 0.080(2) Uani 1 1 d . . . H42 H 0.0255 0.5857 0.8042 0.096 Uiso 1 1 calc R . . C43 C 0.1111(6) 0.4944(5) 0.7455(4) 0.0626(16) Uani 1 1 d . . . H43 H 0.1981 0.5492 0.7558 0.075 Uiso 1 1 calc R . . C45 C 0.3454(9) 0.7614(7) 1.1438(5) 0.096(2) Uiso 1 1 d . . . C47 C 0.012(6) 1.013(3) 0.982(2) 0.182(13) Uiso 0.50 1 d P . . O3 O 0.258(2) 0.9288(15) 1.0963(14) 0.207(7) Uiso 0.50 1 d P . . C44 C 0.367(2) 0.8482(15) 1.1874(12) 0.243(8) Uiso 1 1 d . . . C46 C 0.097(4) 0.998(2) 1.001(2) 0.175(12) Uiso 0.50 1 d P . . O3' O 0.402(3) 0.9040(19) 1.1363(17) 0.251(10) Uiso 0.50 1 d P . . C47' C 0.225(4) 0.958(3) 1.011(3) 0.233(16) Uiso 0.50 1 d P . . C46' C 0.208(4) 1.020(3) 1.038(2) 0.189(12) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0383(3) 0.0446(3) 0.0436(3) 0.0122(2) 0.01747(19) 0.01497(19) Cl1 0.0437(7) 0.0546(9) 0.0620(9) 0.0183(7) 0.0240(6) 0.0216(6) O1 0.0427(19) 0.040(2) 0.046(2) 0.0120(17) 0.0114(16) 0.0149(15) O2 0.0431(19) 0.051(2) 0.041(2) 0.0096(17) 0.0155(16) 0.0089(17) O4 0.177(7) 0.139(6) 0.206(8) 0.011(6) 0.054(6) 0.092(5) N1 0.037(2) 0.042(3) 0.042(3) 0.010(2) 0.016(2) 0.0144(19) N2 0.043(2) 0.046(3) 0.043(3) 0.015(2) 0.016(2) 0.012(2) N3 0.040(3) 0.060(3) 0.046(3) 0.014(2) 0.015(2) 0.013(2) C1 0.036(3) 0.044(3) 0.043(3) 0.012(3) 0.012(2) 0.017(2) C2 0.040(3) 0.041(3) 0.050(3) 0.013(3) 0.013(2) 0.017(2) C3 0.046(3) 0.038(3) 0.053(4) 0.010(3) 0.021(3) 0.020(2) C4 0.057(3) 0.055(4) 0.053(4) 0.024(3) 0.022(3) 0.027(3) C5 0.065(4) 0.057(4) 0.064(4) 0.032(3) 0.034(3) 0.026(3) C6 0.052(3) 0.045(3) 0.059(4) 0.017(3) 0.024(3) 0.014(3) C7 0.042(3) 0.037(3) 0.048(3) 0.011(3) 0.020(3) 0.013(2) C8 0.039(3) 0.044(3) 0.047(3) 0.009(3) 0.015(2) 0.009(2) C9 0.041(3) 0.041(3) 0.045(3) 0.003(3) 0.013(2) 0.008(2) C10 0.035(3) 0.044(3) 0.043(3) 0.008(3) 0.012(2) 0.014(2) C11 0.046(3) 0.055(4) 0.097(5) 0.026(4) 0.026(3) 0.022(3) C12 0.056(4) 0.053(4) 0.098(5) 0.031(4) 0.027(3) 0.016(3) C13 0.041(3) 0.070(5) 0.108(6) 0.030(4) 0.028(3) 0.013(3) C14 0.045(4) 0.077(5) 0.191(9) 0.065(6) 0.034(5) 0.028(4) C15 0.044(3) 0.055(4) 0.138(7) 0.039(4) 0.023(4) 0.020(3) C16 0.039(3) 0.041(3) 0.052(4) 0.011(3) 0.019(3) 0.012(2) C17 0.079(4) 0.059(4) 0.060(4) 0.019(3) 0.033(3) 0.028(3) C18 0.112(6) 0.066(5) 0.066(5) 0.021(4) 0.046(4) 0.025(4) C19 0.082(5) 0.077(5) 0.077(6) -0.006(4) 0.048(4) 0.007(4) C20 0.048(4) 0.075(5) 0.094(6) -0.015(4) 0.023(4) 0.017(3) C21 0.047(3) 0.056(4) 0.062(4) 0.004(3) 0.018(3) 0.020(3) C22 0.042(3) 0.054(4) 0.045(3) 0.005(3) 0.011(3) 0.012(3) C23 0.055(4) 0.077(5) 0.076(5) 0.029(4) 0.019(3) 0.022(3) C24 0.076(5) 0.098(6) 0.090(6) 0.050(5) 0.021(4) 0.037(4) C25 0.064(5) 0.125(7) 0.068(5) 0.023(5) 0.010(4) 0.046(5) C26 0.055(4) 0.090(6) 0.071(5) 0.005(4) 0.002(4) 0.006(4) C27 0.058(4) 0.072(5) 0.067(4) 0.021(4) 0.012(3) 0.014(3) C28 0.048(3) 0.052(4) 0.055(4) 0.006(3) 0.013(3) 0.014(3) C29 0.090(5) 0.084(5) 0.065(5) 0.005(4) 0.030(4) 0.038(4) C30 0.119(7) 0.116(7) 0.093(6) 0.003(6) 0.047(5) 0.070(6) C31 0.156(9) 0.102(7) 0.129(9) -0.004(6) 0.053(7) 0.083(7) C32 0.159(8) 0.088(6) 0.114(7) 0.015(5) 0.043(6) 0.080(6) C33 0.109(6) 0.065(5) 0.087(5) 0.014(4) 0.038(4) 0.042(4) C34 0.115(6) 0.069(5) 0.051(4) 0.016(4) 0.035(4) 0.017(4) C35 0.163(8) 0.129(8) 0.053(5) 0.054(6) 0.051(5) 0.055(7) C36 0.264(11) 0.036(4) 0.029(4) 0.019(3) 0.048(5) 0.005(5) C37 0.126(6) 0.045(4) 0.102(7) 0.037(4) 0.035(5) 0.013(4) C38 0.084(4) 0.056(4) 0.056(4) 0.015(3) 0.019(3) 0.019(3) C39 0.056(4) 0.079(5) 0.070(4) 0.024(4) 0.033(3) 0.027(3) C40 0.051(4) 0.127(7) 0.093(6) 0.053(5) 0.043(4) 0.038(4) C41 0.085(6) 0.147(8) 0.070(5) 0.046(5) 0.040(4) 0.080(6) C42 0.082(5) 0.099(6) 0.072(5) 0.011(4) 0.027(4) 0.062(5) C43 0.053(4) 0.068(4) 0.063(4) 0.008(3) 0.017(3) 0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O2 1.987(4) . ? Ru1 O1 1.999(3) . ? Ru1 N1 2.084(4) . ? Ru1 N2 2.103(4) . ? Ru1 N3 2.126(4) . ? Ru1 Cl1 2.3946(14) . ? O1 C1 1.411(6) . ? O2 C9 1.405(6) . ? O4 C44 1.856(18) 1_554 ? N1 C7 1.351(6) . ? N1 C3 1.370(6) . ? N2 C38 1.372(7) . ? N2 C34 1.391(7) . ? N3 C43 1.321(7) . ? N3 C39 1.332(7) . ? C1 C2 1.529(6) . ? C1 C16 1.537(7) . ? C1 C10 1.547(6) . ? C2 C3 1.508(7) . ? C3 C4 1.364(7) . ? C4 C5 1.378(7) . ? C5 C6 1.379(7) . ? C6 C7 1.382(7) . ? C7 C8 1.508(7) . ? C8 C9 1.538(7) . ? C9 C28 1.532(7) . ? C9 C22 1.544(7) . ? C10 C15 1.356(7) . ? C10 C11 1.365(7) . ? C11 C12 1.370(7) . ? C12 C13 1.371(8) . ? C13 C14 1.347(8) . ? C14 C15 1.390(8) . ? C16 C21 1.378(7) . ? C16 C17 1.391(7) . ? C17 C18 1.378(8) . ? C18 C19 1.352(9) . ? C19 C20 1.378(10) . ? C20 C21 1.386(8) . ? C22 C23 1.380(8) . ? C22 C27 1.389(8) . ? C23 C24 1.393(8) . ? C24 C25 1.350(10) . ? C25 C26 1.378(9) . ? C26 C27 1.396(8) . ? C28 C33 1.366(9) . ? C28 C29 1.390(8) . ? C29 C30 1.369(9) . ? C30 C31 1.355(11) . ? C31 C32 1.372(12) . ? C32 C33 1.393(9) . ? C34 C35 1.470(9) . ? C35 C36 1.272(9) . ? C36 C37 1.292(9) . ? C37 C38 1.468(8) . ? C39 C40 1.379(8) . ? C40 C41 1.354(10) . ? C41 C42 1.372(10) . ? C42 C43 1.372(8) . ? C45 C44 1.208(18) . ? C45 O3' 1.93(3) . ? C47 C47 0.81(7) 2_577 ? C47 C46 0.93(6) . ? C47 C46 1.20(5) 2_577 ? O3 C46' 1.83(4) . ? O3 O3' 1.59(2) . ? O3 C47' 1.50(4) . ? C44 O3' 1.30(3) . ? C44 O4 1.856(18) 1_556 ? C46 C47' 1.54(4) . ? C46 C46' 1.04(4) . ? C46 C47 1.20(5) 2_577 ? C47' C46' 0.98(4) . ? 