# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2170 data_s9723 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H H50 B Cl2 F3 N P4 Ru' _chemical_formula_weight 1077.62 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' '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' '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 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 12.2534(19) _cell_length_b 22.046(3) _cell_length_c 19.251(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.157(13) _cell_angle_gamma 90.00 _cell_volume 4941.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 12.42 _cell_measurement_theta_max 12.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7810 _exptl_absorpt_correction_T_max 0.7984 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1997)' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.51 _diffrn_reflns_number 12465 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.00 _reflns_number_total 11926 _reflns_number_gt 9116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0595P)^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 11926 _refine_ls_number_parameters 600 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.816125(16) 0.243218(8) 0.130978(10) 0.01528(6) Uani 1 1 d . . . H1RU H 0.788(3) 0.2188(14) 0.2056(17) 0.030(8) Uiso 1 1 d . . . P1 P 0.98003(5) 0.18501(3) 0.18511(3) 0.01783(13) Uani 1 1 d . . . P2 P 0.92500(5) 0.31942(3) 0.20686(3) 0.01744(13) Uani 1 1 d . . . P3 P 0.70308(5) 0.16558(3) 0.06298(3) 0.01785(13) Uani 1 1 d . . . P4 P 0.64161(5) 0.29738(3) 0.08897(3) 0.01732(13) Uani 1 1 d . . . F1 F 0.99522(18) 0.26153(12) -0.08878(11) 0.0584(6) Uani 1 1 d . . . F2 F 0.8674(2) 0.33835(11) -0.11705(12) 0.0657(7) Uani 1 1 d . . . F3 F 0.80656(17) 0.24200(10) -0.13931(10) 0.0476(5) Uani 1 1 d . . . N1 N 0.8724(2) 0.27478(11) -0.01535(12) 0.0269(5) Uani 1 1 d . . . C1 C 1.0511(2) 0.21861(12) 0.27526(13) 0.0213(5) Uani 1 1 d . . . H1A H 1.0051 0.2108 0.3084 0.026 Uiso 1 1 calc R . . H1B H 1.1279 0.2002 0.2969 0.026 Uiso 1 1 calc R . . C2 C 1.0628(2) 0.28641(11) 0.26603(14) 0.0218(5) Uani 1 1 d . . . H2A H 1.1242 0.2942 0.2437 0.026 Uiso 1 1 calc R . . H2B H 1.0850 0.3063 0.3145 0.026 Uiso 1 1 calc R . . C3 C 0.5962(2) 0.20316(11) -0.01416(13) 0.0217(5) Uani 1 1 d . . . H3A H 0.6344 0.2229 -0.0466 0.026 Uiso 1 1 calc R . . H3B H 0.5401 0.1732 -0.0431 0.026 Uiso 1 1 calc R . . C4 C 0.5358(2) 0.25046(11) 0.01879(14) 0.0218(5) Uani 1 1 d . . . H4A H 0.4838 0.2298 0.0416 0.026 Uiso 1 1 calc R . . H4B H 0.4887 0.2772 -0.0205 0.026 Uiso 1 1 calc R . . C5 C 0.8553(2) 0.26509(11) 0.03943(14) 0.0206(5) Uani 1 1 d . . . C11 C 1.0922(2) 0.18177(11) 0.14117(13) 0.0196(5) Uani 1 1 d . . . C12 C 1.0610(2) 0.16536(12) 0.06771(14) 0.0243(5) Uani 1 1 d . . . H12A H 0.9827 0.1570 0.0420 0.029 Uiso 1 1 calc R . . C13 C 1.1426(2) 0.16098(13) 0.03147(15) 0.0286(6) Uani 1 1 d . . . H13A H 1.1205 0.1491 -0.0184 0.034 Uiso 1 1 calc R . . C14 C 1.2569(3) 0.17404(13) 0.06865(17) 0.0317(6) Uani 1 1 d . . . H14A H 1.3130 0.1713 0.0441 0.038 Uiso 1 1 calc R . . C15 C 1.2890(2) 0.19104(14) 0.14110(18) 0.0335(7) Uani 1 1 d . . . H15A H 1.3670 0.2004 0.1661 0.040 Uiso 1 1 calc R . . C16 C 1.2076(2) 0.19455(13) 0.17793(15) 0.0274(6) Uani 1 1 d . . . H16A H 1.2306 0.2056 0.2281 0.033 Uiso 1 1 calc R . . C21 C 0.9712(2) 0.10591(11) 0.21308(13) 0.0215(5) Uani 1 1 d . . . C22 C 1.0452(2) 0.06081(12) 0.20445(15) 0.0268(6) Uani 1 1 d . . . H22A H 1.1024 0.0701 0.1823 0.032 Uiso 1 1 calc R . . C23 C 1.0355(3) 0.00223(13) 0.22822(17) 0.0344(7) Uani 1 1 d . . . H23A H 1.0859 -0.0285 0.2218 0.041 Uiso 1 1 calc R . . C24 C 0.9530(3) -0.01195(13) 0.26132(17) 0.0336(7) Uani 1 1 d . . . H24A H 0.9459 -0.0523 0.2767 0.040 Uiso 1 1 calc R . . C25 C 0.8814(3) 0.03312(13) 0.27173(16) 0.0319(6) Uani 1 1 d . . . H25A H 0.8262 0.0239 0.2955 0.038 Uiso 1 1 calc R . . C26 C 0.8896(2) 0.09169(12) 0.24773(15) 0.0256(6) Uani 1 1 d . . . H26A H 0.8395 0.1223 0.2548 0.031 Uiso 1 1 calc R . . C31 C 0.9803(2) 0.38690(12) 0.17294(15) 0.0229(5) Uani 1 1 d . . . C32 C 1.0725(3) 0.41956(13) 0.21964(16) 0.0305(6) Uani 1 1 d . . . H32A H 1.1068 0.4065 0.2686 0.037 Uiso 1 1 calc R . . C33 C 1.1136(3) 0.47082(15) 0.19442(18) 0.0374(7) Uani 1 1 d . . . H33A H 1.1772 0.4921 0.2261 0.045 Uiso 1 1 calc R . . C34 C 1.0639(3) 0.49134(15) 0.12427(19) 0.0429(8) Uani 1 1 d . . . H34A H 1.0917 0.5270 0.1078 0.051 Uiso 1 1 calc R . . C35 C 0.9718(3) 0.45914(15) 0.07741(18) 0.0397(8) Uani 1 1 d . . . H35A H 0.9364 0.4731 0.0289 0.048 Uiso 1 1 calc R . . C36 C 0.9321(2) 0.40685(13) 0.10165(15) 0.0284(6) Uani 1 1 d . . . H36A H 0.8712 0.3845 0.0690 0.034 Uiso 1 1 calc R . . C41 C 0.8692(2) 0.35138(12) 0.27710(13) 0.0211(5) Uani 1 1 d . . . C42 C 0.8567(2) 0.41356(13) 0.28593(16) 0.0294(6) Uani 1 1 d . . . H42A H 0.8735 0.4415 0.2531 0.035 Uiso 1 1 calc R . . C43 C 0.8195(3) 0.43470(14) 0.34297(18) 0.0368(7) Uani 1 1 d . . . H43A H 0.8126 0.4771 0.3492 0.044 Uiso 1 1 calc R . . C44 C 0.7925(3) 0.39485(15) 0.39045(16) 0.0348(7) Uani 1 1 d . . . H44A H 0.7665 0.4098 0.4288 0.042 Uiso 1 1 calc R . . C45 C 0.8033(3) 0.33332(15) 0.38197(15) 0.0315(6) Uani 1 1 d . . . H45A H 0.7849 0.3057 0.4145 0.038 Uiso 1 1 calc R . . C46 C 0.8415(2) 0.31172(12) 0.32539(14) 0.0252(6) Uani 1 1 d . . . H46A H 0.8487 0.2692 0.3197 0.030 Uiso 1 1 calc R . . C51 C 0.7626(2) 0.10783(11) 0.01701(14) 0.0206(5) Uani 1 1 d . . . C52 C 0.8028(2) 0.05278(12) 0.05121(15) 0.0246(5) Uani 1 1 d . . . H52A H 0.7977 0.0449 0.0986 0.030 Uiso 1 1 calc R . . C53 C 0.8502(2) 0.00956(13) 0.01702(17) 0.0306(6) Uani 1 1 d . . . H53A H 0.8777 -0.0276 0.0412 0.037 Uiso 1 1 calc R . . C54 C 0.8576(3) 0.02009(15) -0.05215(17) 0.0359(7) Uani 1 1 d . . . H54A H 0.8887 -0.0100 -0.0759 0.043 Uiso 1 1 calc R . . C55 C 0.8196(3) 0.07453(15) -0.08665(16) 0.0358(7) Uani 1 1 d . . . H55A H 0.8256 0.0821 -0.1339 0.043 Uiso 1 1 calc R . . C56 C 0.7726(2) 0.11816(14) -0.05263(15) 0.0284(6) Uani 1 1 d . . . H56A H 0.7469 0.1555 -0.0768 0.034 Uiso 1 1 calc R . . C61 C 0.6075(2) 0.11983(11) 0.09948(14) 0.0218(5) Uani 1 1 d . . . C62 C 0.6047(2) 0.12697(13) 0.17067(15) 0.0273(6) Uani 1 1 d . . . H62A H 0.6541 0.1555 0.2023 0.033 Uiso 1 1 calc R . . C63 C 0.5291(3) 0.09220(14) 0.19589(17) 0.0356(7) Uani 1 1 d . . . H63B H 0.5291 0.0963 0.2450 0.043 Uiso 1 1 calc R . . C64 C 0.4547(3) 0.05207(14) 0.14973(19) 0.0369(7) Uani 1 1 d . . . H64A H 0.4027 0.0291 0.1668 0.044 Uiso 1 1 calc R . . C65 C 0.4557(3) 0.04518(13) 0.07858(18) 0.0335(7) Uani 1 1 d . . . H65A H 0.4043 0.0175 0.0469 0.040 Uiso 1 1 calc R . . C66 C 0.5318(2) 0.07876(12) 0.05327(16) 0.0258(6) Uani 1 1 d . . . H66A H 0.5323 0.0738 0.0044 0.031 Uiso 1 1 calc R . . C71 C 0.6396(2) 0.36865(12) 0.03993(13) 0.0205(5) Uani 1 1 d . . . C72 C 0.6457(2) 0.42456(13) 0.07491(16) 0.0288(6) Uani 1 1 d . . . H72A H 0.6481 0.4259 0.1247 0.035 Uiso 1 1 calc R . . C73 C 0.6484(3) 0.47821(14) 0.03766(19) 0.0379(7) Uani 1 1 d . . . H73A H 0.6517 0.5161 0.0618 0.046 Uiso 1 1 calc R . . C74 C 0.6462(3) 0.47639(14) -0.03475(19) 0.0399(8) Uani 1 1 d . . . H74A H 0.6476 0.5131 -0.0603 0.048 Uiso 1 1 calc R . . C75 C 0.6419(3) 0.42140(14) -0.06970(16) 0.0358(7) Uani 1 1 d . . . H75A H 0.6413 0.4202 -0.1192 0.043 Uiso 1 1 calc R . . C76 C 0.6385(2) 0.36781(13) -0.03261(15) 0.0275(6) Uani 1 1 d . . . H76A H 0.6355 0.3301 -0.0570 0.033 Uiso 1 1 calc R . . C81 C 0.5524(2) 0.31517(11) 0.14729(14) 0.0209(5) Uani 1 1 d . . . C82 C 0.5799(2) 0.29276(13) 0.21746(15) 0.0271(6) Uani 1 1 d . . . H82A H 0.6496 0.2710 0.2374 0.033 Uiso 1 1 calc R . . C83 C 0.5066(3) 0.30164(14) 0.25981(16) 0.0334(7) Uani 1 1 d . . . H83A H 0.5267 0.2861 0.3082 0.040 Uiso 1 1 calc R . . C84 C 0.4055(3) 0.33282(14) 0.23102(17) 0.0350(7) Uani 1 1 d . . . H84A H 0.3557 0.3388 0.2596 0.042 Uiso 1 1 calc R . . C85 C 0.3759(3) 0.35547(14) 0.16084(18) 0.0339(7) Uani 1 1 d . . . H85A H 0.3054 0.3766 0.1411 0.041 Uiso 1 1 calc R . . C86 C 0.4494(2) 0.34734(13) 0.11874(15) 0.0275(6) Uani 1 1 d . . . H86A H 0.4296 0.3636 0.0707 0.033 Uiso 1 1 calc R . . B1 B 0.8864(3) 0.28015(18) -0.09302(18) 0.0339(7) Uani 1 1 d . . . Cl1 Cl 0.77818(14) 0.15098(6) 0.38879(8) 0.0867(4) Uani 1 1 d D . . Cl2 Cl 0.65811(11) 0.11274(7) 0.49043(7) 0.0803(4) Uani 1 1 d D . . C1S C 0.6507(6) 0.1209(4) 0.4008(3) 0.065(3) Uiso 0.542(9) 1 d PD A 1 H1SA H 0.5856 0.1480 0.3764 0.078 Uiso 0.542(9) 1 calc PR A 1 H1SB H 0.6348 0.0808 0.3765 0.078 Uiso 0.542(9) 1 calc PR A 1 C1S* C 0.6974(9) 0.1720(4) 0.4439(5) 0.077(4) Uiso 0.458(9) 1 d PD A 2 H1SD H 0.6269 0.1924 0.4133 0.092 Uiso 0.458(9) 1 calc PR A 2 H1SC H 0.7418 0.2019 0.4801 0.092 Uiso 0.458(9) 1 calc PR A 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 0.01617(10) 0.01623(10) 0.01305(9) -0.00162(7) 0.00399(7) 0.00077(7) P1 0.0187(3) 0.0183(3) 0.0160(3) -0.0012(2) 0.0046(2) 0.0018(2) P2 0.0183(3) 0.0178(3) 0.0156(3) -0.0021(2) 0.0044(2) 0.0002(2) P3 0.0189(3) 0.0179(3) 0.0161(3) -0.0025(2) 0.0045(2) 0.0002(2) P4 0.0175(3) 0.0183(3) 0.0162(3) -0.0012(2) 0.0053(2) 0.0011(2) F1 0.0354(11) 0.111(2) 0.0345(10) -0.0073(11) 0.0192(9) 0.0059(11) F2 0.107(2) 0.0561(14) 0.0424(12) 0.0169(10) 0.0358(13) 0.0037(14) F3 0.0441(11) 0.0716(14) 0.0226(9) -0.0033(9) 0.0038(8) -0.0102(10) N1 0.0269(12) 0.0327(13) 0.0231(11) 0.0016(9) 0.0104(9) 0.0042(10) C1 0.0216(12) 0.0238(13) 0.0160(11) -0.0016(9) 0.0025(10) 0.0028(10) C2 0.0199(12) 0.0220(13) 0.0213(12) -0.0058(10) 0.0032(10) 0.0017(10) C3 0.0235(13) 0.0209(12) 0.0173(11) -0.0020(9) 