Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'A von Zelewsky' _publ_contact_author_address ; Institute of Inorganic Chemistry University of Fribourg Perolles Fribourg 1700 SWITZERLAND ; _publ_contact_author_email ALEXANDER.VONZELEWSKY@UNIFR.CH _publ_section_title ; Stereoselectivity in the formation of tris-diimine complexes of Fe(II), Ru(II), and Os(II) with a C2-symmetric chiral derivative of 2,2'-bipyridine ; loop_ _publ_author_name 'A. von Zelewsky' 'Thomas Belser' 'Susan Drahonovsky' 'Laurence Jungo' 'Ulrich Knof' 'Gael Labat' ; A.Neels ; 'Helen Stoeckli-Evans' data_1a _database_code_depnum_ccdc_archive 'CCDC 281496' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H78 Fe N6, 2(P F6), 4.75(C H Cl3)' _chemical_formula_weight 1940.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.6777(10) _cell_length_b 15.3081(14) _cell_length_c 15.8171(14) _cell_angle_alpha 103.645(10) _cell_angle_beta 109.925(10) _cell_angle_gamma 110.641(10) _cell_volume 2274.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description bloc _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Stoe IPDS' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17894 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.89 _reflns_number_total 14809 _reflns_number_gt 11284 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie Company, Germany)' _computing_cell_refinement 'CELL (Stoe & Cie Company, Germany)' _computing_data_reduction 'XRED (Stoe & Cie Company, Germany)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON97 (Spek, 1997)' _computing_publication_material SHELXL-97 _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 w=1/[\s^2^(Fo^2^)+(0.1038P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(17) _refine_ls_number_reflns 14809 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.52153(5) 0.52415(4) 0.19034(4) 0.02134(15) Uani 1 d . . . C2 C 0.3544(5) 0.6183(3) 0.1996(3) 0.0270(10) Uani 1 d . . . C3 C 0.3117(5) 0.6846(4) 0.2377(3) 0.0323(11) Uani 1 d . . . H3 H 0.2451 0.6958 0.1948 0.039 Uiso 1 calc R . . C4 C 0.3664(6) 0.7346(4) 0.3387(4) 0.0348(12) Uani 1 d . . . C5 C 0.3334(7) 0.8144(5) 0.3867(4) 0.0526(16) Uani 1 d . . . H5 H 0.2740 0.8365 0.3525 0.063 Uiso 1 calc R . . C6 C 0.4096(7) 0.8528(5) 0.4970(5) 0.0531(16) Uani 1 d . . . H6 H 0.3908 0.9034 0.5337 0.064 Uiso 1 calc R . . C7 C 0.5676(7) 0.8823(5) 0.5361(4) 0.0519(16) Uani 1 d . . . C8 C 0.5149(6) 0.7652(4) 0.5080(4) 0.0407(13) Uani 1 d . . . H8 H 0.5769 0.7460 0.5508 0.049 Uiso 1 calc R . . C9 C 0.4609(5) 0.7116(4) 0.3989(3) 0.0313(11) Uani 1 d . . . C10 C 0.5014(5) 0.6473(3) 0.3566(3) 0.0288(11) Uani 1 d . . . H10 H 0.5667 0.6342 0.3983 0.035 Uiso 1 calc R . . C11 C 0.3902(7) 0.7599(6) 0.5252(5) 0.0568(17) Uani 1 d . . . H11A H 0.4075 0.7746 0.5935 0.068 Uiso 1 calc R . . H11B H 0.3028 0.6977 0.4791 0.068 Uiso 1 calc R . . C12 C 0.6437(8) 0.9337(5) 0.4857(6) 0.070(2) Uani 1 d . . . H12A H 0.7335 0.9361 0.5082 0.105 Uiso 1 calc R . . H12B H 0.6557 1.0026 0.5019 0.105 Uiso 1 calc R . . H12C H 0.5902 0.8951 0.4151 0.105 Uiso 1 calc R . . C13 C 0.6479(10) 0.9446(7) 0.6475(5) 0.088(3) Uani 1 d . . . H13A H 0.7411 0.9532 0.6717 0.132 Uiso 1 calc R . . H13B H 0.6018 0.9090 0.6791 0.132 Uiso 1 calc R . . H13C H 0.6516 1.0110 0.6623 0.132 Uiso 1 calc R . . C2' C 0.3045(5) 0.5619(3) 0.0941(3) 0.0235(9) Uani 1 d . . . C3' C 0.1820(5) 0.5480(3) 0.0196(3) 0.0284(10) Uani 1 d . . . H3' H 0.1287 0.5764 0.0354 0.034 Uiso 1 calc R . . C4' C 0.1425(5) 0.4916(4) -0.0773(3) 0.0290(10) Uani 1 d . . . C5' C 0.0064(5) 0.4662(4) -0.1617(3) 0.0347(12) Uani 1 d . . . H5' H -0.0562 0.4890 -0.1549 0.042 Uiso 1 calc R . . C6' C -0.0132(6) 0.3979(4) -0.2590(4) 0.0352(12) Uani 1 d . . . H6' H -0.0980 0.3791 -0.3183 0.042 Uiso 1 calc R . . C7' C 0.0173(6) 0.3071(4) -0.2496(4) 0.0394(13) Uani 1 d . . . C8' C 0.1731(6) 0.3870(4) -0.2036(3) 0.0353(11) Uani 1 d . . . H8' H 0.2347 0.3616 -0.2176 0.042 Uiso 1 calc R . . C9' C 0.2216(5) 0.4509(4) -0.0984(4) 0.0310(12) Uani 1 d . . . C10' C 0.3399(5) 0.4659(3) -0.0208(3) 0.0261(10) Uani 1 d . . . H10' H 0.3941 0.4379 -0.0357 0.031 Uiso 1 calc R . . C11' C 0.1233(6) 0.4445(5) -0.2647(4) 0.0418(13) Uani 1 d . . . H11C H 0.1766 0.5190 -0.2308 0.050 Uiso 1 calc R . . H11D H 0.1131 0.4210 -0.3314 0.050 Uiso 1 calc R . . C13' C -0.0324(8) 0.2271(5) -0.3502(4) 0.062(2) Uani 1 d . . . H13D H 0.0004 0.1781 -0.3421 0.093 Uiso 1 calc R . . H13E H 0.0036 0.2601 -0.3876 0.093 Uiso 1 calc R . . H13F H -0.1327 0.1922 -0.3851 0.093 Uiso 1 calc R . . C12' C -0.0310(6) 0.2548(4) -0.1886(4) 0.0488(15) Uani 1 d . . . H12D H 0.0077 0.2090 -0.1799 0.073 Uiso 1 calc R . . H12E H -0.1311 0.2162 -0.2222 0.073 Uiso 1 calc R . . H12F H -0.0003 0.3059 -0.1249 0.073 Uiso 1 calc R . . C22 C 0.4485(5) 0.3656(3) 0.2550(3) 0.0286(10) Uani 1 d . . . C23 C 0.3757(6) 0.2711(4) 0.2531(4) 0.0375(12) Uani 1 d . . . H23 H 0.4168 0.2520 0.3028 0.045 Uiso 1 calc R . . C24 C 0.2432(5) 0.2048(3) 0.1788(4) 0.0342(12) Uani 1 d . . . C25 C 0.1608(6) 0.0947(4) 0.1646(4) 0.0481(15) Uani 1 d . . . H25 H 0.1941 0.0629 0.2039 0.058 Uiso 1 calc R . . C26 C 0.0163(6) 0.0439(4) 0.0771(4) 0.0502(17) Uani 1 d . . . H26 H -0.0452 -0.0266 0.0651 0.060 Uiso 1 calc R . . C27 C 0.0235(8) 0.0589(4) -0.0168(4) 0.056(2) Uani 1 d . . . C28 C 0.0342(6) 0.1670(4) 0.0326(4) 0.0485(16) Uani 1 d . . . H28 H -0.0103 0.1935 -0.0126 0.058 Uiso 1 calc R . . C29 C 0.1822(5) 0.2385(3) 0.1098(4) 0.0308(11) Uani 1 d . . . C30 C 0.2601(5) 0.3331(3) 0.1144(3) 0.0280(10) Uani 1 d . . . H30 H 0.2195 0.3548 0.0670 0.034 Uiso 1 calc R . . C31 C -0.0463(6) 0.1182(5) 0.0847(5) 0.0564(18) Uani 1 d . . . H31A H -0.0147 0.1637 0.1522 0.068 Uiso 1 calc R . . H31B H -0.1472 0.0851 0.0461 0.068 Uiso 1 calc R . . C32 C 0.1386(11) 0.0577(5) -0.0375(6) 0.079(3) Uani 1 d . . . H32A H 0.1412 0.0846 -0.0869 0.118 Uiso 1 calc R . . H32B H 0.1237 -0.0118 -0.0613 0.118 Uiso 1 calc R . . H32C H 0.2258 0.0996 0.0225 0.118 Uiso 1 calc R . . C33 C -0.1142(10) -0.0102(5) -0.1090(5) 0.099(4) Uani 1 d . . . H33A H -0.1258 0.0236 -0.1537 0.148 Uiso 1 calc R . . H33B H -0.1886 -0.0248 -0.0915 0.148 Uiso 1 calc R . . H33C H -0.1160 -0.0735 -0.1408 0.148 Uiso 1 calc R . . C22' C 0.5903(5) 0.4418(3) 0.3300(3) 0.0284(10) Uani 1 d . . . C23' C 0.6609(6) 0.4350(4) 0.4179(4) 0.0409(13) Uani 1 d . . . H23' H 0.6204 0.3769 0.4293 0.049 Uiso 1 calc R . . C24' C 0.7903(6) 0.5140(4) 0.4874(4) 0.0406(13) Uani 1 d . . . C25' C 0.8673(6) 0.5178(5) 0.5876(4) 0.062(2) Uani 1 d . . . H25' H 0.8350 0.4676 0.6105 0.074 Uiso 1 calc R . . C26' C 1.0056(6) 0.6154(5) 0.6462(5) 0.0578(19) Uani 1 d . . . H26' H 1.0635 0.6232 0.7129 0.069 Uiso 1 calc R . . C27' C 0.9887(7) 0.7124(5) 0.6419(4) 0.0550(18) Uani 1 d . . . C28' C 0.9920(5) 0.6782(4) 0.5419(4) 0.0457(15) Uani 1 d . . . H28' H 1.0368 0.7336 0.5237 0.055 Uiso 1 calc R . . C29' C 0.8514(5) 0.5959(4) 0.4656(4) 0.0337(12) Uani 1 d . . . C30' C 0.7749(5) 0.5955(3) 0.3755(4) 0.0307(11) Uani 1 d . . . H30' H 0.8165 0.6498 0.3599 0.037 Uiso 1 calc R . . C31' C 1.0785(6) 0.6282(6) 0.5833(5) 0.0590(19) Uani 1 d . . . H31C