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 O2 Ru1 O1 173.29(13) . . ? O2 Ru1 N1 92.28(15) . . ? O1 Ru1 N1 93.07(15) . . ? O2 Ru1 N2 87.42(15) . . ? O1 Ru1 N2 87.53(15) . . ? N1 Ru1 N2 175.80(14) . . ? O2 Ru1 N3 88.23(15) . . ? O1 Ru1 N3 87.15(15) . . ? N1 Ru1 N3 96.55(16) . . ? N2 Ru1 N3 87.64(16) . . ? O2 Ru1 Cl1 93.52(10) . . ? O1 Ru1 Cl1 90.49(10) . . ? N1 Ru1 Cl1 90.29(11) . . ? N2 Ru1 Cl1 85.55(11) . . ? N3 Ru1 Cl1 172.88(13) . . ? C1 O1 Ru1 126.6(3) . . ? C9 O2 Ru1 126.1(3) . . ? C7 N1 C3 118.4(4) . . ? C7 N1 Ru1 120.6(3) . . ? C3 N1 Ru1 120.4(3) . . ? C38 N2 C34 117.8(5) . . ? C38 N2 Ru1 120.0(4) . . ? C34 N2 Ru1 121.7(4) . . ? C43 N3 C39 117.7(5) . . ? C43 N3 Ru1 122.9(4) . . ? C39 N3 Ru1 119.3(4) . . ? O1 C1 C2 111.0(4) . . ? O1 C1 C16 111.0(4) . . ? C2 C1 C16 109.7(4) . . ? O1 C1 C10 105.5(4) . . ? C2 C1 C10 111.9(4) . . ? C16 C1 C10 107.6(4) . . ? C3 C2 C1 116.0(4) . . ? C4 C3 N1 121.3(5) . . ? C4 C3 C2 120.8(5) . . ? N1 C3 C2 117.8(5) . . ? C3 C4 C5 120.6(5) . . ? C6 C5 C4 118.0(5) . . ? C5 C6 C7 120.3(5) . . ? N1 C7 C6 121.3(5) . . ? N1 C7 C8 119.7(4) . . ? C6 C7 C8 118.9(5) . . ? C7 C8 C9 119.0(4) . . ? O2 C9 C28 108.3(4) . . ? O2 C9 C8 112.0(4) . . ? C28 C9 C8 114.0(5) . . ? O2 C9 C22 108.5(4) . . ? C28 C9 C22 108.0(4) . . ? C8 C9 C22 105.8(4) . . ? C15 C10 C11 117.3(5) . . ? C15 C10 C1 123.4(5) . . ? C11 C10 C1 119.3(4) . . ? C10 C11 C12 122.3(5) . . ? C13 C12 C11 119.8(6) . . ? C14 C13 C12 118.5(5) . . ? C13 C14 C15 121.2(6) . . ? C10 C15 C14 120.8(6) . . ? C21 C16 C17 117.9(5) . . ? C21 C16 C1 121.3(5) . . ? C17 C16 C1 120.7(4) . . ? C18 C17 C16 121.3(6) . . ? C19 C18 C17 120.4(7) . . ? C18 C19 C20 119.3(6) . . ? C19 C20 C21 121.0(6) . . ? C16 C21 C20 120.0(6) . . ? C23 C22 C27 118.8(5) . . ? C23 C22 C9 120.9(5) . . ? C27 C22 C9 120.3(5) . . ? C22 C23 C24 119.6(6) . . ? C25 C24 C23 122.0(7) . . ? C24 C25 C26 119.1(6) . . ? C25 C26 C27 120.1(6) . . ? C22 C27 C26 120.4(6) . . ? C33 C28 C29 117.1(6) . . ? C33 C28 C9 125.0(6) . . ? C29 C28 C9 117.8(6) . . ? C30 C29 C28 121.2(7) . . ? C31 C30 C29 120.9(8) . . ? C30 C31 C32 119.7(8) . . ? C31 C32 C33 119.2(9) . . ? C28 C33 C32 121.9(7) . . ? N2 C34 C35 116.8(6) . . ? C36 C35 C34 122.1(7) . . ? C35 C36 C37 121.4(7) . . ? C36 C37 C38 119.8(7) . . ? N2 C38 C37 118.7(6) . . ? N3 C39 C40 122.3(6) . . ? C41 C40 C39 119.8(7) . . ? C40 C41 C42 117.8(6) . . ? C41 C42 C43 119.6(7) . . ? N3 C43 C42 122.7(6) . . ? C44 C45 O3' 41.2(11) . . ? C47 C47 C46 88(7) 2_577 . ? C47 C47 C46 50(6) 2_577 2_577 ? C46 C47 C46 138(4) . 2_577 ? C46' O3 O3' 137(2) . . ? C46' O3 C47' 32.2(17) . . ? O3' O3 C47' 122(2) . . ? C45 C44 O3' 101.0(19) . . ? C45 C44 O4 125.5(14) . 1_556 ? O3' C44 O4 100.3(17) . 1_556 ? C47 C46 C47' 167(5) . . ? C47 C46 C46' 152(6) . . ? C47' C46 C46' 38(3) . . ? C47 C46 C47 42(4) . 2_577 ? C47' C46 C47 143(4) . 2_577 ? C46' C46 C47 136(5) . 2_577 ? C44 O3' O3 103(2) . . ? C44 O3' C45 37.8(12) . . ? O3 O3' C45 109.6(15) . . ? C46' C47' C46 41(3) . . ? C46' C47' O3 93(4) . . ? C46 C47' O3 108(3) . . ? C47' C46' O3 55(3) . . ? C47' C46' C46 100(5) . . ? O3 C46' C46 116(4) . . ? _diffrn_measured_fraction_theta_max 0.739 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.739 _refine_diff_density_max 0.680 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.141 data_mar477 _database_code_CSD 209736 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H45 Cl N7 O4 Ru' _chemical_formula_sum 'C43 H45 Cl N7 O4 Ru' _chemical_formula_weight 860.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.621(2) _cell_length_b 35.268(7) _cell_length_c 11.953(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.79(3) _cell_angle_gamma 90.00 _cell_volume 4018.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.508 _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 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15534 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6103 _reflns_number_gt 4089 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6103 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.05160(3) 0.131312(11) 0.41182(3) 0.03644(14) Uani 1 1 d . . . O1 O 0.1408(3) 0.17939(9) 0.4673(2) 0.0393(7) Uani 1 1 d . . . O2 O -0.0324(3) 0.07965(10) 0.3839(3) 0.0444(8) Uani 1 1 d . . . N1 N 0.0380(3) 0.14494(11) 0.2420(3) 0.0373(9) Uani 1 1 d . . . N2 N 0.2520(3) 0.10866(12) 0.4039(3) 0.0427(9) Uani 1 1 d . . . N3 N 0.3539(3) 0.10783(13) 0.4930(3) 0.0483(10) Uani 1 1 d . . . H3 H 0.3462 0.1168 0.5587 0.058 Uiso 1 1 calc R . . N4 N 0.0724(3) 0.11536(12) 0.5813(3) 0.0395(9) Uani 1 1 d . . . N5 N 0.0621(4) 0.07852(14) 0.6076(4) 0.0614(12) Uani 1 1 d . . . H5 H 0.0360 0.0610 0.5591 0.074 Uiso 1 1 calc R . . N6 N -0.1473(3) 0.15419(11) 0.4187(3) 0.0402(9) Uani 1 1 d . . . N7 N -0.2163(4) 0.15024(13) 0.5079(3) 0.0496(10) Uani 1 1 d . . . H7 H -0.1864 0.1371 0.5670 0.060 Uiso 1 1 calc R . . C1 C 0.1736(4) 0.20922(14) 0.3952(4) 0.0389(11) Uani 1 1 d . . . C2 C 0.2289(4) 0.19233(14) 0.2912(3) 0.0412(11) Uani 1 1 d . . . H2A H 0.2689 0.2128 0.2518 0.049 Uiso 1 1 calc R . . H2B H 0.3047 0.1751 0.3176 0.049 Uiso 1 1 calc R . . C3 C 0.1272(4) 0.17159(14) 0.2074(4) 0.0410(11) Uani 1 1 d . . . C4 C 0.1258(5) 0.17910(16) 0.0939(4) 0.0533(13) Uani 1 1 d . . . H4 H 0.1887 0.1965 0.0707 0.064 Uiso 1 1 calc R . . C5 C 0.0309(6) 0.16085(18) 0.0148(4) 0.0627(15) Uani 1 1 d . . . H5A H 0.0286 0.1659 -0.0618 0.075 Uiso 1 1 calc R . . C6 C -0.0601(6) 0.13504(16) 0.0514(5) 0.0570(14) Uani 1 1 d . . . H6 H -0.1258 0.1229 -0.0009 0.068 Uiso 1 1 calc R . . C7 C -0.0553(5) 0.12696(14) 0.1640(4) 0.0451(12) Uani 1 1 d . . . C8 C -0.1530(4) 0.09787(15) 0.2028(4) 0.0483(12) Uani 1 1 d . . . H8A H -0.2063 0.0868 0.1361 0.058 Uiso 1 1 calc R . . H8B H -0.2192 0.1111 0.2433 0.058 Uiso 1 1 calc R . . C9 C -0.0899(4) 0.06550(15) 0.2776(4) 0.0434(11) Uani 1 1 d . . . C10 C 0.2917(4) 0.23316(14) 0.4592(4) 0.0392(11) Uani 1 1 d . . . C11 C 0.3560(4) 0.22279(16) 0.5643(4) 0.0481(12) Uani 1 1 d . . . H11 H 0.3272 0.2008 0.5975 0.058 Uiso 1 1 calc R . . C12 C 0.4646(5) 0.24467(18) 0.6228(4) 0.0585(15) Uani 1 1 d . . . H12 H 0.5058 0.2376 0.6946 0.070 Uiso 1 1 calc R . . C13 C 0.5091(5) 0.27686(19) 0.5717(5) 0.0641(17) Uani 1 1 d . . . H13 H 0.5812 0.2915 0.6091 0.077 Uiso 1 1 calc R . . C14 C 0.4469(5) 0.28720(17) 0.4656(5) 0.0619(15) Uani 1 1 d . . . H14 H 0.4776 0.3086 0.4308 0.074 Uiso 1 1 calc R . . C15 C 0.3386(4) 0.26559(15) 0.4111(4) 0.0488(12) Uani 1 1 d . . . H15 H 0.2961 0.2730 0.3399 0.059 Uiso 1 1 calc R . . C16 C 0.0458(4) 0.23479(14) 0.3661(4) 0.0384(11) Uani 1 1 d . . . C17 C -0.0387(4) 