0.0016(10) -0.0010(10) C4 0.0187(11) 0.0221(13) 0.0206(12) -0.0013(10) 0.0006(9) -0.0004(10) C5 0.0191(12) 0.0198(12) 0.0218(12) -0.0025(9) 0.0048(10) 0.0018(9) C11 0.0192(12) 0.0181(11) 0.0224(12) -0.0006(9) 0.0080(10) 0.0040(9) C12 0.0227(13) 0.0259(13) 0.0246(13) -0.0013(10) 0.0080(11) 0.0009(10) C13 0.0322(15) 0.0332(15) 0.0242(13) -0.0008(11) 0.0142(12) 0.0048(12) C14 0.0289(15) 0.0334(15) 0.0397(16) -0.0007(13) 0.0204(13) 0.0029(12) C15 0.0208(13) 0.0359(16) 0.0443(17) -0.0086(13) 0.0111(13) -0.0028(12) C16 0.0214(13) 0.0311(14) 0.0287(14) -0.0072(11) 0.0066(11) 0.0000(11) C21 0.0240(13) 0.0208(12) 0.0176(12) -0.0011(9) 0.0037(10) 0.0017(10) C22 0.0276(14) 0.0254(13) 0.0298(14) 0.0005(11) 0.0124(11) 0.0046(11) C23 0.0420(17) 0.0226(14) 0.0400(17) 0.0017(12) 0.0149(14) 0.0100(12) C24 0.0415(17) 0.0232(14) 0.0366(16) 0.0077(12) 0.0132(14) 0.0011(12) C25 0.0340(16) 0.0317(15) 0.0318(15) 0.0074(12) 0.0127(13) -0.0022(12) C26 0.0280(14) 0.0235(13) 0.0255(13) 0.0024(10) 0.0085(11) 0.0052(11) C31 0.0235(13) 0.0196(12) 0.0269(13) -0.0020(10) 0.0095(11) -0.0024(10) C32 0.0302(15) 0.0299(15) 0.0289(14) -0.0030(11) 0.0056(12) -0.0053(12) C33 0.0316(16) 0.0366(17) 0.0434(18) -0.0066(14) 0.0108(14) -0.0149(13) C34 0.048(2) 0.0388(18) 0.0472(19) 0.0045(15) 0.0226(16) -0.0150(15) C35 0.0424(18) 0.0435(18) 0.0337(16) 0.0111(14) 0.0124(14) -0.0089(15) C36 0.0270(14) 0.0328(15) 0.0251(14) -0.0006(11) 0.0077(11) -0.0055(11) C41 0.0192(12) 0.0243(13) 0.0179(12) -0.0051(9) 0.0031(10) 0.0023(10) C42 0.0321(15) 0.0241(14) 0.0338(15) -0.0040(11) 0.0130(12) 0.0022(11) C43 0.0382(17) 0.0305(15) 0.0435(18) -0.0160(13) 0.0154(14) 0.0021(13) C44 0.0289(15) 0.0479(19) 0.0285(15) -0.0170(13) 0.0103(12) 0.0028(13) C45 0.0298(15) 0.0444(17) 0.0208(13) -0.0013(12) 0.0083(11) 0.0020(13) C46 0.0273(14) 0.0264(13) 0.0208(12) -0.0031(10) 0.0059(11) 0.0041(11) C51 0.0172(11) 0.0207(12) 0.0230(12) -0.0071(10) 0.0049(10) -0.0014(9) C52 0.0242(13) 0.0224(13) 0.0273(14) -0.0032(10) 0.0081(11) -0.0025(10) C53 0.0256(14) 0.0229(14) 0.0442(17) -0.0066(12) 0.0123(13) 0.0005(11) C54 0.0292(15) 0.0392(17) 0.0397(17) -0.0186(14) 0.0115(13) 0.0041(13) C55 0.0356(16) 0.0483(19) 0.0246(14) -0.0087(13) 0.0109(12) 0.0057(14) C56 0.0273(14) 0.0346(15) 0.0214(13) -0.0033(11) 0.0050(11) 0.0046(12) C61 0.0203(12) 0.0190(12) 0.0262(13) 0.0010(10) 0.0074(10) 0.0011(10) C62 0.0262(14) 0.0290(14) 0.0258(14) 0.0013(11) 0.0069(11) 0.0005(11) C63 0.0370(17) 0.0410(17) 0.0330(16) 0.0050(13) 0.0167(13) -0.0025(14) C64 0.0308(16) 0.0324(16) 0.0516(19) 0.0121(14) 0.0187(14) -0.0030(13) C65 0.0259(14) 0.0221(14) 0.0503(19) -0.0022(13) 0.0087(13) -0.0040(11) C66 0.0251(13) 0.0212(13) 0.0302(14) -0.0029(11) 0.0073(11) -0.0010(10) C71 0.0180(12) 0.0235(12) 0.0194(12) 0.0005(10) 0.0049(9) 0.0009(10) C72 0.0330(15) 0.0249(14) 0.0308(15) -0.0030(11) 0.0134(12) -0.0013(11) C73 0.0452(19) 0.0216(14) 0.0501(19) 0.0004(13) 0.0193(16) 0.0006(13) C74 0.0444(19) 0.0296(16) 0.0463(19) 0.0142(14) 0.0151(15) 0.0012(14) C75 0.0437(18) 0.0375(17) 0.0256(14) 0.0095(12) 0.0097(13) -0.0003(14) C76 0.0313(15) 0.0279(14) 0.0234(13) 0.0027(11) 0.0085(11) 0.0031(11) C81 0.0210(12) 0.0211(12) 0.0227(12) -0.0029(10) 0.0097(10) -0.0012(10) C82 0.0281(14) 0.0296(14) 0.0249(13) -0.0024(11) 0.0100(11) 0.0002(11) C83 0.0392(17) 0.0392(17) 0.0271(14) -0.0026(12) 0.0181(13) -0.0040(13) C84 0.0350(16) 0.0389(17) 0.0412(17) -0.0116(14) 0.0264(14) -0.0074(13) C85 0.0279(15) 0.0342(16) 0.0434(17) -0.0037(13) 0.0167(13) 0.0035(12) C86 0.0272(14) 0.0301(14) 0.0280(14) -0.0005(11) 0.0126(12) 0.0048(11) B1 0.0359(18) 0.046(2) 0.0216(15) 0.0013(14) 0.0116(14) -0.0005(15) Cl1 0.1203(12) 0.0732(8) 0.0834(9) -0.0155(7) 0.0563(8) -0.0277(8) Cl2 0.0628(7) 0.0898(9) 0.0838(9) 0.0280(7) 0.0162(6) -0.0029(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 H1RU 1.67(3) . ? Ru1 C5 2.024(3) . ? Ru1 P3 2.3307(7) . ? Ru1 P1 2.3370(7) . ? Ru1 P2 2.3497(7) . ? Ru1 P4 2.3611(7) . ? P1 C11 1.826(3) . ? P1 C1 1.838(2) . ? P1 C21 1.838(3) . ? P2 C41 1.836(3) . ? P2 C31 1.837(3) . ? P2 C2 1.866(3) . ? P3 C51 1.827(3) . ? P3 C61 1.842(3) . ? P3 C3 1.843(3) . ? P4 C71 1.829(3) . ? P4 C81 1.837(3) . ? P4 C4 1.867(2) . ? F1 B1 1.373(4) . ? F2 B1 1.359(4) . ? F3 B1 1.384(4) . ? N1 C5 1.157(3) . ? N1 B1 1.562(4) . ? C1 C2 1.517(4) . ? C3 C4 1.526(4) . ? C11 C12 1.393(3) . ? C11 C16 1.398(4) . ? C12 C13 1.390(4) . ? C13 C14 1.389(4) . ? C14 C15 1.378(4) . ? C15 C16 1.395(4) . ? C21 C22 1.390(4) . ? C21 C26 1.400(4) . ? C22 C23 1.388(4) . ? C23 C24 1.389(4) . ? C24 C25 1.381(4) . ? C25 C26 1.385(4) . ? C31 C36 1.386(4) . ? C31 C32 1.403(4) . ? C32 C33 1.385(4) . ? C33 C34 1.374(5) . ? C34 C35 1.399(5) . ? C35 C36 1.387(4) . ? C41 C46 1.393(4) . ? C41 C42 1.396(4) . ? C42 C43 1.394(4) . ? C43 C44 1.380(5) . ? C44 C45 1.378(4) . ? C45 C46 1.396(4) . ? C51 C52 1.396(4) . ? C51 C56 1.403(4) . ? C52 C53 1.384(4) . ? C53 C54 1.382(4) . ? C54 C55 1.380(5) . ? C55 C56 1.386(4) . ? C61 C62 1.391(4) . ? C61 C66 1.399(4) . ? C62 C63 1.400(4) . ? C63 C64 1.378(4) . ? C64 C65 1.382(5) . ? C65 C66 1.393(4) . ? C71 C76 1.393(4) . ? C71 C72 1.396(4) . ? C72 C73 1.389(4) . ? C73 C74 1.386(5) . ? C74 C75 1.380(5) . ? C75 C76 1.388(4) . ? C81 C82 1.378(4) . ? C81 C86 1.402(4) . ? C82 C83 1.403(4) . ? C83 C84 1.373(4) . ? C84 C85 1.379(4) . ? C85 C86 1.399(4) . ? Cl1 C1S* 1.724(6) . ? Cl1 C1S 1.777(5) . ? Cl2 C1S 1.709(5) . ? Cl2 C1S* 1.735(6) . ? 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 H1RU Ru1 C5 174.8(11) . . ? H1RU Ru1 P3 90.0(11) . . ? C5 Ru1 P3 86.94(7) . . ? H1RU Ru1 P1 79.6(11) . . ? C5 Ru1 P1 96.61(7) . . ? P3 Ru1 P1 97.18(3) . . ? H1RU Ru1 P2 85.7(11) . . ? C5 Ru1 P2 97.37(7) . . ? P3 Ru1 P2 175.68(2) . . ? P1 Ru1 P2 82.69(3) . . ? H1RU Ru1 P4 92.8(11) . . ? C5 Ru1 P4 90.95(7) . . ? P3 Ru1 P4 82.11(3) . . ? P1 Ru1 P4 172.37(2) . . ? P2 Ru1 P4 97.44(3) . . ? C11 P1 C1 104.46(12) . . ? C11 P1 C21 102.72(12) . . ? C1 P1 C21 99.18(12) . . ? C11 P1 Ru1 118.76(8) . . ? C1 P1 Ru1 106.76(9) . . ? C21 P1 Ru1 122.05(9) . . ? C41 P2 C31 102.39(12) . . ? C41 P2 C2 100.04(11) . . ? C31 P2 C2 99.72(12) . . ? C41 P2 Ru1 117.56(9) . . ? C31 P2 Ru1 123.98(9) . . ? C2 P2 Ru1 109.35(8) . . ? C51 P3 C61 101.56(12) . . ? C51 P3 C3 102.34(12) . . ? C61 P3 C3 100.19(12) . . ? C51 P3 Ru1 121.78(8) . . ? C61 P3 Ru1 121.67(9) . . ? C3 P3 Ru1 105.74(8) . . ? C71 P4 C81 102.54(12) . . ? C71 P4 C4 101.99(11) . . ? C81 P4 C4 98.60(12) . . ? C71 P4 Ru1 118.44(8) . . ? C81 P4 Ru1 123.13(9) . . ? C4 P4 Ru1 108.56(8) . . ? C5 N1 B1 172.5(3) . . ? C2 C1 P1 108.71(17) . . ? C1 C2 P2 110.79(17) . . ? C4 C3 P3 106.69(17) . . ? C3 C4 P4 111.24(17) . . ? N1 C5 Ru1 175.5(2) . . ? C12 C11 C16 118.7(2) . . ? C12 C11 P1 118.17(19) . . ? C16 C11 P1 123.1(2) . . ? C13 C12 C11 121.0(3) . . ? C14 C13 C12 119.6(3) . . ? C15 C14 C13 120.1(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C11 120.1(3) . . ? C22 C21 C26 119.1(2) . . ? C22 C21 P1 122.9(2) . . ? C26 C21 P1 117.9(2) . . ? C23 C22 C21 120.0(3) . . ? C22 C23 C24 120.7(3) . . ? C25 C24 C23 119.4(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 120.3(3) . . ? C36 C31 C32 118.8(3) . . ? C36 C31 P2 121.2(2) . . ? C32 C31 P2 120.0(2) . . ? C33 C32 C31 120.1(3) . . ? C34 C33 C32 121.0(3) . . ? C33 C34 C35 119.3(3) . . ? C36 C35 C34 120.1(3) . . ? C31 C36 C35 120.7(3) . . ? C46 C41 C42 118.5(2) . . ? C46 C41 P2 118.35(19) . . ? C42 C41 P2 123.2(2) . . ? C43 C42 C41 120.0(3) . . ? C44 C43 C42 120.9(3) . . ? C45 C44 C43 119.7(3) . . ? C44 C45 C46 119.8(3) . . ? C41 C46 C45 121.1(3) . . ? C52 C51 C56 118.0(2) . . ? C52 C51 P3 120.9(2) . . ? C56 C51 P3 121.1(2) . . ? C53 C52 C51 120.9(3) . . ? C54 C53 C52 120.4(3) . . ? C55 C54 C53 119.7(3) . . ? C54 C55 C56 120.2(3) . . ? C55 C56 C51 120.8(3) . . ? C62 C61 C66 119.0(3) . . ? C62 C61 P3 121.9(2) . . ? C66 C61 P3 119.1(2) . . ? C61 C62 C63 120.2(3) . . ? C64 C63 C62 120.2(3) . . ? C63 C64 C65 120.1(3) . . ? C64 C65 C66 120.1(3) . . ? C65 C66 C61 120.4(3) . . ? C76 C71 C72 118.6(2) . . ? C76 C71 P4 120.0(2) . . ? C72 C71 P4 121.3(2) . . ? C73 C72 C71 120.6(3) . . ? C74 C73 C72 119.9(3) . . ? C75 C74 C73 120.1(3) . . ? C74 C75 C76 120.0(3) . . ? C75 C76 C71 120.8(3) . . ? C82 C81 C86 118.8(2) . . ? C82 C81 P4 120.8(2) . . ? C86 C81 P4 120.2(2) . . ? C81 C82 C83 121.0(3) . . ? C84 C83 C82 119.7(3) . . ? C83 C84 C85 120.4(3) . . ? C84 C85 C86 120.1(3) . . ? C85 C86 C81 120.1(3) . . ? F2 B1 F1 111.2(3) . . ? F2 B1 F3 110.1(3) . . ? F1 B1 F3 109.6(3) . . ? F2 B1 N1 109.8(3) . . ? F1 B1 N1 108.3(3) . . ? F3 B1 N1 107.7(3) . . ? C1S* Cl1 C1S 47.5(4) . . ? C1S Cl2 C1S* 48.3(4) . . ? Cl2 C1S Cl1 113.5(4) . . ? Cl1 C1S* Cl2 114.9(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.048 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.084 data_s9685 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H H65 B Cl2 N P4 Ru' _chemical_formula_weight 1251.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'B' 'B' 0.0013 0.0007 '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 P2(1)/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 14.9769(11) _cell_length_b 22.955(3) _cell_length_c 18.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.859(9) _cell_angle_gamma 90.00 _cell_volume 6137.