H 1.0575 0.5639 0.5351 0.071 Uiso 1 calc R . . H31D H 1.1784 0.6745 0.6207 0.071 Uiso 1 calc R . . C32' C 0.8624(8) 0.7181(6) 0.6427(5) 0.070(2) Uani 1 d . . . H32D H 0.8488 0.7670 0.6166 0.105 Uiso 1 calc R . . H32E H 0.8756 0.7396 0.7096 0.105 Uiso 1 calc R . . H32F H 0.7818 0.6514 0.6024 0.105 Uiso 1 calc R . . C33' C 1.1173(8) 0.8123(5) 0.7198(6) 0.078(3) Uani 1 d . . . H33D H 1.1134 0.8687 0.7034 0.117 Uiso 1 calc R . . H33E H 1.1995 0.8089 0.7217 0.117 Uiso 1 calc R . . H33F H 1.1205 0.8226 0.7836 0.117 Uiso 1 calc R . . C42 C 0.6943(5) 0.5213(3) 0.1022(3) 0.0282(10) Uani 1 d . . . C43 C 0.7439(5) 0.4856(4) 0.0410(4) 0.0336(11) Uani 1 d . . . H43 H 0.8159 0.5320 0.0351 0.040 Uiso 1 calc R . . C44 C 0.6873(6) 0.3815(4) -0.0116(4) 0.0359(11) Uani 1 d . . . C45 C 0.7277(7) 0.3368(4) -0.0855(5) 0.0531(16) Uani 1 d . . . H45 H 0.7943 0.3751 -0.1010 0.064 Uiso 1 calc R . . C46 C 0.6438(7) 0.2191(4) -0.1319(5) 0.0533(17) Uani 1 d . . . H46 H 0.6658 0.1837 -0.1802 0.064 Uiso 1 calc R . . C47 C 0.4888(7) 0.1815(5) -0.1644(5) 0.0534(17) Uani 1 d . . . C48 C 0.5251(6) 0.2026(4) -0.0543(4) 0.0415(13) Uani 1 d . . . H48 H 0.4555 0.1557 -0.0419 0.050 Uiso 1 calc R . . C49 C 0.5851(5) 0.3148(4) 0.0037(4) 0.0317(11) Uani 1 d . . . C50 C 0.5399(5) 0.3553(3) 0.0649(3) 0.0299(11) Uani 1 d . . . H50 H 0.4701 0.3101 0.0735 0.036 Uiso 1 calc R . . C51 C 0.6522(8) 0.1833(5) -0.0464(5) 0.0572(17) Uani 1 d . . . H51A H 0.7372 0.2285 0.0158 0.069 Uiso 1 calc R . . H51B H 0.6315 0.1117 -0.0638 0.069 Uiso 1 calc R . . C52 C 0.4188(8) 0.2385(6) -0.2118(5) 0.068(2) Uani 1 d . . . H52A H 0.3217 0.2062 -0.2280 0.101 Uiso 1 calc R . . H52B H 0.4270 0.2359 -0.2712 0.101 Uiso 1 calc R . . H52C H 0.4635 0.3091 -0.1659 0.101 Uiso 1 calc R . . C53 C 0.4014(10) 0.0675(6) -0.2304(6) 0.084(3) Uani 1 d . . . H53A H 0.3059 0.0459 -0.2441 0.126 Uiso 1 calc R . . H53B H 0.4360 0.0295 -0.1973 0.126 Uiso 1 calc R . . H53C H 0.4068 0.0548 -0.2916 0.126 Uiso 1 calc R . . C42' C 0.7465(5) 0.6298(3) 0.1598(3) 0.0259(10) Uani 1 d . . . C43' C 0.8682(5) 0.7091(3) 0.1756(3) 0.0302(10) Uani 1 d . . . H43' H 0.9210 0.6953 0.1461 0.036 Uiso 1 calc R . . C44' C 0.9106(5) 0.8090(3) 0.2356(3) 0.0273(10) Uani 1 d . . . C45' C 1.0477(5) 0.8988(4) 0.2658(4) 0.0321(11) Uani 1 d . . . H45' H 1.1134 0.8947 0.2458 0.038 Uiso 1 calc R . . C46' C 1.0637(5) 0.9958(3) 0.3326(4) 0.0327(11) Uani 1 d . . . H46' H 1.1497 1.0584 0.3536 0.039 Uiso 1 calc R . . C47' C 1.0287(6) 0.9812(4) 0.4182(4) 0.0408(13) Uani 1 d . . . C48' C 0.8732(5) 0.9345(3) 0.3386(4) 0.0362(12) Uani 1 d . . . H48' H 0.8097 0.9471 0.3621 0.043 Uiso 1 calc R . . C49' C 0.8243(5) 0.8264(3) 0.2728(4) 0.0302(11) Uani 1 d . . . C50' C 0.7065(5) 0.7447(3) 0.2542(3) 0.0268(10) Uani 1 d . . . H50' H 0.6499 0.7580 0.2799 0.032 Uiso 1 calc R . . C51' C 0.9295(6) 1.0027(4) 0.2876(4) 0.0427(14) Uani 1 d . . . H51C H 0.8794 0.9703 0.2156 0.051 Uiso 1 calc R . . H51D H 0.9405 1.0717 0.3125 0.051 Uiso 1 calc R . . C52' C 1.0733(7) 0.9155(5) 0.4649(4) 0.0509(15) Uani 1 d . . . H52D H 1.0280 0.9004 0.5047 0.076 Uiso 1 calc R . . H52E H 1.1727 0.9517 0.5060 0.076 Uiso 1 calc R . . H52F H 1.0477 0.8523 0.4138 0.076 Uiso 1 calc R . . C53' C 1.0736(7) 1.0831(5) 0.4993(5) 0.0599(18) Uani 1 d . . . H53D H 1.0262 1.0702 0.5384 0.090 Uiso 1 calc R . . H53E H 1.0503 1.1270 0.4695 0.090 Uiso 1 calc R . . H53F H 1.1727 1.1163 0.5413 0.090 Uiso 1 calc R . . C14 C 0.4553(11) 0.8285(7) -0.0153(8) 0.095(3) Uani 1 d . . . H14 H 0.3776 0.8309 -0.0045 0.114 Uiso 1 calc R . . C15 C 1.0118(9) 0.4541(7) 0.2793(7) 0.089(3) Uani 1 d . . . H15 H 1.0855 0.4628 0.3401 0.107 Uiso 1 calc R . . C16 C 0.3029(9) 0.3826(6) 0.4848(6) 0.078(2) Uani 1 d . . . H16 H 0.3657 0.3523 0.4991 0.094 Uiso 0.50 calc PR A 1 H16A H 0.3627 0.3587 0.5227 0.094 Uiso 0.50 d PR A 2 C17 C -0.3570(10) -0.3990(7) -0.1897(8) 0.092(3) Uani 1 d . . . H17 H -0.2602 -0.3542 -0.1375 0.110 Uiso 1 calc R . . C18 C 0.5657(19) 0.0910(12) 0.2835(9) 0.112(6) Uani 0.75 d P B 1 H18 H 0.5339 0.1182 0.3290 0.135 Uiso 0.75 calc PR B 1 Cl1 Cl 0.5226(5) 0.7726(4) 0.0579(3) 0.1815(19) Uani 1 d . . . Cl2 Cl 0.5657(8) 0.9479(4) 0.0130(5) 0.270(4) Uani 1 d . . . Cl3 Cl 0.3862(5) 0.7502(4) -0.1351(3) 0.188(2) Uani 1 d . . . Cl4 Cl 0.8578(4) 0.3640(3) 0.2595(3) 0.1531(14) Uani 1 d . . . Cl5 Cl 1.0161(3) 0.5712(2) 0.2947(2) 0.1042(8) Uani 1 d . . . Cl6 Cl 1.0484(4) 0.4157(2) 0.1818(3) 0.1328(12) Uani 1 d . . . Cl7 Cl 0.3775(15) 0.4827(8) 0.4476(11) 0.081(2) Uani 0.50 d P C 1 Cl8 Cl 0.154(2) 0.2926(11) 0.3837(13) 0.244(10) Uani 0.50 d P C 1 Cl9 Cl 0.2677(19) 0.4047(11) 0.5764(11) 0.156(7) Uani 0.50 d P C 1 Cl7A Cl 0.390(2) 0.4797(13) 0.4681(15) 0.156(8) Uani 0.50 d P C 2 Cl8A Cl 0.1621(8) 0.2799(4) 0.3764(5) 0.0757(18) Uani 0.50 d P C 2 Cl9A Cl 0.245(3) 0.4421(16) 0.5597(17) 0.211(11) Uani 0.50 d P C 2 Cl10 Cl -0.3633(4) -0.5057(2) -0.2654(2) 0.1176(9) Uani 1 d . . . Cl11 Cl -0.4580(4) -0.4322(3) -0.1343(3) 0.1252(10) Uani 1 d . . . Cl12 Cl -0.4048(4) -0.3293(2) -0.2577(2) 0.1192(10) Uani 1 d . . . Cl13 Cl 0.4827(10) -0.0280(4) 0.2372(4) 0.250(5) Uani 0.75 d P B 1 Cl14 Cl 0.5514(5) 0.1487(4) 0.1958(3) 0.1260(14) Uani 0.75 d P B 1 Cl15 Cl 0.7505(5) 0.1384(6) 0.3510(4) 0.179(3) Uani 0.75 d P B 1 P1 P 0.0544(2) -0.24072(12) -0.00388(12) 0.0538(4) Uani 1 d . . . P2 P 1.52307(17) 1.19653(13) 0.53324(12) 0.0522(4) Uani 1 d . . . F1 F -0.0593(6) -0.2147(4) 0.0151(4) 0.0874(15) Uani 1 d . . . F2 F -0.0440(6) -0.3562(3) -0.0290(5) 0.0956(16) Uani 1 d . . . F3 F 0.1624(6) -0.2709(3) -0.0215(4) 0.0945(16) Uani 1 d . . . F4 F 0.1519(7) -0.1264(4) 0.0243(5) 0.129(2) Uani 1 d . . . F5 F 0.1254(7) -0.2279(5) 0.1073(4) 0.111(2) Uani 1 d . . . F6 F -0.0245(7) -0.2601(6) -0.1137(4) 0.126(2) Uani 1 d . . . F7 F 1.6152(8) 1.2131(11) 0.6373(7) 0.234(6) Uani 1 d . . . F8 F 1.4311(7) 1.1800(7) 0.4271(5) 0.154(3) Uani 1 d . . . F9 F 1.630(2) 1.1711(19) 0.5125(13) 0.107(5) Uiso 0.34 d P D 1 F10 F 1.6183(16) 1.3193(11) 0.5689(11) 0.077(3) Uiso 0.34 d P D 1 F11 F 1.4218(14) 1.2377(12) 0.5653(9) 0.069(3) Uiso 0.33 d P E 1 F12 F 1.4180(17) 1.0815(13) 0.5079(14) 0.086(4) Uiso 0.33 d P D 1 F9A F 1.6393(17) 1.2751(13) 0.5227(12) 0.075(4) Uiso 0.33 d P D 2 F10A F 1.511(3) 1.301(2) 0.546(2) 0.159(8) Uiso 0.34 d P D 2 F11A F 1.4054(15) 1.1161(14) 0.5440(11) 0.075(4) Uiso 0.34 d P D 2 F12A F 1.572(3) 1.115(2) 0.5091(17) 0.127(7) Uiso 0.33 d P D 2 F9B F 1.464(3) 1.0826(17) 0.4560(18) 0.133(7) Uiso 0.33 d P D 3 F10B F 1.6579(16) 1.2363(16) 0.5089(11) 0.079(4) Uiso 0.33 d P F 3 F11B F 1.589(3) 1.2957(19) 0.620(2) 0.145(8) Uiso 0.33 d P D 3 F12B F 1.4007(17) 1.1780(16) 0.5580(11) 0.088(4) Uiso 0.33 d P D 3 N1 N 0.4537(4) 0.6018(3) 0.2593(3) 0.0222(8) Uani 1 d . . . N1' N 0.3800(4) 0.5188(3) 0.0746(3) 0.0234(9) Uani 1 d . . . N21 N 0.3925(4) 0.3956(3) 0.1845(3) 0.0254(9) Uani 1 d . . . N21' N 0.6463(4) 0.5226(3) 0.3104(3) 0.0238(9) Uani 1 d . . . N41 N 0.5908(4) 0.4569(3) 0.1134(3) 0.0256(9) Uani 1 d . . . N41' N 0.6666(4) 0.6469(3) 0.2016(3) 0.0240(9) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0222(3) 0.0219(3) 0.0252(3) 0.0134(2) 0.0129(3) 