# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cla1 _database_code_depnum_ccdc_archive 'CCDC 887598' #TrackingRef 'Dalton complex3h.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C39H36F6N5O2PRuS, 0.5 CH2Cl2' _chemical_formula_sum 'C78.50 H73 Cl F12 N10 O4 P2 Ru2 S2' _chemical_formula_weight 1812.12 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.3379(5) _cell_length_b 14.9255(5) _cell_length_c 37.3985(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8003.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.7177 _cell_measurement_theta_max 29.0203 _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3684 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8437 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1903 _diffrn_standards_number 0 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26584 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.1384 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14228 _reflns_number_gt 10555 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration rmad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 14228 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.002 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 0.67668(4) 0.31147(4) 0.756816(14) 0.01841(13) Uani 1 1 d . . . P1 P 0.32983(15) 0.54992(14) 0.91550(5) 0.0309(5) Uani 1 1 d . . . Ru2 Ru 0.73640(4) 0.42648(4) 0.989967(15) 0.02085(14) Uani 1 1 d . . . P2 P 0.55545(17) 0.42007(16) 1.16264(5) 0.0370(5) Uani 1 1 d . . . F11 F 0.3785(4) 0.6117(4) 0.88739(16) 0.087(2) Uani 1 1 d . . . S11 S 0.87296(14) 0.58502(15) 0.80097(5) 0.0345(5) Uani 1 1 d . . . O11 O 0.5763(3) 0.2976(3) 0.71845(12) 0.0277(12) Uani 1 1 d . . . N11 N 0.6744(4) 0.4487(3) 0.74784(13) 0.0199(13) Uani 1 1 d . . . F12 F 0.2958(3) 0.4829(4) 0.88526(12) 0.0670(17) Uani 1 1 d . . . O12 O 0.6231(4) 0.5769(3) 0.72419(12) 0.0307(13) Uani 1 1 d . . . N12 N 0.7643(4) 0.2820(3) 0.71484(13) 0.0199(13) Uani 1 1 d . . . F13 F 0.4226(3) 0.4937(4) 0.92078(13) 0.0556(15) Uani 1 1 d . . . N13 N 0.6767(4) 0.1760(3) 0.75925(14) 0.0230(13) Uani 1 1 d . . . F14 F 0.2806(3) 0.4883(3) 0.94484(12) 0.0526(14) Uani 1 1 d . . . N14 N 0.7639(4) 0.3172(4) 0.79952(13) 0.0218(13) Uani 1 1 d . . . F15 F 0.3613(4) 0.6149(3) 0.94752(14) 0.0632(16) Uani 1 1 d . . . N15 N 0.5847(4) 0.3344(4) 0.79686(15) 0.0229(15) Uani 1 1 d . . . F16 F 0.2359(3) 0.6056(3) 0.91110(12) 0.0530(14) Uani 1 1 d . . . F21 F 0.5712(4) 0.4766(3) 1.12725(12) 0.0543(15) Uani 1 1 d . . . S21 S 0.48907(17) 0.62477(14) 1.04832(6) 0.0393(6) Uani 1 1 d . . . O21 O 0.7373(3) 0.3134(3) 0.95871(12) 0.0303(12) Uani 1 1 d . . . N21 N 0.5954(4) 0.4076(4) 0.99918(14) 0.0210(14) Uani 1 1 d . . . F22 F 0.4488(3) 0.4084(3) 1.15313(14) 0.0567(15) Uani 1 1 d . . . O22 O 0.4552(3) 0.3429(3) 0.99451(11) 0.0245(11) Uani 1 1 d . . . N22 N 0.8717(4) 0.4419(4) 0.97524(15) 0.0283(15) Uani 1 1 d . . . F23 F 0.5321(4) 0.5105(3) 1.18393(12) 0.0521(14) Uani 1 1 d . . . N23 N 0.7223(4) 0.4994(4) 0.94364(15) 0.0272(15) Uani 1 1 d . . . F24 F 0.6626(3) 0.4325(4) 1.17270(12) 0.0593(15) Uani 1 1 d . . . N24 N 0.7512(4) 0.5287(4) 1.02592(15) 0.0253(14) Uani 1 1 d . . . F25 F 0.5802(3) 0.3292(3) 1.14240(11) 0.0451(13) Uani 1 1 d . . . N25 N 0.7540(4) 0.3575(4) 1.03651(15) 0.0252(14) Uani 1 1 d . . . F26 F 0.5409(4) 0.3650(3) 1.19908(12) 0.0600(16) Uani 1 1 d . . . C111 C 0.5635(5) 0.3522(5) 0.69168(19) 0.0225(17) Uani 1 1 d . . . C112 C 0.5209(6) 0.3157(6) 0.66028(18) 0.038(2) Uani 1 1 d . . . H11A H 0.5061 0.2538 0.6592 0.046 Uiso 1 1 calc R . . C113 C 0.5011(7) 0.3712(7) 0.6314(2) 0.049(3) Uani 1 1 d . . . H11B H 0.4751 0.3457 0.6104 0.059 Uiso 1 1 calc R . . C114 C 0.5180(6) 0.4625(6) 0.6323(2) 0.036(2) Uani 1 1 d . . . H11C H 0.5011 0.4996 0.6127 0.043 Uiso 1 1 calc R . . C115 C 0.5596(5) 0.4981(5) 0.6621(2) 0.033(2) Uani 1 1 d . . . H11D H 0.5732 0.5603 0.6625 0.039 Uiso 1 1 calc R . . C116 C 0.5827(5) 0.4456(5) 0.69171(17) 0.0201(16) Uani 1 1 d . . . C121 C 0.8107(5) 0.3389(5) 0.69462(17) 0.0255(17) Uani 1 1 d . . . H12A H 0.8189 0.3984 0.7030 0.031 Uiso 1 1 calc R . . C122 C 0.8481(5) 0.3160(5) 0.66160(19) 0.0328(19) Uani 1 1 d . . . H12B H 0.8813 0.3584 0.6476 0.039 Uiso 1 1 calc R . . C123 C 0.8352(6) 0.2287(5) 0.64982(18) 0.0311(19) Uani 1 1 d . . . H12C H 0.8591 0.2109 0.6272 0.037 Uiso 1 1 calc R . . C124 C 0.7883(5) 0.1682(5) 0.67040(17) 0.0252(18) Uani 1 1 d . . . H12D H 0.7788 0.1086 0.6622 0.030 Uiso 1 1 calc R . . C125 C 0.7549(5) 0.1952(5) 0.70354(16) 0.0218(15) Uani 1 1 d . . . C131 C 0.6430(6) 0.1226(5) 0.7858(2) 0.033(2) Uani 1 1 d . . . H13A H 0.6178 0.1503 0.8065 0.040 Uiso 1 1 calc R . . C132 C 0.6437(6) 0.0315(5) 0.7841(2) 0.035(2) Uani 1 1 d . . . H13B H 0.6203 -0.0030 0.8034 0.041 Uiso 1 1 calc R . . C133 C 0.6780(6) -0.0094(4) 0.7546(2) 0.038(2) Uani 1 1 d . . . H13C H 0.6786 -0.0730 0.7532 0.045 Uiso 1 1 calc R . . C134 C 0.7127(5) 0.0416(5) 0.7261(2) 0.032(2) Uani 1 1 d . . . H13D H 0.7360 0.0139 0.7051 0.039 Uiso 1 1 calc R . . C135 C 0.7115(5) 0.1342(4) 0.72982(17) 0.0199(16) Uani 1 1 d . . . C141 C 0.8562(5) 0.2997(5) 0.7997(2) 0.0267(18) Uani 1 1 d . . . H14A H 0.8857 0.2847 0.7777 0.032 Uiso 1 1 calc R . . C142 C 0.9092(6) 0.3028(5) 0.8301(2) 0.034(2) Uani 1 1 d . . . H14B H 0.9739 0.2893 0.8291 0.041 Uiso 1 1 calc R . . C143 C 0.8688(6) 0.3253(6) 0.8618(2) 0.041(2) Uani 1 1 d . . . H14C H 0.9055 0.3290 0.8829 0.049 Uiso 1 1 calc R . . C144 C 0.7739(6) 0.3428(5) 0.8631(2) 0.035(2) Uani 1 1 d . . . H14D H 0.7449 0.3582 0.8851 0.042 Uiso 1 1 calc R . . C145 C 0.7220(5) 0.3374(5) 0.83187(19) 0.0257(18) Uani 1 1 d . . . C151 C 0.4922(5) 0.3392(6) 0.7930(2) 0.034(2) Uani 1 1 d . . . H15A H 0.4667 0.3312 0.7697 0.041 Uiso 1 1 calc R . . C152 C 0.4333(6) 0.3549(6) 0.8202(2) 0.040(2) Uani 1 1 d . . . H15B H 0.3679 0.3577 0.8163 0.048 Uiso 1 1 calc R . . C153 C 0.4704(7) 0.3668(6) 0.8544(3) 0.051(3) Uani 1 1 d . . . H15C H 0.4304 0.3774 0.8742 0.062 Uiso 1 1 calc R . . C154 C 0.5632(6) 0.3632(5) 0.8590(2) 0.039(2) Uani 1 1 d . . . H15D H 0.5894 0.3719 0.8821 0.047 Uiso 1 1 calc R . . C155 C 0.6206(5) 0.3465(5) 0.82982(18) 0.0202(16) Uani 1 1 d . . . C160 C 0.9916(5) 0.5868(5) 0.7863(2) 0.036(2) Uani 1 1 d . . . H16A H 0.9926 0.5999 0.7604 0.043 Uiso 1 1 calc R . . H16B H 1.0242 0.6364 0.7986 0.043 Uiso 1 1 calc R . . C161 C 1.0460(5) 0.4997(5) 0.7929(2) 0.0311(19) Uani 1 1 d . . . C162 C 1.0802(6) 0.4780(6) 0.82558(19) 0.034(2) Uani 1 1 d . . . H16C H 1.0704 0.5177 0.8451 0.041 Uiso 1 1 calc R . . C163 C 1.1286(5) 0.4001(6) 0.8312(2) 0.038(2) Uani 1 1 d . . . H16D H 1.1514 0.3865 0.8544 0.046 Uiso 1 1 calc R . . C164 C 1.1442(6) 0.3428(6) 0.8040(2) 0.039(2) Uani 1 1 d . . . H16E H 1.1786 0.2894 0.8082 0.047 Uiso 1 1 calc R . . C165 C 1.1110(6) 0.3607(6) 0.7704(2) 0.043(2) Uani 1 1 d . . . H16F H 1.1217 0.3196 0.7515 0.051 Uiso 1 1 calc R . . C166 C 1.0618(5) 0.4393(6) 0.7644(2) 0.043(2) Uani 1 1 d . . . H16G H 1.0387 0.4526 0.7411 0.051 Uiso 1 1 calc R . . C171 C 0.6277(5) 0.4876(5) 0.72221(19) 0.0265(18) Uani 1 1 d . . . C172 C 0.6544(6) 0.6017(5) 0.7599(2) 0.0322(19) Uani 1 1 d . . . C173 C 0.5691(6) 0.6100(6) 0.7830(2) 0.046(2) Uani 1 1 d . . . H17A H 0.5328 0.6624 0.7755 0.069 Uiso 1 1 calc R . . H17B H 0.5879 0.6170 0.8080 0.069 Uiso 1 1 calc R . . H17C H 0.5308 0.5559 0.7805 0.069 Uiso 1 1 calc R . . C174 C 0.7047(6) 0.6911(5) 0.7561(3) 0.060(3) Uani 1 1 d . . . H17D H 0.6600 0.7375 0.7490 0.089 Uiso 1 1 calc R . . H17E H 0.7535 0.6859 0.7379 0.089 Uiso 1 1 calc R . . H17F H 0.7331 0.7075 0.7791 0.089 Uiso 1 1 calc R . . C175 C 0.7143(5) 0.5192(4) 0.77065(17) 0.0193(16) Uani 1 1 d . . . H17G H 0.7012 0.5042 0.7962 0.023 Uiso 1 1 calc R . . C176 C 0.8179(5) 0.5223(5) 0.76522(17) 0.0260(18) Uani 1 1 d . . . H17H H 0.8321 0.5509 0.7420 0.031 Uiso 1 1 calc R . . H17I H 0.8431 0.4605 0.7647 0.031 Uiso 1 1 calc R . . C211 C 0.6653(5) 0.2719(5) 0.94559(17) 0.0229(17) Uani 1 1 d . . . C212 C 0.6824(5) 0.2042(4) 0.91936(17) 0.0262(17) Uani 1 1 d . . . H21A H 0.7449 0.1891 0.9134 0.031 Uiso 1 1 calc R . . C213 C 0.6110(6) 0.1608(5) 0.90269(19) 0.031(2) Uani 1 1 d . . . H21B H 0.6248 0.1174 0.8849 0.038 Uiso 1 1 calc R . . C214 C 0.5178(5) 0.1787(6) 0.91115(19) 0.034(2) Uani 1 1 d . . . H21C H 0.4684 0.1484 0.8993 0.041 Uiso 1 1 calc R . . C215 C 