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.28 _cell_measurement_theta_max 12.51 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7949 _exptl_absorpt_correction_T_max 0.8431 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1997)' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 14.99 _diffrn_reflns_number 13869 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13363 _reflns_number_gt 9513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0256P)^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 13363 _refine_ls_number_parameters 734 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _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 Ru1 Ru 0.288447(12) 0.443002(7) 0.263622(9) 0.01293(4) Uani 1 1 d . . . H1RU H 0.4009(15) 0.4487(9) 0.2846(12) 0.016(6) Uiso 1 1 d . . . P1 P 0.30918(4) 0.51235(2) 0.35728(3) 0.01649(12) Uani 1 1 d . . . P2 P 0.33250(4) 0.37568(2) 0.36317(3) 0.01689(12) Uani 1 1 d . . . P3 P 0.25888(4) 0.51153(2) 0.16806(3) 0.01580(12) Uani 1 1 d . . . P4 P 0.29193(4) 0.38228(2) 0.16445(3) 0.01577(11) Uani 1 1 d . . . N1 N 0.06389(13) 0.42532(8) 0.22771(10) 0.0184(4) Uani 1 1 d . . . C1 C 0.38305(17) 0.47943(10) 0.44624(13) 0.0242(5) Uani 1 1 d . . . H1A H 0.4502 0.4833 0.4499 0.029 Uiso 1 1 calc R . . H1B H 0.3735 0.5013 0.4885 0.029 Uiso 1 1 calc R . . C2 C 0.36156(17) 0.41578(10) 0.45383(13) 0.0243(5) Uani 1 1 d . . . H2A H 0.3077 0.4127 0.4732 0.029 Uiso 1 1 calc R . . H2B H 0.4169 0.3972 0.4908 0.029 Uiso 1 1 calc R . . C3 C 0.17813(16) 0.47486(9) 0.08499(12) 0.0209(5) Uani 1 1 d . . . H3A H 0.1177 0.4654 0.0933 0.025 Uiso 1 1 calc R . . H3B H 0.1648 0.5004 0.0405 0.025 Uiso 1 1 calc R . . C4 C 0.22736(17) 0.41898(10) 0.07317(12) 0.0222(5) Uani 1 1 d . . . H4A H 0.2726 0.4285 0.0466 0.027 Uiso 1 1 calc R . . H4B H 0.1798 0.3918 0.0413 0.027 Uiso 1 1 calc R . . C5 C 0.14427(15) 0.43204(8) 0.24041(12) 0.0165(4) Uani 1 1 d . . . C11 C 0.20672(15) 0.54168(9) 0.37842(12) 0.0198(5) Uani 1 1 d . . . C12 C 0.16519(19) 0.50858(12) 0.42099(16) 0.0366(6) Uani 1 1 d . . . H12A H 0.1908 0.4715 0.4391 0.044 Uiso 1 1 calc R . . C13 C 0.0865(2) 0.52892(14) 0.43759(17) 0.0431(7) Uani 1 1 d . . . H13A H 0.0590 0.5058 0.4668 0.052 Uiso 1 1 calc R . . C14 C 0.04862(18) 0.58247(13) 0.41160(15) 0.0368(6) Uani 1 1 d . . . H14A H -0.0043 0.5967 0.4237 0.044 Uiso 1 1 calc R . . C15 C 0.08771(18) 0.61555(11) 0.36790(15) 0.0338(6) Uani 1 1 d . . . H15A H 0.0611 0.6523 0.3495 0.041 Uiso 1 1 calc R . . C16 C 0.16589(17) 0.59518(10) 0.35073(14) 0.0261(5) Uani 1 1 d . . . H16A H 0.1916 0.6179 0.3199 0.031 Uiso 1 1 calc R . . C21 C 0.38205(16) 0.57729(10) 0.35985(12) 0.0204(5) Uani 1 1 d . . . C22 C 0.37834(17) 0.62635(10) 0.40259(13) 0.0260(5) Uani 1 1 d . . . H22A H 0.3349 0.6275 0.4297 0.031 Uiso 1 1 calc R . . C23 C 0.43776(19) 0.67369(11) 0.40583(15) 0.0323(6) Uani 1 1 d . . . H23A H 0.4341 0.7069 0.4348 0.039 Uiso 1 1 calc R . . C24 C 0.50169(18) 0.67267(11) 0.36728(14) 0.0316(6) Uani 1 1 d . . . H24A H 0.5403 0.7057 0.3680 0.038 Uiso 1 1 calc R . . C25 C 0.50939(18) 0.62342(11) 0.32754(15) 0.0344(6) Uani 1 1 d . . . H25A H 0.5555 0.6218 0.3028 0.041 Uiso 1 1 calc R . . C26 C 0.44976(17) 0.57612(11) 0.32359(14) 0.0276(5) Uani 1 1 d . . . H26A H 0.4553 0.5426 0.2958 0.033 Uiso 1 1 calc R . . C31 C 0.25348(16) 0.31967(10) 0.37916(13) 0.0213(5) Uani 1 1 d . . . C32 C 0.26810(17) 0.29880(11) 0.45222(14) 0.0294(6) Uani 1 1 d . . . H32A H 0.3177 0.3142 0.4931 0.035 Uiso 1 1 calc R . . C33 C 0.20979(19) 0.25560(11) 0.46432(15) 0.0345(6) Uani 1 1 d . . . H33A H 0.2190 0.2422 0.5138 0.041 Uiso 1 1 calc R . . C34 C 0.1386(2) 0.23192(12) 0.40537(16) 0.0385(7) Uani 1 1 d . . . H34A H 0.0991 0.2024 0.4142 0.046 Uiso 1 1 calc R . . C35 C 0.12533(19) 0.25153(11) 0.33341(15) 0.0330(6) Uani 1 1 d . . . H35A H 0.0774 0.2347 0.2925 0.040 Uiso 1 1 calc R . . C36 C 0.18189(17) 0.29580(10) 0.32065(13) 0.0250(5) Uani 1 1 d . . . H36A H 0.1711 0.3097 0.2711 0.030 Uiso 1 1 calc R . . C41 C 0.43941(16) 0.33112(11) 0.37702(12) 0.0236(5) Uani 1 1 d . . . C42 C 0.43429(19) 0.27093(11) 0.36515(14) 0.0317(6) Uani 1 1 d . . . H42A H 0.3747 0.2520 0.3498 0.038 Uiso 1 1 calc R . . C43 C 0.5162(2) 0.23859(14) 0.37578(17) 0.0488(8) Uani 1 1 d . . . H43A H 0.5124 0.1978 0.3670 0.059 Uiso 1 1 calc R . . C44 C 0.6029(2) 0.26583(17) 0.39905(17) 0.0542(9) Uani 1 1 d . . . H44A H 0.6588 0.2437 0.4062 0.065 Uiso 1 1 calc R . . C45 C 0.60876(19) 0.32524(16) 0.41195(16) 0.0465(8) Uani 1 1 d . . . H45A H 0.6686 0.3438 0.4289 0.056 Uiso 1 1 calc R . . C46 C 0.52725(17) 0.35770(13) 0.40013(14) 0.0320(6) Uani 1 1 d . . . H46A H 0.5316 0.3986 0.4080 0.038 Uiso 1 1 calc R . . C51 C 0.20178(16) 0.58107(10) 0.17362(12) 0.0201(5) Uani 1 1 d . . . C52 C 0.25318(17) 0.63321(10) 0.18920(13) 0.0246(5) Uani 1 1 d . . . H52A H 0.3190 0.6329 0.1965 0.030 Uiso 1 1 calc R . . C53 C 0.20853(19) 0.68532(10) 0.19406(14) 0.0295(6) Uani 1 1 d . . . H53A H 0.2439 0.7204 0.2045 0.035 Uiso 1 1 calc R . . C54 C 0.11288(19) 0.68641(11) 0.18383(15) 0.0332(6) Uani 1 1 d . . . H54A H 0.0823 0.7223 0.1860 0.040 Uiso 1 1 calc R . . C55 C 0.06180(18) 0.63507(11) 0.17038(15) 0.0327(6) Uani 1 1 d . . . H55A H -0.0037 0.6357 0.1644 0.039 Uiso 1 1 calc R . . C56 C 0.10596(17) 0.58256(10) 0.16564(13) 0.0255(5) Uani 1 1 d . . . H56A H 0.0705 0.5474 0.1569 0.031 Uiso 1 1 calc R . . C61 C 0.35184(16) 0.53358(9) 0.12936(12) 0.0191(5) Uani 1 1 d . . . C62 C 0.44244(16) 0.51058(10) 0.15612(13) 0.0231(5) Uani 1 1 d . . . H62A H 0.4585 0.4850 0.1980 0.028 Uiso 1 1 calc R . . C63 C 0.50983(18) 0.52431(11) 0.12271(15) 0.0321(6) Uani 1 1 d . . . H63A H 0.5716 0.5084 0.1418 0.039 Uiso 1 1 calc R . . C64 C 0.48655(18) 0.56163(12) 0.06096(15) 0.0358(6) Uani 1 1 d . . . H64A H 0.5323 0.5712 0.0377 0.043 Uiso 1 1 calc R . . C65 C 0.39627(18) 0.58457(11) 0.03381(15) 0.0324(6) Uani 1 1 d . . . H65A H 0.3802 0.6100 -0.0082 0.039 Uiso 1 1 calc R . . C66 C 0.32924(17) 0.57086(10) 0.06729(13) 0.0256(5) Uani 1 1 d . . . H66A H 0.2676 0.5868 0.0481 0.031 Uiso 1 1 calc R . . C71 C 0.23701(15) 0.31018(9) 0.15413(12) 0.0176(4) Uani 1 1 d . . . C72 C 0.29120(16) 0.26063(9) 0.18201(13) 0.0220(5) Uani 1 1 d . . . H72A H 0.3578 0.2638 0.2031 0.026 Uiso 1 1 calc R . . C73 C 0.24789(18) 0.20688(10) 0.17897(15) 0.0303(6) Uani 1 1 d . . . H73A H 0.2849 0.1733 0.1982 0.036 Uiso 1 1 calc R . . C74 C 0.15059(18) 0.20197(10) 0.14788(15) 0.0315(6) Uani 1 1 d . . . H74A H 0.1212 0.1651 0.1460 0.038 Uiso 1 1 calc R . . C75 C 0.09657(17) 0.25042(11) 0.11973(14) 0.0293(6) Uani 1 1 d . . . H75A H 0.0301 0.2468 0.0977 0.035 Uiso 1 1 calc R . . C76 C 0.13947(16) 0.30459(10) 0.12360(13) 0.0232(5) Uani 1 1 d . . . H76A H 0.1019 0.3381 0.1052 0.028 Uiso 1 1 calc R . . C81 C 0.40452(15) 0.36243(9) 0.15035(12) 0.0186(5) Uani 1 1 d . . . C82 C 0.48885(16) 0.36541(10) 0.20766(13) 0.0243(5) Uani 1 1 d . . . H82A H 0.4898 0.3793 0.2553 0.029 Uiso 1 1 calc R . . C83 C 0.57337(18) 0.34845(11) 0.19721(15) 0.0308(6) Uani 1 1 d . . . H83A H 0.6311 0.3505 0.2375 0.037 Uiso 1 1 calc R . . C84 C 0.57207(18) 0.32854(11) 0.12750(15) 0.0314(6) Uani 1 1 d . . . H84A H 0.6293 0.3173 0.1198 0.038 Uiso 1 1 calc R . . C85 C 0.48806(18) 0.32497(10) 0.06920(14) 0.0273(5) Uani 1 1 d . . . H85A H 0.4875 0.3112 0.0216 0.033 Uiso 1 1 calc R . . C86 C 0.40423(17) 0.34157(10) 0.08020(13) 0.0236(5) Uani 1 1 d . . . H86A H 0.3464 0.3388 0.0401 0.028 Uiso 1 1 calc R . . C91 C -0.07923(15) 0.36460(10) 0.14452(13) 0.0223(5) Uani 1 1 d . . . C92 C -0.12355(17) 0.31139(10) 0.14807(15) 0.0302(6) Uani 1 1 d . . . H92A H -0.1289 0.2993 0.1947 0.036 Uiso 1 1 calc R . . C93 C -0.1602(2) 0.27541(12) 0.08561(18) 0.0422(7) Uani 1 1 d . . . H93A H -0.1913 0.2402 0.0899 0.051 Uiso 1 1 calc R . . C94 C -0.1509(2) 0.29126(13) 0.01732(16) 0.0432(7) Uani 1 1 d . . . H94A H -0.1754 0.2670 -0.0254 0.052 Uiso 1 1 calc R . . C95 C -0.10553(19) 0.34262(13) 0.01232(15) 0.0373(7) Uani 1 1 d . . . H95A H -0.0976 0.3535 -0.0339 0.045 Uiso 1 1 calc R . . C96 C -0.07141(17) 0.37856(11) 0.07453(13) 0.0275(5) Uani 1 1 d . . . H96A H -0.0415 0.4141 0.0693 0.033 Uiso 1 1 calc R . . C101 C -0.05686(16) 0.38776(9) 0.29093(13) 0.0211(5) Uani 1 1 d . . . C102 C -0.14713(18) 0.37293(11) 0.29276(15) 0.0301(6) Uani 1 1 d . . . H10A H -0.2001 0.3784 0.2490 0.036 Uiso 1 1 calc R . . C103 C -0.1612(2) 0.35035(12) 0.35692(16) 0.0374(7) Uani 1 1 d . . . H10B H -0.2229 0.3398 0.3559 0.045 Uiso 1 1 calc R . . C104 C -0.0864(2) 0.34327(11) 0.42160(16) 0.0387(7) Uani 1 1 d . . . H10C H -0.0962 0.3280 0.4653 0.046 Uiso 1 1 calc R . . C105 C 0.0033(2) 0.35859(12) 0.42249(15) 0.0388(7) Uani 1 1 d . . . H10D H 0.0553 0.3544 0.4671 0.047 Uiso 1 1 calc R . . C106 C 0.01696(17) 0.38011(11) 0.35812(13) 0.0282(5) Uani 1 1 d . . . H10E H 0.0791 0.3901 0.3597 0.034 Uiso 1 1 calc R . . C111 C -0.10466(16) 0.47209(10) 0.18957(13) 0.0217(5) Uani 1 1 d . . . C112 C -0.07565(17) 0.52358(10) 0.23013(14) 0.0290(5) Uani 1 1 d . . . H11A H -0.0171 0.5239 0.2697 0.035 Uiso 1 1 calc R . . C113 C -0.1294(2) 0.57434(11) 0.21459(17) 0.0382(7) Uani 1 1 d . . . H11B H -0.1073 0.6084 0.2436 0.046 Uiso 1 1 calc R . . C114 C -0.21496(19) 0.57547(12) 0.15685(17) 0.0378(7) Uani 1 1 d . . . H11C H -0.2514 0.6102 0.1458 0.045 Uiso 1 1 calc R . . C115 C -0.24632(19) 0.52551(12) 0.11588(16) 0.0359(6) Uani 1 1 d . . . H11D H -0.3049 0.5256 0.0764 0.043 Uiso 1 1 calc R . . C116 C -0.19219(17) 0.47470(11) 0.13222(14) 0.0287(5) Uani 1 1 d . . . H11E H -0.2154 0.4407 0.1035 0.034 Uiso 1 1 calc R . . B1 B -0.04487(17) 0.41153(11) 0.21301(14) 0.0195(5) Uani 1 1 d . . . C1S C 0.7709(2) 0.49729(14) 0.3515(2) 0.0580(9) Uani 1 1 d . . . H1SA H 0.7846 0.5021 0.3038 0.070 Uiso 1 1 calc R . . H1SB H 0.8169 0.4691 0.3830 0.070 Uiso 1 1 calc R . . Cl2 Cl 0.78396(6) 0.56471(3) 