0.0115(2) C2 0.025(2) 0.025(2) 0.033(2) 0.0123(19) 0.014(2) 0.0131(19) C3 0.036(3) 0.037(3) 0.030(2) 0.010(2) 0.015(2) 0.027(2) C4 0.042(3) 0.035(3) 0.036(3) 0.013(2) 0.019(2) 0.027(2) C5 0.073(4) 0.060(4) 0.038(3) 0.013(3) 0.023(3) 0.051(4) C6 0.060(4) 0.061(4) 0.047(3) 0.014(3) 0.029(3) 0.039(3) C7 0.060(4) 0.045(3) 0.031(3) -0.002(2) 0.014(3) 0.024(3) C8 0.047(3) 0.047(3) 0.034(3) 0.012(2) 0.023(2) 0.027(3) C9 0.028(3) 0.036(3) 0.027(2) 0.010(2) 0.011(2) 0.016(2) C10 0.029(2) 0.025(2) 0.030(2) 0.0124(19) 0.012(2) 0.0116(19) C11 0.059(4) 0.077(4) 0.040(3) 0.019(3) 0.026(3) 0.039(4) C12 0.071(5) 0.035(3) 0.070(4) 0.006(3) 0.026(4) 0.007(3) C13 0.099(7) 0.083(5) 0.037(3) -0.013(3) 0.002(4) 0.050(5) C2' 0.027(2) 0.021(2) 0.026(2) 0.0115(17) 0.0134(19) 0.0141(18) C3' 0.026(2) 0.030(2) 0.032(2) 0.013(2) 0.013(2) 0.016(2) C4' 0.029(3) 0.034(2) 0.031(2) 0.019(2) 0.015(2) 0.018(2) C5' 0.032(3) 0.048(3) 0.021(2) 0.011(2) 0.005(2) 0.025(2) C6' 0.034(3) 0.040(3) 0.029(3) 0.016(2) 0.009(2) 0.020(2) C7' 0.040(3) 0.040(3) 0.034(3) 0.010(2) 0.012(2) 0.023(2) C8' 0.039(3) 0.048(3) 0.028(2) 0.015(2) 0.018(2) 0.026(2) C9' 0.030(3) 0.031(2) 0.035(3) 0.018(2) 0.015(2) 0.015(2) C10' 0.026(2) 0.031(2) 0.031(2) 0.0146(19) 0.017(2) 0.018(2) C11' 0.048(3) 0.063(4) 0.030(3) 0.026(3) 0.023(3) 0.032(3) C13' 0.062(4) 0.066(4) 0.033(3) -0.003(3) 0.004(3) 0.036(4) C12' 0.045(3) 0.041(3) 0.050(3) 0.019(3) 0.016(3) 0.015(3) C22 0.031(3) 0.034(2) 0.031(2) 0.018(2) 0.019(2) 0.018(2) C23 0.044(3) 0.033(3) 0.042(3) 0.023(2) 0.022(3) 0.017(2) C24 0.041(3) 0.027(2) 0.034(3) 0.016(2) 0.016(2) 0.013(2) C25 0.044(3) 0.031(3) 0.048(3) 0.023(3) 0.011(3) 0.002(2) C26 0.050(4) 0.030(3) 0.046(3) 0.022(2) 0.009(3) 0.004(3) C27 0.071(5) 0.029(3) 0.035(3) 0.014(2) 0.009(3) 0.004(3) C28 0.036(3) 0.039(3) 0.046(3) 0.025(3) 0.004(3) 0.003(2) C29 0.030(3) 0.025(2) 0.032(2) 0.012(2) 0.014(2) 0.007(2) C30 0.035(3) 0.027(2) 0.032(2) 0.0158(19) 0.020(2) 0.018(2) C31 0.033(3) 0.049(3) 0.072(4) 0.032(3) 0.020(3) 0.003(3) C32 0.131(8) 0.043(4) 0.061(4) 0.020(3) 0.053(5) 0.032(4) C33 0.112(7) 0.048(4) 0.045(4) 0.019(3) -0.010(4) -0.011(4) C22' 0.027(2) 0.027(2) 0.031(2) 0.0134(19) 0.011(2) 0.0132(19) C23' 0.044(3) 0.038(3) 0.044(3) 0.031(2) 0.015(3) 0.018(2) C24' 0.040(3) 0.047(3) 0.039(3) 0.031(2) 0.013(2) 0.020(2) C25' 0.046(3) 0.066(4) 0.048(3) 0.045(3) -0.002(3) 0.011(3) C26' 0.036(3) 0.057(4) 0.056(4) 0.039(3) 0.000(3) 0.008(3) C27' 0.049(4) 0.056(4) 0.035(3) 0.019(3) 0.002(3) 0.016(3) C28' 0.024(3) 0.055(3) 0.043(3) 0.031(3) 0.004(2) 0.006(2) C29' 0.024(3) 0.034(3) 0.032(3) 0.017(2) 0.004(2) 0.010(2) C30' 0.033(3) 0.028(2) 0.037(3) 0.020(2) 0.018(2) 0.015(2) C31' 0.027(3) 0.076(4) 0.053(4) 0.033(3) -0.003(3) 0.020(3) C32' 0.065(5) 0.073(5) 0.052(4) 0.017(3) 0.021(4) 0.025(4) C33' 0.062(5) 0.049(4) 0.062(4) 0.024(3) -0.009(4) 0.001(3) C42 0.027(2) 0.028(2) 0.034(2) 0.017(2) 0.016(2) 0.0125(19) C43 0.033(3) 0.028(2) 0.038(3) 0.011(2) 0.021(2) 0.011(2) C44 0.038(3) 0.029(2) 0.044(3) 0.013(2) 0.027(2) 0.013(2) C45 0.064(4) 0.038(3) 0.068(4) 0.015(3) 0.051(4) 0.020(3) C46 0.066(4) 0.038(3) 0.059(4) 0.008(3) 0.043(3) 0.022(3) C47 0.056(4) 0.040(3) 0.050(4) 0.002(3) 0.032(3) 0.011(3) C48 0.048(3) 0.033(3) 0.049(3) 0.014(2) 0.032(3) 0.019(2) C49 0.033(3) 0.025(2) 0.038(3) 0.009(2) 0.020(2) 0.014(2) C50 0.030(3) 0.026(2) 0.032(2) 0.014(2) 0.015(2) 0.009(2) C51 0.075(5) 0.042(3) 0.072(4) 0.018(3) 0.047(4) 0.037(3) C52 0.072(5) 0.073(5) 0.038(3) 0.011(3) 0.017(3) 0.030(4) C53 0.086(6) 0.056(4) 0.073(5) -0.011(4) 0.049(5) 0.008(4) C42' 0.033(3) 0.025(2) 0.027(2) 0.0148(18) 0.017(2) 0.0146(19) C43' 0.030(3) 0.028(2) 0.030(2) 0.0090(19) 0.018(2) 0.008(2) C44' 0.027(2) 0.029(2) 0.032(2) 0.018(2) 0.018(2) 0.013(2) C45' 0.027(3) 0.031(2) 0.039(3) 0.010(2) 0.024(2) 0.008(2) C46' 0.033(3) 0.022(2) 0.041(3) 0.012(2) 0.022(2) 0.008(2) C47' 0.045(3) 0.029(3) 0.043(3) 0.009(2) 0.025(3) 0.010(2) C48' 0.037(3) 0.023(2) 0.052(3) 0.013(2) 0.026(3) 0.013(2) C49' 0.035(3) 0.024(2) 0.034(2) 0.014(2) 0.015(2) 0.014(2) C50' 0.025(2) 0.029(2) 0.034(2) 0.0141(19) 0.017(2) 0.017(2) C51' 0.046(3) 0.028(3) 0.057(3) 0.023(3) 0.025(3) 0.015(2) C52' 0.051(4) 0.051(3) 0.040(3) 0.018(3) 0.018(3) 0.016(3) C53' 0.059(4) 0.041(3) 0.053(4) 0.001(3) 0.031(3) 0.004(3) C14 0.083(6) 0.090(6) 0.105(7) 0.047(5) 0.036(5) 0.037(5) C15 0.070(5) 0.108(7) 0.094(6) 0.048(5) 0.038(5) 0.043(5) C16 0.083(6) 0.073(5) 0.090(5) 0.041(4) 0.055(5) 0.029(4) C17 0.075(6) 0.082(6) 0.101(6) 0.028(5) 0.039(5) 0.029(5) C18 0.189(16) 0.156(13) 0.068(7) 0.054(8) 0.070(9) 0.143(13) Cl1 0.185(4) 0.238(5) 0.167(3) 0.134(4) 0.066(3) 0.126(4) Cl2 0.345(8) 0.117(3) 0.287(7) 0.086(4) 0.191(7) 0.002(4) Cl3 0.164(4) 0.196(4) 0.129(3) 0.030(3) -0.003(3) 0.102(3) Cl4 0.111(2) 0.164(3) 0.178(3) 0.083(3) 0.087(2) 0.031(2) Cl5 0.0748(14) 0.1123(18) 0.1055(17) 0.0138(14) 0.0345(13) 0.0511(13) Cl6 0.136(3) 0.0968(19) 0.182(3) 0.0260(18) 0.118(3) 0.0497(18) Cl7 0.102(5) 0.053(3) 0.105(6) 0.041(3) 0.073(4) 0.026(3) Cl8 0.215(15) 0.138(10) 0.198(13) 0.076(9) -0.014(11) 0.001(9) Cl9 0.151(10) 0.137(8) 0.105(5) -0.007(5) 0.102(6) -0.012(8) Cl7A 0.172(12) 0.112(8) 0.123(9) 0.042(6) 0.081(8) -0.003(7) Cl8A 0.094(4) 0.036(2) 0.065(3) 0.0050(19) 0.046(3) 0.000(2) Cl9A 0.187(11) 0.219(19) 0.201(14) 0.002(11) 0.159(12) 0.058(12) Cl10 0.133(2) 0.1041(19) 0.121(2) 0.0363(16) 0.0635(19) 0.0626(18) Cl11 0.149(3) 0.162(3) 0.145(2) 0.103(2) 0.103(2) 0.095(2) Cl12 0.151(3) 0.1053(19) 0.124(2) 0.0641(17) 0.079(2) 0.0581(18) Cl13 0.368(11) 0.125(4) 0.111(3) 0.041(3) 0.102(5) -0.017(5) Cl14 0.128(3) 0.184(4) 0.149(3) 0.107(3) 0.081(3) 0.116(3) Cl15 0.127(4) 0.343(8) 0.172(5) 0.147(5) 0.091(4) 0.168(5) P1 0.0840(13) 0.0468(8) 0.0567(9) 0.0291(7) 0.0419(9) 0.0434(9) P2 0.0491(9) 0.0553(9) 0.0524(9) 0.0272(8) 0.0228(8) 0.0221(8) F1 0.110(4) 0.106(4) 0.089(3) 0.045(3) 0.046(3) 0.089(3) F2 0.103(4) 0.069(3) 0.169(5) 0.063(3) 0.102(4) 0.049(3) F3 0.108(4) 0.072(3) 0.173(5) 0.064(3) 0.114(4) 0.056(3) F4 0.121(4) 0.050(3) 0.181(6) 0.050(3) 0.032(4) 0.040(3) F5 0.126(5) 0.176(6) 0.083(3) 0.069(4) 0.047(3) 0.113(5) F6 0.125(5) 0.183(6) 0.065(3) 0.063(3) 0.050(3) 0.054(4) F7 0.117(6) 0.363(15) 0.150(7) 0.174(9) 0.010(5) 0.047(8) F8 0.111(5) 0.255(9) 0.098(4) 0.115(5) 0.035(4) 0.074(5) N1 0.025(2) 0.0205(19) 0.0247(19) 0.0114(16) 0.0130(17) 0.0113(16) N1' 0.025(2) 0.0182(18) 0.028(2) 0.0117(16) 0.0138(18) 0.0076(16) N21 0.025(2) 0.025(2) 0.030(2) 0.0144(17) 0.0129(18) 0.0122(17) N21' 0.026(2) 0.025(2) 0.030(2) 0.0134(17) 0.0170(18) 0.0163(17) N41 0.023(2) 0.028(2) 0.028(2) 0.0152(17) 0.0128(17) 0.0110(17) N41' 0.027(2) 0.026(2) 0.0238(19) 0.0114(16) 0.0140(18) 0.0147(18) _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 Fe1 N41' 1.956(4) . ? Fe1 N1' 1.966(4) . ? Fe1 N41 1.966(4) . ? Fe1 N1 1.968(4) . ? Fe1 N21 1.970(4) . ? Fe1 N21' 1.972(4) . ? C2 N1 1.368(6) . ? C2 C3 1.384(7) . ? C2 C2' 1.474(6) . ? C3 C4 1.390(7) . ? C4 C9 1.401(7) . ? C4 C5 1.519(7) . ? C5 C6 1.507(9) . ? C6 C11 1.554(9) . ? C6 C7 1.578(10) . ? C7 C12 1.526(10) . ? C7 C13 1.531(8) . ? C7 C8 1.565(8) . ? C8 