0.5001(5) 0.2412(5) 0.93695(19) 0.0299(19) Uani 1 1 d . . . H21D H 0.4371 0.2532 0.9432 0.036 Uiso 1 1 calc R . . C216 C 0.5702(5) 0.2879(5) 0.95447(17) 0.0181(16) Uani 1 1 d . . . C221 C 0.9461(5) 0.4090(5) 0.9930(2) 0.040(2) Uani 1 1 d . . . H22A H 0.9361 0.3805 1.0154 0.048 Uiso 1 1 calc R . . C222 C 1.0358(6) 0.4149(6) 0.9801(3) 0.052(3) Uani 1 1 d . . . H22B H 1.0867 0.3920 0.9935 0.062 Uiso 1 1 calc R . . C223 C 1.0500(6) 0.4546(6) 0.9475(3) 0.053(3) Uani 1 1 d . . . H22C H 1.1110 0.4577 0.9376 0.064 Uiso 1 1 calc R . . C224 C 0.9761(6) 0.4897(6) 0.9293(2) 0.042(2) Uani 1 1 d . . . H22D H 0.9857 0.5192 0.9071 0.051 Uiso 1 1 calc R . . C225 C 0.8861(6) 0.4822(5) 0.9434(2) 0.0312(19) Uani 1 1 d . . . C231 C 0.6421(5) 0.5267(5) 0.92858(19) 0.033(2) Uani 1 1 d . . . H23A H 0.5853 0.5134 0.9406 0.040 Uiso 1 1 calc R . . C232 C 0.6377(6) 0.5723(6) 0.89712(18) 0.037(2) Uani 1 1 d . . . H23B H 0.5791 0.5889 0.8873 0.044 Uiso 1 1 calc R . . C233 C 0.7171(7) 0.5935(7) 0.8803(2) 0.052(3) Uani 1 1 d . . . H23C H 0.7156 0.6258 0.8584 0.063 Uiso 1 1 calc R . . C234 C 0.8017(6) 0.5677(7) 0.8952(2) 0.051(3) Uani 1 1 d . . . H23D H 0.8584 0.5845 0.8839 0.061 Uiso 1 1 calc R . . C235 C 0.8040(5) 0.5181(5) 0.92611(18) 0.0276(19) Uani 1 1 d . . . C241 C 0.7576(6) 0.6178(4) 1.01793(19) 0.0288(18) Uani 1 1 d . . . H24A H 0.7497 0.6363 0.9938 0.035 Uiso 1 1 calc R . . C242 C 0.7746(6) 0.6804(5) 1.0432(2) 0.037(2) Uani 1 1 d . . . H24B H 0.7794 0.7417 1.0365 0.045 Uiso 1 1 calc R . . C243 C 0.7849(6) 0.6570(5) 1.0780(2) 0.040(2) Uani 1 1 d . . . H24C H 0.7958 0.7009 1.0959 0.047 Uiso 1 1 calc R . . C244 C 0.7792(5) 0.5677(5) 1.08657(19) 0.0351(19) Uani 1 1 d . . . H24D H 0.7863 0.5493 1.1107 0.042 Uiso 1 1 calc R . . C245 C 0.7634(5) 0.5047(5) 1.06047(17) 0.0226(16) Uani 1 1 d . . . C251 C 0.7495(5) 0.2680(5) 1.0396(2) 0.0301(19) Uani 1 1 d . . . H25A H 0.7442 0.2324 1.0186 0.036 Uiso 1 1 calc R . . C252 C 0.7524(5) 0.2261(5) 1.0727(2) 0.036(2) Uani 1 1 d . . . H25B H 0.7500 0.1626 1.0742 0.044 Uiso 1 1 calc R . . C253 C 0.7588(6) 0.2763(5) 1.1035(2) 0.040(2) Uani 1 1 d . . . H25C H 0.7599 0.2486 1.1263 0.048 Uiso 1 1 calc R . . C254 C 0.7638(6) 0.3684(5) 1.1001(2) 0.037(2) Uani 1 1 d . . . H25D H 0.7699 0.4048 1.1208 0.044 Uiso 1 1 calc R . . C255 C 0.7598(5) 0.4079(5) 1.06658(17) 0.0234(17) Uani 1 1 d . . . C260 C 0.4557(6) 0.7222(5) 1.0221(2) 0.047(2) Uani 1 1 d . . . H26A H 0.4061 0.7045 1.0051 0.056 Uiso 1 1 calc R . . H26B H 0.4293 0.7680 1.0383 0.056 Uiso 1 1 calc R . . C261 C 0.5357(6) 0.7634(5) 1.0013(2) 0.038(2) Uani 1 1 d . . . C262 C 0.5548(6) 0.7394(5) 0.9662(2) 0.036(2) Uani 1 1 d . . . H26C H 0.5171 0.6960 0.9545 0.043 Uiso 1 1 calc R . . C263 C 0.6283(7) 0.7785(5) 0.9482(2) 0.046(2) Uani 1 1 d . . . H26D H 0.6407 0.7615 0.9242 0.055 Uiso 1 1 calc R . . C264 C 0.6841(7) 0.8416(6) 0.9644(2) 0.051(3) Uani 1 1 d . . . H26E H 0.7343 0.8680 0.9516 0.062 Uiso 1 1 calc R . . C265 C 0.6669(8) 0.8662(6) 0.9991(3) 0.067(3) Uani 1 1 d . . . H26F H 0.7052 0.9097 1.0105 0.081 Uiso 1 1 calc R . . C266 C 0.5924(7) 0.8269(6) 1.0177(2) 0.051(3) Uani 1 1 d . . . H26G H 0.5806 0.8439 1.0418 0.061 Uiso 1 1 calc R . . C271 C 0.5456(5) 0.3491(5) 0.98332(18) 0.0214(16) Uani 1 1 d . . . C272 C 0.4511(5) 0.3931(5) 1.02897(17) 0.0238(18) Uani 1 1 d . . . C273 C 0.4643(6) 0.3244(5) 1.05853(17) 0.0312(19) Uani 1 1 d . . . H27A H 0.4096 0.2851 1.0596 0.047 Uiso 1 1 calc R . . H27B H 0.4716 0.3553 1.0815 0.047 Uiso 1 1 calc R . . H27C H 0.5200 0.2885 1.0536 0.047 Uiso 1 1 calc R . . C274 C 0.3548(5) 0.4342(5) 1.0307(2) 0.0339(19) Uani 1 1 d . . . H27D H 0.3080 0.3866 1.0323 0.051 Uiso 1 1 calc R . . H27E H 0.3436 0.4698 1.0090 0.051 Uiso 1 1 calc R . . H27F H 0.3503 0.4730 1.0517 0.051 Uiso 1 1 calc R . . C275 C 0.5370(5) 0.4550(4) 1.02646(18) 0.0206(16) Uani 1 1 d . . . H27G H 0.5703 0.4574 1.0499 0.025 Uiso 1 1 calc R . . C276 C 0.5194(5) 0.5502(4) 1.01231(19) 0.0281(17) Uani 1 1 d . . . H27H H 0.4681 0.5489 0.9946 0.034 Uiso 1 1 calc R . . H27I H 0.5762 0.5726 1.0002 0.034 Uiso 1 1 calc R . . C1S C 0.8622(7) 0.8948(8) 0.8612(4) 0.033(4) Uani 0.50 1 d PDU . . H1SA H 0.8012 0.9133 0.8712 0.040 Uiso 0.50 1 calc PR A 1 H1SB H 0.9086 0.9426 0.8568 0.040 Uiso 0.50 1 calc PR A 1 Cl1A Cl 0.9032(7) 0.7756(6) 0.8675(3) 0.059(3) Uani 0.25 1 d PDU B 1 Cl1B Cl 0.8702(6) 0.7993(5) 0.8391(2) 0.0323(19) Uani 0.25 1 d PDU B 1 Cl2A Cl 0.7405(10) 0.8796(11) 0.8591(4) 0.048(4) Uani 0.17 1 d PDU B 2 Cl2B Cl 0.7406(10) 0.9159(10) 0.8689(4) 0.020(4) Uani 0.17 1 d PDU B 2 Cl2C Cl 0.7539(8) 0.9420(9) 0.8763(4) 0.015(3) Uani 0.17 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0185(3) 0.0181(3) 0.0187(2) -0.0014(2) 0.0003(3) -0.0001(3) P1 0.0249(10) 0.0331(12) 0.0348(11) -0.0010(9) -0.0053(11) 0.0007(12) Ru2 0.0151(3) 0.0228(3) 0.0247(3) -0.0023(3) 0.0007(3) -0.0012(3) P2 0.0423(13) 0.0378(13) 0.0309(11) -0.0057(10) 0.0043(11) -0.0101(14) F11 0.067(4) 0.108(5) 0.087(4) 0.048(4) 0.014(4) -0.018(4) S11 0.0280(11) 0.0419(13) 0.0336(11) -0.0136(10) -0.0043(10) -0.0028(12) O11 0.026(3) 0.033(3) 0.024(3) 0.007(2) -0.003(2) -0.007(3) N11 0.021(3) 0.018(3) 0.020(3) -0.005(2) 0.003(3) -0.001(3) F12 0.054(4) 0.093(4) 0.054(3) -0.040(3) -0.021(3) 0.016(3) O12 0.039(3) 0.015(2) 0.038(3) 0.000(2) -0.006(3) 0.004(3) N12 0.024(3) 0.018(3) 0.018(3) 0.002(2) 0.005(3) -0.003(3) F13 0.030(3) 0.075(4) 0.062(3) -0.014(3) -0.012(3) 0.020(3) N13 0.022(3) 0.025(3) 0.022(3) 0.001(3) 0.001(3) 0.001(3) F14 0.052(3) 0.046(3) 0.060(3) 0.010(2) 0.003(3) 0.003(3) N14 0.024(3) 0.018(3) 0.024(3) 0.003(2) 0.003(3) 0.003(4) F15 0.065(4) 0.043(3) 0.081(4) -0.025(3) -0.025(3) 0.000(3) N15 0.025(3) 0.016(3) 0.028(3) -0.003(3) 0.007(3) -0.002(3) F16 0.045(3) 0.061(3) 0.053(3) 0.008(2) -0.003(3) 0.026(3) F21 0.078(4) 0.045(3) 0.040(3) 0.002(2) 0.008(3) -0.011(3) S21 0.0474(14) 0.0308(11) 0.0397(12) -0.0047(9) 0.0091(12) 0.0063(12) O21 0.018(2) 0.033(3) 0.039(3) -0.019(2) 0.001(3) 0.004(3) N21 0.019(3) 0.021(3) 0.023(3) -0.002(2) -0.001(3) -0.003(3) F22 0.036(3) 0.055(3) 0.079(4) -0.019(3) -0.005(3) -0.007(3) O22 0.019(2) 0.034(3) 0.020(2) -0.001(2) 0.004(2) -0.003(3) N22 0.028(4) 0.025(4) 0.032(3) -0.007(3) 0.005(3) -0.002(3) F23 0.060(3) 0.041(3) 0.056(3) -0.018(2) 0.006(3) -0.007(3) N23 0.025(3) 0.034(4) 0.023(3) -0.008(3) 0.004(3) -0.006(4) F24 0.043(3) 0.084(4) 0.051(3) -0.019(3) 0.001(3) -0.011(4) N24 0.018(4) 0.022(3) 0.035(3) -0.004(3) 0.003(3) -0.003(3) F25 0.056(3) 0.042(3) 0.037(2) -0.007(2) 0.006(2) -0.003(3) N25 0.011(3) 0.026(3) 0.038(3) -0.001(3) 0.008(3) -0.005(3) F26 0.092(4) 0.054(3) 0.035(3) 0.005(2) 0.012(3) -0.016(4) C111 0.011(4) 0.030(4) 0.027(4) 0.005(3) 0.000(3) -0.005(4) C112 0.049(5) 0.039(5) 0.027(4) -0.003(4) -0.007(4) -0.006(5) C113 0.056(7) 0.070(7) 0.021(4) -0.009(4) -0.017(5) -0.011(6) C114 0.045(5) 0.039(5) 0.025(4) -0.002(4) -0.007(4) 0.007(5) C115 0.030(5) 0.034(5) 0.034(4) 0.014(4) 0.011(4) 0.005(4) C116 0.016(4) 0.024(4) 0.021(3) -0.005(3) -0.008(3) -0.001(4) C121 0.025(4) 0.030(4) 0.022(4) -0.001(3) 0.001(4) -0.004(4) C122 0.031(5) 0.033(4) 0.034(4) 0.004(4) 0.007(4) -0.009(5) C123 0.036(5) 0.036(4) 0.022(4) -0.007(3) 0.006(4) 0.010(5) C124 0.029(4) 0.022(4) 0.024(4) -0.003(3) -0.005(3) 0.007(4) C125 0.017(4) 0.020(3) 0.029(4) -0.001(3) -0.003(3) 0.003(4) C131 0.033(5) 0.034(5) 0.033(4) 0.004(4) 0.004(4) 0.004(5) C132 0.033(5) 0.026(4) 0.044(5) 0.013(4) 0.015(4) -0.004(4) C133 0.035(4) 0.009(3) 0.070(6) 0.002(4) 0.007(6) -0.002(4) C134 0.032(5) 0.018(4) 0.047(5) -0.001(3) 0.010(4) 0.001(4) C135 0.015(4) 0.020(4) 0.025(4) 0.001(3) -0.004(3) 0.000(3) C141 0.021(4) 0.023(4) 0.036(4) -0.002(3) -0.004(4) 0.003(4) C142 0.025(4) 0.024(4) 0.052(5) 0.014(4) -0.009(4) 0.001(4) C143 0.041(5) 0.051(6) 0.032(5) 0.005(4) -0.014(5) -0.012(6) C144 0.044(5) 0.038(5) 0.023(4) 0.006(3) -0.003(4) -0.011(5) C145 0.031(4) 0.017(4) 0.030(4) -0.003(3) 0.004(4) -0.005(4) C151 0.025(4) 0.043(5) 0.035(4) 0.001(4) -0.001(4) 0.011(5) C152 0.026(5) 0.050(6) 0.043(5) 0.007(4) 0.011(4) 0.006(5) C153 0.050(6) 0.051(6) 0.052(6) 0.004(5) 0.035(6) 0.012(6) C154 0.051(6) 0.033(5) 0.034(5) -0.006(4) 0.011(5) -0.012(5) C155 0.026(4) 0.015(4) 0.020(4) -0.001(3) 0.003(4) -0.005(4) C160 0.029(4) 0.036(5) 0.043(5) 0.005(4) -0.009(4) -0.004(5) C161 0.013(4) 0.042(5) 0.038(5) 