0.39790(5) 0.0515(2) Uani 1 1 d . . . Cl1 Cl 0.65632(7) 0.46984(4) 0.33267(7) 0.0756(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 0.01277(8) 0.01342(8) 0.01252(8) -0.00044(7) 0.00396(6) -0.00078(7) P1 0.0169(3) 0.0168(3) 0.0155(3) -0.0033(2) 0.0048(2) -0.0015(2) P2 0.0175(3) 0.0177(3) 0.0145(3) 0.0018(2) 0.0037(2) 0.0006(2) P3 0.0157(3) 0.0154(3) 0.0166(3) 0.0014(2) 0.0056(2) 0.0004(2) P4 0.0178(3) 0.0150(3) 0.0145(3) -0.0010(2) 0.0052(2) -0.0002(2) N1 0.0165(9) 0.0207(9) 0.0181(9) 0.0000(7) 0.0060(8) 0.0005(7) C1 0.0248(12) 0.0261(12) 0.0186(12) -0.0050(10) 0.0026(10) -0.0007(10) C2 0.0271(13) 0.0270(12) 0.0167(11) 0.0003(10) 0.0041(10) 0.0015(10) C3 0.0209(11) 0.0213(12) 0.0190(11) 0.0025(9) 0.0044(9) -0.0007(9) C4 0.0292(13) 0.0204(11) 0.0153(11) -0.0005(9) 0.0047(10) -0.0002(10) C5 0.0229(11) 0.0131(11) 0.0152(10) -0.0010(8) 0.0084(9) -0.0011(8) C11 0.0206(11) 0.0199(11) 0.0186(11) -0.0082(9) 0.0061(9) -0.0008(9) C12 0.0340(15) 0.0356(15) 0.0468(17) 0.0089(13) 0.0224(13) 0.0084(12) C13 0.0366(16) 0.0585(19) 0.0445(18) 0.0093(15) 0.0275(14) 0.0064(14) C14 0.0266(14) 0.0525(17) 0.0349(15) -0.0108(13) 0.0148(12) 0.0075(13) C15 0.0291(14) 0.0290(13) 0.0395(15) -0.0069(12) 0.0058(12) 0.0076(11) C16 0.0241(12) 0.0250(12) 0.0286(13) -0.0036(10) 0.0077(10) -0.0011(10) C21 0.0200(11) 0.0205(11) 0.0193(11) -0.0025(9) 0.0043(9) -0.0025(9) C22 0.0290(13) 0.0217(12) 0.0279(13) -0.0050(10) 0.0099(11) -0.0042(10) C23 0.0379(15) 0.0192(12) 0.0368(15) -0.0054(11) 0.0078(12) -0.0036(11) C24 0.0312(14) 0.0256(13) 0.0350(15) 0.0032(11) 0.0064(12) -0.0102(11) C25 0.0298(14) 0.0378(15) 0.0374(15) -0.0030(12) 0.0134(12) -0.0111(12) C26 0.0250(12) 0.0275(12) 0.0304(13) -0.0068(10) 0.0092(11) -0.0045(10) C31 0.0207(11) 0.0209(11) 0.0238(12) 0.0071(9) 0.0094(10) 0.0024(9) C32 0.0278(13) 0.0343(14) 0.0244(13) 0.0108(11) 0.0063(11) -0.0015(11) C33 0.0390(15) 0.0342(14) 0.0328(15) 0.0155(12) 0.0152(13) -0.0006(12) C34 0.0411(16) 0.0370(15) 0.0420(17) 0.0062(13) 0.0197(14) -0.0128(13) C35 0.0354(15) 0.0332(14) 0.0317(14) -0.0041(11) 0.0126(12) -0.0136(12) C36 0.0287(13) 0.0250(12) 0.0230(12) 0.0005(10) 0.0107(10) -0.0022(10) C41 0.0217(12) 0.0322(13) 0.0172(11) 0.0049(10) 0.0066(9) 0.0062(10) C42 0.0327(14) 0.0314(14) 0.0312(14) 0.0069(11) 0.0105(12) 0.0116(11) C43 0.056(2) 0.0488(18) 0.0465(19) 0.0123(15) 0.0230(16) 0.0302(16) C44 0.0382(18) 0.085(3) 0.0409(18) 0.0125(17) 0.0153(14) 0.0361(18) C45 0.0220(14) 0.088(3) 0.0304(15) 0.0039(16) 0.0096(12) 0.0061(15) C46 0.0230(13) 0.0478(16) 0.0256(13) 0.0023(12) 0.0082(11) 0.0016(12) C51 0.0246(12) 0.0185(11) 0.0175(11) 0.0032(9) 0.0074(9) 0.0038(9) C52 0.0253(12) 0.0238(12) 0.0241(12) -0.0002(10) 0.0069(10) 0.0005(10) C53 0.0418(15) 0.0179(12) 0.0307(14) 0.0001(10) 0.0144(12) 0.0020(11) C54 0.0422(16) 0.0238(13) 0.0358(15) 0.0042(11) 0.0156(13) 0.0115(11) C55 0.0292(13) 0.0320(14) 0.0411(16) 0.0087(12) 0.0172(12) 0.0113(11) C56 0.0256(12) 0.0229(12) 0.0297(13) 0.0049(10) 0.0112(11) 0.0043(10) C61 0.0222(11) 0.0177(10) 0.0194(11) -0.0004(9) 0.0097(9) -0.0042(9) C62 0.0226(12) 0.0218(12) 0.0263(13) 0.0045(10) 0.0099(10) 0.0014(9) C63 0.0237(13) 0.0383(15) 0.0396(16) 0.0082(12) 0.0175(12) 0.0038(11) C64 0.0304(14) 0.0435(16) 0.0420(15) 0.0091(13) 0.0236(12) -0.0011(12) C65 0.0348(14) 0.0344(14) 0.0303(14) 0.0106(12) 0.0137(12) -0.0012(12) C66 0.0232(12) 0.0269(13) 0.0265(13) 0.0077(10) 0.0080(10) 0.0010(9) C71 0.0205(11) 0.0173(11) 0.0165(11) -0.0051(9) 0.0079(9) -0.0020(9) C72 0.0208(11) 0.0202(11) 0.0251(12) -0.0004(9) 0.0076(10) 0.0015(9) C73 0.0323(14) 0.0197(12) 0.0395(15) 0.0017(11) 0.0127(12) 0.0017(10) C74 0.0323(14) 0.0202(12) 0.0464(16) -0.0092(11) 0.0191(13) -0.0104(10) C75 0.0208(12) 0.0327(14) 0.0339(14) -0.0104(11) 0.0081(11) -0.0083(10) C76 0.0195(11) 0.0229(12) 0.0267(13) -0.0054(10) 0.0066(10) 0.0015(9) C81 0.0215(11) 0.0143(10) 0.0227(12) -0.0012(9) 0.0109(9) -0.0022(9) C82 0.0230(12) 0.0272(12) 0.0241(12) -0.0007(10) 0.0096(10) 0.0004(10) C83 0.0234(13) 0.0338(14) 0.0368(15) 0.0021(11) 0.0120(11) 0.0026(11) C84 0.0325(14) 0.0282(13) 0.0431(16) 0.0031(12) 0.0256(13) 0.0027(11) C85 0.0373(15) 0.0239(12) 0.0291(13) -0.0009(10) 0.0221(12) 0.0014(11) C86 0.0278(13) 0.0218(12) 0.0235(12) -0.0017(10) 0.0115(10) -0.0008(10) C91 0.0138(10) 0.0252(12) 0.0253(12) -0.0021(10) 0.0028(9) 0.0034(9) C92 0.0283(13) 0.0262(13) 0.0342(14) -0.0044(11) 0.0074(11) -0.0001(10) C93 0.0314(15) 0.0296(14) 0.058(2) -0.0138(14) 0.0045(14) 0.0013(12) C94 0.0356(16) 0.0434(17) 0.0369(16) -0.0193(13) -0.0071(13) 0.0131(13) C95 0.0319(15) 0.0503(18) 0.0228(13) -0.0044(12) -0.0005(11) 0.0171(13) C96 0.0250(12) 0.0326(13) 0.0227(12) 0.0010(10) 0.0047(10) 0.0091(11) C101 0.0223(11) 0.0199(11) 0.0222(12) -0.0022(9) 0.0090(10) -0.0001(9) C102 0.0253(13) 0.0365(14) 0.0319(14) -0.0026(11) 0.0141(11) -0.0045(11) C103 0.0452(17) 0.0350(15) 0.0429(17) -0.0046(13) 0.0296(14) -0.0122(13) C104 0.062(2) 0.0328(15) 0.0319(15) 0.0000(12) 0.0295(15) -0.0092(13) C105 0.0473(17) 0.0444(16) 0.0233(14) 0.0048(12) 0.0098(13) 0.0041(14) C106 0.0258(13) 0.0342(14) 0.0250(13) 0.0001(11) 0.0087(10) 0.0012(11) C111 0.0196(11) 0.0263(12) 0.0211(12) 0.0026(10) 0.0090(9) -0.0004(9) C112 0.0243(13) 0.0284(13) 0.0346(14) -0.0050(11) 0.0099(11) -0.0019(10) C113 0.0384(16) 0.0259(13) 0.0542(18) -0.0071(12) 0.0203(14) -0.0025(11) C114 0.0358(15) 0.0311(14) 0.0524(18) 0.0115(13) 0.0224(14) 0.0131(12) C115 0.0270(14) 0.0438(16) 0.0373(16) 0.0083(13) 0.0111(12) 0.0113(12) C116 0.0212(12) 0.0322(14) 0.0303(14) -0.0003(11) 0.0051(10) 0.0013(10) B1 0.0158(12) 0.0220(13) 0.0198(13) -0.0015(10) 0.0045(10) -0.0024(10) C1S 0.050(2) 0.0401(17) 0.094(3) -0.0139(18) 0.038(2) -0.0095(15) Cl2 0.0615(5) 0.0312(4) 0.0638(5) 0.0028(3) 0.0231(4) -0.0076(3) Cl1 0.0469(5) 0.0619(6) 0.1120(9) -0.0174(6) 0.0177(5) -0.0151(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1RU 1.61(2) . ? Ru1 C5 2.075(2) . ? Ru1 P1 2.3231(6) . ? Ru1 P3 2.3247(6) . ? Ru1 P4 2.3470(6) . ? Ru1 P2 2.3556(6) . ? P1 C11 1.834(2) . ? P1 C21 1.839(2) . ? P1 C1 1.847(2) . ? P2 C31 1.837(2) . ? P2 C41 1.846(2) . ? P2 C2 1.866(2) . ? P3 C51 1.830(2) . ? P3 C61 1.840(2) . ? P3 C3 1.844(2) . ? P4 C71 1.830(2) . ? P4 C81 1.847(2) . ? P4 C4 1.880(2) . ? N1 C5 1.159(3) . ? N1 B1 1.593(3) . ? C1 C2 1.513(3) . ? C3 C4 1.531(3) . ? C11 C12 1.390(3) . ? C11 C16 1.396(3) . ? C12 C13 1.395(4) . ? C13 C14 1.376(4) . ? C14 C15 1.382(4) . ? C15 C16 1.393(3) . ? C21 C26 1.395(3) . ? C21 C22 1.397(3) . ? C22 C23 1.393(3) . ? C23 C24 1.377(4) . ? C24 C25 1.382(4) . ? C25 C26 1.392(3) . ? C31 C36 1.379(3) . ? C31 C32 1.408(3) . ? C32 C33 1.388(3) . ? C33 C34 1.379(4) . ? C34 C35 1.382(4) . ? C35 C36 1.393(3) . ? C41 C46 1.386(3) . ? C41 C42 1.398(3) . ? C42 C43 1.392(4) . ? C43 C44 1.379(5) . ? C44 C45 1.383(5) . ? C45 C46 1.385(4) . ? C51 C56 1.394(3) . ? C51 C52 1.402(3) . ? C52 C53 1.388(3) . ? C53 C54 1.382(4) . ? C54 C55 1.383(4) . ? C55 C56 1.392(3) . ? C61 C62 1.390(3) . ? C61 C66 1.401(3) . ? C62 C63 1.388(3) . ? C63 C64 1.396(4) . ? C64 C65 1.386(4) . ? C65 C66 1.384(3) . ? C71 C76 1.392(3) . ? C71 C72 1.398(3) . ? C72 C73 1.387(3) . ? C73 C74 1.388(3) . ? C74 C75 1.377(4) . ? C75 C76 1.391(3) . ? C81 C82 1.373(3) . ? C81 C86 1.406(3) . ? C82 C83 1.398(3) . ? C83 C84 1.386(3) . ? C84 C85 1.380(4) . ? C85 C86 1.390(3) . ? C91 C96 1.400(3) . ? C91 C92 1.402(3) . ? C91 B1 1.633(3) . ? C92 C93 1.398(4) . ? C93 C94 1.388(4) . ? C94 C95 1.379(4) . ? C95 C96 1.390(3) . ? C101 C106 1.398(3) . ? C101 C102 1.405(3) . ? C101 B1 1.631(3) . ? C102 C103 1.394(3) . ? C103 C104 1.373(4) . ? C104 C105 1.383(4) . ? C105 C106 1.386(3) . ? C111 C112 1.399(3) . ? C111 C116 1.406(3) . ? C111 B1 1.635(3) . ? C112 C113 1.392(3) . ? C113 C114 1.389(4) . ? C114 C115 1.378(4) . ? C115 C116 1.397(3) . ? C1S Cl1 1.753(3) . ? C1S Cl2 1.758(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 H1RU Ru1 C5 177.0(8) . . ? H1RU Ru1 P1 83.4(7) . . ? C5 Ru1 P1 96.76(6) . . ? H1RU Ru1 P3 93.3(7) . . ? C5 Ru1 P3 89.66(6) . . ? P1 Ru1 P3 94.08(2) . . ? H1RU Ru1 P4 87.3(7) . . ? C5 Ru1 P4 92.84(6) . . ? P1 Ru1 P4 168.86(2) . . ? P3 Ru1 P4 80.30(2) . . ? H1RU Ru1 P2 81.7(7) . . ? C5 Ru1 P2 95.33(6) . . ? P1 Ru1 P2 84.78(2) . . ? P3 Ru1 P2 174.98(2) . . ? P4 Ru1 P2 99.97(2) . . ? C11 P1 C21 103.17(10) . . ? C11 P1 C1 104.49(11) . . ? C21 P1 C1 97.56(11) . . ? C11 P1 Ru1 120.10(7) . . ? C21 P1 Ru1 120.52(7) . . ? C1 P1 Ru1 107.71(8) . . ? C31 P2 C41 99.45(10) . . ? C31 P2 C2 99.59(11) . . ? C41 P2 C2 102.07(11) . . ? C31 P2 Ru1 124.10(8) . . ? C41 P2 Ru1 118.88(7) . . ? C2 P2 Ru1 109.23(8) . . ? C51 P3 C61 102.15(10) . . ? C51 P3 C3 104.87(10) . . ? C61 P3 C3 99.26(10) . . ? C51 P3 Ru1 121.42(7) . . ? C61 P3 Ru1 121.00(8) . . ? C3 P3 Ru1 104.96(7) . . ? C71 P4 C81 99.28(9) . . ? C71 P4 C4 103.15(10) . . ? C81 P4 C4 101.66(10) . . ? C71 P4 Ru1 119.78(7) . . ? C81 P4 Ru1 121.19(7) . . ? C4 P4 Ru1 109.06(7) . . ? C5 N1 B1 175.8(2) . . ? C2 C1 P1 113.44(16) . . ? C1 C2 P2 112.56(16) . . ? C4 C3 P3 106.96(15) . . ? C3 C4 P4 111.80(15) . . ? N1 C5 Ru1 179.3(2) . . ? C12 C11 C16 118.3(2) . . ? C12 C11 P1 119.15(18) . . ? C16 C11 P1 122.54(17) . . ? C11 C12 C13 121.0(2) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 119.9(2) . . ? C14 C15 C16 120.3(2) . . ? C15 C16 C11 120.5(2) . . ? C26 C21 C22 118.0(2) . . ? C26 C21 P1 119.40(17) . . ? C22 C21 P1 122.34(17) . . ? C23 C22 C21 120.7(2) . . ? C24 C23 C22 120.5(2) . . ? C23 C24 C25 119.6(2) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 