C9 1.508(7) . ? C8 C11 1.549(9) . ? C9 C10 1.369(7) . ? C10 N1 1.341(6) . ? C2' N1' 1.344(6) . ? C2' C3' 1.414(6) . ? C3' C4' 1.386(7) . ? C4' C9' 1.368(7) . ? C4' C5' 1.527(6) . ? C5' C6' 1.532(7) . ? C6' C11' 1.544(8) . ? C6' C7' 1.579(7) . ? C7' C12' 1.518(8) . ? C7' C13' 1.522(8) . ? C7' C8' 1.564(8) . ? C8' C9' 1.499(7) . ? C8' C11' 1.558(7) . ? C9' C10' 1.398(7) . ? C10' N1' 1.351(6) . ? C22 N21 1.356(6) . ? C22 C23 1.383(6) . ? C22 C22' 1.468(7) . ? C23 C24 1.377(7) . ? C24 C29 1.400(7) . ? C24 C25 1.533(6) . ? C25 C26 1.530(8) . ? C26 C31 1.557(10) . ? C26 C27 1.581(8) . ? C27 C32 1.493(12) . ? C27 C33 1.518(9) . ? C27 C28 1.593(9) . ? C28 C29 1.508(7) . ? C28 C31 1.564(9) . ? C29 C30 1.381(6) . ? C30 N21 1.350(6) . ? C22' N21' 1.342(6) . ? C22' C23' 1.404(6) . ? C23' C24' 1.381(7) . ? C24' C29' 1.392(7) . ? C24' C25' 1.508(7) . ? C25' C26' 1.525(8) . ? C26' C31' 1.518(10) . ? C26' C27' 1.579(9) . ? C27' C32' 1.512(11) . ? C27' C33' 1.530(9) . ? C27' C28' 1.564(9) . ? C28' C29' 1.487(7) . ? C28' C31' 1.538(8) . ? C29' C30' 1.397(6) . ? C30' N21' 1.336(6) . ? C42 N41 1.361(6) . ? C42 C43 1.389(7) . ? C42 C42' 1.468(6) . ? C43 C44 1.386(7) . ? C44 C49 1.407(7) . ? C44 C45 1.511(8) . ? C45 C46 1.545(8) . ? C46 C47 1.537(10) . ? C46 C51 1.561(9) . ? C47 C53 1.528(9) . ? C47 C52 1.545(11) . ? C47 C48 1.565(8) . ? C48 C49 1.501(7) . ? C48 C51 1.584(9) . ? C49 C50 1.376(7) . ? C50 N41 1.354(6) . ? C42' N41' 1.373(7) . ? C42' C43' 1.399(6) . ? C43' C44' 1.395(7) . ? C44' C49' 1.397(7) . ? C44' C45' 1.516(6) . ? C45' C46' 1.512(7) . ? C46' C51' 1.538(8) . ? C46' C47' 1.584(7) . ? C47' C52' 1.512(8) . ? C47' C53' 1.540(8) . ? C47' C48' 1.580(8) . ? C48' C49' 1.505(7) . ? C48' C51' 1.564(7) . ? C49' C50' 1.371(7) . ? C50' N41' 1.344(6) . ? C14 Cl2 1.662(10) . ? C14 Cl3 1.698(11) . ? C14 Cl1 1.735(10) . ? C15 Cl4 1.703(10) . ? C15 Cl5 1.731(10) . ? C15 Cl6 1.762(11) . ? C16 Cl7A 1.617(18) . ? C16 Cl9 1.630(16) . ? C16 Cl8 1.688(18) . ? C16 Cl8A 1.760(11) . ? C16 Cl9A 1.78(2) . ? C16 Cl7 1.813(14) . ? C17 Cl11 1.706(11) . ? C17 Cl10 1.743(10) . ? C17 Cl12 1.777(10) . ? C18 Cl13 1.561(17) . ? C18 Cl14 1.805(13) . ? C18 Cl15 1.812(17) . ? P1 F6 1.557(5) . ? P1 F4 1.562(5) . ? P1 F3 1.572(5) . ? P1 F2 1.590(5) . ? P1 F5 1.596(5) . ? P1 F1 1.612(5) . ? P2 F11B 1.51(3) . ? P2 F7 1.528(7) . ? P2 F9 1.54(2) . ? P2 F8 1.554(5) . ? P2 F9A 1.555(16) . ? P2 F12B 1.557(18) . ? P2 F12A 1.57(2) . ? P2 F11A 1.581(15) . ? P2 F12 1.605(16) . ? P2 F9B 1.61(2) . ? P2 F10A 1.63(3) . ? P2 F10 1.639(14) . ? F7 F11B 1.47(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 N41' Fe1 N1' 92.41(15) . . ? N41' Fe1 N41 82.02(17) . . ? N1' Fe1 N41 93.72(16) . . ? N41' Fe1 N1 93.19(16) . . ? N1' Fe1 N1 81.99(16) . . ? N41 Fe1 N1 173.46(16) . . ? N41' Fe1 N21 173.21(18) . . ? N1' Fe1 N21 93.16(15) . . ? N41 Fe1 N21 93.74(17) . . ? N1 Fe1 N21 91.44(16) . . ? N41' Fe1 N21' 93.21(16) . . ? N1' Fe1 N21' 173.38(18) . . ? N41 Fe1 N21' 90.52(16) . . ? N1 Fe1 N21' 94.20(16) . . ? N21 Fe1 N21' 81.48(16) . . ? N1 C2 C3 121.6(4) . . ? N1 C2 C2' 113.2(4) . . ? C3 C2 C2' 125.2(4) . . ? C2 C3 C4 120.5(4) . . ? C3 C4 C9 117.2(5) . . ? C3 C4 C5 123.9(4) . . ? C9 C4 C5 118.9(5) . . ? C6 C5 C4 110.1(5) . . ? C5 C6 C11 108.8(5) . . ? C5 C6 C7 112.4(6) . . ? C11 C6 C7 87.6(5) . . ? C12 C7 C13 110.2(6) . . ? C12 C7 C8 119.0(5) . . ? C13 C7 C8 112.4(6) . . ? C12 C7 C6 118.0(6) . . ? C13 C7 C6 110.6(6) . . ? C8 C7 C6 84.5(5) . . ? C9 C8 C11 107.5(5) . . ? C9 C8 C7 109.2(4) . . ? C11 C8 C7 88.3(5) . . ? C10 C9 C4 119.3(4) . . ? C10 C9 C8 125.1(4) . . ? C4 C9 C8 115.6(5) . . ? N1 C10 C9 124.0(4) . . ? C8 C11 C6 85.8(5) . . ? N1' C2' C3' 122.4(4) . . ? N1' C2' C2 114.5(4) . . ? C3' C2' C2 123.0(4) . . ? C4' C3' C2' 118.3(5) . . ? C9' C4' C3' 119.7(4) . . ? C9' C4' C5' 118.3(4) . . ? C3' C4' C5' 121.8(5) . . ? C4' C5' C6' 110.0(4) . . ? C5' C6' C11' 108.2(4) . . ? C5' C6' C7' 111.6(4) . . ? C11' C6' C7' 86.9(4) . . ? C12' C7' C13' 109.5(5) . . ? C12' C7' C8' 118.8(4) . . ? C13' C7' C8' 111.5(5) . . ? C12' C7' C6' 118.3(5) . . ? C13' C7' C6' 111.3(5) . . ? C8' C7' C6' 85.6(4) . . ? C9' C8' C11' 106.4(4) . . ? C9' C8' C7' 108.5(4) . . ? C11' C8' C7' 87.0(4) . . ? C4' C9' C10' 118.8(5) . . ? C4' C9' C8' 118.3(4) . . ? C10' C9' C8' 122.8(5) . . ? N1' C10' C9' 123.0(5) . . ? C6' C11' C8' 87.0(4) . . ? N21 C22 C23 121.5(4) . . ? N21 C22 C22' 113.6(4) . . ? C23 C22 C22' 124.9(4) . . ? C24 C23 C22 120.3(4) . . ? C23 C24 C29 118.1(4) . . ? C23 C24 C25 123.8(4) . . ? C29 C24 C25 118.0(4) . . ? C26 C25 C24 110.0(4) . . ? C25 C26 C31 109.0(5) . . ? C25 C26 C27 111.4(5) . . ? C31 C26 C27 88.5(5) . . ? C32 C27 C33 109.9(7) . . ? C32 C27 C26 120.2(6) . . ? C33 C27 C26 111.7(6) . . ? C32 C27 C28 117.9(5) . . ? C33 C27 C28 110.6(7) . . ? C26 C27 C28 84.3(5) . . ? C29 C28 C31 107.5(4) . . ? C29 C28 C27 107.8(5) . . ? C31 C28 C27 87.8(5) . . ? C30 C29 C24 119.0(4) . . ? C30 C29 C28 123.7(4) . . ? C24 C29 C28 117.2(4) . . ? N21 C30 C29 122.4(4) . . ? C26 C31 C28 86.1(5) . . ? N21' C22' C23' 121.8(4) . . ? N21' C22' C22 114.5(4) . . ? C23' C22' C22 123.7(4) . . ? C24' C23' C22' 119.6(4) . . ? C23' C24' C29' 118.8(4) . . ? C23' C24' C25' 123.1(4) . . ? C29' C24' C25' 118.1(5) . . ? C24' C25' C26' 109.6(4) . . ? C31' C26' C25' 109.5(6) . . ? C31' C26' C27' 88.5(5) . . ? C25' C26' C27' 111.9(5) . . ? C32' C27' C33' 108.5(7) . . ? C32' C27' C28' 119.3(5) . . ? C33' C27' C28' 112.6(6) . . ? C32' C27' C26' 119.1(6) . . ? C33' C27' C26' 112.4(5) . . ? C28' C27' C26' 83.2(5) . . ? C29' C28' C31' 108.4(5) . . ? C29' C28' C27' 108.3(5) . . ? C31' C28' C27' 88.3(5) . . ? C24' C29' C30' 117.7(4) . . ? C24' C29' C28' 116.9(4) . . ? C30' C29' C28' 125.4(4) . . ? N21' C30' C29' 124.0(4) . . ? C26' C31' C28' 86.1(5) . . ? N41 C42 C43 121.9(4) . . ? N41 C42 C42' 114.0(4) . . ? C43 C42 C42' 124.1(4) . . ? C44 C43 C42 120.1(5) . . ? C43 C44 C49 117.9(5) . . ? C43 C44 C45 123.4(5) . . ? C49 C44 C45 118.7(4) . . ? C44 C45 C46 110.2(5) . . ? C47 C46 C45 112.2(5) . . ? C47 C46 C51 88.0(5) . . ? C45 C46 C51 107.6(5) . . ? C53 C47 C46 112.3(6) . . ? C53 C47 C52 108.3(6) . . ? C46 C47 C52 119.0(6) . . ? C53 C47 C48 111.7(6) . . ? C46 C47 C48 86.9(5) . . ? C52 C47 C48 117.4(6) . . ? C49 C48 C47 109.7(4) . . ? C49 C48 C51 106.1(5) . . ? C47 C48 C51 86.3(5) . . ? C50 C49 C44 118.9(4) . . ? C50 C49 C48 124.1(5) . . ? C44 C49 C48 116.8(5) . . ? N41 C50 C49 123.4(4) . . ? C46 C51 C48 85.4(5) . . ? N41' C42' C43' 122.1(4) . . ? N41' C42' C42 113.3(4) . . ? C43' C42' C42 124.6(5) . . ? C44' C43' C42' 119.3(5) . . ? C43' C44' C49' 118.2(4) . . ? C43' C44' C45' 123.4(5) . . ? C49' C44' C45' 118.4(4) . . ? C46' C45' C44' 110.4(4) . . ? C45' C46' C51' 109.0(4) . . ? C45' C46' C47' 111.9(4) . . ? C51' C46' C47' 87.7(4) . . ? C52' C47' C53' 109.4(5) . . ? C52' C47' C48' 119.1(4) . . ? C53' C47' C48' 110.6(5) . . ? C52' C47' C46' 118.2(5) . . ? C53' C47' C46' 112.8(4) . . ? C48' C47' C46' 84.8(4) . . ? C49' C48' C51' 106.1(4) . . ? C49' C48' C47' 108.9(4) . . ? C51' C48' C47' 86.9(4) . . ? C50' C49' C44' 119.1(4) . . ? C50' C49' C48' 