0.004(4) 0.005(4) -0.005(4) C162 0.033(5) 0.044(5) 0.024(4) 0.004(4) -0.007(4) -0.012(5) C163 0.024(4) 0.050(6) 0.041(5) 0.016(4) 0.000(4) -0.016(5) C164 0.031(5) 0.034(5) 0.052(5) 0.005(4) -0.001(5) -0.002(5) C165 0.043(5) 0.038(5) 0.046(5) -0.010(4) 0.000(5) -0.001(5) C166 0.028(4) 0.069(7) 0.031(5) -0.002(4) 0.004(4) -0.015(5) C171 0.020(4) 0.025(4) 0.035(4) 0.008(3) 0.010(4) 0.003(4) C172 0.039(5) 0.020(4) 0.037(4) -0.005(3) -0.009(4) 0.006(4) C173 0.040(5) 0.048(6) 0.050(5) -0.011(4) -0.006(5) 0.014(5) C174 0.061(6) 0.018(4) 0.100(7) 0.002(5) -0.037(6) 0.001(5) C175 0.017(4) 0.022(4) 0.019(3) -0.005(3) 0.001(3) 0.000(4) C176 0.027(4) 0.028(4) 0.023(4) 0.000(3) 0.002(4) -0.001(4) C211 0.024(4) 0.023(4) 0.022(4) -0.003(3) -0.004(4) -0.004(4) C212 0.019(4) 0.030(4) 0.030(4) -0.004(3) 0.003(4) -0.003(4) C213 0.041(5) 0.026(4) 0.027(4) -0.010(3) -0.006(4) -0.010(4) C214 0.023(4) 0.044(5) 0.037(4) -0.009(4) 0.004(4) -0.005(5) C215 0.022(4) 0.036(5) 0.031(4) -0.004(4) 0.004(4) 0.000(4) C216 0.015(3) 0.024(4) 0.016(3) 0.002(3) -0.002(3) -0.006(4) C221 0.022(4) 0.037(5) 0.060(6) -0.003(4) -0.002(5) -0.003(4) C222 0.019(4) 0.048(6) 0.089(8) 0.000(5) -0.013(5) 0.004(5) C223 0.022(5) 0.058(7) 0.079(7) -0.009(6) 0.021(5) -0.011(5) C224 0.036(5) 0.056(6) 0.035(5) -0.003(4) 0.008(5) -0.001(5) C225 0.027(4) 0.036(5) 0.031(4) -0.012(4) 0.012(4) -0.004(4) C231 0.024(4) 0.047(5) 0.028(4) -0.002(4) -0.007(4) -0.005(4) C232 0.031(4) 0.057(6) 0.023(4) 0.008(4) 0.004(4) 0.010(5) C233 0.056(6) 0.078(7) 0.024(4) 0.012(4) -0.005(5) 0.011(6) C234 0.041(5) 0.082(7) 0.029(4) 0.007(5) 0.010(4) -0.037(6) C235 0.020(4) 0.041(5) 0.022(4) -0.005(3) 0.004(4) -0.011(4) C241 0.031(5) 0.025(4) 0.031(4) 0.005(3) 0.006(4) 0.007(4) C242 0.033(5) 0.020(4) 0.059(5) -0.007(4) 0.006(5) -0.012(5) C243 0.037(5) 0.036(5) 0.046(5) -0.020(4) 0.003(5) -0.007(5) C244 0.034(5) 0.042(5) 0.030(4) -0.007(4) -0.005(4) 0.002(5) C245 0.018(4) 0.026(4) 0.024(4) 0.001(3) 0.003(4) -0.001(4) C251 0.017(4) 0.027(4) 0.046(5) -0.001(3) -0.001(4) 0.002(4) C252 0.018(4) 0.027(4) 0.065(6) 0.015(4) 0.004(5) 0.002(4) C253 0.031(5) 0.047(5) 0.042(5) 0.021(4) 0.006(5) 0.000(5) C254 0.032(5) 0.039(5) 0.039(4) 0.012(4) 0.009(5) 0.010(5) C255 0.015(4) 0.034(4) 0.021(3) -0.001(3) -0.002(3) 0.004(4) C260 0.047(6) 0.026(5) 0.066(6) -0.007(4) 0.004(5) 0.015(5) C261 0.042(5) 0.019(4) 0.054(5) 0.009(4) -0.008(5) 0.008(4) C262 0.049(6) 0.024(4) 0.035(5) 0.005(4) -0.015(5) 0.000(5) C263 0.063(6) 0.028(5) 0.048(5) 0.014(4) -0.020(5) -0.006(5) C264 0.058(6) 0.045(5) 0.051(6) 0.019(4) -0.016(6) -0.009(6) C265 0.064(7) 0.054(6) 0.084(8) 0.006(5) -0.025(7) -0.020(7) C266 0.071(7) 0.037(5) 0.045(5) -0.010(4) -0.019(5) 0.005(6) C271 0.016(4) 0.027(4) 0.021(4) 0.007(3) -0.002(3) -0.004(4) C272 0.025(4) 0.034(4) 0.013(3) 0.000(3) 0.007(3) 0.009(4) C273 0.037(4) 0.033(5) 0.024(4) 0.007(3) 0.011(4) -0.010(5) C274 0.028(4) 0.032(4) 0.042(4) -0.009(4) 0.011(4) 0.004(4) C275 0.018(4) 0.020(4) 0.025(4) 0.002(3) 0.005(3) -0.004(4) C276 0.021(4) 0.029(4) 0.034(4) 0.002(4) 0.004(4) 0.004(4) C1S 0.022(7) 0.036(7) 0.042(7) -0.002(6) 0.015(6) -0.017(7) Cl1A 0.056(6) 0.040(5) 0.081(6) -0.049(5) 0.029(5) -0.029(5) Cl1B 0.043(4) 0.013(3) 0.041(4) -0.016(3) 0.006(4) -0.015(4) Cl2A 0.028(7) 0.059(8) 0.057(8) 0.040(6) -0.017(6) -0.021(7) Cl2B 0.023(7) 0.011(7) 0.027(7) -0.025(5) -0.010(5) -0.002(6) Cl2C 0.004(5) 0.027(7) 0.014(6) -0.011(5) 0.002(5) -0.007(5) _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 N13 2.024(5) . ? Ru1 N15 2.025(6) . ? Ru1 N14 2.030(6) . ? Ru1 O11 2.043(5) . ? Ru1 N12 2.058(5) . ? Ru1 N11 2.075(5) . ? P1 F11 1.563(6) . ? P1 F13 1.586(5) . ? P1 F12 1.587(5) . ? P1 F16 1.591(5) . ? P1 F14 1.597(5) . ? P1 F15 1.606(5) . ? Ru2 N22 2.029(6) . ? Ru2 N25 2.038(6) . ? Ru2 N24 2.045(5) . ? Ru2 O21 2.053(5) . ? Ru2 N23 2.056(6) . ? Ru2 N21 2.071(6) . ? P2 F22 1.580(5) . ? P2 F21 1.585(5) . ? P2 F24 1.592(5) . ? P2 F25 1.593(5) . ? P2 F23 1.603(5) . ? P2 F26 1.605(5) . ? S11 C160 1.787(8) . ? S11 C176 1.813(7) . ? O11 C111 1.303(8) . ? N11 C171 1.306(8) . ? N11 C175 1.471(8) . ? O12 C171 1.338(8) . ? O12 C172 1.457(8) . ? N12 C121 1.317(8) . ? N12 C125 1.369(8) . ? N13 C135 1.360(8) . ? N13 C131 1.360(9) . ? N14 C141 1.349(9) . ? N14 C145 1.384(8) . ? N15 C151 1.336(9) . ? N15 C155 1.348(8) . ? S21 C276 1.800(7) . ? S21 C260 1.818(8) . ? O21 C211 1.300(8) . ? N21 C271 1.275(8) . ? N21 C275 1.497(8) . ? O22 C271 1.366(8) . ? O22 C272 1.492(8) . ? N22 C221 1.349(9) . ? N22 C225 1.350(9) . ? N23 C231 1.344(9) . ? N23 C235 1.371(9) . ? N24 C245 1.353(8) . ? N24 C241 1.365(8) . ? N25 C251 1.343(8) . ? N25 C255 1.356(8) . ? C111 C116 1.421(9) . ? C111 C112 1.431(10) . ? C112 C113 1.389(11) . ? C112 H11A 0.9500 . ? C113 C114 1.384(11) . ? C113 H11B 0.9500 . ? C114 C115 1.369(10) . ? C114 H11C 0.9500 . ? C115 C116 1.397(9) . ? C115 H11D 0.9500 . ? C116 C171 1.453(9) . ? C121 C122 1.389(9) . ? C121 H12A 0.9500 . ? C122 C123 1.388(10) . ? C122 H12B 0.9500 . ? C123 C124 1.363(9) . ? C123 H12C 0.9500 . ? C124 C125 1.389(9) . ? C124 H12D 0.9500 . ? C125 C135 1.477(9) . ? C131 C132 1.361(10) . ? C131 H13A 0.9500 . ? C132 C133 1.353(10) . ? C132 H13B 0.9500 . ? C133 C134 1.400(10) . ? C133 H13C 0.9500 . ? C134 C135 1.390(9) . ? C134 H13D 0.9500 . ? C141 C142 1.369(10) . ? C141 H14A 0.9500 . ? C142 C143 1.361(10) . ? C142 H14B 0.9500 . ? C143 C144 1.386(11) . ? C143 H14C 0.9500 . ? C144 C145 1.387(10) . ? C144 H14D 0.9500 . ? C145 C155 1.462(10) . ? C151 C152 1.344(10) . ? C151 H15A 0.9500 . ? C152 C153 1.397(12) . ? C152 H15B 0.9500 . ? C153 C154 1.342(12) . ? C153 H15C 0.9500 . ? C154 C155 1.391(10) . ? C154 H15D 0.9500 . ? C160 C161 1.536(10) . ? C160 H16A 0.9900 . ? C160 H16B 0.9900 . ? C161 C162 1.355(10) . ? C161 C166 1.416(11) . ? C162 C163 1.370(11) . ? C162 H16C 0.9500 . ? C163 C164 1.346(11) . ? C163 H16D 0.9500 . ? C164 C165 1.370(10) . ? C164 H16E 0.9500 . ? C165 C166 1.389(11) . ? C165 H16F 0.9500 . ? C166 H16G 0.9500 . ? C172 C173 1.502(11) . ? C172 C174 1.525(10) . ? C172 C175 1.553(9) . ? C173 H17A 0.9800 . ? C173 H17B 0.9800 . ? C173 H17C 0.9800 . ? C174 H17D 0.9800 . ? C174 H17E 0.9800 . ? C174 H17F 0.9800 . ? C175 C176 1.501(9) . ? C175 H17G 1.0000 . ? C176 H17H 0.9900 . ? C176 H17I 0.9900 . ? C211 C216 1.422(10) . ? C211 C212 1.430(9) . ? C212 C213 1.362(9) . ? C212 H21A 0.9500 . ? C213 C214 1.399(10) . ? C213 H21B 0.9500 . ? C214 C215 1.366(10) . ? C214 H21C 0.9500 . ? C215 C216 1.388(9) . ? C215 H21D 0.9500 . ? C216 C271 1.457(9) . ? C221 C222 1.376(11) . ? C221 H22A 0.9500 . ? C222 C223 1.371(12) . ? C222 H22B 0.9500 . ? C223 C224 1.364(12) . ? C223 H22C 0.9500 . ? C224 C225 1.398(10) . ? C224 H22D 0.9500 . ? C225 C235 1.446(11) . ? C231 C232 1.361(10) . ? C231 H23A 0.9500 . ? C232 C233 1.340(11) . ? C232 H23B 0.9500 . ? C233 C234 1.390(11) . ? C233 H23C 0.9500 . ? C234 C235 1.373(10) . ? C234 H23D 0.9500 . ? C241 C242 1.353(9) . ? C241 H24A 0.9500 . ? C242 C243 1.355(10) . ? C242 H24B 0.9500 . ? C243 C244 1.372(10) . ? C243 H24C 0.9500 . ? C244 C245 1.375(9) . ? C244 H24D 0.9500 . ? C245 C255 1.463(9) . ? C251 C252 1.389(10) . ? C251 H25A 0.9500 . ? C252 C253 1.375(10) . ? C252 H25B 0.9500 . ? C253 C254 1.382(10) . ? C253 H25C 0.9500 . ? C254 C255 1.386(9) . ? C254 H25D 0.9500 . ? C260 C261 1.516(12) . ? C260 H26A 0.9900 . ? C260 H26B 0.9900 . ? C261 C262 1.390(11) . ? C261 C266 1.391(11) . ? C262 C263 1.379(11) . ? C262 H26C 0.9500 . ? C263 C264 1.377(11) . ? C263 H26D 0.9500 . ? C264 C265 1.371(12) . ? C264 H26E 0.9500 . ? C265 C266 1.404(13) . ? C265 H26F 0.9500 . ? C266 H26G 0.9500 . ? C272 C274 1.513(9) . ? C272 C273 1.519(9) . ? C272 C275 1.543(10) . ? C273 H27A 0.9800 . ? C273 H27B 0.9800 . ? C273 H27C 0.9800 . ? C274 H27D 0.9800 . ? C274 H27E 0.9800 . ? C274 H27F 0.9800 . ? C275 C276 1.537(9) . ? C275 H27G 1.0000 . ? C276 H27H 0.9900 . ? C276 H27I 0.9900 . ? C1S Cl1B 1.651(12) . ? C1S Cl2A 1.761(15) . ? C1S Cl2B 1.795(16) . ? C1S Cl2C 1.796(14) . ? C1S Cl1A 1.888(13) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? Cl1A Cl1B 1.216(12) . ? Cl2A Cl2B 0.656(17) . ? Cl2A Cl2C 1.15(2) . ? Cl2B Cl2C 0.514(15) . ? 