121.0(2) . . ? C36 C31 C32 118.9(2) . . ? C36 C31 P2 121.46(17) . . ? C32 C31 P2 119.62(18) . . ? C33 C32 C31 119.8(2) . . ? C34 C33 C32 120.8(2) . . ? C33 C34 C35 119.5(2) . . ? C34 C35 C36 120.3(2) . . ? C31 C36 C35 120.7(2) . . ? C46 C41 C42 118.9(2) . . ? C46 C41 P2 119.47(19) . . ? C42 C41 P2 121.66(19) . . ? C43 C42 C41 120.3(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 120.2(3) . . ? C44 C45 C46 120.0(3) . . ? C45 C46 C41 120.7(3) . . ? C56 C51 C52 118.6(2) . . ? C56 C51 P3 119.94(18) . . ? C52 C51 P3 121.44(17) . . ? C53 C52 C51 120.4(2) . . ? C54 C53 C52 120.4(2) . . ? C53 C54 C55 119.8(2) . . ? C54 C55 C56 120.2(2) . . ? C55 C56 C51 120.6(2) . . ? C62 C61 C66 118.6(2) . . ? C62 C61 P3 121.77(17) . . ? C66 C61 P3 119.37(17) . . ? C63 C62 C61 121.1(2) . . ? C62 C63 C64 119.7(2) . . ? C65 C64 C63 119.5(2) . . ? C66 C65 C64 120.7(2) . . ? C65 C66 C61 120.4(2) . . ? C76 C71 C72 119.0(2) . . ? C76 C71 P4 120.18(17) . . ? C72 C71 P4 120.64(17) . . ? C73 C72 C71 120.1(2) . . ? C72 C73 C74 120.2(2) . . ? C75 C74 C73 120.2(2) . . ? C74 C75 C76 119.9(2) . . ? C75 C76 C71 120.6(2) . . ? C82 C81 C86 118.7(2) . . ? C82 C81 P4 121.64(17) . . ? C86 C81 P4 119.62(17) . . ? C81 C82 C83 121.3(2) . . ? C84 C83 C82 119.3(2) . . ? C85 C84 C83 120.3(2) . . ? C84 C85 C86 120.0(2) . . ? C85 C86 C81 120.4(2) . . ? C96 C91 C92 115.5(2) . . ? C96 C91 B1 119.6(2) . . ? C92 C91 B1 124.8(2) . . ? C93 C92 C91 122.5(3) . . ? C94 C93 C92 119.9(3) . . ? C95 C94 C93 119.1(3) . . ? C94 C95 C96 120.3(3) . . ? C95 C96 C91 122.7(2) . . ? C106 C101 C102 115.6(2) . . ? C106 C101 B1 125.0(2) . . ? C102 C101 B1 119.4(2) . . ? C103 C102 C101 121.9(3) . . ? C104 C103 C102 120.4(2) . . ? C103 C104 C105 119.4(2) . . ? C104 C105 C106 119.9(3) . . ? C105 C106 C101 122.8(2) . . ? C112 C111 C116 115.6(2) . . ? C112 C111 B1 121.6(2) . . ? C116 C111 B1 122.5(2) . . ? C113 C112 C111 122.4(2) . . ? C114 C113 C112 120.3(3) . . ? C115 C114 C113 119.0(2) . . ? C114 C115 C116 120.2(3) . . ? C115 C116 C111 122.4(2) . . ? N1 B1 C101 108.29(18) . . ? N1 B1 C91 108.17(18) . . ? C101 B1 C91 113.20(19) . . ? N1 B1 C111 108.54(18) . . ? C101 B1 C111 108.53(18) . . ? C91 B1 C111 110.00(18) . . ? Cl1 C1S Cl2 111.17(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.438 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.061 data_s9717r _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H2 H48 B F4 N Os P4' _chemical_formula_weight 1101.83 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' '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' 'Os' 'Os' -1.2165 7.6030 '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 P2(1)/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 12.825(2) _cell_length_b 21.230(3) _cell_length_c 18.373(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.904(12) _cell_angle_gamma 90.00 _cell_volume 4760.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 12.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.867 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3720 _exptl_absorpt_correction_T_max 0.5585 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1997)' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.32 _diffrn_reflns_number 10732 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10286 _reflns_number_gt 6986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0467P)^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 10286 _refine_ls_number_parameters 579 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.928 _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 -0.087077(17) -0.341941(11) 0.745793(13) 0.02336(7) Uani 1 1 d . . . H1OS H -0.104(4) -0.267(3) 0.712(3) 0.029(15) Uiso 1 1 d . . . P1 P 0.02634(11) -0.33882(8) 0.66764(8) 0.0268(3) Uani 1 1 d . . . P2 P -0.22131(12) -0.36943(7) 0.63149(9) 0.0274(3) Uani 1 1 d . . . P3 P 0.04443(12) -0.30748(7) 0.85853(8) 0.0272(3) Uani 1 1 d . . . P4 P -0.20501(12) -0.32668(7) 0.82033(9) 0.0280(4) Uani 1 1 d . . . N1 N -0.0195(5) -0.4791(3) 0.8067(4) 0.0501(16) Uani 1 1 d D . . H1N H 0.015(5) -0.511(2) 0.843(3) 0.060 Uiso 1 1 d D . . C1 C -0.0628(5) -0.3222(3) 0.5703(3) 0.0347(15) Uani 1 1 d . . . H1A H -0.0857 -0.2775 0.5665 0.042 Uiso 1 1 calc R . . H1B H -0.0219 -0.3295 0.5333 0.042 Uiso 1 1 calc R . . C2 C -0.1626(5) -0.3639(3) 0.5508(3) 0.0314(14) Uani 1 1 d . . . H2A H -0.1425 -0.4066 0.5380 0.038 Uiso 1 1 calc R . . H2B H -0.2188 -0.3469 0.5052 0.038 Uiso 1 1 calc R . . C3 C -0.0051(5) -0.3332(3) 0.9376(3) 0.0343(14) Uani 1 1 d . . . H3A H -0.0026 -0.3797 0.9418 0.041 Uiso 1 1 calc R . . H3B H 0.0414 -0.3153 0.9866 0.041 Uiso 1 1 calc R . . C4 C -0.1220(5) -0.3101(3) 0.9205(3) 0.0353(15) Uani 1 1 d . . . H4A H -0.1215 -0.2642 0.9298 0.042 Uiso 1 1 calc R . . H4B H -0.1562 -0.3309 0.9557 0.042 Uiso 1 1 calc R . . C5 C -0.0459(5) -0.4287(3) 0.7839(4) 0.0345(14) Uani 1 1 d . . . C11 C 0.0988(4) -0.4106(3) 0.6588(4) 0.0299(14) Uani 1 1 d . . . C12 C 0.0884(6) -0.4399(3) 0.5896(4) 0.0428(16) Uani 1 1 d . . . H12A H 0.0420 -0.4226 0.5433 0.051 Uiso 1 1 calc R . . C13 C 0.1460(6) -0.4943(3) 0.5886(4) 0.056(2) Uani 1 1 d . . . H13A H 0.1372 -0.5139 0.5406 0.067 Uiso 1 1 calc R . . C14 C 0.2136(6) -0.5215(3) 0.6511(4) 0.0461(17) Uani 1 1 d . . . H14A H 0.2526 -0.5588 0.6474 0.055 Uiso 1 1 calc R . . C15 C 0.2250(5) -0.4936(3) 0.7215(4) 0.0423(16) Uani 1 1 d . . . H15A H 0.2715 -0.5118 0.7672 0.051 Uiso 1 1 calc R . . C16 C 0.1677(5) -0.4390(3) 0.7244(3) 0.0323(14) Uani 1 1 d . . . H16A H 0.1755 -0.4201 0.7727 0.039 Uiso 1 1 calc R . . C21 C 0.1299(5) -0.2763(3) 0.6753(3) 0.0305(14) Uani 1 1 d . . . C22 C 0.2383(5) -0.2897(3) 0.6799(4) 0.0397(16) Uani 1 1 d . . . H22A H 0.2627 -0.3320 0.6815 0.048 Uiso 1 1 calc R . . C23 C 0.3098(6) -0.2402(4) 0.6819(4) 0.0517(19) Uani 1 1 d . . . H23A H 0.3837 -0.2489 0.6850 0.062 Uiso 1 1 calc R . . C24 C 0.2752(7) -0.1784(4) 0.6796(5) 0.061(2) Uani 1 1 d . . . H24A H 0.3249 -0.1449 0.6811 0.074 Uiso 1 1 calc R . . C25 C 0.1681(7) -0.1659(4) 0.6751(5) 0.063(2) Uani 1 1 d . . . H25A H 0.1439 -0.1234 0.6724 0.075 Uiso 1 1 calc R . . C26 C 0.0950(5) -0.2142(3) 0.6744(4) 0.0423(16) Uani 1 1 d . . . H26A H 0.0220 -0.2050 0.6734 0.051 Uiso 1 1 calc R . . C31 C -0.2797(5) -0.4486(3) 0.6148(4) 0.0346(15) Uani 1 1 d . . . C32 C -0.3301(5) -0.4696(3) 0.5398(4) 0.0410(16) Uani 1 1 d . . . H32A H -0.3327 -0.4428 0.4978 0.049 Uiso 1 1 calc R . . C33 C -0.3762(5) -0.5295(3) 0.5264(5) 0.0486(19) Uani 1 1 d . . . H33A H -0.4097 -0.5432 0.4754 0.058 Uiso 1 1 calc R . . C34 C -0.3741(5) -0.5688(3) 0.5857(5) 0.051(2) Uani 1 1 d . . . H34A H -0.4057 -0.6096 0.5759 0.061 Uiso 1 1 calc R . . C35 C -0.3254(6) -0.5487(3) 0.6606(5) 0.053(2) Uani 1 1 d . . . H35A H -0.3236 -0.5757 0.7022 0.064 Uiso 1 1 calc R . . C36 C -0.2789(5) -0.4883(3) 0.6743(4) 0.0418(17) Uani 1 1 d . . . H36A H -0.2463 -0.4745 0.7254 0.050 Uiso 1 1 calc R . . C41 C -0.3438(5) -0.3204(3) 0.5969(3) 0.0309(14) Uani 1 1 d . . . C42 C -0.4479(5) -0.3425(3) 0.5954(4) 0.0386(15) Uani 1 1 d . . . H42A H -0.4558 -0.3842 0.6118 0.046 Uiso 1 1 calc R . . C43 C -0.5386(5) -0.3041(4) 0.5701(4) 0.0495(19) Uani 1 1 d . . . H43A H -0.6086 -0.3196 0.5689 0.059 Uiso 1 1 calc R . . C44 C -0.5286(6) -0.2432(4) 0.5465(4) 0.0473(18) Uani 1 1 d . . . H44A H -0.5910 -0.2167 0.5294 0.057 Uiso 1 1 calc R . . C45 C -0.4257(6) -0.2212(4) 0.5481(4) 0.0463(17) Uani 1 1 d . . . H45A H -0.4179 -0.1798 0.5310 0.056 Uiso 1 1 calc R . . C46 C -0.3354(5) -0.2593(3) 0.5744(4) 0.0380(15) Uani 1 1 d . . . H46A H -0.2653 -0.2430 0.5770 0.046 Uiso 1 1 calc R . . C51 C 0.1845(4) -0.3375(3) 0.8838(3) 0.0295(13) Uani 1 1 d . . . C52 C 0.2632(5) -0.3056(3) 0.8615(3) 0.0378(15) Uani 1 1 d . . . H52A H 0.2471 -0.2656 0.8376 0.045 Uiso 1 1 calc R . . C53 C 0.3668(5) -0.3324(3) 0.8739(4) 0.0438(17) Uani 1 1 d . . . H53A H 0.4202 -0.3108 0.8572 0.053 Uiso 1 1 calc R . . C54 C 0.3927(6) -0.3905(4) 0.9108(4) 0.054(2) Uani 1 1 d . . . H54A H 0.4632 -0.4085 0.9192 0.064 Uiso 1 1 calc R . . C55 C 0.3155(6) -0.4212(4) 0.9348(4) 0.055(2) Uani 1 1 d . . . H55A H 0.3331 -0.4604 0.9605 0.066 Uiso 1 1 calc R . . C56 C 0.2108(5) -0.3956(3) 0.9218(4) 0.0430(16) Uiso 1 1 d . . . H56A H 0.1577 -0.4173 0.9386 0.052 Uiso 1 1 calc R . . C61 C 0.0667(5) -0.2226(3) 0.8771(3) 0.0275(13) Uani 1 1 d . . . C62 C 0.0042(5) -0.1784(3) 0.8282(4) 0.0350(15) Uani 1 1 d . . . H62A H -0.0515 -0.1916 0.7835 0.042 Uiso 1 1 calc R . . C63 C 0.0222(6) -0.1138(3) 0.8436(4) 0.0421(16) Uani 1 1 d . . . H63A H -0.0205 -0.0832 0.8095 0.051 Uiso 1 1 calc R . . C64 C 0.1020(5) -0.0957(3) 0.9083(4) 0.0438(17) Uani 1 1 d . . . H64A H 0.1152 -0.0521 0.9188 0.053 Uiso 1 1 calc R . . C65 C 0.1641(5) -0.1395(3) 0.9591(4) 0.0458(18) Uani 1 1 d . . . H65A H 0.2189 -0.1259 1.0041 0.055 Uiso 1 1 calc R . . C66 C 0.1464(5) -0.2032(3) 0.9446(4) 0.0344(14) Uani 1 1 d . . . H66A H 0.1878 -0.2335 0.9798 0.041 Uiso 1 1 calc R . . C71 C -0.2937(5) -0.3922(3) 0.8275(4) 0.0349(15) Uani 1 1 d . . . C72 C -0.4028(5) -0.3947(3) 0.7829(4) 0.0472(18) Uani 1 1 d . . . H72A H -0.4352 -0.3605 0.7506 0.057 Uiso 1 1 calc R . . C73 C -0.4640(7) -0.4484(4) 0.7861(5) 0.068(3) Uani 1 1 d . . . H73A H -0.5385 -0.4503 0.7553 0.081 Uiso 1 1 calc R . . C74 C -0.4190(9) -0.4992(4) 0.8331(6) 0.074(3) Uani 1 1 d . . . H74A H -0.4617 -0.5356 0.8342 0.089 Uiso 1 1 calc R . . C75 C -0.3138(8) -0.4956(4) 0.8767(5) 0.065(2) Uani 1 1 d . . . H75A H -0.2824 -0.5296 0.9098 0.079 Uiso 1 1 calc R . . C76 C -0.2499(6) -0.4434(4) 0.8745(4) 0.0520(19) Uani 1 1 d . . . H76A