0.24184(15) 0.4513(4) 0.0465(12) Uani 1 1 d . . . H17 H -0.0158 0.2306 0.5217 0.056 Uiso 1 1 calc R . . C18 C -0.1548(5) 0.26519(17) 0.4324(5) 0.0595(15) Uani 1 1 d . . . H18 H -0.2086 0.2696 0.4901 0.071 Uiso 1 1 calc R . . C19 C -0.1909(5) 0.28179(18) 0.3293(5) 0.0616(15) Uani 1 1 d . . . H19 H -0.2707 0.2969 0.3157 0.074 Uiso 1 1 calc R . . C20 C -0.1073(5) 0.27592(18) 0.2457(4) 0.0630(16) Uani 1 1 d . . . H20 H -0.1295 0.2878 0.1761 0.076 Uiso 1 1 calc R . . C21 C 0.0094(5) 0.25257(16) 0.2645(4) 0.0547(14) Uani 1 1 d . . . H21 H 0.0641 0.2489 0.2069 0.066 Uiso 1 1 calc R . . C22 C 0.0236(4) 0.04232(15) 0.2262(4) 0.0480(12) Uani 1 1 d . . . C23 C 0.0411(5) 0.04342(18) 0.1152(5) 0.0637(16) Uani 1 1 d . . . H23 H -0.0172 0.0587 0.0658 0.076 Uiso 1 1 calc R . . C24 C 0.1459(6) 0.0217(2) 0.0739(6) 0.087(2) Uani 1 1 d . . . H24 H 0.1592 0.0234 -0.0016 0.104 Uiso 1 1 calc R . . C25 C 0.2296(5) -0.0022(2) 0.1474(7) 0.098(3) Uani 1 1 d . . . H25 H 0.2982 -0.0170 0.1209 0.118 Uiso 1 1 calc R . . C26 C 0.2105(5) -0.0040(2) 0.2582(6) 0.085(2) Uani 1 1 d . . . H26 H 0.2645 -0.0204 0.3072 0.102 Uiso 1 1 calc R . . C27 C 0.1105(5) 0.01883(18) 0.2975(5) 0.0633(16) Uani 1 1 d . . . H27 H 0.1014 0.0184 0.3739 0.076 Uiso 1 1 calc R . . C28 C -0.2056(4) 0.03687(14) 0.2933(4) 0.0454(12) Uani 1 1 d . . . C29 C -0.2822(4) 0.01978(17) 0.1980(5) 0.0579(14) Uani 1 1 d . . . H29 H -0.2683 0.0271 0.1255 0.069 Uiso 1 1 calc R . . C30 C -0.3797(5) -0.00832(18) 0.2143(6) 0.0706(17) Uani 1 1 d . . . H30 H -0.4294 -0.0199 0.1512 0.085 Uiso 1 1 calc R . . C31 C -0.4050(5) -0.01948(18) 0.3178(6) 0.0693(17) Uani 1 1 d . . . H31 H -0.4700 -0.0384 0.3262 0.083 Uiso 1 1 calc R . . C32 C -0.3319(5) -0.00203(19) 0.4102(5) 0.0685(17) Uani 1 1 d . . . H32 H -0.3483 -0.0092 0.4821 0.082 Uiso 1 1 calc R . . C33 C -0.2349(4) 0.02584(17) 0.3987(5) 0.0574(14) Uani 1 1 d . . . H33 H -0.1883 0.0375 0.4628 0.069 Uiso 1 1 calc R . . C34 C 0.3059(4) 0.09290(15) 0.3190(4) 0.0475(12) Uani 1 1 d . . . H34 H 0.2584 0.0899 0.2465 0.057 Uiso 1 1 calc R . . C35 C 0.4434(4) 0.08144(16) 0.3534(5) 0.0568(14) Uani 1 1 d . . . H35 H 0.5043 0.0698 0.3099 0.068 Uiso 1 1 calc R . . C36 C 0.4695(4) 0.09098(17) 0.4644(5) 0.0579(15) Uani 1 1 d . . . H36 H 0.5526 0.0866 0.5122 0.069 Uiso 1 1 calc R . . C37 C 0.1152(5) 0.13301(19) 0.6771(5) 0.0597(15) Uani 1 1 d . . . H37 H 0.1316 0.1589 0.6859 0.072 Uiso 1 1 calc R . . C38 C 0.1315(6) 0.1056(3) 0.7639(5) 0.075(2) Uani 1 1 d . . . H38 H 0.1610 0.1100 0.8401 0.090 Uiso 1 1 calc R . . C39 C 0.0969(6) 0.0724(2) 0.7164(6) 0.080(2) Uani 1 1 d . . . H39 H 0.0971 0.0492 0.7530 0.096 Uiso 1 1 calc R . . C40 C -0.2278(4) 0.17630(15) 0.3473(4) 0.0501(13) Uani 1 1 d . . . H40 H -0.2059 0.1840 0.2773 0.060 Uiso 1 1 calc R . . C41 C -0.3485(4) 0.18635(16) 0.3908(5) 0.0581(14) Uani 1 1 d . . . H41 H -0.4215 0.2015 0.3572 0.070 Uiso 1 1 calc R . . C42 C -0.3371(5) 0.16920(17) 0.4938(5) 0.0609(15) Uani 1 1 d . . . H42 H -0.4018 0.1705 0.5449 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.48815(16) 0.36216(6) 0.23992(13) 0.0850(5) Uani 1 1 d . . . O3 O 0.7673(6) 0.3943(2) 0.2021(5) 0.164(3) Uani 1 1 d . . . O4 O 0.5705(6) 0.4119(2) 0.4614(5) 0.157(3) Uani 1 1 d . . . C43 C 0.4658(9) 0.4044(3) 0.5294(7) 0.136(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0346(2) 0.0390(2) 0.0363(3) 0.0009(2) 0.00652(14) 0.00246(15) O1 0.0423(14) 0.042(2) 0.0335(18) 0.0038(15) 0.0063(12) 0.0005(13) O2 0.0440(16) 0.041(2) 0.046(2) -0.0017(16) -0.0003(13) 0.0029(13) N1 0.0433(19) 0.038(2) 0.032(2) -0.0019(18) 0.0085(15) 0.0049(16) N2 0.0388(18) 0.045(3) 0.045(2) 0.001(2) 0.0085(17) 0.0027(17) N3 0.0381(19) 0.061(3) 0.044(2) 0.004(2) -0.0013(16) 0.0063(18) N4 0.0409(18) 0.041(2) 0.037(2) 0.002(2) 0.0078(16) 0.0020(16) N5 0.064(2) 0.051(3) 0.070(3) 0.013(3) 0.010(2) 0.005(2) N6 0.0347(17) 0.044(3) 0.042(2) -0.002(2) 0.0088(16) -0.0010(16) N7 0.043(2) 0.053(3) 0.054(3) 0.003(2) 0.0113(18) 0.0008(18) C1 0.038(2) 0.043(3) 0.037(3) 0.001(2) 0.0091(18) 0.0016(19) C2 0.046(2) 0.041(3) 0.039(3) 0.000(2) 0.0160(19) 0.0006(19) C3 0.047(2) 0.041(3) 0.038(3) -0.003(2) 0.015(2) 0.003(2) C4 0.072(3) 0.044(3) 0.047(3) 0.004(3) 0.021(2) -0.001(2) C5 0.098(4) 0.057(4) 0.033(3) 0.002(3) 0.010(3) 0.008(3) C6 0.078(3) 0.048(3) 0.041(3) -0.003(3) -0.006(3) 0.000(3) C7 0.053(3) 0.038(3) 0.041(3) 0.000(2) -0.002(2) 0.005(2) C8 0.046(2) 0.055(4) 0.041(3) -0.003(3) -0.005(2) 0.003(2) C9 0.041(2) 0.043(3) 0.045(3) -0.007(2) 0.0025(19) 0.000(2) C10 0.040(2) 0.039(3) 0.041(3) 0.002(2) 0.0143(19) 0.0037(18) C11 0.044(2) 0.050(3) 0.052(3) 0.003(3) 0.010(2) 0.001(2) C12 0.046(3) 0.075(4) 0.053(3) -0.007(3) 0.002(2) -0.003(3) C13 0.042(3) 0.083(5) 0.069(4) -0.022(3) 0.014(2) -0.011(3) C14 0.063(3) 0.052(4) 0.075(4) -0.007(3) 0.025(3) -0.013(3) C15 0.051(3) 0.049(3) 0.048(3) 0.002(3) 0.013(2) 0.002(2) C16 0.038(2) 0.044(3) 0.034(3) -0.001(2) 0.0092(18) 0.0017(19) C17 0.048(2) 0.049(3) 0.043(3) -0.003(2) 0.008(2) 0.002(2) C18 0.048(3) 0.064(4) 0.070(4) -0.014(3) 0.019(2) 0.006(2) C19 0.054(3) 0.061(4) 0.068(4) -0.005(3) 0.000(3) 0.022(3) C20 0.073(3) 0.069(4) 0.045(3) 0.004(3) 0.001(3) 0.022(3) C21 0.064(3) 0.061(4) 0.041(3) 0.002(3) 0.015(2) 0.017(3) C22 0.042(2) 0.049(3) 0.053(3) -0.011(3) 0.008(2) -0.003(2) C23 0.056(3) 0.066(4) 0.070(4) -0.020(3) 0.009(3) 0.000(3) C24 0.066(4) 0.104(6) 0.093(5) -0.049(5) 0.024(3) -0.006(4) C25 0.048(3) 0.119(7) 0.127(7) -0.045(6) 0.005(4) 0.022(4) C26 0.057(3) 0.098(6) 0.097(5) -0.025(5) -0.004(3) 0.023(3) C27 0.051(3) 0.066(4) 0.072(4) -0.009(3) 0.003(2) 0.015(3) C28 0.039(2) 0.040(3) 0.057(3) -0.005(3) 0.007(2) 0.0057(19) C29 0.044(2) 0.058(4) 0.070(4) -0.009(3) 0.004(2) -0.004(2) C30 0.049(3) 0.060(4) 0.100(5) -0.014(4) -0.003(3) -0.006(3) C31 0.047(3) 0.058(4) 0.102(5) 0.011(4) 0.006(3) -0.007(2) C32 0.049(3) 0.075(5) 0.082(4) 0.015(4) 0.011(3) -0.004(3) C33 0.043(3) 0.065(4) 0.062(4) -0.001(3) 0.002(2) 0.002(2) C34 0.045(2) 0.052(3) 