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 N13 Ru1 N15 97.8(2) . . ? N13 Ru1 N14 90.4(2) . . ? N15 Ru1 N14 79.2(2) . . ? N13 Ru1 O11 86.0(2) . . ? N15 Ru1 O11 94.5(2) . . ? N14 Ru1 O11 172.2(2) . . ? N13 Ru1 N12 79.7(2) . . ? N15 Ru1 N12 176.3(2) . . ? N14 Ru1 N12 103.5(2) . . ? O11 Ru1 N12 82.7(2) . . ? N13 Ru1 N11 173.2(2) . . ? N15 Ru1 N11 86.7(2) . . ? N14 Ru1 N11 95.5(2) . . ? O11 Ru1 N11 88.6(2) . . ? N12 Ru1 N11 95.6(2) . . ? F11 P1 F13 91.2(3) . . ? F11 P1 F12 91.7(3) . . ? F13 P1 F12 90.8(3) . . ? F11 P1 F16 90.0(3) . . ? F13 P1 F16 178.7(3) . . ? F12 P1 F16 89.7(3) . . ? F11 P1 F14 178.8(3) . . ? F13 P1 F14 88.9(3) . . ? F12 P1 F14 89.4(3) . . ? F16 P1 F14 89.9(3) . . ? F11 P1 F15 91.1(3) . . ? F13 P1 F15 89.5(3) . . ? F12 P1 F15 177.1(3) . . ? F16 P1 F15 89.9(3) . . ? F14 P1 F15 87.7(3) . . ? N22 Ru2 N25 99.8(2) . . ? N22 Ru2 N24 89.7(2) . . ? N25 Ru2 N24 78.6(2) . . ? N22 Ru2 O21 86.2(2) . . ? N25 Ru2 O21 94.0(2) . . ? N24 Ru2 O21 170.8(2) . . ? N22 Ru2 N23 78.8(2) . . ? N25 Ru2 N23 177.9(3) . . ? N24 Ru2 N23 99.7(2) . . ? O21 Ru2 N23 87.5(2) . . ? N22 Ru2 N21 173.7(2) . . ? N25 Ru2 N21 84.9(2) . . ? N24 Ru2 N21 95.4(2) . . ? O21 Ru2 N21 89.4(2) . . ? N23 Ru2 N21 96.7(2) . . ? F22 P2 F21 90.5(3) . . ? F22 P2 F24 179.2(3) . . ? F21 P2 F24 89.9(3) . . ? F22 P2 F25 90.8(3) . . ? F21 P2 F25 91.4(3) . . ? F24 P2 F25 89.8(3) . . ? F22 P2 F23 90.1(3) . . ? F21 P2 F23 89.8(3) . . ? F24 P2 F23 89.2(3) . . ? F25 P2 F23 178.4(3) . . ? F22 P2 F26 90.5(3) . . ? F21 P2 F26 178.5(3) . . ? F24 P2 F26 89.1(3) . . ? F25 P2 F26 89.8(3) . . ? F23 P2 F26 89.0(3) . . ? C160 S11 C176 101.3(4) . . ? C111 O11 Ru1 125.1(5) . . ? C171 N11 C175 107.8(6) . . ? C171 N11 Ru1 124.5(5) . . ? C175 N11 Ru1 127.4(4) . . ? C171 O12 C172 106.7(5) . . ? C121 N12 C125 118.8(6) . . ? C121 N12 Ru1 127.4(4) . . ? C125 N12 Ru1 112.2(4) . . ? C135 N13 C131 116.8(6) . . ? C135 N13 Ru1 114.9(4) . . ? C131 N13 Ru1 128.2(5) . . ? C141 N14 C145 117.7(6) . . ? C141 N14 Ru1 126.8(5) . . ? C145 N14 Ru1 115.5(5) . . ? C151 N15 C155 118.2(7) . . ? C151 N15 Ru1 125.1(5) . . ? C155 N15 Ru1 116.7(5) . . ? C276 S21 C260 98.9(4) . . ? C211 O21 Ru2 127.0(4) . . ? C271 N21 C275 109.2(5) . . ? C271 N21 Ru2 124.2(5) . . ? C275 N21 Ru2 126.5(4) . . ? C271 O22 C272 105.5(5) . . ? C221 N22 C225 118.3(7) . . ? C221 N22 Ru2 125.5(5) . . ? C225 N22 Ru2 115.9(5) . . ? C231 N23 C235 118.0(6) . . ? C231 N23 Ru2 126.7(5) . . ? C235 N23 Ru2 115.3(5) . . ? C245 N24 C241 117.3(6) . . ? C245 N24 Ru2 116.3(4) . . ? C241 N24 Ru2 126.1(5) . . ? C251 N25 C255 118.9(6) . . ? C251 N25 Ru2 124.7(5) . . ? C255 N25 Ru2 115.9(4) . . ? O11 C111 C116 125.8(6) . . ? O11 C111 C112 116.9(7) . . ? C116 C111 C112 117.1(6) . . ? C113 C112 C111 119.8(8) . . ? C113 C112 H11A 120.1 . . ? C111 C112 H11A 120.1 . . ? C114 C113 C112 122.2(8) . . ? C114 C113 H11B 118.9 . . ? C112 C113 H11B 118.9 . . ? C115 C114 C113 118.5(7) . . ? C115 C114 H11C 120.8 . . ? C113 C114 H11C 120.8 . . ? C114 C115 C116 122.1(7) . . ? C114 C115 H11D 119.0 . . ? C116 C115 H11D 119.0 . . ? C115 C116 C111 120.2(6) . . ? C115 C116 C171 119.1(7) . . ? C111 C116 C171 120.6(6) . . ? N12 C121 C122 123.1(7) . . ? N12 C121 H12A 118.4 . . ? C122 C121 H12A 118.4 . . ? C123 C122 C121 117.5(7) . . ? C123 C122 H12B 121.3 . . ? C121 C122 H12B 121.3 . . ? C124 C123 C122 120.6(6) . . ? C124 C123 H12C 119.7 . . ? C122 C123 H12C 119.7 . . ? C123 C124 C125 118.8(6) . . ? C123 C124 H12D 120.6 . . ? C125 C124 H12D 120.6 . . ? N12 C125 C124 121.1(6) . . ? N12 C125 C135 114.8(5) . . ? C124 C125 C135 124.1(6) . . ? N13 C131 C132 123.3(7) . . ? N13 C131 H13A 118.4 . . ? C132 C131 H13A 118.4 . . ? C133 C132 C131 119.4(7) . . ? C133 C132 H13B 120.3 . . ? C131 C132 H13B 120.3 . . ? C132 C133 C134 120.2(6) . . ? C132 C133 H13C 119.9 . . ? C134 C133 H13C 119.9 . . ? C135 C134 C133 117.4(7) . . ? C135 C134 H13D 121.3 . . ? C133 C134 H13D 121.3 . . ? N13 C135 C134 122.8(6) . . ? N13 C135 C125 114.3(6) . . ? C134 C135 C125 122.8(6) . . ? N14 C141 C142 122.7(7) . . ? N14 C141 H14A 118.6 . . ? C142 C141 H14A 118.6 . . ? C143 C142 C141 119.7(7) . . ? C143 C142 H14B 120.1 . . ? C141 C142 H14B 120.1 . . ? C142 C143 C144 119.7(8) . . ? C142 C143 H14C 120.2 . . ? C144 C143 H14C 120.2 . . ? C143 C144 C145 119.1(8) . . ? C143 C144 H14D 120.5 . . ? C145 C144 H14D 120.5 . . ? N14 C145 C144 121.1(7) . . ? N14 C145 C155 113.9(6) . . ? C144 C145 C155 124.9(7) . . ? N15 C151 C152 123.4(8) . . ? N15 C151 H15A 118.3 . . ? C152 C151 H15A 118.3 . . ? C151 C152 C153 118.5(8) . . ? C151 C152 H15B 120.7 . . ? C153 C152 H15B 120.7 . . ? C154 C153 C152 119.3(8) . . ? C154 C153 H15C 120.4 . . ? C152 C153 H15C 120.4 . . ? C153 C154 C155 119.6(8) . . ? C153 C154 H15D 120.2 . . ? C155 C154 H15D 120.2 . . ? N15 C155 C154 121.0(7) . . ? N15 C155 C145 114.6(6) . . ? C154 C155 C145 124.4(7) . . ? C161 C160 S11 114.9(5) . . ? C161 C160 H16A 108.5 . . ? S11 C160 H16A 108.5 . . ? C161 C160 H16B 108.5 . . ? S11 C160 H16B 108.5 . . ? H16A C160 H16B 107.5 . . ? C162 C161 C166 118.0(8) . . ? C162 C161 C160 122.1(8) . . ? C166 C161 C160 119.8(7) . . ? C161 C162 C163 121.6(8) . . ? C161 C162 H16C 119.2 . . ? C163 C162 H16C 119.2 . . ? C164 C163 C162 120.5(8) . . ? C164 C163 H16D 119.7 . . ? C162 C163 H16D 119.7 . . ? C163 C164 C165 120.7(8) . . ? C163 C164 H16E 119.7 . . ? C165 C164 H16E 119.7 . . ? C164 C165 C166 119.4(8) . . ? C164 C165 H16F 120.3 . . ? C166 C165 H16F 120.3 . . ? C165 C166 C161 119.7(8) . . ? C165 C166 H16G 120.2 . . ? C161 C166 H16G 120.2 . . ? N11 C171 O12 115.4(7) . . ? N11 C171 C116 127.8(7) . . ? O12 C171 C116 116.8(6) . . ? O12 C172 C173 107.3(6) . . ? O12 C172 C174 106.4(6) . . ? C173 C172 C174 111.5(7) . . ? O12 C172 C175 101.9(5) . . ? C173 C172 C175 111.5(6) . . ? C174 C172 C175 117.1(6) . . ? C172 C173 H17A 109.5 . . ? C172 C173 H17B 109.5 . . ? H17A C173 H17B 109.5 . . ? C172 C173 H17C 109.5 . . ? H17A C173 H17C 109.5 . . ? H17B C173 H17C 109.5 . . ? C172 C174 H17D 109.5 . . ? C172 C174 H17E 109.5 . . ? H17D C174 H17E 109.5 . . ? C172 C174 H17F 109.5 . . ? H17D C174 H17F 109.5 . . ? H17E C174 H17F 109.5 . . ? N11 C175 C176 109.1(6) . . ? N11 C175 C172 101.7(5) . . ? C176 C175 C172 119.3(6) . . ? N11 C175 H17G 108.8 . . ? C176 C175 H17G 108.8 . . ? C172 C175 H17G 108.8 . . ? C175 C176 S11 110.3(5) . . ? C175 C176 H17H 109.6 . . ? S11 C176 H17H 109.6 . . ? C175 C176 H17I 109.6 . . ? S11 C176 H17I 109.6 . . ? H17H C176 H17I 108.1 . . ? O21 C211 C216 126.3(6) . . ? O21 C211 C212 117.3(7) . . ? C216 C211 C212 116.3(7) . . ? C213 C212 C211 121.4(7) . . ? C213 C212 H21A 119.3 . . ? C211 C212 H21A 119.3 . . ? C212 C213 C214 121.5(7) . . ? C212 C213 H21B 119.2 . . ? C214 C213 H21B 119.2 . . ? C215 C214 C213 117.9(7) . . ? C215 C214 H21C 121.0 . . ? C213 C214 H21C 121.1 . . ? C214 C215 C216 122.8(7) . . ? C214 C215 H21D 118.6 . . ? C216 C215 H21D 118.6 . . ? C215 C216 C211 119.9(6) . . ? C215 C216 C271 119.3(6) . . ? C211 C216 C271 120.7(6) . . ? N22 C221 C222 122.9(9) . . ? N22 C221 H22A 118.5 . . ? C222 C221 H22A 118.5 . . ? C223 C222 C221 118.6(9) . . ? C223 C222 H22B 120.7 . . ? C221 C222 H22B 120.7 . . ? C224 C223 C222 119.6(8) . . ? C224 C223 H22C 120.2 . . ? C222 C223 H22C 120.2 . . ? C223 C224 C225 119.9(8) . . ? C223 C224 H22D 120.0 . . ? C225 C224 H22D 120.0 . . ? N22 C225 C224 120.6(8) . . ? N22 C225 C235 115.8(7) . . ? C224 C225 C235 123.6(7) . . ? N23 C231 C232 123.6(8) . . ? N23 C231 H23A 118.2 . . ? C232 C231 H23A 118.2 . . ? C233 C232 C231 119.0(8) . . ? C233 C232 H23B 120.5 . . ? C231 C232 H23B 120.5 . . ? C232 C233 C234 119.2(7) . . ? C232 C233 H23C 120.4 . . ? C234 C233 H23C 120.4 . . ? C235 C234 C233 120.6(8) . . ? C235 C234 H23D 119.7 . . ? C233 C234 H23D 119.7 . . ? N23 C235 C234 119.5(7) . . ? N23 C235 C225 114.0(6) . . ? C234 C235 C225 126.5(7) . . ? C242 C241 N24 122.1(7) . . ? C242 C241 H24A 118.9 . . ? N24 C241 H24A 118.9 . . ? C241 C242 C243 120.8(7) . . ? C241 C242 H24B 119.6 . . ? C243 C242 H24B 119.6 . . ? C242 C243 C244 117.9(7) . . ? C242 C243 H24C 121.1 . . ? C244 C243 H24C 121.0 . . ? C243 C244 C245 120.6(7) . . ? C243 C244 H24D 119.7 . . ? C245 C244 H24D 119.7 . . ? N24 C245 C244 121.2(6) . . ? N24 C245 C255 114.0(6) . . ? C244 C245 C255 124.8(6) . . ? N25 C251 C252 121.5(7) . . ? N25 C251 H25A 119.2 . . ? C252 C251 H25A 119.2 . . ? C253 C252 C251 120.2(7) . . ? C253 C252 H25B 119.9 . . ? C251 C252 H25B 119.9 . . ? C252 C253 C254 