H -0.1754 -0.4425 0.9053 0.062 Uiso 1 1 calc R . . C81 C -0.3004(5) -0.2593(3) 0.8059(3) 0.0310(14) Uani 1 1 d . . . C82 C -0.3046(5) -0.2131(3) 0.7524(4) 0.0357(14) Uani 1 1 d . . . H82A H -0.2622 -0.2172 0.7184 0.043 Uiso 1 1 calc R . . C83 C -0.3710(5) -0.1604(3) 0.7482(4) 0.0446(16) Uani 1 1 d . . . H83A H -0.3757 -0.1291 0.7104 0.054 Uiso 1 1 calc R . . C84 C -0.4301(5) -0.1539(4) 0.7996(4) 0.0494(18) Uani 1 1 d . . . H84A H -0.4757 -0.1182 0.7966 0.059 Uiso 1 1 calc R . . C85 C -0.4232(6) -0.1988(3) 0.8547(4) 0.0475(18) Uani 1 1 d . . . H85A H -0.4619 -0.1931 0.8908 0.057 Uiso 1 1 calc R . . C86 C -0.3608(5) -0.2518(3) 0.8578(4) 0.0424(17) Uani 1 1 d . . . H86A H -0.3582 -0.2833 0.8950 0.051 Uiso 1 1 calc R . . F1 F 0.1396(5) -0.5485(2) 0.9433(3) 0.163(3) Uani 1 1 d D . . F2 F 0.1652(6) -0.6513(2) 0.9281(4) 0.175(4) Uani 1 1 d D . . F3 F 0.1033(7) -0.5889(3) 0.8258(3) 0.228(6) Uani 1 1 d D . . F4 F 0.2769(5) -0.5804(3) 0.9010(5) 0.201(5) Uani 1 1 d D . . B1 B 0.1713(4) -0.59229(18) 0.8995(2) 0.092(4) Uani 1 1 d 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 0.02263(10) 0.02364(11) 0.02363(11) -0.00628(12) 0.00684(7) -0.00372(11) P1 0.0268(7) 0.0311(8) 0.0230(7) -0.0051(7) 0.0082(6) -0.0041(7) P2 0.0234(7) 0.0273(8) 0.0298(8) -0.0109(7) 0.0057(6) -0.0038(6) P3 0.0272(7) 0.0291(9) 0.0238(8) -0.0038(6) 0.0057(6) -0.0023(7) P4 0.0290(7) 0.0287(9) 0.0294(8) -0.0080(6) 0.0137(7) -0.0057(6) N1 0.062(4) 0.027(3) 0.069(5) 0.010(3) 0.032(4) 0.007(3) C1 0.033(3) 0.044(4) 0.026(3) -0.004(3) 0.008(3) 0.002(3) C2 0.027(3) 0.040(4) 0.025(3) -0.012(3) 0.005(2) 0.001(3) C3 0.039(3) 0.041(4) 0.024(3) -0.006(3) 0.011(3) -0.005(3) C4 0.044(4) 0.043(4) 0.024(3) -0.014(3) 0.018(3) -0.007(3) C5 0.033(3) 0.034(4) 0.043(4) -0.009(3) 0.020(3) -0.004(3) C11 0.023(3) 0.030(3) 0.039(4) -0.009(3) 0.014(3) -0.005(3) C12 0.048(4) 0.046(4) 0.034(4) -0.003(3) 0.013(3) 0.003(3) C13 0.070(5) 0.046(5) 0.049(5) -0.017(4) 0.015(4) 0.010(4) C14 0.048(4) 0.035(4) 0.056(5) -0.002(4) 0.017(4) 0.006(3) C15 0.042(4) 0.040(4) 0.042(4) -0.003(3) 0.009(3) 0.007(3) C16 0.035(3) 0.030(3) 0.031(3) -0.007(3) 0.009(3) -0.001(3) C21 0.031(3) 0.033(4) 0.026(3) -0.007(3) 0.006(3) -0.011(3) C22 0.039(4) 0.041(4) 0.043(4) -0.011(3) 0.019(3) -0.010(3) C23 0.045(4) 0.058(5) 0.059(5) -0.017(4) 0.025(4) -0.018(4) C24 0.062(5) 0.054(5) 0.077(6) -0.012(4) 0.035(5) -0.033(4) C25 0.076(6) 0.035(5) 0.076(6) 0.000(4) 0.021(5) -0.019(4) C26 0.041(4) 0.035(4) 0.052(4) 0.000(3) 0.016(3) -0.006(3) C31 0.028(3) 0.034(4) 0.042(4) -0.013(3) 0.010(3) -0.006(3) C32 0.030(3) 0.035(4) 0.050(4) -0.014(3) 0.002(3) 0.002(3) C33 0.033(3) 0.039(4) 0.067(5) -0.029(4) 0.005(3) -0.006(3) C34 0.040(4) 0.035(4) 0.082(6) -0.022(4) 0.025(4) -0.012(3) C35 0.052(4) 0.036(4) 0.080(6) -0.011(4) 0.032(4) -0.013(3) C36 0.037(3) 0.039(4) 0.055(4) -0.025(3) 0.022(3) -0.007(3) C41 0.028(3) 0.033(3) 0.027(3) -0.016(3) 0.001(2) -0.004(3) C42 0.032(3) 0.039(3) 0.044(4) -0.019(3) 0.010(3) -0.001(3) C43 0.031(3) 0.062(5) 0.050(4) -0.020(4) 0.004(3) 0.002(3) C44 0.041(4) 0.059(5) 0.036(4) -0.009(3) 0.004(3) 0.020(4) C45 0.049(4) 0.048(4) 0.039(4) 0.001(3) 0.009(3) 0.011(4) C46 0.037(3) 0.041(4) 0.035(4) -0.003(3) 0.009(3) -0.002(3) C51 0.027(3) 0.029(3) 0.031(3) -0.007(3) 0.007(2) 0.001(3) C52 0.033(3) 0.044(4) 0.030(3) -0.009(3) 0.002(3) -0.002(3) C53 0.034(3) 0.051(5) 0.046(4) -0.012(3) 0.012(3) 0.003(3) C54 0.043(4) 0.072(6) 0.039(4) -0.010(4) 0.001(3) 0.023(4) C55 0.065(5) 0.051(5) 0.040(4) 0.003(4) 0.003(4) 0.021(4) C61 0.028(3) 0.028(3) 0.025(3) -0.006(3) 0.007(2) -0.002(3) C62 0.035(3) 0.031(3) 0.034(3) -0.003(3) 0.003(3) 0.001(3) C63 0.045(4) 0.042(4) 0.042(4) -0.005(3) 0.018(3) -0.006(3) C64 0.039(4) 0.034(4) 0.058(5) -0.014(3) 0.015(3) 0.001(3) C65 0.035(3) 0.045(4) 0.053(4) -0.028(3) 0.007(3) -0.007(3) C66 0.027(3) 0.033(4) 0.041(4) -0.006(3) 0.007(3) -0.001(3) C71 0.041(4) 0.035(4) 0.036(4) -0.013(3) 0.022(3) -0.009(3) C72 0.043(4) 0.047(4) 0.060(5) -0.023(4) 0.028(4) -0.019(3) C73 0.054(5) 0.074(6) 0.091(7) -0.045(5) 0.045(5) -0.037(5) C74 0.097(7) 0.047(5) 0.101(8) -0.027(5) 0.065(6) -0.037(5) C75 0.096(7) 0.046(5) 0.074(6) -0.002(4) 0.054(6) -0.012(5) C76 0.062(5) 0.053(5) 0.052(5) -0.002(4) 0.034(4) -0.013(4) C81 0.032(3) 0.036(4) 0.030(3) -0.010(3) 0.016(3) -0.006(3) C82 0.032(3) 0.034(4) 0.042(4) -0.007(3) 0.013(3) -0.003(3) C83 0.038(3) 0.044(4) 0.049(4) -0.003(4) 0.010(3) 0.004(4) C84 0.036(3) 0.045(4) 0.066(5) -0.019(4) 0.016(3) 0.004(4) C85 0.045(4) 0.043(4) 0.062(5) -0.017(4) 0.028(4) 0.001(3) C86 0.039(4) 0.038(4) 0.055(4) -0.008(3) 0.023(3) -0.005(3) F1 0.187(8) 0.104(6) 0.184(8) -0.029(6) 0.035(7) 0.043(6) F2 0.291(11) 0.101(5) 0.193(8) 0.089(5) 0.161(8) 0.086(6) F3 0.397(15) 0.131(7) 0.083(5) 0.020(5) -0.032(8) -0.017(9) F4 0.144(7) 0.118(7) 0.329(14) -0.022(8) 0.054(8) 0.009(6) B1 0.115(11) 0.094(10) 0.051(7) 0.016(7) 0.004(7) -0.029(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 H1OS 1.70(5) . ? Os1 C5 1.983(7) . ? Os1 P1 2.3380(14) . ? Os1 P2 2.3434(15) . ? Os1 P3 2.3499(15) . ? Os1 P4 2.3539(15) . ? P1 C11 1.818(6) . ? P1 C1 1.837(6) . ? P1 C21 1.853(6) . ? P2 C41 1.827(6) . ? P2 C31 1.828(6) . ? P2 C2 1.861(6) . ? P3 C51 1.827(6) . ? P3 C3 1.839(6) . ? P3 C61 1.840(6) . ? P4 C71 1.828(6) . ? P4 C81 1.848(6) . ? P4 C4 1.854(6) . ? N1 H1N 0.954(10) . ? N1 C5 1.162(8) . ? H1N F3 2.09(6) . ? C1 C2 1.507(8) . ? C3 C4 1.515(8) . ? C11 C12 1.385(8) . ? C11 C16 1.393(8) . ? C12 C13 1.373(9) . ? C13 C14 1.338(9) . ? C14 C15 1.391(9) . ? C15 C16 1.383(8) . ? C21 C26 1.391(9) . ? C21 C22 1.396(8) . ? C22 C23 1.387(9) . ? C23 C24 1.380(10) . ? C24 C25 1.376(11) . ? C25 C26 1.388(9) . ? C31 C36 1.377(9) . ? C31 C32 1.403(8) . ? C32 C33 1.391(9) . ? C33 C34 1.366(10) . ? C34 C35 1.391(10) . ? C35 C36 1.405(9) . ? C41 C46 1.376(9) . ? C41 C42 1.408(8) . ? C42 C43 1.380(9) . ? C43 C44 1.382(10) . ? C44 C45 1.391(10) . ? C45 C46 1.372(9) . ? C51 C52 1.379(8) . ? C51 C56 1.406(9) . ? C52 C53 1.397(8) . ? C53 C54 1.398(10) . ? C54 C55 1.365(11) . ? C55 C56 1.400(9) . ? C61 C62 1.375(8) . ? C61 C66 1.405(8) . ? C62 C63 1.405(9) . ? C63 C64 1.365(9) . ? C64 C65 1.384(9) . ? C65 C66 1.383(9) . ? C71 C72 1.388(9) . ? C71 C76 1.393(10) . ? C72 C73 1.395(10) . ? C73 C74 1.392(13) . ? C74 C75 1.343(12) . ? C75 C76 1.387(10) . ? C81 C82 1.378(9) . ? C81 C86 1.411(8) . ? C82 C83 1.394(9) . ? C83 C84 1.388(10) . ? C84 C85 1.372(10) . ? C85 C86 1.372(9) . ? F1 B1 1.3698(9) . ? F2 B1 1.3698(9) . ? F3 B1 1.3698(9) . ? F4 B1 1.3699(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 H1OS Os1 C5 171.9(18) . . ? H1OS Os1 P1 77.5(18) . . ? C5 Os1 P1 95.45(17) . . ? H1OS Os1 P2 86.0(18) . . ? C5 Os1 P2 97.33(19) . . ? P1 Os1 P2 83.17(5) . . ? H1OS Os1 P3 90.4(18) . . ? C5 Os1 P3 86.38(19) . . ? P1 Os1 P3 96.84(5) . . ? P2 Os1 P3 176.27(6) . . ? H1OS Os1 P4 92.8(18) . . ? C5 Os1 P4 94.08(17) . . ? P1 Os1 P4 170.30(6) . . ? P2 Os1 P4 97.43(5) . . ? P3 Os1 P4 81.94(5) . . ? C11 P1 C1 104.9(3) . . ? C11 P1 C21 103.5(3) . . ? C1 P1 C21 98.8(3) . . ? C11 P1 Os1 117.6(2) . . ? C1 P1 Os1 106.6(2) . . ? C21 P1 Os1 122.7(2) . . ? C41 P2 C31 101.6(3) . . ? C41 P2 C2 101.6(3) . . ? C31 P2 C2 99.7(3) . . ? C41 P2 Os1 119.06(18) . . ? C31 P2 Os1 122.0(2) . . ? C2 P2 Os1 109.43(18) . . ? C51 P3 C3 104.3(3) . . ? C51 P3 C61 102.1(3) . . ? C3 P3 C61 102.5(3) . . ? C51 P3 Os1 119.92(19) . . ? C3 P3 Os1 106.0(2) . . ? C61 P3 Os1 119.80(19) . . ? C71 P4 C81 101.5(3) . . ? C71 P4 C4 104.6(3) . . ? C81 P4 C4 98.6(3) . . ? C71 P4 Os1 117.6(2) . . ? C81 P4 Os1 122.6(2) . . ? C4 P4 Os1 109.13(19) . . ? H1N N1 C5 157(5) . . ? N1 H1N F3 127(6) . . ? C2 C1 P1 110.3(4) . . ? C1 C2 P2 111.7(4) . . ? C4 C3 P3 107.4(4) . . ? C3 C4 P4 112.0(4) . . ? N1 C5 Os1 178.5(6) . . ? C12 C11 C16 117.2(6) . . ? C12 C11 P1 123.5(5) . . ? C16 C11 P1 119.4(5) . . ? C13 C12 C11 119.3(7) . . ? C14 C13 C12 124.1(7) . . ? C13 C14 C15 118.0(7) . . ? C16 C15 C14 119.2(6) . . ? C15 C16 C11 122.2(6) . . ? C26 C21 C22 120.3(6) . . ? C26 C21 P1 117.2(5) . . ? C22 C21 P1 122.4(5) . . ? C23 C22 C21 119.1(7) . . ? C24 C23 C22 121.0(7) . . ? C25 C24 C23 119.4(7) . . ? C24 C25 C26 121.1(7) . . ? C25 C26 C21 119.1(7) . . ? C36 C31 C32 118.3(6) . . ? C36 C31 P2 121.7(5) . . ? C32 C31 P2 119.9(5) . . ? C33 C32 C31 120.4(7) . . ? C34 C33 C32 121.0(7) . . ? C33 C34 C35 119.7(7) . . ? C34 C35 C36 119.6(8) . . ? C31 C36 C35 121.1(7) . . ? C46 C41 C42 118.0(6) . . ? C46 C41 P2 120.2(5) . . ? C42 C41 P2 121.7(5) . . ? C43 C42 C41 120.4(7) . . ? C42 C43 C44 120.6(7) . . ? C43 C44 C45 119.1(7) . . ? C46 C45 C44 120.2(7) . . ? C45 C46 C41 121.7(6) . . ? C52 C51 C56 119.5(6) . . ? C52 C51 P3 120.4(5) . . ? C56 C51 P3 119.9(5) . . ? C51 C52 C53 119.9(6) . . ? C52 C53 C54 120.7(7) . . ? C55 C54 C53 119.3(7) . . ? C54 C55 C56 120.8(7) . . ? C55 C56 C51 119.7(7) . . ? C62 C61 C66 119.8(6) . . ? C62 C61 P3 121.4(4) . . ? C66 C61 P3 118.7(5) . . ? C61 C62 C63 120.6(6) . . ? C64 C63 C62 118.8(7) . . ? C63 C64 C65 121.4(6) . . ? C66 C65 C64 120.1(6) . . ? C65 C66 C61 119.2(6) . . ? C72 C71 C76 118.5(6) . . ? C72 C71 P4 121.5(6) . . ? C76 C71 P4 119.8(5) . . ? C71 C72 C73 119.0(8) . . ? C74 C73 C72 121.9(8) . . ? C75 C74 C73 118.4(8) . . ? C74 C75 C76 121.5(9) . . ? C75 C76 C71 120.8(8) . . ? C82 C81 C86 119.5(6) . . ? C82 C81 P4 122.1(4) . . ? C86 C81 P4 117.9(5) . . ? C81 C82 C83 120.0(6) . . ? C84 C83 C82 119.6(7) . . ? C85 C84 C83 120.5(7) . . ? C84 C85 C86 120.3(7) . . ? C85 C86 C81 120.0(7) . . ? B1 F3 H1N 95.7(15) . . ? F3 B1 F1 