0.047(3) -0.007(3) 0.012(2) 0.005(2) C35 0.045(3) 0.058(4) 0.069(4) -0.008(3) 0.017(2) 0.004(2) C36 0.036(2) 0.067(4) 0.071(4) 0.005(3) 0.007(2) 0.007(2) C37 0.056(3) 0.068(4) 0.055(4) -0.018(4) 0.006(2) 0.001(3) C38 0.078(4) 0.115(7) 0.031(3) -0.003(4) 0.002(3) 0.015(4) C39 0.079(4) 0.101(6) 0.059(5) 0.031(4) 0.009(3) 0.019(4) C40 0.043(2) 0.049(3) 0.057(3) 0.010(3) 0.004(2) 0.006(2) C41 0.042(2) 0.051(3) 0.082(4) 0.006(3) 0.008(2) 0.008(2) C42 0.041(3) 0.059(4) 0.087(4) -0.007(3) 0.022(2) 0.002(2) Cl1 0.0827(10) 0.1099(16) 0.0635(11) 0.0004(9) 0.0146(7) 0.0044(9) O3 0.122(4) 0.211(9) 0.172(6) -0.093(6) 0.063(4) -0.063(5) O4 0.147(5) 0.193(9) 0.125(5) -0.041(5) 0.001(4) -0.013(5) C43 0.128(7) 0.180(13) 0.109(7) -0.028(7) 0.041(5) -0.014(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. ; 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 O1 1.974(3) . ? Ru1 O2 2.003(3) . ? Ru1 N1 2.073(4) . ? Ru1 N4 2.086(4) . ? Ru1 N6 2.089(3) . ? Ru1 N2 2.101(3) . ? O1 C1 1.423(5) . ? O2 C9 1.406(5) . ? N1 C7 1.360(6) . ? N1 C3 1.374(6) . ? N2 C34 1.322(5) . ? N2 N3 1.346(5) . ? N3 C36 1.345(6) . ? N4 C37 1.319(6) . ? N4 N5 1.343(6) . ? N5 C39 1.316(7) . ? N6 C40 1.325(6) . ? N6 N7 1.337(5) . ? N7 C42 1.331(6) . ? C1 C16 1.527(6) . ? C1 C10 1.534(6) . ? C1 C2 1.537(6) . ? C2 C3 1.492(6) . ? C3 C4 1.380(6) . ? C4 C5 1.382(7) . ? C5 C6 1.375(8) . ? C6 C7 1.371(7) . ? C7 C8 1.506(7) . ? C8 C9 1.525(7) . ? C9 C28 1.533(6) . ? C9 C22 1.555(6) . ? C10 C11 1.372(6) . ? C10 C15 1.383(7) . ? C11 C12 1.406(7) . ? C12 C13 1.384(8) . ? C13 C14 1.376(7) . ? C14 C15 1.380(7) . ? C16 C21 1.370(6) . ? C16 C17 1.408(6) . ? C17 C18 1.381(7) . ? C18 C19 1.366(7) . ? C19 C20 1.381(7) . ? C20 C21 1.386(7) . ? C22 C23 1.361(7) . ? C22 C27 1.385(7) . ? C23 C24 1.407(8) . ? C24 C25 1.394(10) . ? C25 C26 1.363(9) . ? C26 C27 1.384(7) . ? C28 C33 1.383(7) . ? C28 C29 1.406(6) . ? C29 C30 1.396(7) . ? C30 C31 1.352(7) . ? C31 C32 1.371(8) . ? C32 C33 1.375(7) . ? C34 C35 1.392(6) . ? C35 C36 1.359(7) . ? C37 C38 1.412(9) . ? C38 C39 1.323(10) . ? C40 C41 1.382(6) . ? C41 C42 1.363(7) . ? O4 C43 1.403(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O2 169.94(12) . . ? O1 Ru1 N1 95.54(14) . . ? O2 Ru1 N1 94.43(14) . . ? O1 Ru1 N4 85.72(14) . . ? O2 Ru1 N4 84.25(15) . . ? N1 Ru1 N4 177.05(14) . . ? O1 Ru1 N6 90.79(13) . . ? O2 Ru1 N6 90.40(13) . . ? N1 Ru1 N6 90.73(14) . . ? N4 Ru1 N6 91.92(14) . . ? O1 Ru1 N2 88.97(14) . . ? O2 Ru1 N2 89.92(14) . . ? N1 Ru1 N2 88.87(14) . . ? N4 Ru1 N2 88.48(14) . . ? N6 Ru1 N2 179.51(16) . . ? C1 O1 Ru1 123.6(3) . . ? C9 O2 Ru1 125.0(3) . . ? C7 N1 C3 119.6(4) . . ? C7 N1 Ru1 120.7(3) . . ? C3 N1 Ru1 119.6(3) . . ? C34 N2 N3 106.2(4) . . ? C34 N2 Ru1 130.7(3) . . ? N3 N2 Ru1 123.2(3) . . ? C36 N3 N2 110.4(4) . . ? C37 N4 N5 106.1(4) . . ? C37 N4 Ru1 133.9(4) . . ? N5 N4 Ru1 119.2(4) . . ? C39 N5 N4 111.9(5) . . ? C40 N6 N7 105.4(4) . . ? C40 N6 Ru1 131.3(3) . . ? N7 N6 Ru1 123.2(3) . . ? C42 N7 N6 111.4(4) . . ? O1 C1 C16 109.6(3) . . ? O1 C1 C10 108.4(3) . . ? C16 C1 C10 107.9(4) . . ? O1 C1 C2 109.5(4) . . ? C16 C1 C2 113.6(4) . . ? C10 C1 C2 107.7(3) . . ? C3 C2 C1 117.8(3) . . ? N1 C3 C4 120.2(4) . . ? N1 C3 C2 120.8(4) . . ? C4 C3 C2 118.9(4) . . ? C3 C4 C5 120.1(5) . . ? C6 C5 C4 118.7(5) . . ? C7 C6 C5 120.8(5) . . ? N1 C7 C6 120.5(5) . . ? N1 C7 C8 119.2(4) . . ? C6 C7 C8 120.3(4) . . ? C7 C8 C9 118.4(4) . . ? O2 C9 C8 109.9(4) . . ? O2 C9 C28 109.1(4) . . ? C8 C9 C28 109.1(3) . . ? O2 C9 C22 109.4(3) . . ? C8 C9 C22 114.0(4) . . ? C28 C9 C22 105.2(4) . . ? C11 C10 C15 118.0(4) . . ? C11 C10 C1 121.4(4) . . ? C15 C10 C1 120.5(4) . . ? C10 C11 C12 121.4(5) . . ? C13 C12 C11 118.9(5) . . ? C14 C13 C12 120.1(5) . . ? C13 C14 C15 119.6(5) . . ? C14 C15 C10 121.9(5) . . ? C21 C16 C17 117.2(4) . . ? C21 C16 C1 125.0(4) . . ? C17 C16 C1 117.7(4) . . ? C18 C17 C16 121.3(5) . . ? C19 C18 C17 120.3(5) . . ? C18 C19 C20 119.1(5) . . ? C19 C20 C21 120.7(5) . . ? C16 C21 C20 121.3(5) . . ? C23 C22 C27 118.2(5) . . ? C23 C22 C9 123.8(5) . . ? C27 C22 C9 118.0(4) . . ? C22 C23 C24 121.1(6) . . ? C25 C24 C23 119.3(6) . . ? C26 C25 C24 119.8(6) . . ? C25 C26 C27 119.6(6) . . ? C26 C27 C22 121.9(6) . . ? C33 C28 C29 117.9(5) . . ? C33 C28 C9 122.5(4) . . ? C29 C28 C9 119.6(4) . . ? C30 C29 C28 118.7(5) . . ? C31 C30 C29 122.8(6) . . ? C30 C31 C32 118.1(6) . . ? C31 C32 C33 121.4(6) . . ? C32 C33 C28 121.1(5) . . ? N2 C34 C35 110.6(4) . . ? C36 C35 C34 105.0(4) . . ? N3 C36 C35 107.9(4) . . ? N4 C37 C38 107.8(6) . . ? C39 C38 C37 107.1(5) . . ? N5 C39 C38 107.2(7) . . ? N6 C40 C41 110.8(4) . . ? C42 C41 C40 104.9(4) . . ? N7 C42 C41 107.4(4) . . ? _diffrn_measured_fraction_theta_max 0.828 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.828 _refine_diff_density_max 1.296 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.146 data_kkcip390_Chan_PM's_Ru_Dec_ _database_code_CSD 213055 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Apr 23 16:47:25 2003' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution SIR92 _computing_structure_refinement teXsan _computing_publication_material teXsan #------------------------------------------------------------------------------ _cell_length_a 12.963(2) _cell_length_b 13.707(2) _cell_length_c 13.287(2) _cell_angle_alpha 90 _cell_angle_beta 117.85(2) _cell_angle_gamma 90 _cell_volume 2087.