117.9(7) . . ? C252 C253 H25C 121.0 . . ? C254 C253 H25C 121.0 . . ? C253 C254 C255 120.3(8) . . ? C253 C254 H25D 119.9 . . ? C255 C254 H25D 119.9 . . ? N25 C255 C254 121.1(7) . . ? N25 C255 C245 114.8(6) . . ? C254 C255 C245 124.0(6) . . ? C261 C260 S21 113.7(6) . . ? C261 C260 H26A 108.8 . . ? S21 C260 H26A 108.8 . . ? C261 C260 H26B 108.8 . . ? S21 C260 H26B 108.8 . . ? H26A C260 H26B 107.7 . . ? C262 C261 C266 118.6(8) . . ? C262 C261 C260 121.9(8) . . ? C266 C261 C260 119.5(8) . . ? C263 C262 C261 120.1(8) . . ? C263 C262 H26C 120.0 . . ? C261 C262 H26C 120.0 . . ? C264 C263 C262 121.4(9) . . ? C264 C263 H26D 119.3 . . ? C262 C263 H26D 119.3 . . ? C265 C264 C263 119.6(9) . . ? C265 C264 H26E 120.2 . . ? C263 C264 H26E 120.2 . . ? C264 C265 C266 119.7(9) . . ? C264 C265 H26F 120.2 . . ? C266 C265 H26F 120.2 . . ? C261 C266 C265 120.7(9) . . ? C261 C266 H26G 119.7 . . ? C265 C266 H26G 119.7 . . ? N21 C271 O22 115.8(6) . . ? N21 C271 C216 129.7(6) . . ? O22 C271 C216 114.5(6) . . ? O22 C272 C274 106.0(6) . . ? O22 C272 C273 106.6(5) . . ? C274 C272 C273 110.9(6) . . ? O22 C272 C275 102.6(5) . . ? C274 C272 C275 119.2(6) . . ? C273 C272 C275 110.5(6) . . ? C272 C273 H27A 109.5 . . ? C272 C273 H27B 109.5 . . ? H27A C273 H27B 109.5 . . ? C272 C273 H27C 109.5 . . ? H27A C273 H27C 109.5 . . ? H27B C273 H27C 109.5 . . ? C272 C274 H27D 109.5 . . ? C272 C274 H27E 109.5 . . ? H27D C274 H27E 109.5 . . ? C272 C274 H27F 109.5 . . ? H27D C274 H27F 109.5 . . ? H27E C274 H27F 109.5 . . ? N21 C275 C276 107.1(5) . . ? N21 C275 C272 101.8(5) . . ? C276 C275 C272 116.3(6) . . ? N21 C275 H27G 110.4 . . ? C276 C275 H27G 110.4 . . ? C272 C275 H27G 110.4 . . ? C275 C276 S21 110.7(5) . . ? C275 C276 H27H 109.5 . . ? S21 C276 H27H 109.5 . . ? C275 C276 H27I 109.5 . . ? S21 C276 H27I 109.5 . . ? H27H C276 H27I 108.1 . . ? Cl1B C1S Cl2A 86.3(9) . . ? Cl1B C1S Cl2B 107.5(8) . . ? Cl2A C1S Cl2B 21.2(6) . . ? Cl1B C1S Cl2C 123.8(9) . . ? Cl2A C1S Cl2C 37.7(7) . . ? Cl2B C1S Cl2C 16.5(5) . . ? Cl1B C1S Cl1A 39.5(5) . . ? Cl2A C1S Cl1A 101.1(9) . . ? Cl2B C1S Cl1A 116.6(9) . . ? Cl2C C1S Cl1A 126.9(9) . . ? Cl1B C1S H1SA 119.4 . . ? Cl2A C1S H1SA 34.7 . . ? Cl2B C1S H1SA 14.6 . . ? Cl2C C1S H1SA 7.5 . . ? Cl1A C1S H1SA 119.4 . . ? Cl1B C1S H1SB 119.4 . . ? Cl2A C1S H1SB 138.6 . . ? Cl2B C1S H1SB 123.5 . . ? Cl2C C1S H1SB 110.5 . . ? Cl1A C1S H1SB 119.4 . . ? H1SA C1S H1SB 117.1 . . ? Cl1B Cl1A C1S 59.7(6) . . ? Cl1A Cl1B C1S 80.9(7) . . ? Cl2B Cl2A Cl2C 9.5(17) . . ? Cl2B Cl2A C1S 82.3(19) . . ? Cl2C Cl2A C1S 72.8(10) . . ? Cl2C Cl2B Cl2A 158(4) . . ? Cl2C Cl2B C1S 82(2) . . ? Cl2A Cl2B C1S 76.5(19) . . ? Cl2B Cl2C Cl2A 12(2) . . ? Cl2B Cl2C C1S 82(2) . . ? Cl2A Cl2C C1S 69.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 Ru1 O11 C111 -148.9(6) . . . . ? N15 Ru1 O11 C111 113.6(6) . . . . ? N14 Ru1 O11 C111 148.3(15) . . . . ? N12 Ru1 O11 C111 -68.8(6) . . . . ? N11 Ru1 O11 C111 27.0(6) . . . . ? N13 Ru1 N11 C171 30(2) . . . . ? N15 Ru1 N11 C171 -101.7(6) . . . . ? N14 Ru1 N11 C171 179.6(5) . . . . ? O11 Ru1 N11 C171 -7.1(5) . . . . ? N12 Ru1 N11 C171 75.4(6) . . . . ? N13 Ru1 N11 C175 -157.6(18) . . . . ? N15 Ru1 N11 C175 70.7(5) . . . . ? N14 Ru1 N11 C175 -8.1(5) . . . . ? O11 Ru1 N11 C175 165.3(5) . . . . ? N12 Ru1 N11 C175 -112.2(5) . . . . ? N13 Ru1 N12 C121 -175.8(6) . . . . ? N15 Ru1 N12 C121 137(3) . . . . ? N14 Ru1 N12 C121 -87.9(6) . . . . ? O11 Ru1 N12 C121 96.9(6) . . . . ? N11 Ru1 N12 C121 9.1(6) . . . . ? N13 Ru1 N12 C125 18.6(5) . . . . ? N15 Ru1 N12 C125 -29(4) . . . . ? N14 Ru1 N12 C125 106.5(5) . . . . ? O11 Ru1 N12 C125 -68.7(5) . . . . ? N11 Ru1 N12 C125 -156.5(5) . . . . ? N15 Ru1 N13 C135 162.8(5) . . . . ? N14 Ru1 N13 C135 -118.1(5) . . . . ? O11 Ru1 N13 C135 68.8(5) . . . . ? N12 Ru1 N13 C135 -14.5(5) . . . . ? N11 Ru1 N13 C135 32(2) . . . . ? N15 Ru1 N13 C131 -14.3(7) . . . . ? N14 Ru1 N13 C131 64.8(6) . . . . ? O11 Ru1 N13 C131 -108.3(6) . . . . ? N12 Ru1 N13 C131 168.4(7) . . . . ? N11 Ru1 N13 C131 -145.5(18) . . . . ? N13 Ru1 N14 C141 75.7(6) . . . . ? N15 Ru1 N14 C141 173.6(7) . . . . ? O11 Ru1 N14 C141 138.2(15) . . . . ? N12 Ru1 N14 C141 -3.8(7) . . . . ? N11 Ru1 N14 C141 -100.8(6) . . . . ? N13 Ru1 N14 C145 -101.2(5) . . . . ? N15 Ru1 N14 C145 -3.3(5) . . . . ? O11 Ru1 N14 C145 -38.7(19) . . . . ? N12 Ru1 N14 C145 179.3(5) . . . . ? N11 Ru1 N14 C145 82.2(5) . . . . ? N13 Ru1 N15 C151 -88.6(7) . . . . ? N14 Ru1 N15 C151 -177.5(7) . . . . ? O11 Ru1 N15 C151 -2.1(7) . . . . ? N12 Ru1 N15 C151 -42(4) . . . . ? N11 Ru1 N15 C151 86.3(7) . . . . ? N13 Ru1 N15 C155 92.1(5) . . . . ? N14 Ru1 N15 C155 3.2(5) . . . . ? O11 Ru1 N15 C155 178.6(5) . . . . ? N12 Ru1 N15 C155 139(3) . . . . ? N11 Ru1 N15 C155 -93.0(5) . . . . ? N22 Ru2 O21 C211 -160.4(6) . . . . ? N25 Ru2 O21 C211 100.0(6) . . . . ? N24 Ru2 O21 C211 136.3(13) . . . . ? N23 Ru2 O21 C211 -81.6(6) . . . . ? N21 Ru2 O21 C211 15.2(6) . . . . ? N22 Ru2 N21 C271 37(2) . . . . ? N25 Ru2 N21 C271 -102.0(6) . . . . ? N24 Ru2 N21 C271 180.0(6) . . . . ? O21 Ru2 N21 C271 -7.9(6) . . . . ? N23 Ru2 N21 C271 79.5(6) . . . . ? N22 Ru2 N21 C275 -147(2) . . . . ? N25 Ru2 N21 C275 74.0(5) . . . . ? N24 Ru2 N21 C275 -4.0(5) . . . . ? O21 Ru2 N21 C275 168.1(5) . . . . ? N23 Ru2 N21 C275 -104.5(5) . . . . ? N25 Ru2 N22 C221 2.4(7) . . . . ? N24 Ru2 N22 C221 80.8(6) . . . . ? O21 Ru2 N22 C221 -91.0(6) . . . . ? N23 Ru2 N22 C221 -179.2(7) . . . . ? N21 Ru2 N22 C221 -136(2) . . . . ? N25 Ru2 N22 C225 176.5(5) . . . . ? N24 Ru2 N22 C225 -105.1(5) . . . . ? O21 Ru2 N22 C225 83.1(5) . . . . ? N23 Ru2 N22 C225 -5.1(5) . . . . ? N21 Ru2 N22 C225 38(2) . . . . ? N22 Ru2 N23 C231 179.6(7) . . . . ? N25 Ru2 N23 C231 -132(7) . . . . ? N24 Ru2 N23 C231 -92.7(7) . . . . ? O21 Ru2 N23 C231 93.0(6) . . . . ? N21 Ru2 N23 C231 3.9(7) . . . . ? N22 Ru2 N23 C235 2.4(5) . . . . ? N25 Ru2 N23 C235 51(7) . . . . ? N24 Ru2 N23 C235 90.1(5) . . . . ? O21 Ru2 N23 C235 -84.2(5) . . . . ? N21 Ru2 N23 C235 -173.3(5) . . . . ? N22 Ru2 N24 C245 -100.8(6) . . . . ? N25 Ru2 N24 C245 -0.8(5) . . . . ? O21 Ru2 N24 C245 -37.9(17) . . . . ? N23 Ru2 N24 C245 -179.4(6) . . . . ? N21 Ru2 N24 C245 82.9(6) . . . . ? N22 Ru2 N24 C241 73.4(7) . . . . ? N25 Ru2 N24 C241 173.5(7) . . . . ? O21 Ru2 N24 C241 136.4(12) . . . . ? N23 Ru2 N24 C241 -5.1(7) . . . . ? N21 Ru2 N24 C241 -102.8(7) . . . . ? N22 Ru2 N25 C251 -96.0(7) . . . . ? N24 Ru2 N25 C251 176.3(7) . . . . ? O21 Ru2 N25 C251 -9.2(7) . . . . ? N23 Ru2 N25 C251 -144(6) . . . . ? N21 Ru2 N25 C251 79.8(7) . . . . ? N22 Ru2 N25 C255 91.9(5) . . . . ? N24 Ru2 N25 C255 4.2(5) . . . . ? O21 Ru2 N25 C255 178.7(5) . . . . ? N23 Ru2 N25 C255 44(7) . . . . ? N21 Ru2 N25 C255 -92.3(5) . . . . ? Ru1 O11 C111 C116 -30.3(10) . . . . ? Ru1 O11 C111 C112 153.9(5) . . . . ? O11 C111 C112 C113 176.9(8) . . . . ? C116 C111 C112 C113 0.7(11) . . . . ? C111 C112 C113 C114 -2.5(14) . . . . ? C112 C113 C114 C115 3.1(15) . . . . ? C113 C114 C115 C116 -2.0(13) . . . . ? C114 C115 C116 C111 0.3(12) . . . . ? C114 C115 C116 C171 179.3(7) . . . . ? O11 C111 C116 C115 -175.4(7) . . . . ? C112 C111 C116 C115 0.4(11) . . . . ? O11 C111 C116 C171 5.6(12) . . . . ? C112 C111 C116 C171 -178.6(7) . . . . ? C125 N12 C121 C122 2.3(11) . . . . ? Ru1 N12 C121 C122 -162.5(6) . . . . ? N12 C121 C122 C123 0.1(11) . . . . ? C121 C122 C123 C124 -0.8(12) . . . . ? C122 C123 C124 C125 -0.8(11) . . . . ? C121 N12 C125 C124 -4.0(10) . . . . ? Ru1 N12 C125 C124 163.0(5) . . . . ? C121 N12 C125 C135 173.2(6) . . . . ? Ru1 N12 C125 C135 -19.8(7) . . . . ? C123 C124 C125 N12 3.2(10) . . . . ? C123 C124 C125 C135 -173.7(7) . . . . ? C135 N13 C131 C132 0.6(12) . . . . ? Ru1 N13 C131 C132 177.6(7) . . . . ? N13 C131 C132 C133 -1.0(14) . . . . ? C131 C132 C133 C134 0.1(13) . . . . ? C132 C133 C134 C135 1.0(12) . . . . ? C131 N13 C135 C134 0.7(10) . . . . ? Ru1 N13 C135 C134 -176.8(6) . . . . ? C131 N13 C135 C125 -174.5(6) . . . . ? Ru1 N13 C135 C125 8.0(7) . . . . ? C133 C134 C135 N13 -1.5(12) . . . . ? C133 C134 C135 C125 173.3(7) . . . . ? N12 C125 C135 N13 8.1(9) . . . . ? C124 C125 C135 N13 -174.8(6) . . . . ? N12 C125 C135 C134 -167.1(7) . . . . ? C124 C125 C135 C134 10.0(11) . . . . ? C145 N14 C141 C142 -1.2(11) . . . . ? Ru1 N14 C141 C142 -178.0(5) . . . . ? N14 C141 C142 C143 -0.8(12) . . . . ? C141 C142 C143 C144 1.6(13) . . . . ? C142 C143 C144 C145 -0.4(13) . . . . ? C141 N14 C145 C144 2.4(10) . . . . ? Ru1 N14 C145 C144 179.6(5) . . . . ? C141 N14 C145 C155 -174.2(7) . . . . ? Ru1 N14 C145 C155 3.1(8) . . . . ? C143 C144 C145 N14 -1.6(12) . . . . ? C143 C144 C145 C155 174.5(8) . . . . ? C155 N15 C151 C152 -0.5(12) . . . . ? Ru1 N15 C151 C152 -179.8(6) . . . . ? N15 C151 C152 C153 0.1(14) . . . . ? C151 C152 C153 C154 0.6(14) . . . . ? C152 C153 C154 C155 -0.8(14) . . . . ? C151 N15 C155 C154 0.3(11) . . . . ? Ru1 N15 C155 C154 179.6(6) . . . . ? C151 N15 C155 C145 178.2(7) . . . . ? Ru1 N15 C155 C145 -2.4(8) . . . . ? C153 C154 C155 N15 0.3(13) . . . . ? C153 C154 C155 C145 -177.4(8) . . . . ? N14 C145 C155 N15 -0.4(10) . . . . ? C144 C145 C155 N15 -176.8(6) . . . . ? N14 C145 C155 C154 177.4(6) . . . . ? C144 C145 C155 C154 1.1(13) . . . . ? C176 S11 C160 C161 -78.4(6) . . . . ? S11 C160 C161 C162 -78.0(9) . . . . ? S11 C160 C161 C166 102.1(8) . . . . ? C166 C161 C162 C163 -0.1(11) . . . . ? C160 C161 C162 C163 180.0(7) . . . . ? C161 C162 C163 C164 0.5(12) . . . . ? C162 C163 C164 C165 -0.8(12) . . . . ? C163 C164 C165 C166 0.7(13) . . . . ? C164 C165 C166 C161 -0.4(12) . . . . ? C162 C161 C166 C165 0.0(11) . . . . ? C160 C161 C166 C165 180.0(7) . . . . ? C175 N11 C171 O12 -3.8(8) . . . . ? Ru1 N11 C171 O12 169.9(5) . . . . ? C175 N11 C171 C116 174.6(7) . . . . ? Ru1 N11 C171 C116 -11.7(10) . . . . ? C172 O12 C171 N11 -13.3(8) . . . . ? C172 O12 C171 C116 168.1(6) . . . . ? C115 C116 C171 N11 -161.6(7) . . . . ? C111 C116 C171 N11 17.4(11) . . . . ? C115 C116 C171 O12 16.8(10) . . . . ? C111 C116 C171 O12 -164.2(7) . . . . ? C171 O12 C172 C173 -94.3(7) . . . . ? C171 O12 C172 C174 146.2(6) . . . . ? C171 O12 C172 C175 23.0(7) . . . . ? C171 N11 C175 C176 -109.1(6) . . . . ? Ru1 N11 C175 C176 77.5(7) . . . . ? C171 N11 C175 C172 17.8(7) . . . . ? Ru1 N11 C175 C172 -155.7(5) . . . . ? O12 C172 C175 N11 -24.1(6) . . . . ? C173 C172 C175 N11 90.1(7) . . . . ? C174 C172 C175 N11 -139.7(7) . . . . ? O12 C172 C175 C176 95.9(7) . . . . ? C173 C172 C175 C176 -149.9(7) . . . . ? C174 C172 C175 C176 -19.8(10) . . . . ? N11 C175 C176 S11 -164.3(4) . . . . ? C172 C175 C176 S11 79.6(7) . . . . ? C160 S11 C176 C175 -175.2(5) . . . . ? Ru2 O21 C211 C216 -10.2(10) . . . . ? Ru2 O21 C211 C212 169.0(4) . . . . ? O21 C211 C212 C213 -176.2(7) . . . . ? C216 C211 C212 C213 3.1(10) . . . . ? C211 C212 C213 C214 -1.8(11) . . . . ? C212 C213 C214 C215 -0.3(12) . . . . ? C213 C214 C215 C216 1.0(12) . . . . ? C214 C215 C216 C211 0.4(11) . . . . ? C214 C215 C216 C271 -175.9(7) . . . . ? O21 C211 C216 C215 176.8(7) . . . . ? C212 C211 C216 C215 -2.4(10) . . . . ? O21 C211 C216 C271 -6.8(11) . . . . ? C212 C211 C216 C271 173.9(6) . . . . ? C225 N22 C221 C222 0.2(12) . . . . ? Ru2 N22 C221 C222 174.2(7) . . . . ? N22 C221 C222 C223 -1.2(14) . . . . ? C221 C222 C223 C224 2.2(14) . . . . ? C222 C223 C224 C225 -2.2(14) . . . . ? C221 N22 C225 C224 -0.3(11) . . . . ? Ru2 N22 C225 C224 -174.8(6) . . . . ? C221 N22 C225 C235 -178.5(7) . . . . ? Ru2 N22 C225 C235 7.0(9) . . . . ? C223 C224 C225 N22 1.3(13) . . . . ? C223 C224 C225 C235 179.3(8) . . . . ? C235 N23 C231 C232 -0.5(12) . . . . ? Ru2 N23 C231 C232 -177.6(6) . . . . ? N23 C231 C232 C233 -1.6(14) . . . . ? C231 C232 C233 C234 0.6(14) . . . . ? C232 C233 C234 C235 2.4(15) . . . . ? C231 N23 C235 C234 3.5(11) . . . . ? Ru2 N23 C235 C234 -179.0(6) . . . . ? C231 N23 C235 C225 -176.9(7) . . . . ? Ru2 N23 C235 C225 0.5(8) . . . . ? C233 C234 C235 N23 -4.5(13) . . . . ? C233 C234 C235 C225 176.0(8) . . . . ? N22 C225 C235 N23 -4.9(10) . . . . ? C224 C225 C235 N23 177.0(7) . . . . ? N22 C225 C235 C234 174.6(8) . . . . ? C224 C225 C235 C234 -3.5(13) . . . . ? C245 N24 C241 C242 -0.5(12) . . . . ? Ru2 N24 C241 C242 -174.7(6) . . . . ? N24 C241 C242 C243 -0.9(13) . . . . ? C241 C242 C243 C244 1.2(13) . . . . ? C242 C243 C244 C245 -0.1(13) . . . . ? C241 N24 C245 C244 1.5(12) . . . . ? Ru2 N24 C245 C244 176.4(6) . . . . ? C241 N24 C245 C255 -177.3(7) . . . . ? Ru2 N24 C245 C255 -2.5(9) . . . . ? C243 C244 C245 N24 -1.3(13) . . . . ? C243 C244 C245 C255 177.5(8) . . . . ? C255 N25 C251 C252 -1.2(12) . . . . ? Ru2 N25 C251 C252 -173.1(5) . . . . ? N25 C251 C252 C253 0.9(13) . . . . ? C251 C252 C253 C254 -1.0(13) . . . . ? C252 C253 C254 C255 1.6(14) . . . . ? C251 N25 C255 C254 1.8(12) . . . . ? Ru2 N25 C255 C254 174.4(6) . . . . ? C251 N25 C255 C245 -179.4(7) . . . . ? Ru2 N25 C255 C245 -6.8(9) . . . . ? C253 C254 C255 N25 -2.0(13) . . . . ? C253 C254 C255 C245 179.2(8) . . . . ? N24 C245 C255 N25 6.1(10) . . . . ? C244 C245 C255 N25 -172.8(7) . . . . ? N24 C245 C255 C254 -175.1(7) . . . . ? C244 C245 C255 C254 6.0(13) . . . . ? C276 S21 C260 C261 -65.4(7) . . . . ? S21 C260 C261 C262 93.0(9) . . . . ? S21 C260 C261 C266 -86.8(8) . . . . ? C266 C261 C262 C263 -0.2(12) . . . . ? C260 C261 C262 C263 -180.0(7) . . . . ? C261 C262 C263 C264 -0.1(12) . . . . ? C262 C263 C264 C265 0.2(13) . . . . ? C263 C264 C265 C266 -0.1(14) . . . . ? C262 C261 C266 C265 0.4(12) . . . . ? C260 C261 C266 C265 -179.9(8) . . . . ? C264 C265 C266 C261 -0.2(14) . . . . ? C275 N21 C271 O22 -0.5(8) . . . . ? Ru2 N21 C271 O22 176.1(4) . . . . ? C275 N21 C271 C216 178.6(7) . . . . ? Ru2 N21 C271 C216 -4.8(10) . . . . ? C272 O22 C271 N21 -14.2(8) . . . . ? C272 O22 C271 C216 166.6(5) . . . . ? C215 C216 C271 N21 -168.3(7) . . . . ? C211 C216 C271 N21 15.3(11) . . . . ? C215 C216 C271 O22 10.8(9) . . . . ? C211 C216 C271 O22 -165.6(6) . . . . ? C271 O22 C272 C274 147.2(6) . . . . ? C271 O22 C272 C273 -94.6(6) . . . . ? C271 O22 C272 C275 21.5(6) . . . . ? C271 N21 C275 C276 -108.4(6) . . . . ? Ru2 N21 C275 C276 75.1(7) . . . . ? C271 N21 C275 C272 14.2(7) . . . . ? Ru2 N21 C275 C272 -162.3(4) . . . . ? O22 C272 C275 N21 -21.0(6) . . . . ? C274 C272 C275 N21 -137.6(6) . . . . ? C273 C272 C275 N21 92.3(6) . . . . ? O22 C272 C275 C276 95.0(7) . . . . ? C274 C272 C275 C276 -21.6(9) . . . . ? C273 C272 C275 C276 -151.7(6) . . . . ? N21 C275 C276 S21 -158.7(4) . . . . ? C272 C275 C276 S21 88.3(6) . . . . ? C260 S21 C276 C275 -171.4(5) . . . . ? Cl2A C1S Cl1A Cl1B 70.0(10) . . . . ? Cl2B C1S Cl1A Cl1B 85.4(11) . . . . ? Cl2C C1S Cl1A Cl1B 100.6(12) . . . . ? Cl2A C1S Cl1B Cl1A -112.5(9) . . . . ? Cl2B C1S Cl1B Cl1A -110.9(11) . . . . ? Cl2C C1S Cl1B Cl1A -108.8(12) . . . . ? Cl1B C1S Cl2A Cl2B 176(2) . . . . ? Cl2C C1S Cl2A Cl2B 1(2) . . . . ? Cl1A C1S Cl2A Cl2B 139(2) . . . . ? Cl1B C1S Cl2A Cl2C 175.0(12) . . . . ? Cl2B C1S Cl2A Cl2C -1(2) . . . . ? Cl1A C1S Cl2A Cl2C 138.2(12) . . . . ? C1S Cl2A Cl2B Cl2C -5(13) . . . . ? Cl2C Cl2A Cl2B C1S 5(13) . . . . ? Cl1B C1S Cl2B Cl2C 174(3) . . . . ? Cl2A C1S Cl2B Cl2C 178(5) . . . . ? Cl1A C1S Cl2B Cl2C 132(3) . . . . ? Cl1B C1S Cl2B Cl2A -4(2) . . . . ? Cl2C C1S Cl2B Cl2A -178(5) . . . . ? Cl1A C1S Cl2B Cl2A -46(2) . . . . ? C1S Cl2B Cl2C Cl2A -5(13) . . . . ? Cl2A Cl2B Cl2C C1S 5(13) . . . . ? C1S Cl2A Cl2C Cl2B 175(13) . . . . ? Cl2B Cl2A Cl2C C1S -175(13) . . . . ? Cl1B C1S Cl2C Cl2B -7(4) . . . . ? Cl2A C1S Cl2C Cl2B -1(3) . . . . ? Cl1A C1S Cl2C Cl2B -56(3) . . . . ? Cl1B C1S Cl2C Cl2A -6.1(15) . . . . ? Cl2B C1S Cl2C Cl2A 1(3) . . . . ? Cl1A C1S Cl2C Cl2A -54.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.774 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.103 data_dxb _database_code_depnum_ccdc_archive 'CCDC 917694' #TrackingRef 'complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety OsSO2N5BC57H52 _chemical_formula_sum 'C57 H52 B N5 O2 Os S' _chemical_formula_weight 1072.11 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4352(19) _cell_length_b 19.433(4) _cell_length_c 25.513(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4677.