109.37(9) . . ? F3 B1 F4 109.52(9) . . ? F1 B1 F4 109.48(9) . . ? F3 B1 F2 109.45(9) . . ? F1 B1 F2 109.55(9) . . ? F4 B1 F2 109.45(9) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.098 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.125 data_s9743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H2 H48 F3 N O3 P4 Ru S' _chemical_formula_weight 1074.96 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' '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' 'Ru' 'Ru' -1.2594 0.8363 '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' '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 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 16.536(4) _cell_length_b 17.005(2) _cell_length_c 22.280(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.73(2) _cell_angle_gamma 90.00 _cell_volume 6222(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 12.54 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8458 _exptl_absorpt_correction_T_max 0.8774 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1997)' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.43 _diffrn_reflns_number 9532 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9202 _reflns_number_gt 7335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0755P)^2^+3.7660P] 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 9202 _refine_ls_number_parameters 647 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.513753(17) 0.230441(17) 0.772020(13) 0.02232(12) Uani 1 1 d . A . H1RU H 0.465(3) 0.258(3) 0.713(2) 0.051(13) Uiso 1 1 d . . . P1 P 0.61183(6) 0.24968(6) 0.70568(5) 0.0253(2) Uani 1 1 d . . . P2 P 0.49371(6) 0.10975(6) 0.72114(5) 0.0270(2) Uani 1 1 d . . . P3 P 0.53023(6) 0.35275(6) 0.81890(5) 0.0288(3) Uani 1 1 d . . . P4 P 0.39735(6) 0.22759(6) 0.82301(5) 0.0264(2) Uani 1 1 d . . . N1 N 0.6293(2) 0.1635(2) 0.88326(16) 0.0373(9) Uani 1 1 d D A . H1N H 0.668(2) 0.147(2) 0.9109(17) 0.045 Uiso 1 1 d D . . C1 C 0.5752(2) 0.1929(2) 0.63822(18) 0.0304(9) Uani 1 1 d . . . H1A H 0.5259 0.2179 0.6171 0.036 Uiso 1 1 calc R . . H1B H 0.6175 0.1916 0.6102 0.036 Uiso 1 1 calc R . . C2 C 0.5556(2) 0.1099(2) 0.65652(18) 0.0324(10) Uani 1 1 d . . . H2A H 0.6070 0.0808 0.6680 0.039 Uiso 1 1 calc R . . H2B H 0.5253 0.0825 0.6217 0.039 Uiso 1 1 calc R . . C3 C 0.4868(2) 0.3430(2) 0.89131(19) 0.0356(10) Uani 1 1 d . . . H3A H 0.5201 0.3065 0.9186 0.043 Uiso 1 1 calc R . . H3B H 0.4857 0.3948 0.9115 0.043 Uiso 1 1 calc R . . C4 C 0.4015(2) 0.3114(3) 0.8767(2) 0.0373(10) Uani 1 1 d . . . H4A H 0.3654 0.3540 0.8590 0.045 Uiso 1 1 calc R . . H4B H 0.3809 0.2940 0.9145 0.045 Uiso 1 1 calc R . . C5 C 0.5866(2) 0.1872(2) 0.84214(19) 0.0295(9) Uani 1 1 d . . . C11 C 0.7159(2) 0.2149(2) 0.72684(19) 0.0285(10) Uani 1 1 d . . . C12 C 0.7618(2) 0.1773(2) 0.6865(2) 0.0373(10) Uani 1 1 d . . . H12A H 0.7385 0.1680 0.6461 0.045 Uiso 1 1 calc R . . C13 C 0.8404(3) 0.1536(3) 0.7045(2) 0.0481(12) Uani 1 1 d . . . H13A H 0.8708 0.1285 0.6763 0.058 Uiso 1 1 calc R . . C14 C 0.8755(3) 0.1656(3) 0.7624(2) 0.0464(12) Uani 1 1 d . . . H14A H 0.9294 0.1479 0.7748 0.056 Uiso 1 1 calc R . . C15 C 0.8320(3) 0.2037(3) 0.8024(2) 0.0452(12) Uani 1 1 d . . . H15A H 0.8563 0.2131 0.8425 0.054 Uiso 1 1 calc R . . C16 C 0.7529(2) 0.2285(2) 0.78489(19) 0.0352(10) Uani 1 1 d . . . H16A H 0.7238 0.2552 0.8131 0.042 Uiso 1 1 calc R . . C21 C 0.6286(2) 0.3463(2) 0.67416(17) 0.0292(9) Uani 1 1 d . . . C22 C 0.7051(3) 0.3793(3) 0.6750(2) 0.0394(10) Uani 1 1 d . . . H22A H 0.7516 0.3502 0.6914 0.047 Uiso 1 1 calc R . . C23 C 0.7153(3) 0.4546(3) 0.6520(2) 0.0506(13) Uani 1 1 d . . . H23A H 0.7682 0.4767 0.6535 0.061 Uiso 1 1 calc R . . C24 C 0.6491(3) 0.4966(3) 0.6275(2) 0.0543(13) Uani 1 1 d . . . H24A H 0.6559 0.5480 0.6122 0.065 Uiso 1 1 calc R . . C25 C 0.5720(3) 0.4642(3) 0.6251(2) 0.0546(13) Uani 1 1 d . . . H25A H 0.5260 0.4931 0.6076 0.066 Uiso 1 1 calc R . . C26 C 0.5617(3) 0.3899(3) 0.6481(2) 0.0430(11) Uani 1 1 d . . . H26A H 0.5086 0.3681 0.6462 0.052 Uiso 1 1 calc R . . C31 C 0.5261(2) 0.0161(2) 0.7574(2) 0.0347(10) Uani 1 1 d . . . C32 C 0.5447(3) -0.0474(2) 0.7225(2) 0.0461(12) Uani 1 1 d . . . H32A H 0.5417 -0.0418 0.6798 0.055 Uiso 1 1 calc R . . C33 C 0.5676(3) -0.1194(3) 0.7491(3) 0.0523(14) Uani 1 1 d . . . H33A H 0.5791 -0.1629 0.7247 0.063 Uiso 1 1 calc R . . C34 C 0.5736(3) -0.1271(3) 0.8108(3) 0.0570(15) Uani 1 1 d . . . H34A H 0.5912 -0.1755 0.8292 0.068 Uiso 1 1 calc R . . C35 C 0.5544(3) -0.0659(3) 0.8455(3) 0.0523(13) Uani 1 1 d . . . H35A H 0.5572 -0.0725 0.8881 0.063 Uiso 1 1 calc R . . C36 C 0.5307(2) 0.0067(2) 0.8198(2) 0.0396(11) Uani 1 1 d . . . H36A H 0.5178 0.0492 0.8447 0.048 Uiso 1 1 calc R . . C41 C 0.3917(2) 0.0821(2) 0.68460(18) 0.0297(9) Uani 1 1 d . . . C42 C 0.3514(3) 0.0151(3) 0.7017(2) 0.0430(11) Uani 1 1 d . . . H42A H 0.3765 -0.0176 0.7332 0.052 Uiso 1 1 calc R . . C43 C 0.2753(3) -0.0040(3) 0.6733(3) 0.0549(13) Uani 1 1 d . . . H43A H 0.2476 -0.0489 0.6859 0.066 Uiso 1 1 calc R . . C44 C 0.2400(3) 0.0411(3) 0.6273(2) 0.0521(13) Uani 1 1 d . . . H44A H 0.1880 0.0269 0.6075 0.063 Uiso 1 1 calc R . . C45 C 0.2785(3) 0.1074(3) 0.6090(2) 0.0514(13) Uani 1 1 d . . . H45A H 0.2531 0.1390 0.5770 0.062 Uiso 1 1 calc R . . C46 C 0.3548(2) 0.1278(3) 0.6377(2) 0.0402(11) Uani 1 1 d . . . H46A H 0.3818 0.1731 0.6250 0.048 Uiso 1 1 calc R . . C51 C 0.6321(2) 0.3911(2) 0.84302(19) 0.0303(9) Uani 1 1 d . . . C52 C 0.6691(2) 0.4426(2) 0.8071(2) 0.0350(10) Uani 1 1 d . . . H52A H 0.6399 0.4615 0.7707 0.042 Uiso 1 1 calc R . . C53 C 0.7485(3) 0.4673(3) 0.8234(2) 0.0423(11) Uani 1 1 d . . . H53A H 0.7737 0.5023 0.7980 0.051 Uiso 1 1 calc R . . C54 C 0.7910(3) 0.4409(3) 0.8766(2) 0.0473(12) Uani 1 1 d . . . H54A H 0.8452 0.4582 0.8882 0.057 Uiso 1 1 calc R . . C55 C 0.7546(3) 0.3894(3) 0.9132(2) 0.0444(12) Uani 1 1 d . . . H55A H 0.7843 0.3715 0.9497 0.053 Uiso 1 1 calc R . . C56 C 0.6764(3) 0.3637(2) 0.8975(2) 0.0389(10) Uani 1 1 d . . . H56A H 0.6521 0.3281 0.9229 0.047 Uiso 1 1 calc R . . C61 C 0.4749(2) 0.4389(2) 0.78705(19) 0.0315(9) Uani 1 1 d . . . C62 C 0.4188(2) 0.4318(3) 0.7360(2) 0.0424(11) Uani 1 1 d . . . H62A H 0.4103 0.3823 0.7165 0.051 Uiso 1 1 calc R . . C63 C 0.3747(3) 0.4977(3) 0.7132(3) 0.0559(14) Uani 1 1 d . . . H63A H 0.3363 0.4934 0.6782 0.067 Uiso 1 1 calc R . . C64 C 0.3876(3) 0.5694(3) 0.7425(3) 0.0588(15) Uani 1 1 d . . . H64A H 0.3579 0.6143 0.7271 0.071 Uiso 1 1 calc R . . C65 C 0.4421(3) 0.5764(3) 0.7931(2) 0.0504(13) Uani 1 1 d . . . H65A H 0.4495 0.6257 0.8130 0.060 Uiso 1 1 calc R . . C66 C 0.4862(3) 0.5121(2) 0.8152(2) 0.0409(11) Uani 1 1 d . . . H66A H 0.5249 0.5175 0.8500 0.049 Uiso 1 1 calc R . . C71 C 0.3845(2) 0.1417(2) 0.87006(19) 0.0335(10) Uani 1 1 d . . . C72 C 0.3368(3) 0.0791(2) 0.8482(2) 0.0407(11) Uani 1 1 d . . . H72A H 0.3058 0.0827 0.8096 0.049 Uiso 1 1 calc R . . C73 C 0.3337(3) 0.0106(3) 0.8824(3) 0.0604(15) Uani 1 1 d . . . H73A H 0.3006 -0.0325 0.8676 0.072 Uiso 1 1 calc R . . C74 C 0.3800(3) 0.0068(3) 0.9385(3) 0.0669(16) Uani 1 1 d . . . H74A H 0.3792 -0.0397 0.9621 0.080 Uiso 1 1 calc R . . C75 C 0.4262(3) 0.0689(3) 0.9601(3) 0.0629(15) Uani 1 1 d . . . H75A H 0.4561 0.0659 0.9991 0.076 Uiso 1 1 calc R . . C76 C 0.4304(3) 0.1356(3) 0.9264(2) 0.0448(12) Uani 1 1 d . . . H76A H 0.4647 0.1778 0.9414 0.054 Uiso 1 1 calc R . . C81 C 0.2944(2) 0.2452(2) 0.78531(19) 0.0275(9) Uani 1 1 d . . . C82 C 0.2803(2) 0.2650(2) 0.7247(2) 0.0350(10) Uani 1 1 d . . . H82A H 0.3234 0.2627 0.7000 0.042 Uiso 1 1 calc R . . C83 C 0.2031(3) 0.2880(3) 0.7001(2) 0.0485(12) Uani 1 1 d . . . H83A H 0.1936 0.3004 0.6583 0.058 Uiso 1 1 calc R . . C84 C 0.1408(3) 0.2932(3) 0.7345(3) 0.0498(13) Uani 1 1 d . . . H84A H 0.0884 0.3097 0.7169 0.060 Uiso 1 1 calc R . . C85 C 0.1536(3) 0.2747(3) 0.7947(2) 0.0449(12) Uani 1 1 d . . . H85A H 0.1102 0.2787 0.8190 0.054 Uiso 1 1 calc R . . C86 C 0.2297(2) 0.2501(2) 0.8200(2) 0.0379(11) Uani 1 1 d . . . H86A H 0.2381 0.2363 0.8616 0.045 Uiso 1 1 calc R . . S1 S 0.77651(12) 0.16298(13) 1.01965(9) 0.0493(6) Uani 0.828(5) 1 d PD A 1 O1 O 0.7849(4) 0.1306(4) 1.07971(19) 0.110(3) Uani 0.828(5) 1 d PD A 1 O2 O 0.7489(4) 0.2421(3) 1.0122(3) 0.107(2) Uani 0.828(5) 1 d PD A 1 O3 O 0.7404(2) 0.1111(2) 0.97275(16) 0.0500(12) Uani 0.828(5) 1 d PD A 1 C1S C 0.8785(4) 0.1708(4) 1.0054(2) 0.073(2) Uani 0.828(5) 1 d PD A 1 F1 F 0.8839(3) 0.1970(4) 0.9509(2) 0.140(3) Uani 0.828(5) 1 d PD A 1 F2 F 0.9235(3) 0.2154(3) 1.04433(19) 0.1005(18) Uani 0.828(5) 1 d PD A 1 F3 F 0.9176(4) 0.1042(5) 1.0090(4) 0.124(3) Uani 0.828(5) 1 d PD A 1 S1* S 0.7916(7) 0.1864(7) 1.0056(5) 0.058(4) Uiso 0.172(5) 1 d PD A 2 O1* O 0.7240(10) 0.1901(15) 1.0406(9) 0.061(6) Uiso 0.172(5) 1 d PD A 2 O2* O 0.841(2) 0.2558(16) 1.0084(19) 0.137(13) Uiso 0.172(5) 1 d PD A 2 O3* O 0.7741(13) 0.1624(13) 0.9438(6) 0.065(6) Uiso 0.172(5) 1 d PD A 2 C1S* C 0.8555(16) 0.1158(14) 1.0439(11) 0.070(10) Uiso 0.172(5) 1 d PD A 2 F1* F 0.862(2) 0.133(2) 1.1013(13) 0.157(13) Uiso 0.172(5) 1 d PD A 2 F2* F 0.808(2) 0.056(2) 1.0477(18) 0.167(14) Uiso 0.172(5) 1 d PD A 2 F3* F 0.9057(18) 0.0779(16) 1.0132(15) 0.060(8) Uiso 0.172(5) 1 d PD A 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 0.02174(16) 0.02221(17) 0.0232(2) 0.00057(13) 0.00334(13) -0.00075(12) P1 0.0240(5) 0.0257(5) 0.0265(6) 0.0013(4) 0.0042(4) 0.0010(4) P2 0.0243(5) 0.0251(5) 0.0314(6) -0.0021(4) 0.0021(4) 0.0001(4) P3 0.0300(5) 0.0256(5) 0.0318(6) -0.0010(5) 0.0081(5) -0.0032(4) P4 0.0244(5) 0.0282(5) 0.0272(6) 0.0001(4) 0.0050(4) -0.0034(4) N1 