123.5(5) . . ? C44' C49' C48' 117.2(4) . . ? N41' C50' C49' 124.4(5) . . ? C46' C51' C48' 86.9(4) . . ? Cl2 C14 Cl3 113.3(7) . . ? Cl2 C14 Cl1 114.3(7) . . ? Cl3 C14 Cl1 108.7(6) . . ? Cl4 C15 Cl5 112.1(6) . . ? Cl4 C15 Cl6 111.2(6) . . ? Cl5 C15 Cl6 109.0(5) . . ? Cl7A C16 Cl9 117.8(10) . . ? Cl7A C16 Cl8 114.1(11) . . ? Cl9 C16 Cl8 107.6(11) . . ? Cl7A C16 Cl8A 114.6(9) . . ? Cl9 C16 Cl8A 113.1(7) . . ? Cl8 C16 Cl8A 8.3(10) . . ? Cl7A C16 Cl9A 99.0(11) . . ? Cl9 C16 Cl9A 25.8(13) . . ? Cl8 C16 Cl9A 103.2(12) . . ? Cl8A C16 Cl9A 111.0(10) . . ? Cl7A C16 Cl7 8.9(12) . . ? Cl9 C16 Cl7 121.9(9) . . ? Cl8 C16 Cl7 105.3(9) . . ? Cl8A C16 Cl7 106.1(7) . . ? Cl9A C16 Cl7 100.6(9) . . ? Cl11 C17 Cl10 111.5(5) . . ? Cl11 C17 Cl12 111.2(6) . . ? Cl10 C17 Cl12 110.3(6) . . ? Cl13 C18 Cl14 114.8(8) . . ? Cl13 C18 Cl15 112.6(8) . . ? Cl14 C18 Cl15 103.0(10) . . ? F6 P1 F4 92.2(4) . . ? F6 P1 F3 92.5(4) . . ? F4 P1 F3 90.2(3) . . ? F6 P1 F2 89.5(4) . . ? F4 P1 F2 178.1(4) . . ? F3 P1 F2 90.4(2) . . ? F6 P1 F5 175.8(4) . . ? F4 P1 F5 91.7(4) . . ? F3 P1 F5 89.1(3) . . ? F2 P1 F5 86.6(3) . . ? F6 P1 F1 88.5(3) . . ? F4 P1 F1 92.3(3) . . ? F3 P1 F1 177.2(3) . . ? F2 P1 F1 87.0(3) . . ? F5 P1 F1 89.7(3) . . ? F11B P2 F7 57.8(11) . . ? F11B P2 F9 113.0(14) . . ? F7 P2 F9 81.9(9) . . ? F11B P2 F8 122.3(13) . . ? F7 P2 F8 179.2(5) . . ? F9 P2 F8 97.4(8) . . ? F11B P2 F9A 73.7(12) . . ? F7 P2 F9A 95.9(7) . . ? F9 P2 F9A 58.9(10) . . ? F8 P2 F9A 83.4(6) . . ? F11B P2 F12B 80.7(13) . . ? F7 P2 F12B 89.6(7) . . ? F9 P2 F12B 155.5(13) . . ? F8 P2 F12B 91.2(6) . . ? F9A P2 F12B 145.3(12) . . ? F11B P2 F12A 132.0(15) . . ? F7 P2 F12A 79.9(10) . . ? F9 P2 F12A 32.0(10) . . ? F8 P2 F12A 99.6(9) . . ? F9A P2 F12A 90.7(12) . . ? F12B P2 F12A 123.9(14) . . ? F11B P2 F11A 106.5(13) . . ? F7 P2 F11A 83.9(6) . . ? F9 P2 F11A 120.7(13) . . ? F8 P2 F11A 96.8(6) . . ? F9A P2 F11A 179.6(10) . . ? F12B P2 F11A 35.1(7) . . ? F12A P2 F11A 88.9(13) . . ? F11B P2 F12 132.6(14) . . ? F7 P2 F12 92.5(7) . . ? F9 P2 F12 95.8(12) . . ? F8 P2 F12 87.9(7) . . ? F9A P2 F12 151.6(11) . . ? F12B P2 F12 61.5(10) . . ? F12A P2 F12 64.1(13) . . ? F11A P2 F12 28.1(7) . . ? F11B P2 F9B 168.8(15) . . ? F7 P2 F9B 111.1(11) . . ? F9 P2 F9B 63.8(12) . . ? F8 P2 F9B 68.8(9) . . ? F9A P2 F9B 110.9(13) . . ? F12B P2 F9B 98.7(12) . . ? F12A P2 F9B 40.0(10) . . ? F11A P2 F9B 68.8(11) . . ? F12 P2 F9B 41.1(9) . . ? F11B P2 F10A 47.2(13) . . ? F7 P2 F10A 104.9(11) . . ? F9 P2 F10A 127.8(15) . . ? F8 P2 F10A 75.3(10) . . ? F9A P2 F10A 68.9(13) . . ? F12B P2 F10A 76.5(13) . . ? F12A P2 F10A 159.4(15) . . ? F11A P2 F10A 111.5(13) . . ? F12 P2 F10A 134.4(13) . . ? F9B P2 F10A 143.7(13) . . ? F11B P2 F10 39.7(11) . . ? F7 P2 F10 85.5(7) . . ? F9 P2 F10 92.8(11) . . ? F8 P2 F10 94.2(6) . . ? F9A P2 F10 37.5(7) . . ? F12B P2 F10 109.5(10) . . ? F12A P2 F10 124.1(12) . . ? F11A P2 F10 142.8(10) . . ? F12 P2 F10 170.9(11) . . ? F9B P2 F10 147.5(12) . . ? F10A P2 F10 38.6(10) . . ? F11B F7 P2 60.3(11) . . ? F7 F11B P2 61.9(11) . . ? C10 N1 C2 117.2(4) . . ? C10 N1 Fe1 127.9(3) . . ? C2 N1 Fe1 114.6(3) . . ? C2' N1' C10' 117.6(4) . . ? C2' N1' Fe1 114.9(3) . . ? C10' N1' Fe1 126.9(3) . . ? C30 N21 C22 118.4(4) . . ? C30 N21 Fe1 126.5(3) . . ? C22 N21 Fe1 114.9(3) . . ? C30' N21' C22' 117.9(4) . . ? C30' N21' Fe1 126.9(3) . . ? C22' N21' Fe1 115.0(3) . . ? C50 N41 C42 117.6(4) . . ? C50 N41 Fe1 127.3(3) . . ? C42 N41 Fe1 114.9(3) . . ? C50' N41' C42' 116.8(4) . . ? C50' N41' Fe1 127.7(4) . . ? C42' N41' Fe1 115.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -1.7(8) . . . . ? C2' C2 C3 C4 -179.5(5) . . . . ? C2 C3 C4 C9 -2.6(8) . . . . ? C2 C3 C4 C5 175.3(5) . . . . ? C3 C4 C5 C6 179.8(6) . . . . ? C9 C4 C5 C6 -2.3(8) . . . . ? C4 C5 C6 C11 -47.3(8) . . . . ? C4 C5 C6 C7 48.0(8) . . . . ? C5 C6 C7 C12 38.0(8) . . . . ? C11 C6 C7 C12 147.4(5) . . . . ? C5 C6 C7 C13 166.1(6) . . . . ? C11 C6 C7 C13 -84.5(6) . . . . ? C5 C6 C7 C8 -82.0(6) . . . . ? C11 C6 C7 C8 27.4(4) . . . . ? C12 C7 C8 C9 -38.6(8) . . . . ? C13 C7 C8 C9 -169.5(6) . . . . ? C6 C7 C8 C9 80.5(5) . . . . ? C12 C7 C8 C11 -146.6(6) . . . . ? C13 C7 C8 C11 82.5(7) . . . . ? C6 C7 C8 C11 -27.5(4) . . . . ? C3 C4 C9 C10 4.2(8) . . . . ? C5 C4 C9 C10 -173.8(5) . . . . ? C3 C4 C9 C8 -178.3(5) . . . . ? C5 C4 C9 C8 3.7(8) . . . . ? C11 C8 C9 C10 -138.6(6) . . . . ? C7 C8 C9 C10 127.0(6) . . . . ? C11 C8 C9 C4 44.1(6) . . . . ? C7 C8 C9 C4 -50.3(7) . . . . ? C4 C9 C10 N1 -1.6(8) . . . . ? C8 C9 C10 N1 -178.8(5) . . . . ? C9 C8 C11 C6 -81.7(5) . . . . ? C7 C8 C11 C6 27.9(4) . . . . ? C5 C6 C11 C8 85.2(6) . . . . ? C7 C6 C11 C8 -27.6(4) . . . . ? N1 C2 C2' N1' -10.9(5) . . . . ? C3 C2 C2' N1' 167.0(4) . . . . ? N1 C2 C2' C3' 164.9(4) . . . . ? C3 C2 C2' C3' -17.1(7) . . . . ? N1' C2' C3' C4' -3.0(7) . . . . ? C2 C2' C3' C4' -178.5(4) . . . . ? C2' C3' C4' C9' 0.3(7) . . . . ? C2' C3' C4' C5' 175.3(4) . . . . ? C9' C4' C5' C6' -1.4(6) . . . . ? C3' C4' C5' C6' -176.5(4) . . . . ? C4' C5' C6' C11' -47.1(5) . . . . ? C4' C5' C6' C7' 47.0(6) . . . . ? C5' C6' C7' C12' 39.4(7) . . . . ? C11' C6' C7' C12' 147.8(5) . . . . ? C5' C6' C7' C13' 167.4(5) . . . . ? C11' C6' C7' C13' -84.1(5) . . . . ? C5' C6' C7' C8' -81.1(5) . . . . ? C11' C6' C7' C8' 27.3(4) . . . . ? C12' C7' C8' C9' -40.7(6) . . . . ? C13' C7' C8' C9' -169.6(5) . . . . ? C6' C7' C8' C9' 79.3(4) . . . . ? C12' C7' C8' C11' -147.0(5) . . . . ? C13' C7' C8' C11' 84.1(5) . . . . ? C6' C7' C8' C11' -27.0(4) . . . . ? C3' C4' C9' C10' 1.0(7) . . . . ? C5' C4' C9' C10' -174.2(4) . . . . ? C3' C4' C9' C8' 177.7(4) . . . . ? C5' C4' C9' C8' 2.5(7) . . . . ? C11' C8' C9' C4' 43.8(6) . . . . ? C7' C8' C9' C4' -48.6(6) . . . . ? C11' C8' C9' C10' -139.7(5) . . . . ? C7' C8' C9' C10' 128.0(5) . . . . ? C4' C9' C10' N1' 0.2(7) . . . . ? C8' C9' C10' N1' -176.3(4) . . . . ? C5' C6' C11' C8' 84.4(4) . . . . ? C7' C6' C11' C8' -27.3(4) . . . . ? C9' C8' C11' C6' -80.8(5) . . . . ? C7' C8' C11' C6' 27.6(4) . . . . ? N21 C22 C23 C24 -0.1(8) . . . . ? C22' C22 C23 C24 -179.4(5) . . . . ? C22 C23 C24 C29 -4.2(8) . . . . ? C22 C23 C24 C25 173.2(5) . . . . ? C23 C24 C25 C26 178.3(6) . . . . ? C29 C24 C25 C26 -4.3(8) . . . . ? C24 C25 C26 C31 -46.3(7) . . . . ? C24 C25 C26 C27 49.7(7) . . . . ? C25 C26 C27 C32 36.2(7) . . . . ? C31 C26 C27 C32 146.1(5) . . . . ? C25 C26 C27 C33 167.2(7) . . . . ? C31 C26 C27 C33 -83.0(7) . . . . ? C25 C26 C27 C28 -82.9(6) . . . . ? C31 C26 C27 C28 27.0(4) . . . . ? C32 C27 C28 C29 -40.4(7) . . . . ? C33 C27 C28 C29 -168.1(6) . . . . ? C26 C27 C28 C29 80.8(5) . . . . ? C32 C27 C28 C31 -148.1(6) . . . . ? C33 C27 C28 C31 84.1(6) . . . . ? C26 C27 C28 C31 -26.9(4) . . . . ? C23 C24 C29 C30 4.9(8) . . . . ? C25 C24 C29 C30 -172.6(5) . . . . ? C23 C24 C29 C28 -176.5(6) . . . . ? C25 C24 C29 C28 6.0(8) . . . . ? C31 C28 C29 C30 -139.3(6) . . . . ? C27 C28 C29 C30 127.3(5) . . . . ? C31 C28 C29 C24 42.2(7) . . . . ? C27 C28 C29 C24 -51.2(7) . . . . ? C24 C29 C30 N21 -1.5(8) . . . . ? C28 C29 C30 N21 180.0(5) . . . . ? C25 C26 C31 C28 84.7(5) . . . . ? C27 C26 C31 C28 -27.5(4) . . . . ? C29 