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_meas ? _chemical_formula_weight 561.34 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H15 Cl2 N3 O5 Ru ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1120.00 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device unknown _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3958 _reflns_number_total 3958 _reflns_number_observed 2824 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.60 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 4 -1.259 0.836 'International Tables' Cl 0 8 0.148 0.159 'International Tables' O 0 20 0.011 0.006 'International Tables' N 0 12 0.006 0.003 'International Tables' C 0 84 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.26800(3) 0.47336(3) 0.04603(3) 0.0316(1) Uij ? ? Cl(1) 0.1655(1) 0.96305(9) 0.0056(1) 0.0612(4) Uij ? ? Cl(2) -0.0804(1) 0.87198(9) -0.1596(1) 0.0505(4) Uij ? ? O(1) 0.4193(2) 0.4183(2) 0.0751(3) 0.0386(9) Uij ? ? O(2) 0.2214(2) 0.3456(2) -0.0310(3) 0.0406(9) Uij ? ? O(3) 0.4659(3) 0.7231(2) 0.0798(3) 0.048(1) Uij ? ? O(4) -0.0365(3) 0.5339(3) -0.2470(3) 0.063(1) Uij ? ? O(5) 0.3696(3) 0.2227(2) -0.0516(3) 0.0447(10) Uij ? ? N(1) 0.2512(3) 0.4660(3) 0.1576(3) 0.041(1) Uij ? ? N(2) 0.3303(3) 0.6108(3) 0.0560(3) 0.0310(10) Uij ? ? N(3) 0.1253(3) 0.5367(2) -0.0736(3) 0.0339(10) Uij ? ? C(1) 0.5227(4) 0.4631(3) 0.1350(4) 0.036(1) Uij ? ? C(2) 0.6212(4) 0.4030(4) 0.1809(4) 0.044(1) Uij ? ? C(3) 0.7299(4) 0.4408(4) 0.2401(4) 0.051(2) Uij ? ? C(4) 0.7462(4) 0.5412(4) 0.2586(5) 0.054(2) Uij ? ? C(5) 0.6507(4) 0.6017(4) 0.2132(4) 0.046(1) Uij ? ? C(6) 0.5365(4) 0.5638(3) 0.1478(4) 0.034(1) Uij ? ? C(7) 0.4415(4) 0.6338(3) 0.0930(4) 0.034(1) Uij ? ? C(8) 0.2375(4) 0.6813(3) 0.0039(4) 0.032(1) Uij ? ? C(9) 0.2482(4) 0.7801(3) 0.0268(4) 0.037(1) Uij ? ? C(10) 0.1504(4) 0.8392(3) -0.0247(4) 0.039(1) Uij ? ? C(11) 0.0430(4) 0.7995(3) -0.0963(4) 0.036(1) Uij ? ? C(12) 0.0305(4) 0.7004(3) -0.1180(4) 0.037(1) Uij ? ? C(13) 0.1280(4) 0.6406(3) -0.0670(4) 0.034(1) Uij ? ? C(14) 0.0321(4) 0.4901(3) -0.1633(4) 0.041(1) Uij ? ? C(15) 0.0172(4) 0.3838(3) -0.1517(4) 0.037(1) Uij ? ? C(16) -0.0971(4) 0.3472(4) -0.2123(4) 0.047(1) Uij ? ? C(17) -0.1198(4) 0.2494(4) -0.2142(5) 0.052(2) Uij ? ? C(18) -0.0289(5) 0.1849(4) -0.1553(4) 0.048(1) Uij ? ? C(19) 0.0837(4) 0.2196(3) -0.0942(4) 0.043(1) Uij ? ? C(20) 0.1076(4) 0.3182(3) -0.0913(4) 0.039(1) Uij ? ? C(21) 0.4176(5) 0.1472(5) 0.0334(5) 0.074(2) Uij ? ? H(1) 0.6124 0.3343 0.1705 0.0533 Uij ? ? H(2) 0.7965 0.3993 0.2699 0.0601 Uij ? ? H(3) 0.8233 0.5668 0.3015 0.0626 Uij ? ? H(4) 0.6618 0.6699 0.2270 0.0552 Uij ? ? H(5) 0.3220 0.8075 0.0778 0.0439 Uij ? ? H(6) -0.0437 0.6736 -0.1678 0.0439 Uij ? ? H(7) -0.1595 0.3914 -0.2529 0.0566 Uij ? ? H(8) -0.1980 0.2259 -0.2560 0.0620 Uij ? ? H(9) -0.0439 0.1166 -0.1566 0.0579 Uij ? ? H(10) 0.1461 0.1751 -0.0546 0.0511 Uij ? ? H(11) 0.5493 0.7351 0.0676 0.0602 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0283(2) 0.0268(2) 0.0365(2) 0.0013(2) 0.0124(2) 0.0009(2) Cl(1) 0.0602(8) 0.0285(7) 0.090(1) 0.0043(6) 0.0305(8) -0.0043(6) Cl(2) 0.0457(7) 0.0456(7) 0.0541(8) 0.0192(6) 0.0182(6) 0.0099(6) O(1) 0.029(2) 0.033(2) 0.048(2) 0.001(1) 0.013(1) -0.005(1) O(2) 0.030(2) 0.028(2) 0.058(2) -0.001(1) 0.016(2) -0.006(1) O(3) 0.034(2) 0.032(2) 0.076(2) -0.003(1) 0.025(2) 0.002(2) O(4) 0.051(2) 0.047(2) 0.047(2) 0.003(2) -0.013(2) 0.001(2) O(5) 0.038(2) 0.037(2) 0.062(2) -0.004(1) 0.026(2) -0.003(2) N(1) 0.047(2) 0.040(2) 0.038(2) 0.003(2) 0.021(2) 0.003(2) N(2) 0.028(2) 0.028(2) 0.033(2) 0.001(2) 0.011(2) 0.002(2) N(3) 0.030(2) 0.028(2) 0.037(2) 0.002(2) 0.009(2) 0.003(2) C(1) 0.032(2) 0.044(3) 0.030(2) 0.005(2) 0.013(2) 0.001(2) C(2) 0.037(3) 0.048(3) 0.043(3) 0.008(2) 0.015(2) 0.008(2) C(3) 0.034(3) 0.062(4) 0.044(3) 0.011(2) 0.010(2) 0.012(3) C(4) 0.026(2) 0.065(4) 0.056(3) -0.003(2) 0.006(2) 0.009(3) C(5) 0.033(3) 0.052(3) 0.044(3) -0.003(2) 0.012(2) 0.001(2) C(6) 0.030(2) 0.039(3) 0.032(2) 0.003(2) 0.014(2) 0.002(2) C(7) 0.033(2) 0.033(3) 0.034(3) -0.002(2) 0.015(2) -0.005(2) C(8) 0.031(2) 0.032(3) 0.036(2) 0.002(2) 0.018(2) 0.001(2) C(9) 0.036(3) 0.030(2) 0.044(3) -0.001(2) 0.018(2) 0.000(2) C(10) 0.043(3) 0.030(3) 0.047(3) 0.003(2) 0.025(2) 0.000(2) C(11) 0.040(3) 0.036(3) 0.034(2) 0.013(2) 0.017(2) 0.007(2) C(12) 0.028(2) 0.041(3) 0.038(2) 0.004(2) 0.013(2) 0.002(2) C(13) 0.037(2) 0.030(2) 0.037(2) 0.002(2) 0.020(2) 0.004(2) C(14) 0.031(2) 0.038(3) 0.046(3) -0.003(2) 0.013(2) -0.008(2) C(15) 0.031(2) 0.036(3) 0.042(3) -0.002(2) 0.016(2) -0.008(2) C(16) 0.031(3) 0.048(3) 0.055(3) -0.002(2) 0.014(2) -0.011(2) C(17) 0.047(3) 0.047(3) 0.069(4) -0.019(3) 0.033(3) -0.018(3) C(18) 0.054(3) 0.036(3) 0.057(3) -0.013(3) 0.027(3) -0.010(2) C(19) 0.041(3) 0.028(3) 0.059(3) -0.004(2) 0.025(2) -0.004(2) C(20) 0.037(3) 0.034(3) 0.048(3) -0.005(2) 0.022(2) -0.007(2) C(21) 0.073(4) 0.072(4) 0.078(4) 0.011(3) 0.037(4) 0.032(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2824 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0488 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.716 _refine_ls_shift/esd_max 0.0780 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.53 _refine_diff_density_max 0.55 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 1.964(3) ? ? yes Ru(1) O(2) 1.975(3) ? ? yes Ru(1) N(1) 1.599(4) ? ? yes Ru(1) N(2) 2.029(4) ? ? yes Ru(1) N(3) 1.988(3) ? ? yes Cl(1) C(10) 1.735(5) ? ? yes Cl(2) C(11) 1.731(4) ? ? yes O(1) C(1) 1.346(5) ? ? yes O(2) C(20) 1.362(5) ? ? yes O(3) C(7) 1.296(5) ? ? yes O(4) C(14) 1.210(6) ? ? yes O(5) C(21) 1.441(6) ? ? yes N(2) C(7) 1.326(5) ? ? yes N(2) C(8) 1.443(5) ? ? yes N(3) C(13) 1.426(5) ? ? yes N(3) C(14) 1.395(6) ? ? yes C(1) C(2) 1.398(6) ? ? yes C(1) C(6) 1.391(6) ? ? yes C(2) C(3) 1.356(7) ? ? yes C(3) C(4) 1.396(8) ? ? yes C(4) C(5) 1.373(7) ? ? yes C(5) C(6) 1.420(6) ? ? yes C(6) C(7) 1.459(6) ? ? yes C(8) C(9) 1.381(6) ? ? yes C(8) C(13) 1.401(6) ? ? yes C(9) C(10) 1.386(6) ? ? yes C(10) C(11) 1.379(6) ? ? yes C(11) C(12) 1.383(6) ? ? yes C(12) C(13) 1.389(6) ? ? yes C(14) C(15) 1.486(6) ? ? yes C(15) C(16) 1.408(6) ? ? yes C(15) C(20) 1.396(6) ? ? yes C(16) C(17) 1.369(7) ? ? yes C(17) C(18) 1.386(7) ? ? yes C(18) C(19) 1.382(6) ? ? yes C(19) C(20) 1.383(6) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ru(1) O(2) 78.3(1) ? ? ? yes O(1) Ru(1) N(1) 110.4(2) ? ? ? yes O(1) Ru(1) N(2) 90.8(1) ? ? ? yes O(1) Ru(1) N(3) 142.7(1) ? ? ? yes O(2) Ru(1) N(1) 106.4(2) ? ? ? yes O(2) Ru(1) N(2) 150.8(1) ? ? ? yes