0.0340(19) 0.039(2) 0.036(2) 0.0060(17) -0.0076(17) -0.0008(16) C1 0.031(2) 0.039(2) 0.022(2) -0.0032(18) 0.0055(17) 0.0005(18) C2 0.029(2) 0.034(2) 0.034(2) -0.0110(19) 0.0035(18) -0.0020(17) C3 0.037(2) 0.038(2) 0.033(2) -0.0050(19) 0.0087(19) -0.0099(19) C4 0.038(2) 0.039(2) 0.037(3) -0.006(2) 0.009(2) -0.0048(19) C5 0.0266(19) 0.029(2) 0.034(2) -0.0003(19) 0.0079(19) -0.0080(17) C11 0.0244(19) 0.0215(19) 0.039(2) 0.0060(18) 0.0023(19) -0.0034(15) C12 0.037(2) 0.041(2) 0.033(2) -0.004(2) 0.005(2) 0.0030(19) C13 0.032(2) 0.042(3) 0.072(4) -0.009(2) 0.011(2) 0.009(2) C14 0.027(2) 0.037(2) 0.075(4) 0.008(2) 0.003(2) 0.0069(19) C15 0.036(2) 0.052(3) 0.045(3) 0.012(2) -0.004(2) -0.002(2) C16 0.032(2) 0.042(2) 0.032(2) 0.004(2) 0.0059(19) -0.0005(19) C21 0.036(2) 0.030(2) 0.023(2) 0.0030(17) 0.0118(18) 0.0075(17) C22 0.036(2) 0.037(2) 0.046(3) 0.005(2) 0.011(2) -0.0009(19) C23 0.054(3) 0.038(3) 0.063(3) 0.013(2) 0.021(3) -0.005(2) C24 0.070(3) 0.042(3) 0.056(3) 0.016(2) 0.025(3) 0.001(3) C25 0.065(3) 0.043(3) 0.057(3) 0.018(3) 0.012(3) 0.018(2) C26 0.040(2) 0.048(3) 0.042(3) 0.012(2) 0.008(2) 0.003(2) C31 0.0252(19) 0.028(2) 0.050(3) 0.002(2) 0.0006(19) -0.0032(16) C32 0.047(3) 0.027(2) 0.068(3) -0.003(2) 0.020(2) 0.0030(19) C33 0.045(3) 0.027(2) 0.091(5) -0.001(3) 0.031(3) 0.006(2) C34 0.033(2) 0.033(3) 0.105(5) 0.023(3) 0.009(3) 0.006(2) C35 0.044(3) 0.040(3) 0.071(4) 0.016(3) -0.005(3) -0.001(2) C36 0.035(2) 0.030(2) 0.051(3) 0.004(2) -0.003(2) -0.0033(18) C41 0.027(2) 0.034(2) 0.028(2) -0.0109(18) 0.0039(18) 0.0013(17) C42 0.035(2) 0.039(2) 0.055(3) -0.007(2) 0.008(2) -0.0037(19) C43 0.037(2) 0.056(3) 0.072(4) -0.008(3) 0.005(3) -0.012(2) C44 0.028(2) 0.068(3) 0.059(3) -0.015(3) -0.004(2) -0.006(2) C45 0.038(2) 0.061(3) 0.052(3) -0.008(3) -0.008(2) 0.004(2) C46 0.034(2) 0.041(2) 0.045(3) -0.009(2) 0.004(2) 0.0017(19) C51 0.033(2) 0.0242(19) 0.035(2) -0.0040(19) 0.0091(19) -0.0020(17) C52 0.031(2) 0.033(2) 0.040(3) 0.000(2) 0.005(2) -0.0007(18) C53 0.041(2) 0.040(2) 0.047(3) -0.001(2) 0.011(2) -0.009(2) C54 0.039(2) 0.048(3) 0.055(3) -0.004(2) 0.001(2) -0.015(2) C55 0.042(2) 0.051(3) 0.038(3) -0.003(2) -0.003(2) -0.005(2) C56 0.047(3) 0.037(2) 0.034(2) 0.000(2) 0.008(2) -0.006(2) C61 0.029(2) 0.031(2) 0.036(2) 0.0023(19) 0.0128(19) 0.0009(17) C62 0.033(2) 0.034(2) 0.061(3) 0.004(2) 0.008(2) 0.0030(19) C63 0.037(2) 0.051(3) 0.077(4) 0.014(3) -0.006(2) 0.009(2) C64 0.051(3) 0.033(3) 0.093(4) 0.014(3) 0.010(3) 0.011(2) C65 0.037(2) 0.036(2) 0.079(4) -0.001(2) 0.011(3) 0.004(2) C66 0.037(2) 0.031(2) 0.056(3) -0.004(2) 0.013(2) 0.0018(19) C71 0.027(2) 0.038(2) 0.036(2) 0.007(2) 0.0079(18) -0.0011(17) C72 0.036(2) 0.039(2) 0.048(3) 0.014(2) 0.005(2) -0.0050(19) C73 0.048(3) 0.045(3) 0.087(4) 0.020(3) 0.005(3) -0.009(2) C74 0.062(3) 0.065(3) 0.073(4) 0.048(3) 0.002(3) 0.000(3) C75 0.060(3) 0.071(4) 0.055(3) 0.022(3) -0.002(3) -0.005(3) C76 0.050(3) 0.052(3) 0.032(3) 0.015(2) 0.003(2) -0.007(2) C81 0.0222(18) 0.0228(19) 0.037(2) -0.0002(17) 0.0037(18) -0.0003(15) C82 0.031(2) 0.036(2) 0.038(3) 0.002(2) 0.0038(19) 0.0021(18) C83 0.039(3) 0.053(3) 0.051(3) 0.006(2) -0.005(2) 0.007(2) C84 0.028(2) 0.045(3) 0.074(4) 0.004(3) -0.002(2) 0.008(2) C85 0.032(2) 0.049(3) 0.057(3) -0.005(2) 0.016(2) 0.002(2) C86 0.033(2) 0.036(2) 0.045(3) 0.002(2) 0.007(2) -0.0032(18) S1 0.0570(11) 0.0510(11) 0.0386(11) -0.0025(9) 0.0001(9) -0.0089(9) O1 0.151(6) 0.142(6) 0.035(3) 0.011(3) 0.008(3) -0.074(5) O2 0.125(5) 0.053(3) 0.135(6) -0.032(4) -0.022(4) 0.032(3) O3 0.052(2) 0.047(2) 0.045(2) -0.0018(19) -0.0180(19) -0.0052(18) C1S 0.071(5) 0.093(6) 0.052(5) -0.009(4) -0.014(4) -0.021(5) F1 0.128(5) 0.248(8) 0.046(3) 0.001(4) 0.015(3) -0.096(5) F2 0.092(3) 0.135(4) 0.071(3) -0.030(3) -0.006(2) -0.056(3) F3 0.057(3) 0.141(8) 0.165(7) -0.065(6) -0.023(3) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 H1RU 1.53(5) . ? Ru1 C5 1.998(4) . ? Ru1 P3 2.3290(11) . ? Ru1 P1 2.3418(13) . ? Ru1 P4 2.3475(12) . ? Ru1 P2 2.3493(11) . ? P1 C21 1.820(4) . ? P1 C11 1.828(4) . ? P1 C1 1.829(4) . ? P2 C31 1.838(4) . ? P2 C41 1.846(4) . ? P2 C2 1.862(4) . ? P3 C61 1.826(4) . ? P3 C51 1.828(4) . ? P3 C3 1.848(4) . ? P4 C71 1.824(4) . ? P4 C81 1.833(4) . ? P4 C4 1.857(4) . ? N1 H1N 0.88(3) . ? N1 C5 1.161(5) . ? H1N O3 1.82(3) . ? H1N O3* 1.84(4) . ? C1 C2 1.514(6) . ? C3 C4 1.510(5) . ? C11 C16 1.384(6) . ? C11 C12 1.398(6) . ? C12 C13 1.375(6) . ? C13 C14 1.365(7) . ? C14 C15 1.372(7) . ? C15 C16 1.386(6) . ? C21 C22 1.383(6) . ? C21 C26 1.400(6) . ? C22 C23 1.397(6) . ? C23 C24 1.366(7) . ? C24 C25 1.384(7) . ? C25 C26 1.381(6) . ? C31 C32 1.387(6) . ? C31 C36 1.392(6) . ? C32 C33 1.393(6) . ? C33 C34 1.373(8) . ? C34 C35 1.356(7) . ? C35 C36 1.398(6) . ? C41 C46 1.384(6) . ? C41 C42 1.397(6) . ? C42 C43 1.379(6) . ? C43 C44 1.356(7) . ? C44 C45 1.381(7) . ? C45 C46 1.390(6) . ? C51 C52 1.378(6) . ? C51 C56 1.421(6) . ? C52 C53 1.386(6) . ? C53 C54 1.381(6) . ? C54 C55 1.380(7) . ? C55 C56 1.370(6) . ? C61 C62 1.386(6) . ? C61 C66 1.396(6) . ? C62 C63 1.399(6) . ? C63 C64 1.388(7) . ? C64 C65 1.363(7) . ? C65 C66 1.373(6) . ? C71 C72 1.380(6) . ? C71 C76 1.393(6) . ? C72 C73 1.397(6) . ? C73 C74 1.390(8) . ? C74 C75 1.359(8) . ? C75 C76 1.367(7) . ? C81 C82 1.385(6) . ? C81 C86 1.394(6) . ? C82 C83 1.385(6) . ? C83 C84 1.357(7) . ? C84 C85 1.371(7) . ? C85 C86 1.383(6) . ? S1 O2 1.425(4) . ? S1 O1 1.438(4) . ? S1 O3 1.443(3) . ? S1 C1S 1.757(8) . ? C1S F3 1.302(6) . ? C1S F1 1.305(5) . ? C1S F2 1.316(5) . ? S1* O2* 1.431(6) . ? S1* O3* 1.432(6) . ? S1* O1* 1.438(6) . ? S1* C1S* 1.753(10) . ? C1S* F2* 1.304(7) . ? C1S* F3* 1.306(7) . ? C1S* F1* 1.306(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 H1RU Ru1 C5 172.7(17) . . ? H1RU Ru1 P3 97.8(17) . . ? C5 Ru1 P3 87.14(11) . . ? H1RU Ru1 P1 75.8(17) . . ? C5 Ru1 P1 98.41(12) . . ? P3 Ru1 P1 96.03(4) . . ? H1RU Ru1 P4 92.1(17) . . ? C5 Ru1 P4 93.86(12) . . ? P3 Ru1 P4 82.00(4) . . ? P1 Ru1 P4 167.46(4) . . ? H1RU Ru1 P2 79.7(17) . . ? C5 Ru1 P2 95.37(11) . . ? P3 Ru1 P2 177.48(4) . . ? P1 Ru1 P2 83.48(4) . . ? P4 Ru1 P2 97.94(4) . . ? C21 P1 C11 102.13(17) . . ? C21 P1 C1 102.15(18) . . ? C11 P1 C1 104.58(18) . . ? C21 P1 Ru1 121.17(13) . . ? C11 P1 Ru1 119.51(14) . . ? C1 P1 Ru1 104.95(14) . . ? C31 P2 C41 100.23(18) . . ? C31 P2 C2 100.54(19) . . ? C41 P2 C2 102.50(18) . . ? C31 P2 Ru1 121.85(14) . . ? C41 P2 Ru1 120.33(13) . . ? C2 P2 Ru1 108.23(13) . . ? C61 P3 C51 103.35(18) . . ? C61 P3 C3 100.5(2) . . ? C51 P3 C3 102.36(19) . . ? C61 P3 Ru1 121.02(14) . . ? C51 P3 Ru1 120.36(13) . . ? C3 P3 Ru1 105.94(14) . . ? C71 P4 C81 103.27(18) . . ? C71 P4 C4 104.0(2) . . ? C81 P4 C4 97.57(18) . . ? C71 P4 Ru1 116.88(14) . . ? C81 P4 Ru1 123.04(14) . . ? C4 P4 Ru1 109.01(14) . . ? H1N N1 C5 171(3) . . ? N1 H1N O3 174(4) . . ? N1 H1N O3* 145(4) . . ? O3 H1N O3* 40.1(9) . . ? C2 C1 P1 109.4(3) . . ? C1 C2 P2 111.3(3) . . ? C4 C3 P3 107.0(3) . . ? C3 C4 P4 112.0(3) . . ? N1 C5 Ru1 178.7(4) . . ? C16 C11 C12 117.6(4) . . ? C16 C11 P1 119.1(3) . . ? C12 C11 P1 123.3(3) . . ? C13 C12 C11 120.8(4) . . ? C14 C13 C12 121.0(5) . . ? C13 C14 C15 119.2(4) . . ? C14 C15 C16 120.6(4) . . ? C11 C16 C15 120.8(4) . . ? C22 C21 C26 117.9(4) . . ? C22 C21 P1 122.8(3) . . ? C26 C21 P1 119.3(3) . . ? C21 C22 C23 121.1(4) . . ? C24 C23 C22 120.1(5) . . ? C23 C24 C25 119.9(4) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C21 120.9(4) . . ? C32 C31 C36 118.8(4) . . ? C32 C31 P2 120.0(4) . . ? C36 C31 P2 121.2(3) . . ? C31 C32 C33 120.8(5) . . ? C34 C33 C32 119.6(5) . . ? C35 C34 C33 120.3(4) . . ? C34 C35 C36 121.1(5) . . ? C31 C36 C35 119.4(4) . . ? C46 C41 C42 118.8(4) . . ? C46 C41 P2 119.3(3) . . ? C42 C41 P2 121.9(3) . . ? C43 C42 C41 120.4(5) . . ? C44 C43 C42 120.2(5) . . ? C43 C44 C45 120.8(4) . . ? C44 C45 C46 119.5(5) . . ? C41 C46 C45 120.3(4) . . ? C52 C51 C56 119.0(4) . . ? C52 C51 P3 120.9(3) . . ? C56 C51 P3 120.0(3) . . ? C51 C52 C53 120.8(4) . . ? C54 C53 C52 119.8(4) . . ? C55 C54 C53 120.0(4) . . ? C56 C55 C54 121.0(4) . . ? C55 C56 C51 119.3(4) . . ? C62 C61 C66 119.2(4) . . ? C62 C61 P3 120.4(3) . . ? C66 C61 P3 120.4(3) . . ? C61 C62 C63 119.9(4) . . ? C64 C63 C62 119.2(5) . . ? C65 C64 C63 121.0(4) . . ? C64 C65 C66 119.9(5) . . ? C65 C66 C61 120.8(4) . . ? C72 C71 C76 119.3(4) . . ? C72 C71 P4 121.0(3) . . ? C76 C71 P4 119.3(3) . . ? C71 C72 C73 120.5(4) . . ? C74 C73 C72 118.6(5) . . ? C75 C74 C73 120.6(5) . . ? C74 C75 C76 121.0(5) . . ? C75 C76 C71 119.9(5) . . ? C82 C81 C86 118.4(4) . . ? C82 C81 P4 121.8(3) . . ? C86 C81 P4 119.2(3) . . ? C83 C82 C81 119.7(4) . . ? C84 C83 C82 121.4(5) . . ? C83 C84 C85 119.8(4) . . ? C84 C85 C86 119.8(4) . . ? C85 C86 C81 120.8(4) . . ? O2 S1 O1 117.7(4) . . ? O2 S1 O3 113.2(3) . . ? O1 S1 O3 115.2(3) . . ? O2 S1 C1S 102.0(4) . . ? O1 S1 C1S 102.0(4) . . ? O3 S1 C1S 103.9(3) . . ? S1 O3 H1N 121.5(14) . . ? F3 C1S F1 105.5(8) . . ? F3 C1S F2 102.8(6) . . ? F1 C1S F2 108.7(6) . . ? F3 C1S S1 113.7(5) . . ? F1 C1S S1 111.5(5) . . ? F2 C1S S1 113.9(5) . . ? O2* S1* O3* 109(2) . . ? O2* S1* O1* 115(2) . . ? O3* S1* O1* 116.9(15) . . ? O2* S1* C1S* 104(2) . . ? O3* S1* C1S* 108.4(14) . . ? O1* S1* C1S* 103.2(15) . . ? S1* O3* H1N 120.0(19) . . ? F2* C1S* F3* 94(3) . . ? F2* C1S* F1* 96(3) . . ? F3* C1S* F1* 130(3) . . ? F2* C1S* S1* 104(2) . . ? F3* C1S* S1* 118(2) . . ? F1* C1S* S1* 107(2) . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.840 _refine_diff_density_max 0.559 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.082