C28 C31 C26 -80.8(5) . . . . ? C27 C28 C31 C26 27.3(4) . . . . ? N21 C22 C22' N21' -7.3(6) . . . . ? C23 C22 C22' N21' 172.1(5) . . . . ? N21 C22 C22' C23' 169.5(5) . . . . ? C23 C22 C22' C23' -11.1(8) . . . . ? N21' C22' C23' C24' 1.4(8) . . . . ? C22 C22' C23' C24' -175.2(5) . . . . ? C22' C23' C24' C29' -4.1(9) . . . . ? C22' C23' C24' C25' 173.8(6) . . . . ? C23' C24' C25' C26' -179.4(6) . . . . ? C29' C24' C25' C26' -1.4(9) . . . . ? C24' C25' C26' C31' -48.3(7) . . . . ? C24' C25' C26' C27' 48.1(8) . . . . ? C31' C26' C27' C32' 147.4(6) . . . . ? C25' C26' C27' C32' 37.0(8) . . . . ? C31' C26' C27' C33' -84.1(7) . . . . ? C25' C26' C27' C33' 165.5(7) . . . . ? C31' C26' C27' C28' 27.6(4) . . . . ? C25' C26' C27' C28' -82.8(6) . . . . ? C32' C27' C28' C29' -38.0(7) . . . . ? C33' C27' C28' C29' -166.9(5) . . . . ? C26' C27' C28' C29' 81.6(5) . . . . ? C32' C27' C28' C31' -146.8(6) . . . . ? C33' C27' C28' C31' 84.3(6) . . . . ? C26' C27' C28' C31' -27.2(4) . . . . ? C23' C24' C29' C30' 2.8(9) . . . . ? C25' C24' C29' C30' -175.2(6) . . . . ? C23' C24' C29' C28' -178.8(6) . . . . ? C25' C24' C29' C28' 3.2(9) . . . . ? C31' C28' C29' C24' 43.2(8) . . . . ? C27' C28' C29' C24' -51.2(7) . . . . ? C31' C28' C29' C30' -138.4(6) . . . . ? C27' C28' C29' C30' 127.1(6) . . . . ? C24' C29' C30' N21' 1.4(8) . . . . ? C28' C29' C30' N21' -176.9(6) . . . . ? C25' C26' C31' C28' 84.7(5) . . . . ? C27' C26' C31' C28' -27.9(4) . . . . ? C29' C28' C31' C26' -80.5(6) . . . . ? C27' C28' C31' C26' 28.2(4) . . . . ? N41 C42 C43 C44 0.5(7) . . . . ? C42' C42 C43 C44 -179.3(4) . . . . ? C42 C43 C44 C49 -3.5(7) . . . . ? C42 C43 C44 C45 175.2(5) . . . . ? C43 C44 C45 C46 -179.0(5) . . . . ? C49 C44 C45 C46 -0.4(8) . . . . ? C44 C45 C46 C47 46.7(7) . . . . ? C44 C45 C46 C51 -48.4(7) . . . . ? C45 C46 C47 C53 167.1(6) . . . . ? C51 C46 C47 C53 -84.7(6) . . . . ? C45 C46 C47 C52 39.2(8) . . . . ? C51 C46 C47 C52 147.4(6) . . . . ? C45 C46 C47 C48 -80.7(6) . . . . ? C51 C46 C47 C48 27.5(4) . . . . ? C53 C47 C48 C49 -168.5(6) . . . . ? C46 C47 C48 C49 78.7(5) . . . . ? C52 C47 C48 C49 -42.6(8) . . . . ? C53 C47 C48 C51 85.7(7) . . . . ? C46 C47 C48 C51 -27.1(4) . . . . ? C52 C47 C48 C51 -148.4(6) . . . . ? C43 C44 C49 C50 3.9(7) . . . . ? C45 C44 C49 C50 -174.8(5) . . . . ? C43 C44 C49 C48 179.8(5) . . . . ? C45 C44 C49 C48 1.0(8) . . . . ? C47 C48 C49 C50 129.5(6) . . . . ? C51 C48 C49 C50 -138.7(5) . . . . ? C47 C48 C49 C44 -46.1(7) . . . . ? C51 C48 C49 C44 45.7(6) . . . . ? C44 C49 C50 N41 -1.4(7) . . . . ? C48 C49 C50 N41 -176.9(5) . . . . ? C47 C46 C51 C48 -27.2(4) . . . . ? C45 C46 C51 C48 85.5(6) . . . . ? C49 C48 C51 C46 -82.7(5) . . . . ? C47 C48 C51 C46 26.7(4) . . . . ? N41 C42 C42' N41' -10.1(5) . . . . ? C43 C42 C42' N41' 169.7(4) . . . . ? N41 C42 C42' C43' 167.2(4) . . . . ? C43 C42 C42' C43' -13.0(7) . . . . ? N41' C42' C43' C44' 0.1(6) . . . . ? C42 C42' C43' C44' -177.0(4) . . . . ? C42' C43' C44' C49' -4.0(6) . . . . ? C42' C43' C44' C45' 173.6(4) . . . . ? C43' C44' C45' C46' -178.7(4) . . . . ? C49' C44' C45' C46' -1.2(6) . . . . ? C44' C45' C46' C51' -47.1(5) . . . . ? C44' C45' C46' C47' 48.2(6) . . . . ? C45' C46' C47' C52' 38.2(7) . . . . ? C51' C46' C47' C52' 147.8(5) . . . . ? C45' C46' C47' C53' 167.6(5) . . . . ? C51' C46' C47' C53' -82.8(6) . . . . ? C45' C46' C47' C48' -82.2(5) . . . . ? C51' C46' C47' C48' 27.4(4) . . . . ? C52' C47' C48' C49' -40.5(7) . . . . ? C53' C47' C48' C49' -168.5(5) . . . . ? C46' C47' C48' C49' 79.0(4) . . . . ? C52' C47' C48' C51' -146.4(5) . . . . ? C53' C47' C48' C51' 85.6(5) . . . . ? C46' C47' C48' C51' -26.9(4) . . . . ? C43' C44' C49' C50' 4.0(6) . . . . ? C45' C44' C49' C50' -173.6(4) . . . . ? C43' C44' C49' C48' 179.1(4) . . . . ? C45' C44' C49' C48' 1.5(6) . . . . ? C51' C48' C49' C50' -140.5(5) . . . . ? C47' C48' C49' C50' 127.2(5) . . . . ? C51' C48' C49' C44' 44.6(6) . . . . ? C47' C48' C49' C44' -47.6(6) . . . . ? C44' C49' C50' N41' -0.1(7) . . . . ? C48' C49' C50' N41' -174.9(4) . . . . ? C45' C46' C51' C48' 84.8(4) . . . . ? C47' C46' C51' C48' -27.6(4) . . . . ? C49' C48' C51' C46' -81.1(5) . . . . ? C47' C48' C51' C46' 27.7(4) . . . . ? F9 P2 F7 F11B 123.8(16) . . . . ? F8 P2 F7 F11B 99(48) . . . . ? F9A P2 F7 F11B 66.5(15) . . . . ? F12B P2 F7 F11B -79.2(15) . . . . ? F12A P2 F7 F11B 156.2(17) . . . . ? F11A P2 F7 F11B -113.9(15) . . . . ? F12 P2 F7 F11B -140.7(15) . . . . ? F9B P2 F7 F11B -178.4(16) . . . . ? F10A P2 F7 F11B -3.3(17) . . . . ? F10 P2 F7 F11B 30.4(14) . . . . ? F9 P2 F11B F7 -63.3(14) . . . . ? F8 P2 F11B F7 -179.0(6) . . . . ? F9A P2 F11B F7 -108.1(11) . . . . ? F12B P2 F11B F7 95.5(11) . . . . ? F12A P2 F11B F7 -32(2) . . . . ? F11A P2 F11B F7 71.5(11) . . . . ? F12 P2 F11B F7 59.3(17) . . . . ? F9B P2 F11B F7 8(8) . . . . ? F10A P2 F11B F7 176(2) . . . . ? F10 P2 F11B F7 -128(2) . . . . ? C9 C10 N1 C2 -2.7(7) . . . . ? C9 C10 N1 Fe1 170.6(4) . . . . ? C3 C2 N1 C10 4.3(7) . . . . ? C2' C2 N1 C10 -177.6(4) . . . . ? C3 C2 N1 Fe1 -169.8(4) . . . . ? C2' C2 N1 Fe1 8.2(5) . . . . ? N41' Fe1 N1 C10 -84.5(4) . . . . ? N1' Fe1 N1 C10 -176.5(4) . . . . ? N41 Fe1 N1 C10 -127.2(15) . . . . ? N21 Fe1 N1 C10 90.5(4) . . . . ? N21' Fe1 N1 C10 9.0(4) . . . . ? N41' Fe1 N1 C2 88.9(3) . . . . ? N1' Fe1 N1 C2 -3.1(3) . . . . ? N41 Fe1 N1 C2 46.2(17) . . . . ? N21 Fe1 N1 C2 -96.1(3) . . . . ? N21' Fe1 N1 C2 -177.6(3) . . . . ? C3' C2' N1' C10' 4.1(6) . . . . ? C2 C2' N1' C10' 180.0(4) . . . . ? C3' C2' N1' Fe1 -167.4(3) . . . . ? C2 C2' N1' Fe1 8.4(5) . . . . ? C9' C10' N1' C2' -2.7(6) . . . . ? C9' C10' N1' Fe1 167.7(3) . . . . ? N41' Fe1 N1' C2' -96.1(3) . . . . ? N41 Fe1 N1' C2' -178.2(3) . . . . ? N1 Fe1 N1' C2' -3.2(3) . . . . ? N21 Fe1 N1' C2' 87.8(3) . . . . ? N21' Fe1 N1' C2' 52.0(16) . . . . ? N41' Fe1 N1' C10' 93.3(4) . . . . ? N41 Fe1 N1' C10' 11.1(4) . . . . ? N1 Fe1 N1' C10' -173.8(4) . . . . ? N21 Fe1 N1' C10' -82.8(4) . . . . ? N21' Fe1 N1' C10' -118.7(15) . . . . ? C29 C30 N21 C22 -2.7(7) . . . . ? C29 C30 N21 Fe1 172.1(4) . . . . ? C23 C22 N21 C30 3.6(7) . . . . ? C22' C22 N21 C30 -177.1(4) . . . . ? C23 C22 N21 Fe1 -171.9(4) . . . . ? C22' C22 N21 Fe1 7.5(5) . . . . ? N41' Fe1 N21 C30 -140.6(14) . . . . ? N1' Fe1 N21 C30 4.4(4) . . . . ? N41 Fe1 N21 C30 -89.5(4) . . . . ? N1 Fe1 N21 C30 86.5(4) . . . . ? N21' Fe1 N21 C30 -179.5(4) . . . . ? N41' Fe1 N21 C22 34.4(18) . . . . ? N1' Fe1 N21 C22 179.5(3) . . . . ? N41 Fe1 N21 C22 85.5(3) . . . . ? N1 Fe1 N21 C22 -98.5(3) . . . . ? N21' Fe1 N21 C22 -4.5(3) . . . . ? C29' C30' N21' C22' -4.2(8) . . . . ? C29' C30' N21' Fe1 171.2(4) . . . . ? C23' C22' N21' C30' 2.7(7) . . . . ? C22 C22' N21' C30' 179.6(4) . . . . ? C23' C22' N21' Fe1 -173.3(4) . . . . ? C22 C22' N21' Fe1 3.6(5) . . . . ? N41' Fe1 N21' C30' 9.0(4) . . . . ? N1' Fe1 N21' C30' -139.1(14) . . . . ? N41 Fe1 N21' C30' 91.0(4) . . . . ? N1 Fe1 N21' C30' -84.5(4) . . . . ? N21 Fe1 N21' C30' -175.3(5) . . . . ? N41' Fe1 N21' C22' -175.5(4) . . . . ? N1' Fe1 N21' C22' 36.5(17) . . . . ? N41 Fe1 N21' C22' -93.4(4) . . . . ? N1 