O(2) Ru(1) N(3) 91.6(1) ? ? ? yes N(1) Ru(1) N(2) 102.7(2) ? ? ? yes N(1) Ru(1) N(3) 106.9(2) ? ? ? yes N(2) Ru(1) N(3) 80.8(1) ? ? ? yes Ru(1) O(1) C(1) 124.6(3) ? ? ? yes Ru(1) O(2) C(20) 122.3(3) ? ? ? yes Ru(1) N(2) C(7) 125.2(3) ? ? ? yes Ru(1) N(2) C(8) 111.9(3) ? ? ? yes C(7) N(2) C(8) 122.4(4) ? ? ? yes Ru(1) N(3) C(13) 113.6(3) ? ? ? yes Ru(1) N(3) C(14) 126.4(3) ? ? ? yes C(13) N(3) C(14) 119.8(4) ? ? ? yes O(1) C(1) C(2) 116.3(4) ? ? ? yes O(1) C(1) C(6) 124.1(4) ? ? ? yes C(2) C(1) C(6) 119.5(4) ? ? ? yes C(1) C(2) C(3) 121.2(5) ? ? ? yes C(2) C(3) C(4) 120.6(4) ? ? ? yes C(3) C(4) C(5) 119.1(4) ? ? ? yes C(4) C(5) C(6) 121.1(5) ? ? ? yes C(1) C(6) C(5) 118.4(4) ? ? ? yes C(1) C(6) C(7) 124.2(4) ? ? ? yes C(5) C(6) C(7) 117.4(4) ? ? ? yes O(3) C(7) N(2) 117.8(4) ? ? ? yes O(3) C(7) C(6) 119.1(4) ? ? ? yes N(2) C(7) C(6) 123.1(4) ? ? ? yes N(2) C(8) C(9) 125.2(4) ? ? ? yes N(2) C(8) C(13) 114.3(4) ? ? ? yes C(9) C(8) C(13) 120.3(4) ? ? ? yes C(8) C(9) C(10) 119.3(4) ? ? ? yes Cl(1) C(10) C(9) 118.6(3) ? ? ? yes Cl(1) C(10) C(11) 121.0(3) ? ? ? yes C(9) C(10) C(11) 120.4(4) ? ? ? yes Cl(2) C(11) C(10) 121.0(4) ? ? ? yes Cl(2) C(11) C(12) 118.1(3) ? ? ? yes C(10) C(11) C(12) 120.9(4) ? ? ? yes C(11) C(12) C(13) 119.1(4) ? ? ? yes N(3) C(13) C(8) 115.2(4) ? ? ? yes N(3) C(13) C(12) 124.6(4) ? ? ? yes C(8) C(13) C(12) 119.9(4) ? ? ? yes O(4) C(14) N(3) 121.9(4) ? ? ? yes O(4) C(14) C(15) 120.5(4) ? ? ? yes N(3) C(14) C(15) 117.6(4) ? ? ? yes C(14) C(15) C(16) 116.3(4) ? ? ? yes C(14) C(15) C(20) 125.2(4) ? ? ? yes C(16) C(15) C(20) 118.4(4) ? ? ? yes C(15) C(16) C(17) 121.3(5) ? ? ? yes C(16) C(17) C(18) 119.7(4) ? ? ? yes C(17) C(18) C(19) 119.9(5) ? ? ? yes C(18) C(19) C(20) 120.9(4) ? ? ? yes O(2) C(20) C(15) 123.2(4) ? ? ? yes O(2) C(20) C(19) 116.9(4) ? ? ? yes C(15) C(20) C(19) 119.8(4) ? ? ? yes data_afc678_Chan_PM's_Ru_ONO_Nov_18_1997 _database_code_CSD 213056 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Dec 22 16:42:26 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement teXsan _computing_publication_material teXsan #------------------------------------------------------------------------------ _cell_length_a 9.243(3) _cell_length_b 11.208(4) _cell_length_c 40.92(1) _cell_angle_alpha 90 _cell_angle_beta 91.00(3) _cell_angle_gamma 90 _cell_volume 4238(2) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 15.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description XDIM _exptl_crystal_colour HABIT _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 882.40 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H49 Cl N O2 P2 Ru ' _chemical_formula_moiety 'C49 H49 Cl N O2 P2 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1828.00 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.652 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device AFC7R _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.97 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 6552 _reflns_number_total 6069 _reflns_number_observed 2638 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 12.70 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.08274 _diffrn_orient_matrix_UB_12 0.02614 _diffrn_orient_matrix_UB_13 0.01369 _diffrn_orient_matrix_UB_21 0.05359 _diffrn_orient_matrix_UB_22 -0.02695 _diffrn_orient_matrix_UB_23 0.02012 _diffrn_orient_matrix_UB_31 0.04461 _diffrn_orient_matrix_UB_32 0.08094 _diffrn_orient_matrix_UB_33 0.00226 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 196 0.003 0.002 'International Tables' H 0 196 0.000 0.000 'International Tables' N 0 4 0.006 0.003 'International Tables' O 0 8 0.011 0.006 'International Tables' P 0 8 0.102 0.094 'International Tables' Cl 0 4 0.148 0.159 'International Tables' Ru 0 4 -1.259 0.836 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.0652(1) 0.0394(1) 0.38601(3) 0.0406 Uij ? ? Cl(1) -0.1938(4) 0.0444(4) 0.39525(9) 0.0588 Uij ? ? P(1) 0.0704(4) 0.2167(4) 0.41557(9) 0.0471 Uij ? ? P(2) 0.3255(4) 0.0289(5) 0.38247(9) 0.0509 Uij ? ? O(1) 0.091(1) -0.0509(10) 0.4279(2) 0.0461 Uij ? ? O(2) 0.054(1) 0.145(1) 0.3463(2) 0.0506 Uij ? ? N(1) 0.026(1) -0.120(1) 0.3588(3) 0.0460 Uij ? ? C(1) 0.073(2) 0.196(2) 0.4595(3) 0.0748 Uij ? ? C(2) -0.085(2) 0.312(2) 0.4091(4) 0.0727 Uij ? ? C(3) 0.210(2) 0.326(2) 0.4085(4) 0.0556 Uij ? ? C(4) 0.312(2) 0.365(2) 0.4315(4) 0.0693 Uij ? ? C(5) 0.410(2) 0.446(2) 0.4243(6) 0.0916 Uij ? ? C(6) 0.416(3) 0.497(2) 0.3935(7) 0.1117 Uij ? ? C(7) 0.318(2) 0.467(2) 0.3698(5) 0.0789 Uij ? ? C(8) 0.216(2) 0.380(2) 0.3771(4) 0.0665 Uij ? ? C(9) 0.429(2) 0.148(2) 0.3630(4) 0.0707 Uij ? ? C(10) 0.415(2) 0.025(2) 0.4222(3) 0.0607 Uij ? ? C(11) 0.404(2) -0.096(2) 0.3603(4) 0.0506 Uij ? ? C(12) 0.525(2) -0.159(2) 0.3718(4) 0.0594 Uij ? ? C(13) 0.584(2) -0.248(2) 0.3530(5) 0.0770 Uij ? ? C(14) 0.522(2) -0.280(2) 0.3228(5) 0.0889 Uij ? ? C(15) 0.402(2) -0.222(2) 0.3115(4) 0.0701 Uij ? ? C(16) 0.344(2) -0.133(2) 0.3302(4) 0.0729 Uij ? ? C(17) 0.082(1) -0.173(1) 0.4325(3) 0.0353 Uij ? ? C(18) 0.174(2) -0.212(2) 0.4633(4) 0.0487 Uij ? ? C(19) 0.227(2) -0.128(2) 0.4833(4) 0.0540 Uij ? ? C(20) 0.308(2) -0.160(2) 0.5117(4) 0.0617 Uij ? ? C(21) 0.329(2) -0.279(2) 0.5188(4) 0.0761 Uij ? ? C(22) 0.272(2) -0.364(2) 0.4994(4) 0.0748 Uij ? ? C(23) 0.191(2) -0.333(2) 0.4711(4) 0.0695 Uij ? ? C(24) -0.077(2) -0.212(2) 0.4389(3) 0.0419 Uij ? ? C(25) -0.164(2) -0.140(2) 0.4573(3) 0.0511 Uij ? ? C(26) -0.302(2) -0.176(2) 0.4660(4) 0.0626 Uij ? ? C(27) -0.349(2) -0.289(2) 0.4574(4) 0.0655 Uij ? ? C(28) -0.266(2) -0.359(2) 0.4394(4) 0.0698 Uij ? ? C(29) -0.127(2) -0.327(2) 0.4307(4) 0.0560 Uij ? ? C(30) 0.145(2) -0.239(1) 0.4026(3) 0.0446 Uij ? ? C(31) 0.058(2) -0.230(2) 0.3705(4) 0.0507 Uij ? ? C(32) 0.023(2) -0.335(2) 0.3536(4) 0.0674 Uij ? ? C(33) -0.053(2) -0.325(2) 0.3239(4) 0.0617 Uij ? ? C(34) -0.085(2) -0.221(2) 0.3118(4) 0.0523 Uij ? ? C(35) -0.053(2) -0.114(2) 0.3291(3) 0.0497 Uij ? ? C(36) -0.112(2) 0.002(2) 