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 2.821 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5056 _exptl_absorpt_correction_T_max 0.6307 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36663 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9190 _reflns_number_gt 8596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration rmad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(7) _refine_ls_number_reflns 9190 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.13659(2) 0.534367(10) 0.107286(8) 0.01837(6) Uani 1 1 d . . . S1 S 0.51823(15) 0.46456(10) -0.03375(6) 0.0351(3) Uani 1 1 d . . . O1 O -0.0604(3) 0.57901(18) 0.10197(15) 0.0229(8) Uani 1 1 d . . . O2 O 0.1488(4) 0.62972(19) -0.04184(14) 0.0285(9) Uani 1 1 d . . . N1 N 0.1747(4) 0.5650(2) 0.02972(16) 0.0185(10) Uani 1 1 d . . . N2 N 0.3341(5) 0.4988(2) 0.12611(16) 0.0195(11) Uani 1 1 d . . . N3 N 0.2365(5) 0.6231(2) 0.12874(17) 0.0189(10) Uani 1 1 d . . . N4 N 0.0764(5) 0.5007(2) 0.18017(17) 0.0200(10) Uani 1 1 d . . . N5 N 0.0318(4) 0.4453(2) 0.08914(16) 0.0162(10) Uani 1 1 d . . . C11 C -0.1129(6) 0.6178(3) 0.0652(2) 0.0213(12) Uani 1 1 d . . . C12 C -0.2464(6) 0.6476(3) 0.0742(2) 0.0286(14) Uani 1 1 d . . . H12A H -0.2929 0.6387 0.1065 0.034 Uiso 1 1 calc R . . C13 C -0.3112(6) 0.6885(3) 0.0387(2) 0.0342(15) Uani 1 1 d . . . H13A H -0.4019 0.7072 0.0464 0.041 Uiso 1 1 calc R . . C14 C -0.2459(7) 0.7035(3) -0.0092(2) 0.0326(15) Uani 1 1 d . . . H14A H -0.2918 0.7316 -0.0344 0.039 Uiso 1 1 calc R . . C15 C -0.1143(6) 0.6766(3) -0.0189(2) 0.0255(13) Uani 1 1 d . . . H15A H -0.0691 0.6871 -0.0512 0.031 Uiso 1 1 calc R . . C16 C -0.0436(6) 0.6340(3) 0.0172(2) 0.0206(12) Uani 1 1 d . . . C21 C 0.3725(7) 0.4316(3) 0.1291(2) 0.0269(13) Uani 1 1 d . . . H21A H 0.3088 0.3975 0.1167 0.032 Uiso 1 1 calc R . . C22 C 0.5005(6) 0.4112(3) 0.1496(2) 0.0277(14) Uani 1 1 d . . . H22A H 0.5240 0.3638 0.1513 0.033 Uiso 1 1 calc R . . C23 C 0.5950(6) 0.4602(3) 0.1677(2) 0.0333(14) Uani 1 1 d . . . H23A H 0.6850 0.4469 0.1809 0.040 Uiso 1 1 calc R . . C24 C 0.5570(6) 0.5275(3) 0.1661(2) 0.0272(13) Uani 1 1 d . . . H24A H 0.6195 0.5617 0.1794 0.033 Uiso 1 1 calc R . . C25 C 0.4274(6) 0.5465(3) 0.14528(19) 0.0202(12) Uani 1 1 d . . . C31 C 0.1766(6) 0.6861(3) 0.1281(2) 0.0256(14) Uani 1 1 d . . . H31A H 0.0795 0.6902 0.1188 0.031 Uiso 1 1 calc R . . C32 C 0.2514(7) 0.7444(3) 0.1406(2) 0.0303(14) Uani 1 1 d . . . H32A H 0.2071 0.7883 0.1391 0.036 Uiso 1 1 calc R . . C33 C 0.3935(6) 0.7386(3) 0.1556(2) 0.0286(14) Uani 1 1 d . . . H33A H 0.4479 0.7784 0.1637 0.034 Uiso 1 1 calc R . . C34 C 0.4521(6) 0.6748(3) 0.1584(2) 0.0229(13) Uani 1 1 d . . . H34A H 0.5468 0.6696 0.1705 0.028 Uiso 1 1 calc R . . C35 C 0.3757(6) 0.6176(3) 0.14397(19) 0.0204(12) Uani 1 1 d . . . C41 C 0.1059(6) 0.5328(3) 0.22543(19) 0.0296(13) Uani 1 1 d . . . H41A H 0.1596 0.5741 0.2246 0.036 Uiso 1 1 calc R . . C42 C 0.0604(8) 0.5074(3) 0.2733(2) 0.0395(17) Uani 1 1 d . . . H42A H 0.0813 0.5315 0.3048 0.047 Uiso 1 1 calc R . . C43 C -0.0143(8) 0.4479(4) 0.2747(3) 0.047(2) Uani 1 1 d . . . H43A H -0.0458 0.4296 0.3072 0.057 Uiso 1 1 calc R . . C44 C -0.0440(7) 0.4142(3) 0.2285(2) 0.0369(16) Uani 1 1 d . . . H44A H -0.0960 0.3724 0.2290 0.044 Uiso 1 1 calc R . . C45 C 0.0018(6) 0.4414(3) 0.1820(2) 0.0231(13) Uani 1 1 d . . . C51 C 0.0034(6) 0.4215(3) 0.0405(2) 0.0228(13) Uani 1 1 d . . . H51A H 0.0427 0.4453 0.0114 0.027 Uiso 1 1 calc R . . C52 C -0.0780(6) 0.3656(3) 0.0312(2) 0.0270(13) Uani 1 1 d . . . H52A H -0.0957 0.3513 -0.0038 0.032 Uiso 1 1 calc R . . C53 C -0.1353(8) 0.3295(3) 0.0726(2) 0.0303(13) Uani 1 1 d . . . H53A H -0.1899 0.2892 0.0666 0.036 Uiso 1 1 calc R . . C54 C -0.1122(6) 0.3527(3) 0.1223(2) 0.0303(14) Uani 1 1 d . . . H54A H -0.1533 0.3294 0.1514 0.036 Uiso 1 1 calc R . . C55 C -0.0280(6) 0.4106(3) 0.1304(2) 0.0232(13) Uani 1 1 d . . . C61 C 0.0953(6) 0.6072(3) 0.00377(19) 0.0211(12) Uani 1 1 d . . . C62 C 0.2823(6) 0.5932(3) -0.0523(2) 0.0282(14) Uani 1 1 d . . . C63 C 0.3083(6) 0.5548(3) 0.0006(2) 0.0229(13) Uani 1 1 d . . . H63A H 0.3868 0.5783 0.0199 0.027 Uiso 1 1 calc R . . C64 C 0.3450(6) 0.4791(3) -0.0052(2) 0.0259(13) Uani 1 1 d . . . H64A H 0.2726 0.4567 -0.0275 0.031 Uiso 1 1 calc R . . H64B H 0.3416 0.4570 0.0297 0.031 Uiso 1 1 calc R . . C65 C 0.6305(8) 0.4859(4) 0.0199(3) 0.055(2) Uani 1 1 d . . . H65A H 0.7297 0.4804 0.0094 0.083 Uiso 1 1 calc R . . H65B H 0.6100 0.4553 0.0495 0.083 Uiso 1 1 calc R . . H65C H 0.6135 0.5337 0.0303 0.083 Uiso 1 1 calc R . . C66 C 0.3962(7) 0.6460(3) -0.0631(3) 0.0417(17) Uani 1 1 d . . . H66A H 0.3766 0.6690 -0.0965 0.063 Uiso 1 1 calc R . . H66B H 0.4886 0.6231 -0.0649 0.063 Uiso 1 1 calc R . . H66C H 0.3974 0.6801 -0.0348 0.063 Uiso 1 1 calc R . . C67 C 0.2500(8) 0.5484(3) -0.0992(2) 0.0450(18) Uani 1 1 d . . . H67A H 0.2355 0.5775 -0.1301 0.067 Uiso 1 1 calc R . . H67B H 0.1640 0.5216 -0.0924 0.067 Uiso 1 1 calc R . . H67C H 0.3296 0.5171 -0.1055 0.067 Uiso 1 1 calc R . . C111 C 0.3907(5) 0.2054(3) 0.1117(2) 0.0224(11) Uani 1 1 d . . . C112 C 0.2479(6) 0.2027(3) 0.0968(2) 0.0302(14) Uani 1 1 d . . . H11A H 0.1869 0.1721 0.1150 0.036 Uiso 1 1 calc R . . C113 C 0.1915(7) 0.2421(3) 0.0573(2) 0.0380(16) Uani 1 1 d . . . H11B H 0.0939 0.2380 0.0487 0.046 Uiso 1 1 calc R . . C114 C 0.2755(8) 0.2873(3) 0.0302(2) 0.0355(16) Uani 1 1 d . . . H11C H 0.2365 0.3145 0.0028 0.043 Uiso 1 1 calc R . . C115 C 0.4163(7) 0.2931(3) 0.0429(2) 0.0320(15) Uani 1 1 d . . . H11D H 0.4753 0.3245 0.0246 0.038 Uiso 1 1 calc R . . C116 C 0.4727(7) 0.2521(3) 0.0833(2) 0.0294(14) Uani 1 1 d . . . H11E H 0.5705 0.2564 0.0916 0.035 Uiso 1 1 calc R . . C121 C 0.4276(6) 0.0771(3) 0.1535(2) 0.0272(13) Uani 1 1 d . . . C122 C 0.3587(6) 0.0466(3) 0.1119(2) 0.0367(13) Uani 1 1 d . . . H12B H 0.3226 0.0749 0.0846 0.044 Uiso 1 1 calc R . . C123 C 0.3402(7) -0.0246(3) 0.1085(3) 0.0495(17) Uani 1 1 d . . . H12C H 0.2932 -0.0441 0.0791 0.059 Uiso 1 1 calc R . . C124 C 0.3904(8) -0.0662(3) 0.1479(3) 0.051(2) Uani 1 1 d . . . H12D H 0.3761 -0.1146 0.1463 0.061 Uiso 1 1 calc R . . C125 C 0.4610(7) -0.0379(4) 0.1895(3) 0.0435(16) Uani 1 1 d . . . H12E H 0.4966 -0.0664 0.2168 0.052 Uiso 1 1 calc R . . C126 C 0.4800(6) 0.0319(3) 0.1916(2) 0.0338(13) Uani 1 1 d . . . H12F H 0.5311 0.0507 0.2203 0.041 Uiso 1 1 calc R . . C131 C 0.3511(6) 0.1868(3) 0.2127(2) 0.0239(12) Uani 1 1 d . . . C132 C 0.3514(7) 0.2559(3) 0.2266(2) 0.0331(14) Uani 1 1 d . . . H13B H 0.4100 0.2869 0.2076 0.040 Uiso 1 1 calc R . . C133 C 0.2688(7) 0.2813(4) 0.2674(3) 0.0417(17) Uani 1 1 d . . . H13C H 0.2712 0.3289 0.2758 0.050 Uiso 1 1 calc R . . C134 C 0.1833(7) 0.2373(4) 0.2957(3) 0.0383(16) Uani 1 1 d . . . H13D H 0.1274 0.2540 0.3239 0.046 Uiso 1 1 calc R . . C135 C 0.1805(6) 0.1687(3) 0.2823(2) 0.0313(14) Uani 1 1 d . . . H13E H 0.1215 0.1379 0.3013 0.038 Uiso 1 1 calc R . . C136 C 0.2630(6) 0.1442(3) 0.2413(2) 0.0264(13) Uani 1 1 d . . . H13F H 0.2588 0.0967 0.2327 0.032 Uiso 1 1 calc R . . C141 C 0.6191(6) 0.1741(3) 0.1703(2) 0.0270(13) Uani 1 1 d . . . C142 C 0.7155(6) 0.1512(3) 0.1323(2) 0.0319(14) Uani 1 1 d . . . H14B H 0.6796 0.1290 0.1019 0.038 Uiso 1 1 calc R . . C143 C 0.8591(7) 0.1595(3) 0.1370(2) 0.0347(14) Uani 1 1 d . . . H14C H 0.9196 0.1437 0.1097 0.042 Uiso 1 1 calc R . . C144 C 0.9175(7) 0.1905(3) 0.1808(3) 0.0347(15) Uani 1 1 d . . . H14D H 1.0171 0.1962 0.1843 0.042 Uiso 1 1 calc R . . C145 C 0.8263(7) 0.2126(3) 0.2188(2) 0.0342(16) Uani 1 1 d . . . H14E H 0.8633 0.2333 0.2496 0.041 Uiso 1 1 calc R . . C146 C 0.6795(6) 0.2054(3) 0.2132(2) 0.0326(15) Uani 1 1 d . . . H14F H 0.6194 0.2228 0.2400 0.039 Uiso 1 1 calc R . . B1 B 0.4482(7) 0.1604(4) 0.1615(3) 0.0266(15) 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 Os1 0.02036(9) 0.01913(9) 0.01562(9) -0.00027(9) -0.00084(9) 0.00009(9) S1 0.0306(8) 0.0427(9) 0.0321(8) -0.0065(8) 0.0075(6) 0.0075(8) O1 0.0164(18) 0.032(2) 0.020(2) 0.0016(18) 0.0020(18) 0.0069(15) O2 0.028(2) 0.035(2) 0.023(2) 0.0085(16) 0.0063(19) 0.000(2) N1 0.022(3) 0.022(2) 0.011(2) 0.0036(18) 0.0026(18) -0.0004(18) N2 0.017(3) 0.027(2) 0.014(2) 0.0010(19) -0.0034(17) 0.003(2) N3 0.021(2) 0.018(2) 0.017(2) -0.0050(18) -0.0025(19) -0.0077(19) N4 0.024(2) 0.023(2) 0.013(2) 0.0085(19) 0.006(2) 0.002(2) N5 0.013(2) 0.014(2) 0.022(2) -0.0016(16) -0.0040(17) 0.0002(16) C11 0.023(3) 0.025(3) 0.017(3) -0.002(2) -0.002(2) 0.003(2) C12 0.027(3) 0.036(4) 0.023(3) 0.004(3) 0.005(3) 0.002(3) C13 0.024(3) 0.041(4) 0.038(4) 0.000(3) 0.000(3) 0.012(3) C14 0.036(4) 0.035(4) 0.027(3) 0.004(3) -0.006(3) 0.012(3) C15 0.031(4) 0.026(3) 0.020(3) 0.006(2) 0.005(3) 0.001(3) C16 0.022(3) 0.021(3) 0.019(3) 0.002(2) 0.000(2) 0.000(2) C21 0.036(3) 0.024(3) 0.021(3) -0.003(2) 0.001(3) 0.001(3) C22 