Fe1 N21' C22' 91.1(4) . . . . ? N21 Fe1 N21' C22' 0.3(3) . . . . ? C49 C50 N41 C42 -1.6(7) . . . . ? C49 C50 N41 Fe1 172.4(4) . . . . ? C43 C42 N41 C50 2.1(6) . . . . ? C42' C42 N41 C50 -178.0(4) . . . . ? C43 C42 N41 Fe1 -172.7(4) . . . . ? C42' C42 N41 Fe1 7.1(5) . . . . ? N41' Fe1 N41 C50 -176.3(4) . . . . ? N1' Fe1 N41 C50 -84.4(4) . . . . ? N1 Fe1 N41 C50 -133.2(14) . . . . ? N21 Fe1 N41 C50 9.0(4) . . . . ? N21' Fe1 N41 C50 90.5(4) . . . . ? N41' Fe1 N41 C42 -2.1(3) . . . . ? N1' Fe1 N41 C42 89.8(3) . . . . ? N1 Fe1 N41 C42 41.0(17) . . . . ? N21 Fe1 N41 C42 -176.8(3) . . . . ? N21' Fe1 N41 C42 -95.3(3) . . . . ? C49' C50' N41' C42' -3.7(6) . . . . ? C49' C50' N41' Fe1 167.9(4) . . . . ? C43' C42' N41' C50' 3.7(6) . . . . ? C42 C42' N41' C50' -178.9(4) . . . . ? C43' C42' N41' Fe1 -168.9(3) . . . . ? C42 C42' N41' Fe1 8.4(4) . . . . ? N1' Fe1 N41' C50' 91.1(4) . . . . ? N41 Fe1 N41' C50' -175.5(4) . . . . ? N1 Fe1 N41' C50' 9.0(4) . . . . ? N21 Fe1 N41' C50' -123.8(15) . . . . ? N21' Fe1 N41' C50' -85.4(4) . . . . ? N1' Fe1 N41' C42' -97.2(3) . . . . ? N41 Fe1 N41' C42' -3.7(3) . . . . ? N1 Fe1 N41' C42' -179.3(3) . . . . ? N21 Fe1 N41' C42' 47.9(17) . . . . ? N21' Fe1 N41' C42' 86.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.748 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.069 data_2a _database_code_depnum_ccdc_archive 'CCDC 281497' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H78 N6 Ru, 2(P F6), 5(C H Cl3)' _chemical_formula_weight 2015.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.8288(11) _cell_length_b 15.4650(14) _cell_length_c 15.8323(14) _cell_angle_alpha 117.650(9) _cell_angle_beta 93.330(11) _cell_angle_gamma 110.796(10) _cell_volume 2309.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.00 _exptl_crystal_description bloc _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'IPDS, Stoe & Cie Company, Germany' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17663 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.83 _reflns_number_total 14765 _reflns_number_gt 14101 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie Company, Germany)' _computing_cell_refinement 'CELL (Stoe & Cie Company, Germany)' _computing_data_reduction 'XRED (Stoe & Cie Company, Germany)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON97 (Spek, 1997)' _computing_publication_material SHELXL-97 _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 w=1/[\s^2^(Fo^2^)+(0.1418P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 14765 _refine_ls_number_parameters 1016 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.193899(18) 0.209440(17) 0.098590(17) 0.02183(11) Uani 1 d . . . N1 N 0.2231(5) 0.0960(4) -0.0203(4) 0.0252(11) Uani 1 d . . . N1' N 0.3371(5) 0.1984(4) 0.1673(4) 0.0258(11) Uani 1 d . . . N21 N 0.0513(5) 0.0941(4) 0.1083(4) 0.0283(12) Uani 1 d . . . N21' N 0.0393(5) 0.1975(4) 0.0193(4) 0.0265(11) Uani 1 d . . . N41 N 0.3219(5) 0.3377(4) 0.0945(4) 0.0256(11) Uani 1 d . . . N41' N 0.1939(5) 0.3379(4) 0.2249(4) 0.0269(12) Uani 1 d . . . C2 C 0.3186(5) 0.0737(4) -0.0001(4) 0.0278(11) Uani 1 d . . . C3 C 0.3629(5) 0.0134(4) -0.0755(4) 0.0325(11) Uani 1 d . . . H3 H 0.4307 0.0006 -0.0596 0.039 Uiso 1 calc R . . C4 C 0.3081(5) -0.0269(4) -0.1722(4) 0.0291(11) Uani 1 d . . . C5 C 0.3564(6) -0.0851(5) -0.2579(5) 0.0381(14) Uani 1 d . . . H5 H 0.4240 -0.1022 -0.2517 0.046 Uiso 1 calc R . . C6 C 0.2808(6) -0.1125(5) -0.3558(5) 0.0417(15) Uani 1 d . . . H6 H 0.3071 -0.1515 -0.4149 0.050 Uiso 1 calc R . . C7 C 0.2617(7) -0.0137(6) -0.3465(5) 0.0424(15) Uani 1 d . . . C8 C 0.1507(5) -0.0479(5) -0.2999(5) 0.0388(13) Uani 1 d . . . H8 H 0.0764 -0.0364 -0.3143 0.047 Uiso 1 calc R . . C9 C 0.2066(6) -0.0069(5) -0.1943(5) 0.0301(14) Uani 1 d . . . C10 C 0.1681(5) 0.0534(4) -0.1166(4) 0.0295(11) Uani 1 d . . . H10 H 0.0992 0.0657 -0.1313 0.035 Uiso 1 calc R . . C11 C 0.1393(6) -0.1672(5) -0.3634(5) 0.0432(15) Uani 1 d . . . H11A H 0.1204 -0.2083 -0.3300 0.052 Uiso 1 calc R . . H11B H 0.0841 -0.2094 -0.4308 0.052 Uiso 1 calc R . . C12 C 0.3668(7) 0.0971(6) -0.2848(6) 0.0521(17) Uani 1 d . . . H12A H 0.3391 0.1499 -0.2827 0.078 Uiso 1 calc R . . H12B H 0.4374 0.1010 -0.3135 0.078 Uiso 1 calc R . . H12C H 0.3922 0.1125 -0.2181 0.078 Uiso 1 calc R . . C13 C 0.2095(11) -0.0349(10) -0.4486(7) 0.073(3) Uani 1 d . . . H13A H 0.1584 0.0037 -0.4427 0.109 Uiso 1 calc R . . H13B H 0.1585 -0.1119 -0.4934 0.109 Uiso 1 calc R . . H13C H 0.2785 -0.0099 -0.4742 0.109 Uiso 1 calc R . . C2' C 0.3726(5) 0.1221(4) 0.1053(4) 0.0288(11) Uani 1 d . . . C3' C 0.4548(6) 0.0938(5) 0.1433(5) 0.0396(13) Uani 1 d . . . H3' H 0.4785 0.0408 0.1002 0.048 Uiso 1 calc R . . C4' C 0.5001(6) 0.1445(5) 0.2443(5) 0.0381(13) Uani 1 d . . . C5' C 0.5794(7) 0.1101(7) 0.2922(6) 0.054(2) Uani 1 d . . . H5' H 0.6015 0.0528 0.2578 0.065 Uiso 1 calc R . . C6' C 0.6167(9) 0.1853(8) 0.4062(7) 0.063(3) Uani 1 d . . . H6' H 0.6709 0.1715 0.4438 0.075 Uiso 1 calc R . . C7' C 0.4970(9) 0.1921(9) 0.4425(7) 0.061(2) Uani 1 d . . . C8' C 0.5233(6) 0.2819(6) 0.4172(5) 0.0459(15) Uani 1 d . . . H8' H 0.5041 0.3429 0.4605 0.055 Uiso 1 calc R . . C9' C 0.4701(6) 0.2278(5) 0.3075(5) 0.0315(13) Uani 1 d . . . C10' C 0.3854(5) 0.2497(4) 0.2645(4) 0.0303(11) Uani 1 d . . . H10' H 0.3616 0.3032 0.3064 0.036 Uiso 1 calc R . . C11' C 0.6638(7) 0.3043(8) 0.4340(6) 0.063(2) Uani 1 d . . . H11C H 0.7039 0.3201 0.3872 0.075 Uiso 1 calc R . . H11D H 0.7148 0.3574 0.5025 0.075 Uiso 1 calc R . . C13' C 0.3712(11) 0.0928(8) 0.3933(8) 0.079(3) Uani 1 d . . . H13D H 0.3066 0.1131 0.4194 0.118 Uiso 1 calc R . . H13E H 0.3761 0.0388 0.4066 0.118 Uiso 1 calc R . . H13F H 0.3507 0.0631 0.3224 0.118 Uiso 1 calc R . . C12' C 0.5249(13) 0.2395(11) 0.5551(7) 0.088(4) Uani 1 d . . . H12D H 0.4720 0.2756 0.5815 0.132 Uiso 1 calc R . . H12E H 0.6124 0.2911 0.5862 0.132 Uiso 1 calc R . . H12F H 0.5079 0.1815 0.5684 0.132 Uiso 1 calc R . . C22 C -0.0671(5) 0.0712(4) 0.0664(4) 0.0277(10) Uani 1 d . . . C23 C -0.1710(5) 0.0094(4) 0.0839(4) 0.0314(11) Uani 1 d . . . H23 H -0.2524 -0.0058 0.0546 0.038 Uiso 1 calc R . . C24 C -0.1540(5) -0.0297(4) 0.1445(4) 0.0315(11) Uani 1 d . . . C25 C -0.2606(5) -0.0891(5) 0.1755(5) 0.0353(14) Uani 1 d . . . H25 H -0.3455 -0.1055 0.1550 0.042 Uiso 1 calc R . . C27 C -0.0910(6) -0.0201(6) 0.3288(6) 0.0450(16) Uani 1 d . . . C26 C -0.2091(6) -0.1180(5) 0.2441(5) 0.0379(13) Uani 1 d . . . H26 H -0.2732 -0.1587 0.2659 0.045 Uiso 1 calc R . . C28 C -0.0173(5) -0.0514(5) 0.2492(5) 0.0391(13) Uani 1 d . . . H28 H 0.0687 -0.0403 0.2733 0.047 Uiso 1 calc R . . C29 C -0.0321(5) -0.0103(5) 0.1838(5) 0.0295(13) Uani 1 d . . . C30 C 0.0660(5) 0.0514(4) 0.1631(4) 0.0275(11) Uani 1 d . . . H30 H 0.1478 0.0644 0.1889 0.033 Uiso 1 calc R . . C31 C -0.1230(6) -0.1704(5) 0.1982(6) 0.0460(16) Uani 1 d . . . H31A H -0.1457 -0.2099 0.1257 0.055 Uiso 1 calc R . . H31B H -0.1086 -0.2135 0.2238 0.055 Uiso 1 calc R . . C32 C -0.0572(7) -0.0390(8) 0.4099(7) 0.063(2) Uani 1 d . . . H32A H 0.0080 0.0277 0.4650 0.095 Uiso 1 calc R . . H32B H -0.0270 -0.0946 0.3850 