0.3179(3) 0.0497 Uij ? ? C(37) -0.012(2) 0.107(2) 0.3156(4) 0.0544 Uij ? ? C(38) 0.116(2) 0.091(2) 0.2906(4) 0.0570 Uij ? ? C(39) 0.106(2) -0.001(2) 0.2672(4) 0.0671 Uij ? ? C(40) 0.225(3) -0.012(2) 0.2458(5) 0.0971 Uij ? ? C(41) 0.338(3) 0.060(2) 0.2470(6) 0.1060 Uij ? ? C(42) 0.341(2) 0.150(2) 0.2696(5) 0.0987 Uij ? ? C(43) 0.228(2) 0.166(2) 0.2912(4) 0.0588 Uij ? ? C(44) -0.104(2) 0.215(2) 0.3042(4) 0.0609 Uij ? ? C(45) -0.089(2) 0.275(2) 0.2737(4) 0.0742 Uij ? ? C(46) -0.175(2) 0.371(2) 0.2652(4) 0.0793 Uij ? ? C(47) -0.279(2) 0.413(2) 0.2864(6) 0.0825 Uij ? ? C(48) -0.295(2) 0.356(2) 0.3160(5) 0.0895 Uij ? ? C(49) -0.208(2) 0.260(2) 0.3250(4) 0.0657 Uij ? ? H(1) -0.0148 0.1596 0.4659 0.0897 Uij ? ? H(2) 0.1523 0.1468 0.4657 0.0897 Uij ? ? H(3) 0.0825 0.2716 0.4699 0.0897 Uij ? ? H(4) -0.0821 0.3760 0.4245 0.0873 Uij ? ? H(5) -0.0839 0.3441 0.3876 0.0873 Uij ? ? H(6) -0.1712 0.2675 0.4119 0.0873 Uij ? ? H(7) 0.3098 0.3330 0.4530 0.0835 Uij ? ? H(8) 0.4790 0.4691 0.4406 0.1095 Uij ? ? H(9) 0.4898 0.5538 0.3890 0.1333 Uij ? ? H(10) 0.3196 0.5041 0.3489 0.0949 Uij ? ? H(11) 0.1476 0.3560 0.3607 0.0798 Uij ? ? H(12) 0.5295 0.1359 0.3670 0.0847 Uij ? ? H(13) 0.4099 0.1478 0.3401 0.0847 Uij ? ? H(14) 0.4014 0.2232 0.3718 0.0847 Uij ? ? H(15) 0.3708 -0.0346 0.4354 0.0729 Uij ? ? H(16) 0.5142 0.0060 0.4197 0.0729 Uij ? ? H(17) 0.4061 0.1003 0.4325 0.0729 Uij ? ? H(18) 0.5662 -0.1403 0.3926 0.0713 Uij ? ? H(19) 0.6678 -0.2881 0.3607 0.0926 Uij ? ? H(20) 0.5632 -0.3418 0.3102 0.1066 Uij ? ? H(21) 0.3590 -0.2418 0.2910 0.0843 Uij ? ? H(22) 0.2583 -0.0944 0.3224 0.0875 Uij ? ? H(23) 0.2111 -0.0456 0.4786 0.0644 Uij ? ? H(24) 0.3480 -0.1006 0.5257 0.0742 Uij ? ? H(25) 0.3842 -0.3010 0.5377 0.0912 Uij ? ? H(26) 0.2872 -0.4458 0.5046 0.0896 Uij ? ? H(27) 0.1482 -0.3925 0.4576 0.0833 Uij ? ? H(28) -0.1294 -0.0647 0.4642 0.0611 Uij ? ? H(29) -0.3629 -0.1229 0.4776 0.0748 Uij ? ? H(30) -0.4405 -0.3171 0.4645 0.0787 Uij ? ? H(31) -0.3028 -0.4336 0.4322 0.0837 Uij ? ? H(32) -0.0674 -0.3811 0.4194 0.0673 Uij ? ? H(33) 0.2391 -0.2081 0.3989 0.0537 Uij ? ? H(34) 0.1529 -0.3217 0.4080 0.0537 Uij ? ? H(35) 0.0495 -0.4106 0.3621 0.0807 Uij ? ? H(36) -0.0806 -0.3951 0.3125 0.0741 Uij ? ? H(37) -0.1313 -0.2162 0.2909 0.0629 Uij ? ? H(38) -0.1528 -0.0108 0.2967 0.0597 Uij ? ? H(39) -0.1859 0.0229 0.3326 0.0597 Uij ? ? H(40) 0.0246 -0.0517 0.2657 0.0804 Uij ? ? H(41) 0.2235 -0.0745 0.2301 0.1169 Uij ? ? H(42) 0.4153 0.0509 0.2323 0.1271 Uij ? ? H(43) 0.4220 0.2019 0.2707 0.1177 Uij ? ? H(44) 0.2304 0.2299 0.3064 0.0707 Uij ? ? H(45) -0.0184 0.2488 0.2589 0.0890 Uij ? ? H(46) -0.1638 0.4081 0.2446 0.0950 Uij ? ? H(47) -0.3369 0.4799 0.2806 0.0987 Uij ? ? H(48) -0.3679 0.3825 0.3305 0.1073 Uij ? ? H(49) -0.2192 0.2241 0.3458 0.0788 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0396(7) 0.0431(10) 0.0394(7) -0.0033(8) 0.0096(5) 0.0015(7) Cl(1) 0.041(2) 0.075(4) 0.060(2) -0.003(3) 0.011(2) 0.005(2) P(1) 0.043(2) 0.049(3) 0.049(2) 0.000(3) 0.011(2) 0.001(2) P(2) 0.045(3) 0.058(3) 0.050(2) -0.001(3) 0.012(2) 0.005(2) O(1) 0.059(7) 0.049(8) 0.030(5) 0.007(7) 0.004(4) 0.006(5) O(2) 0.063(7) 0.061(8) 0.028(5) 0.002(7) -0.007(4) -0.003(5) N(1) 0.036(7) 0.05(1) 0.052(8) -0.025(8) 0.025(6) 0.000(8) C(1) 0.11(1) 0.08(2) 0.037(9) 0.02(1) 0.018(9) -0.014(9) C(2) 0.07(1) 0.07(1) 0.08(1) 0.02(1) 0.002(9) -0.02(1) C(3) 0.05(1) 0.04(1) 0.07(1) -0.01(1) 0.006(9) 0.004(9) C(4) 0.06(1) 0.07(2) 0.08(1) -0.03(1) -0.004(9) 0.01(1) C(5) 0.05(1) 0.07(2) 0.15(2) -0.03(1) -0.01(1) -0.02(2) C(6) 0.11(2) 0.09(2) 0.13(2) 0.00(2) 0.02(2) 0.05(2) C(7) 0.08(1) 0.07(2) 0.09(1) -0.01(1) 0.01(1) 0.04(1) C(8) 0.07(1) 0.06(1) 0.07(1) -0.01(1) 0.013(9) 0.01(1) C(9) 0.06(1) 0.07(1) 0.09(1) 0.00(1) 0.019(9) 0.02(1) C(10) 0.06(1) 0.08(1) 0.048(9) 0.00(1) 0.002(7) -0.013(9) C(11) 0.06(1) 0.05(1) 0.05(1) -0.01(1) 0.018(8) -0.012(9) C(12) 0.032(9) 0.07(2) 0.07(1) 0.01(1) 0.011(8) -0.01(1) C(13) 0.07(1) 0.08(2) 0.09(1) 0.04(1) 0.02(1) 0.01(1) C(14) 0.11(2) 0.09(2) 0.07(1) 0.04(2) 0.03(1) -0.01(1) C(15) 0.10(2) 0.05(1) 0.06(1) 0.01(1) 0.02(1) -0.01(1) C(16) 0.07(1) 0.09(2) 0.06(1) 0.02(1) 0.016(9) 0.00(1) C(17) 0.021(8) 0.03(1) 0.050(9) 0.020(9) 0.006(6) 0.009(8) C(18) 0.05(1) 0.05(1) 0.051(10) -0.02(1) 0.015(7) 0.004(10) C(19) 0.06(1) 0.04(1) 0.06(1) 0.00(1) 0.001(8) 0.009(10) C(20) 0.05(1) 0.08(2) 0.06(1) 0.02(1) -0.003(8) 0.01(1) C(21) 0.06(1) 0.11(2) 0.05(1) 0.02(2) 0.004(9) 0.00(1) C(22) 0.09(1) 0.08(2) 0.06(1) 0.04(1) 0.00(1) 0.03(1) C(23) 0.07(1) 0.07(2) 0.07(1) -0.02(1) 0.006(10) -0.01(1) C(24) 0.05(1) 0.03(1) 0.041(9) 0.00(1) 0.002(7) 0.007(8) C(25) 0.04(1) 0.06(1) 0.047(9) 0.00(1) 0.002(7) -0.002(9) C(26) 0.05(1) 0.07(2) 0.07(1) 0.00(1) 0.029(8) 0.00(1) C(27) 0.06(1) 0.06(2) 0.07(1) -0.02(1) 0.011(9) 0.01(1) C(28) 0.08(1) 0.05(1) 0.08(1) -0.02(1) 0.015(10) -0.01(1) C(29) 0.05(1) 0.05(1) 0.07(1) 0.00(1) 0.014(8) 0.000(9) C(30) 0.047(9) 0.03(1) 0.054(10) -0.007(9) 0.007(7) 0.007(8) C(31) 0.05(1) 0.04(1) 0.06(1) 0.00(1) 0.028(8) 0.002(10) C(32) 0.09(1) 0.05(1) 0.07(1) -0.02(1) 0.02(1) 0.00(1) C(33) 0.08(1) 0.05(2) 0.05(1) -0.01(1) 0.014(9) -0.01(1) C(34) 0.08(1) 0.04(1) 0.045(10) -0.01(1) 0.001(8) -0.006(10) C(35) 0.05(1) 0.06(1) 0.036(9) 0.00(1) 0.012(7) -0.003(10) C(36) 0.06(1) 0.05(1) 0.036(8) -0.01(1) 0.007(7) 0.002(8) C(37) 0.05(1) 0.06(1) 0.05(1) 0.00(1) 0.004(8) 0.018(9) C(38) 0.06(1) 0.05(1) 0.06(1) 0.04(1) 0.009(8) 0.010(10) C(39) 0.11(2) 0.04(1) 0.047(10) 0.01(1) 0.020(10) 0.009(9) C(40) 0.15(2) 0.07(2) 0.06(1) 0.01(2) 0.05(1) 0.01(1) C(41) 0.13(2) 0.10(2) 0.09(2) 0.02(2) 0.07(2) 0.03(2) C(42) 0.09(2) 0.13(2) 0.08(1) 0.03(2) 0.05(1) 0.05(2) C(43) 0.05(1) 0.05(1) 0.08(1) 0.00(1) 0.019(9) 0.007(10) C(44) 0.07(1) 0.08(2) 0.036(9) -0.01(1) 0.001(8) 0.001(10) C(45) 0.09(1) 0.08(2) 0.06(1) 0.00(1) 0.011(9) 0.01(1) C(46) 0.09(2) 0.07(2) 0.07(1) 0.04(1) -0.02(1) 0.00(1) C(47) 0.09(2) 0.06(2) 0.10(2) 0.01(1) -0.03(1) 0.00(1) C(48) 0.10(2) 0.09(2) 0.07(1) 