0.031(4) 0.028(3) 0.024(3) 0.000(3) 0.004(3) 0.003(3) C23 0.028(3) 0.040(4) 0.032(3) 0.001(3) -0.005(2) 0.011(3) C24 0.030(3) 0.030(3) 0.022(3) -0.005(3) -0.005(2) -0.004(3) C25 0.024(3) 0.026(3) 0.011(2) 0.000(2) 0.001(2) 0.003(2) C31 0.036(4) 0.015(3) 0.026(3) 0.000(2) 0.003(2) 0.002(2) C32 0.045(4) 0.019(3) 0.027(3) 0.000(3) 0.000(3) 0.004(3) C33 0.038(4) 0.025(3) 0.024(3) 0.000(2) 0.003(3) -0.007(3) C34 0.025(3) 0.021(3) 0.023(3) 0.002(2) -0.003(2) -0.003(2) C35 0.024(3) 0.021(3) 0.016(2) -0.004(2) 0.002(2) -0.002(3) C41 0.040(4) 0.032(3) 0.017(3) 0.000(3) -0.006(2) -0.001(3) C42 0.060(5) 0.043(4) 0.015(3) 0.002(3) -0.002(3) -0.006(3) C43 0.068(5) 0.053(5) 0.020(3) 0.011(3) -0.001(3) -0.015(4) C44 0.052(4) 0.029(4) 0.029(3) 0.005(3) 0.003(3) -0.007(3) C45 0.025(3) 0.026(3) 0.019(3) 0.002(2) 0.002(2) -0.001(2) C51 0.024(3) 0.021(3) 0.024(3) -0.003(2) 0.001(2) -0.004(2) C52 0.024(3) 0.032(3) 0.024(3) -0.007(3) -0.004(3) 0.003(3) C53 0.029(3) 0.028(3) 0.035(3) -0.004(2) 0.005(3) -0.005(3) C54 0.027(4) 0.028(3) 0.036(4) 0.003(2) 0.010(3) -0.006(3) C55 0.020(3) 0.027(3) 0.023(3) -0.001(2) 0.009(2) 0.004(2) C61 0.028(3) 0.020(3) 0.015(3) -0.002(2) 0.002(2) -0.002(2) C62 0.022(3) 0.041(4) 0.021(3) 0.004(3) 0.002(2) 0.001(3) C63 0.023(3) 0.032(3) 0.014(3) -0.001(2) 0.003(2) 0.000(2) C64 0.024(3) 0.030(3) 0.023(3) -0.004(2) 0.004(2) -0.004(3) C65 0.032(4) 0.080(6) 0.055(4) -0.016(4) 0.007(4) 0.009(4) C66 0.032(4) 0.048(4) 0.045(4) 0.017(3) 0.009(3) 0.000(3) C67 0.055(4) 0.060(5) 0.020(3) -0.007(3) -0.008(3) 0.013(3) C111 0.026(3) 0.023(3) 0.018(3) -0.009(2) 0.004(3) 0.003(2) C112 0.029(3) 0.031(3) 0.031(4) -0.005(3) 0.006(3) -0.002(3) C113 0.033(4) 0.044(4) 0.038(4) -0.012(3) -0.008(3) 0.015(3) C114 0.056(5) 0.031(4) 0.019(3) -0.004(3) -0.009(3) 0.019(3) C115 0.047(4) 0.028(3) 0.021(3) 0.003(3) 0.007(3) 0.005(3) C116 0.033(3) 0.025(3) 0.030(3) -0.004(3) -0.001(3) 0.005(3) C121 0.026(3) 0.030(3) 0.026(3) 0.001(3) 0.006(3) 0.004(3) C122 0.037(3) 0.034(3) 0.039(3) 0.003(3) -0.004(4) 0.000(3) C123 0.046(4) 0.032(4) 0.071(5) -0.007(4) -0.010(4) -0.003(3) C124 0.048(5) 0.023(3) 0.080(6) -0.001(4) 0.005(4) 0.003(3) C125 0.047(4) 0.035(4) 0.049(4) 0.014(4) 0.010(3) 0.012(4) C126 0.040(3) 0.030(3) 0.031(3) 0.005(3) 0.005(3) 0.004(3) C131 0.016(3) 0.032(3) 0.023(3) 0.004(2) -0.007(3) 0.001(3) C132 0.041(4) 0.028(3) 0.031(3) 0.002(2) 0.007(3) -0.005(3) C133 0.043(4) 0.038(4) 0.044(4) -0.012(3) 0.000(3) 0.010(3) C134 0.028(4) 0.051(4) 0.035(4) -0.008(3) 0.002(3) 0.007(3) C135 0.023(3) 0.047(4) 0.023(3) 0.001(3) -0.002(2) -0.002(3) C136 0.018(3) 0.036(3) 0.025(3) -0.004(3) -0.005(2) -0.001(3) C141 0.033(3) 0.025(3) 0.023(3) 0.008(2) 0.002(3) 0.002(3) C142 0.033(4) 0.029(3) 0.034(3) -0.002(3) 0.001(3) 0.007(3) C143 0.027(3) 0.035(3) 0.042(4) 0.004(3) 0.008(3) 0.001(3) C144 0.026(3) 0.038(4) 0.040(4) 0.011(3) -0.002(3) -0.003(3) C145 0.036(4) 0.044(4) 0.023(3) 0.007(3) -0.007(3) -0.010(3) C146 0.034(4) 0.044(4) 0.020(3) 0.005(3) 0.003(3) -0.004(3) B1 0.031(4) 0.029(4) 0.020(3) 0.004(3) -0.001(3) -0.002(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 Os1 N3 2.041(4) . ? Os1 N2 2.045(4) . ? Os1 N5 2.047(4) . ? Os1 N4 2.051(4) . ? Os1 O1 2.056(3) . ? Os1 N1 2.098(4) . ? S1 C65 1.779(7) . ? S1 C64 1.811(6) . ? O1 C11 1.301(6) . ? O2 C61 1.341(6) . ? O2 C62 1.470(7) . ? N1 C61 1.293(6) . ? N1 C63 1.477(7) . ? N2 C21 1.359(7) . ? N2 C25 1.368(7) . ? N3 C31 1.347(7) . ? N3 C35 1.374(7) . ? N4 C41 1.342(7) . ? N4 C45 1.351(7) . ? N5 C51 1.351(7) . ? N5 C55 1.371(7) . ? C11 C12 1.406(8) . ? C11 C16 1.424(7) . ? C12 C13 1.349(8) . ? C13 C14 1.399(8) . ? C14 C15 1.370(8) . ? C15 C16 1.405(7) . ? C16 C61 1.452(7) . ? C21 C22 1.374(9) . ? C22 C23 1.383(8) . ? C23 C24 1.356(8) . ? C24 C25 1.384(7) . ? C25 C35 1.466(7) . ? C31 C32 1.373(7) . ? C32 C33 1.399(8) . ? C33 C34 1.360(8) . ? C34 C35 1.374(7) . ? C41 C42 1.385(8) . ? C42 C43 1.355(9) . ? C43 C44 1.375(9) . ? C44 C45 1.371(8) . ? C45 C55 1.473(8) . ? C51 C52 1.351(7) . ? C52 C53 1.379(8) . ? C53 C54 1.365(8) . ? C54 C55 1.392(8) . ? C62 C67 1.511(8) . ? C62 C66 1.511(8) . ? C62 C63 1.562(7) . ? C63 C64 1.518(7) . ? C111 C116 1.396(8) . ? C111 C112 1.400(8) . ? C111 B1 1.635(8) . ? C112 C113 1.372(8) . ? C113 C114 1.371(9) . ? C114 C115 1.372(9) . ? C115 C116 1.406(8) . ? C121 C122 1.379(8) . ? C121 C126 1.400(8) . ? C121 B1 1.643(9) . ? C122 C123 1.396(8) . ? C123 C124 1.375(10) . ? C124 C125 1.369(10) . ? C125 C126 1.370(9) . ? C131 C136 1.383(8) . ? C131 C132 1.390(8) . ? C131 B1 1.676(9) . ? C132 C133 1.390(8) . ? C133 C134 1.379(9) . ? C134 C135 1.375(9) . ? C135 C136 1.388(8) . ? C141 C146 1.375(8) . ? C141 C142 1.403(8) . ? C141 B1 1.650(9) . ? C142 C143 1.370(9) . ? C143 C144 1.384(9) . ? C144 C145 1.365(9) . ? C145 C146 1.400(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 N3 Os1 N2 78.55(18) . . ? N3 Os1 N5 177.30(17) . . ? N2 Os1 N5 101.99(17) . . ? N3 Os1 N4 98.87(18) . . ? N2 Os1 N4 86.08(17) . . ? N5 Os1 N4 78.55(17) . . ? N3 Os1 O1 94.50(16) . . ? N2 Os1 O1 169.16(16) . . ? N5 Os1 O1 84.57(15) . . ? N4 Os1 O1 86.81(16) . . ? N3 Os1 N1 86.20(17) . . ? N2 Os1 N1 99.28(17) . . ? N5 Os1 N1 96.30(17) . . ? N4 Os1 N1 173.30(18) . . ? O1 Os1 N1 88.44(16) . . ? C65 S1 C64 101.1(3) . . ? C11 O1 Os1 129.5(3) . . ? C61 O2 C62 108.8(4) . . ? C61 N1 C63 108.8(4) . . ? C61 N1 Os1 124.3(3) . . ? C63 N1 Os1 125.6(3) . . ? C21 N2 C25 117.3(5) . . ? C21 N2 Os1 125.5(4) . . ? C25 N2 Os1 116.2(3) . . ? C31 N3 C35 118.4(4) . . ? C31 N3 Os1 124.8(4) . . ? C35 N3 Os1 116.8(3) . . ? C41 N4 C45 118.4(5) . . ? C41 N4 Os1 125.1(4) . . ? C45 N4 Os1 116.5(4) . . ? C51 N5 C55 117.1(4) . . ? C51 N5 Os1 126.3(4) . . ? C55 N5 Os1 116.2(3) . . ? O1 C11 C12 117.6(5) . . ? O1 C11 C16 125.1(5) . . ? C12 C11 C16 117.4(5) . . ? C13 C12 C11 122.7(6) . . ? C12 C13 C14 120.5(6) . . ? C15 C14 C13 118.6(5) . . ? C14 C15 C16 122.4(5) . . ? C15 C16 C11 118.4(5) . . ? C15 C16 C61 119.0(5) . . ? C11 C16 C61 122.5(5) . . ? N2 C21 C22 122.2(6) . . ? C21 C22 C23 119.7(6) . . ? C24 C23 C22 118.9(5) . . ? C23 C24 C25 120.1(5) . . ? N2 C25 C24 121.7(5) . . ? N2 C25 C35 114.6(5) . . ? C24 C25 C35 123.6(5) . . ? N3 C31 C32 122.1(5) . . ? C31 C32 C33 119.3(5) . . ? C34 C33 C32 118.5(5) . . ? C33 C34 C35 120.7(5) . . ? C34 C35 N3 120.9(5) . . ? C34 C35 C25 125.5(5) . . ? N3 C35 C25 113.5(5) . . ? N4 C41 C42 121.9(6) . . ? C43 C42 C41 119.2(6) . . ? C42 C43 C44 119.3(6) . . ? C45 C44 C43 119.6(6) . . ? N4 C45 C44 121.5(5) . . ? N4 C45 C55 114.6(5) . . ? C44 C45 C55 123.9(5) . . ? N5 C51 C52 123.3(5) . . ? C51 C52 C53 119.9(5) . . ? C54 C53 C52 118.8(5) . . ? C53 C54 C55 119.7(5) . . ? N5 C55 C54 121.3(5) . . ? N5 C55 C45 114.0(5) . . ? C54 C55 C45 124.7(5) . . ? N1 C61 O2 115.7(5) . . ? N1 C61 C16 129.1(5) . . ? O2 C61 C16 115.3(5) . . ? O2 C62 C67 104.4(5) . . ? O2 C62 C66 108.4(5) . . ? C67 C62 C66 113.0(5) . . ? O2 C62 C63 102.0(4) . . ? C67 C62 C63 116.1(5) . . ? C66 C62 C63 111.8(5) . . ? N1 C63 C64 112.0(4) . . ? N1 C63 C62 103.6(4) . . ? C64 C63 C62 114.5(5) . . ? C63 C64 S1 113.3(4) . . ? C116 C111 C112 114.7(5) . . ? C116 C111 B1 124.5(5) . . ? C112 C111 B1 120.7(5) . . ? C113 C112 C111 123.4(6) . . ? C114 C113 C112 120.3(6) . . ? C113 C114 C115 119.5(6) . . ? C114 C115 C116 119.6(6) . . ? C111 C116 C115 122.6(6) . . ? C122 C121 C126 115.6(5) . . ? C122 C121 B1 125.1(5) . . ? C126 C121 B1 119.3(6) . . ? C121 C122 C123 122.2(6) . . ? C124 C123 C122 119.6(7) . . ? C125 C124 C123 119.9(6) . . ? C124 C125 C126 119.5(6) . . ? C125 C126 C121 123.2(6) . . ? C136 C131 C132 116.4(5) . . ? C136 C131 B1 123.9(5) . . ? C132 C131 B1 119.6(5) . . ? C131 C132 C133 122.2(6) . . ? C134 C133 C132 120.0(6) . . ? C135 C134 C133 118.8(6) . . ? C134 C135 C136 120.6(6) . . ? C131 C136 C135 122.0(6) . . ? C146 C141 C142 115.0(6) . . ? C146 C141 B1 125.8(5) . . ? C142 C141 B1 119.2(5) . . ? C143 C142 C141 122.9(6) . . ? C142 C143 C144 121.1(6) . . ? C145 C144 C143 117.3(6) . . ? C144 C145 C146 121.4(6) . . ? C141 C146 C145 122.3(6) . . ? C111 B1 C121 113.0(5) . . ? C111 B1 C141 110.1(5) . . ? C121 B1 C141 107.0(5) . . ? C111 B1 C131 105.1(5) . . ? C121 B1 C131 109.5(5) . . ? C141 B1 C131 112.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.698 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.116