0.02(2) 0.01(1) -0.01(1) C(49) 0.06(1) 0.06(1) 0.08(1) 0.01(1) 0.013(10) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2638 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0774 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1020 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.099 _refine_ls_shift/esd_max 0.0320 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.45 _refine_diff_density_max 1.29 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.431(4) ? ? yes Ru(1) P(1) 2.326(5) ? ? yes Ru(1) P(2) 2.415(4) ? ? yes Ru(1) O(1) 2.001(9) ? ? yes Ru(1) O(2) 2.008(9) ? ? yes Ru(1) N(1) 2.13(1) ? ? yes P(1) C(1) 1.81(1) ? ? yes P(1) C(2) 1.81(2) ? ? yes P(1) C(3) 1.81(2) ? ? yes P(2) C(9) 1.84(2) ? ? yes P(2) C(10) 1.81(1) ? ? yes P(2) C(11) 1.83(2) ? ? yes O(1) C(17) 1.39(2) ? ? yes O(2) C(37) 1.45(2) ? ? yes N(1) C(31) 1.35(2) ? ? yes N(1) C(35) 1.41(2) ? ? yes C(3) C(4) 1.39(2) ? ? yes C(3) C(8) 1.42(2) ? ? yes C(4) C(5) 1.32(2) ? ? yes C(5) C(6) 1.39(3) ? ? yes C(6) C(7) 1.36(3) ? ? yes C(7) C(8) 1.40(2) ? ? yes C(11) C(12) 1.39(2) ? ? yes C(11) C(16) 1.41(2) ? ? yes C(12) C(13) 1.38(2) ? ? yes C(13) C(14) 1.40(3) ? ? yes C(14) C(15) 1.36(3) ? ? yes C(15) C(16) 1.37(2) ? ? yes C(17) C(18) 1.57(2) ? ? yes C(17) C(24) 1.56(2) ? ? yes C(17) C(30) 1.55(2) ? ? yes C(18) C(19) 1.34(2) ? ? yes C(18) C(23) 1.40(2) ? ? yes C(19) C(20) 1.42(2) ? ? yes C(20) C(21) 1.37(3) ? ? yes C(21) C(22) 1.34(3) ? ? yes C(22) C(23) 1.42(2) ? ? yes C(24) C(25) 1.38(2) ? ? yes C(24) C(29) 1.40(2) ? ? yes C(25) C(26) 1.38(2) ? ? yes C(26) C(27) 1.39(2) ? ? yes C(27) C(28) 1.33(2) ? ? yes C(28) C(29) 1.38(2) ? ? yes C(30) C(31) 1.53(2) ? ? yes C(31) C(32) 1.40(2) ? ? yes C(32) C(33) 1.39(2) ? ? yes C(33) C(34) 1.30(2) ? ? yes C(34) C(35) 1.42(2) ? ? yes C(35) C(36) 1.48(2) ? ? yes C(36) C(37) 1.50(2) ? ? yes C(37) C(38) 1.59(2) ? ? yes C(37) C(44) 1.55(2) ? ? yes C(38) C(39) 1.40(2) ? ? yes C(38) C(43) 1.33(2) ? ? yes C(39) C(40) 1.42(3) ? ? yes C(40) C(41) 1.33(3) ? ? yes C(41) C(42) 1.36(3) ? ? yes C(42) C(43) 1.39(2) ? ? yes C(44) C(45) 1.43(2) ? ? yes C(44) C(49) 1.39(2) ? ? yes C(45) C(46) 1.37(2) ? ? yes C(46) C(47) 1.38(3) ? ? yes C(47) C(48) 1.38(3) ? ? yes C(48) C(49) 1.39(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru(1) P(1) 84.9(2) ? ? ? yes Cl(1) Ru(1) P(2) 174.3(1) ? ? ? yes Cl(1) Ru(1) O(1) 89.0(3) ? ? ? yes Cl(1) Ru(1) O(2) 94.4(3) ? ? ? yes Cl(1) Ru(1) N(1) 86.8(3) ? ? ? yes P(1) Ru(1) P(2) 93.5(2) ? ? ? yes P(1) Ru(1) O(1) 89.2(3) ? ? ? yes P(1) Ru(1) O(2) 85.3(3) ? ? ? yes P(1) Ru(1) N(1) 171.5(3) ? ? ? yes P(2) Ru(1) O(1) 85.5(3) ? ? ? yes P(2) Ru(1) O(2) 90.9(3) ? ? ? yes P(2) Ru(1) N(1) 94.9(3) ? ? ? yes O(1) Ru(1) O(2) 173.3(4) ? ? ? yes O(1) Ru(1) N(1) 92.3(5) ? ? ? yes O(2) Ru(1) N(1) 93.7(5) ? ? ? yes Ru(1) P(1) C(1) 114.0(6) ? ? ? yes Ru(1) P(1) C(2) 114.9(6) ? ? ? yes Ru(1) P(1) C(3) 120.3(6) ? ? ? yes C(1) P(1) C(2) 102.5(8) ? ? ? yes C(1) P(1) C(3) 104.4(8) ? ? ? yes C(2) P(1) C(3) 98.2(8) ? ? ? yes Ru(1) P(2) C(9) 121.2(6) ? ? ? yes Ru(1) P(2) C(10) 112.7(5) ? ? ? yes Ru(1) P(2) C(11) 118.2(5) ? ? ? yes C(9) P(2) C(10) 100.1(8) ? ? ? yes C(9) P(2) C(11) 97.4(7) ? ? ? yes C(10) P(2) C(11) 104.3(8) ? ? ? yes Ru(1) O(1) C(17) 127.6(8) ? ? ? yes Ru(1) O(2) C(37) 122.9(10) ? ? ? yes Ru(1) N(1) C(31) 122(1) ? ? ? yes Ru(1) N(1) C(35) 119(1) ? ? ? yes C(31) N(1) C(35) 117(1) ? ? ? yes P(1) C(3) C(4) 125(1) ? ? ? yes P(1) C(3) C(8) 117(1) ? ? ? yes C(4) C(3) C(8) 116(1) ? ? ? yes C(3) C(4) C(5) 121(1) ? ? ? yes C(4) C(5) C(6) 121(2) ? ? ? yes C(5) C(6) C(7) 120(2) ? ? ? yes C(6) C(7) C(8) 117(1) ? ? ? yes C(3) C(8) C(7) 121(1) ? ? ? yes P(2) C(11) C(12) 122(1) ? ? ? yes P(2) C(11) C(16) 120(1) ? ? ? yes C(12) C(11) C(16) 116(1) ? ? ? yes C(11) C(12) C(13) 119(1) ? ? ? yes C(12) C(13) C(14) 121(1) ? ? ? yes C(13) C(14) C(15) 119(1) ? ? ? yes C(14) C(15) C(16) 118(1) ? ? ? yes C(11) C(16) C(15) 123(1) ? ? ? yes O(1) C(17) C(18) 110(1) ? ? ? yes O(1) C(17) C(24) 111(1) ? ? ? yes O(1) C(17) C(30) 109(1) ? ? ? yes C(18) C(17) C(24) 106(1) ? ? ? yes C(18) C(17) C(30) 107(1) ? ? ? yes C(24) C(17) C(30) 111(1) ? ? ? yes C(17) C(18) C(19) 119(1) ? ? ? yes C(17) C(18) C(23) 120(1) ? ? ? yes C(19) C(18) C(23) 120(1) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes C(19) C(20) C(21) 119(1) ? ? ? yes C(20) C(21) C(22) 120(1) ? ? ? yes C(21) C(22) C(23) 120(1) ? ? ? yes C(18) C(23) C(22) 118(1) ? ? ? yes C(17) C(24) C(25) 119(1) ? ? ? yes C(17) C(24) C(29) 121(1) ? ? ? yes C(25) C(24) C(29) 117(1) ? ? ? yes C(24) C(25) C(26) 121(1) ? ? ? yes C(25) C(26) C(27) 118(1) ? ? ? yes C(26) C(27) C(28) 119(1) ? ? ? yes C(27) C(28) C(29) 122(1) ? ? ? yes C(24) C(29) C(28) 118(1) ? ? ? yes C(17) C(30) C(31) 116(1) ? ? ? yes N(1) C(31) C(30) 118(1) ? ? ? yes N(1) C(31) C(32) 122(1) ? ? ? yes C(30) C(31) C(32) 118(1) ? ? ? yes C(31) C(32) C(33) 118(1) ? ? ? yes C(32) C(33) C(34) 120(1) ? ? ? yes C(33) C(34) C(35) 121(1) ? ? ? yes N(1) C(35) C(34) 119(1) ? ? ? yes N(1) C(35) C(36) 119(1) ? ? ? yes C(34) C(35) C(36) 120(1) ? ? ? yes C(35) C(36) C(37) 119(1) ? ? ? yes O(2) C(37) C(36) 115(1) ? ? ? yes O(2) C(37) C(38) 106(1) ? ? ? yes O(2) C(37) C(44) 104(1) ? ? ? yes C(36) C(37) C(38) 114(1) ? ? ? yes C(36) C(37) C(44) 107(1) ? ? ? yes C(38) C(37) C(44) 107(1) ? ? ? yes C(37) C(38) C(39) 118(1) ? ? ? yes C(37) C(38) C(43) 120(1) ? ? ? yes C(39) C(38) C(43) 120(1) ? ? ? yes C(38) C(39) C(40) 116(1) ? ? ? yes C(39) C(40) C(41) 122(2) ? ? ? yes C(40) C(41) C(42) 118(2) ? ? ? yes C(41) C(42) C(43) 121(2) ? ? ? yes C(38) C(43) C(42) 119(1) ? ? ? yes C(37) C(44) C(45) 125(1) ? ? ? yes C(37) C(44) C(49) 118(1) ? ? ? yes C(45) C(44) C(49) 116(1) ? ? ? yes C(44) C(45) C(46) 121(1) ? ? ? yes C(45) C(46) C(47) 120(1) ? ? ? yes C(46) C(47) C(48) 118(1) ? ? ? yes C(47) C(48) C(49) 120(1) ? ? ? yes C(44) C(49) C(48) 121(1) ? ? ? yes #------------------------------------------------------------------------------