0.095 Uiso 1 calc R . . H32C H -0.1308 -0.0623 0.4321 0.095 Uiso 1 calc R . . C33 C -0.0861(7) 0.0928(6) 0.3752(6) 0.0561(18) Uani 1 d . . . H33A H -0.0004 0.1466 0.4115 0.084 Uiso 1 calc R . . H33B H -0.1393 0.1007 0.4200 0.084 Uiso 1 calc R . . H33C H -0.1155 0.1030 0.3235 0.084 Uiso 1 calc R . . C22' C -0.0734(5) 0.1220(4) 0.0097(4) 0.0292(11) Uani 1 d . . . C23' C -0.1828(5) 0.0961(5) -0.0525(5) 0.0362(12) Uani 1 d . . . H23' H -0.2594 0.0430 -0.0594 0.043 Uiso 1 calc R . . C24' C -0.1799(5) 0.1480(5) -0.1045(5) 0.0393(13) Uani 1 d . . . C25' C -0.2942(6) 0.1184(7) -0.1796(7) 0.0565(19) Uani 1 d . . . H25' H -0.3754 0.0652 -0.1953 0.068 Uiso 1 calc R . . C26' C -0.2563(7) 0.1887(8) -0.2259(7) 0.060(2) Uani 1 d . . . H26' H -0.3259 0.1760 -0.2745 0.072 Uiso 1 calc R . . C27' C -0.1355(8) 0.1956(9) -0.2587(7) 0.062(3) Uani 1 d . . . C28' C -0.0637(6) 0.2846(6) -0.1479(6) 0.0460(15) Uani 1 d . . . H28' H 0.0166 0.3444 -0.1353 0.055 Uiso 1 calc R . . C29' C -0.0635(6) 0.2307(5) -0.0897(5) 0.0328(14) Uani 1 d . . . C30' C 0.0419(5) 0.2504(4) -0.0280(4) 0.0309(11) Uani 1 d . . . H30' H 0.1196 0.3039 -0.0188 0.037 Uiso 1 calc R . . C31' C -0.1803(8) 0.3078(7) -0.1419(8) 0.064(2) Uani 1 d . . . H31C H -0.1783 0.3605 -0.1603 0.077 Uiso 1 calc R . . H31D H -0.2023 0.3251 -0.0791 0.077 Uiso 1 calc R . . C32' C -0.1203(10) 0.2395(11) -0.3294(9) 0.088(3) Uani 1 d . . . H32D H -0.0406 0.2473 -0.3452 0.133 Uiso 1 calc R . . H32E H -0.1226 0.3095 -0.2976 0.133 Uiso 1 calc R . . H32F H -0.1882 0.1895 -0.3898 0.133 Uiso 1 calc R . . C33' C -0.1125(9) 0.0964(8) -0.3047(6) 0.071(2) Uani 1 d . . . H33D H -0.0268 0.1158 -0.3098 0.107 Uiso 1 calc R . . H33E H -0.1702 0.0446 -0.3702 0.107 Uiso 1 calc R . . H33F H -0.1258 0.0644 -0.2638 0.107 Uiso 1 calc R . . C42 C 0.3366(5) 0.4377(4) 0.1669(4) 0.0300(11) Uani 1 d . . . C43 C 0.4050(6) 0.5293(4) 0.1650(5) 0.0395(13) Uani 1 d . . . H43 H 0.4137 0.5972 0.2151 0.047 Uiso 1 calc R . . C44 C 0.4609(6) 0.5209(4) 0.0889(5) 0.0379(13) Uani 1 d . . . C45 C 0.5297(8) 0.6174(5) 0.0751(6) 0.0533(18) Uani 1 d . . . H45 H 0.5378 0.6880 0.1159 0.064 Uiso 1 calc R . . C46 C 0.5820(9) 0.5810(5) -0.0139(6) 0.054(2) Uani 1 d . . . H46 H 0.6295 0.6386 -0.0270 0.065 Uiso 1 calc R . . C47 C 0.4776(13) 0.4716(7) -0.1083(7) 0.077(3) Uani 1 d . . . C48 C 0.5195(7) 0.4139(5) -0.0602(6) 0.0515(18) Uani 1 d . . . H48 H 0.5177 0.3427 -0.1063 0.062 Uiso 1 calc R . . C49 C 0.4537(6) 0.4205(5) 0.0191(5) 0.0320(14) Uani 1 d . . . C50 C 0.3817(5) 0.3321(4) 0.0253(4) 0.0297(12) Uani 1 d . . . H50 H 0.3747 0.2639 -0.0226 0.036 Uiso 1 calc R . . C51 C 0.6523(9) 0.5146(7) -0.0080(8) 0.068(3) Uani 1 d . . . H51A H 0.6892 0.5358 0.0595 0.082 Uiso 1 calc R . . H51B H 0.7128 0.5096 -0.0478 0.082 Uiso 1 calc R . . C52 C 0.5307(18) 0.4531(8) -0.1998(9) 0.126(7) Uani 1 d . . . H52A H 0.4796 0.3800 -0.2548 0.189 Uiso 1 calc R . . H52B H 0.6165 0.4631 -0.1835 0.189 Uiso 1 calc R . . H52C H 0.5290 0.5045 -0.2180 0.189 Uiso 1 calc R . . C53 C 0.3457(11) 0.4550(7) -0.1270(8) 0.081(3) Uani 1 d . . . H53A H 0.2908 0.3781 -0.1651 0.121 Uiso 1 calc R . . H53B H 0.3338 0.4881 -0.1639 0.121 Uiso 1 calc R . . H53C H 0.3258 0.4880 -0.0644 0.121 Uiso 1 calc R . . C42' C 0.2717(5) 0.4369(4) 0.2429(4) 0.0309(11) Uani 1 d . . . C43' C 0.2892(6) 0.5306(4) 0.3321(5) 0.0430(15) Uani 1 d . . . H43' H 0.3403 0.5995 0.3435 0.052 Uiso 1 calc R . . C44' C 0.2314(6) 0.5213(5) 0.4024(5) 0.0453(16) Uani 1 d . . . C45' C 0.2540(9) 0.6166(5) 0.5036(6) 0.067(3) Uani 1 d . . . H45' H 0.3087 0.6889 0.5265 0.081 Uiso 1 calc R . . C46' C 0.1745(9) 0.5782(6) 0.5635(6) 0.059(2) Uani 1 d . . . H46' H 0.1840 0.6362 0.6307 0.071 Uiso 1 calc R . . C47' C 0.1846(9) 0.4759(6) 0.5574(6) 0.059(2) Uani 1 d . . . C48' C 0.0840(6) 0.4115(5) 0.4578(5) 0.0484(17) Uani 1 d . . . H48' H 0.0208 0.3388 0.4391 0.058 Uiso 1 calc R . . C49' C 0.1457(7) 0.4197(5) 0.3816(6) 0.0385(16) Uani 1 d . . . C50' C 0.1314(5) 0.3291(4) 0.2899(4) 0.0316(12) Uani 1 d . . . H50' H 0.0751 0.2597 0.2743 0.038 Uiso 1 calc R . . C51' C 0.0408(9) 0.5055(6) 0.4994(7) 0.063(3) Uani 1 d . . . H51C H 0.0164 0.5220 0.4504 0.076 Uiso 1 calc R . . H51D H -0.0220 0.4976 0.5363 0.076 Uiso 1 calc R . . C52' C 0.1361(13) 0.4571(8) 0.6356(8) 0.088(4) Uani 1 d . . . H52D H 0.1226 0.3852 0.6204 0.131 Uiso 1 calc R . . H52E H 0.0574 0.4633 0.6375 0.131 Uiso 1 calc R . . H52F H 0.1969 0.5106 0.6994 0.131 Uiso 1 calc R . . C53' C 0.3109(9) 0.4682(8) 0.5577(7) 0.075(3) Uani 1 d . . . H53D H 0.2994 0.3984 0.5476 0.112 Uiso 1 calc R . . H53E H 0.3716 0.5254 0.6208 0.112 Uiso 1 calc R . . H53F H 0.3414 0.4759 0.5049 0.112 Uiso 1 calc R . . C54 C 0.0573(11) -0.2980(9) -0.1055(8) 0.101(4) Uani 1 d D . . H54A H 0.1410 -0.2946 -0.0874 0.122 Uiso 0.50 calc PR A 1 H54B H 0.1465 -0.2848 -0.0991 0.122 Uiso 0.50 d PR A 2 C55 C 0.2373(16) -0.2702(12) 0.1951(13) 0.073(5) Uiso 0.50 d PD B 1 H55 H 0.2981 -0.2549 0.2515 0.087 Uiso 0.50 calc PR B 1 C55A C 0.226(5) -0.260(4) 0.199(4) 0.25(4) Uiso 0.50 d PD C 2 H55A H 0.3080 -0.2262 0.2471 0.300 Uiso 0.50 calc PR C 2 C56 C 0.7080(8) 0.6415(8) 0.3937(8) 0.090(3) Uani 1 d D . . H56A H 0.6739 0.6937 0.4311 0.107 Uiso 0.50 calc PR D 1 H56B H 0.6686 0.6922 0.4128 0.107 Uiso 0.50 d PR D 2 C57 C -0.2056(14) 0.3735(14) 0.1914(11) 0.120(5) Uani 1 d . . . H57 H -0.2169 0.4249 0.2534 0.145 Uiso 1 calc R . . C58 C 0.6970(13) -0.2411(12) 0.7229(10) 0.100(4) Uani 1 d . . . H58 H 0.6538 -0.2321 0.7759 0.120 Uiso 1 calc R . . P1 P 0.4671(2) -0.21731(14) -0.09618(16) 0.0561(5) Uani 1 d . . . P2 P 0.53363(18) -0.12187(15) 0.44090(15) 0.0534(5) Uani 1 d D . . F1 F 0.4352(8) -0.3066(7) -0.2064(6) 0.135(3) Uani 1 d . . . F2 F 0.5059(7) -0.1216(6) 0.0141(6) 0.116(3) Uani 1 d . . . F3 F 0.5961(7) -0.2244(5) -0.0776(5) 0.0896(19) Uani 1 d . . . F4 F 0.3984(9) -0.3056(7) -0.0714(8) 0.137(3) Uani 1 d . . . F5 F 0.3410(5) -0.2061(5) -0.1139(6) 0.099(2) Uani 1 d . . . F6 F 0.5378(5) -0.1246(5) -0.1165(7) 0.107(3) Uani 1 d . . . F7 F 0.5090(10) -0.2027(9) 0.3242(8) 0.067(2) Uiso 0.50 d PD E 1 F8 F 0.5598(12) -0.0425(11) 0.5565(10) 0.090(3) Uiso 0.50 d PD E 1 F9 F 0.6638(14) -0.1319(12) 0.4682(12) 0.104(4) Uiso 0.50 d PD E 1 F10 F 0.4301(18) -0.0920(16) 0.4187(15) 0.131(6) Uiso 0.50 d PD E 1 F11 F 0.4622(16) -0.2147(14) 0.4648(14) 0.110(4) Uiso 0.50 d PD E 1 F12 F 0.6290(16) -0.0274(13) 0.4285(13) 0.112(4) Uiso 0.50 d PD E 1 F7A F 0.5308(18) -0.2238(15) 0.3503(15) 0.125(6) Uiso 0.50 d PD E 2 F8A F 0.511(3) -0.020(2) 0.517(2) 0.176(9) Uiso 0.50 d PD E 2 F9A F 0.6695(15) -0.0494(13) 0.4611(13) 0.109(4) Uiso 0.50 d PD E 2 F10A F 0.3827(11) -0.2013(9) 0.4173(9) 0.078(3) Uiso 0.50 d PD E 2 F11A F 0.517(3) -0.087(2) 0.364(2) 0.190(10) Uiso 0.50 d PD E 2 F12A F 0.533(4) -0.143(3) 0.531(3) 0.225(13) Uiso 0.50 d PD E 2 Cl1A Cl -0.0476(11) -0.3727(9) -0.0640(9) 0.148(3) Uiso 0.50 d PD F 1 Cl1 Cl -0.0095(12) -0.4120(10) -0.0945(10) 0.159(4) Uiso 0.50 d PD F 2 Cl2 Cl 0.0344(10) -0.3121(8) -0.2174(7) 0.118(3) Uiso 0.50 d PD F 1 Cl2A Cl -0.0157(9) -0.3551(8) -0.2321(7) 0.115(2) Uiso 0.50 d PD F 2 Cl3 Cl 0.0607(7) -0.1739(5) -0.0283(4) 0.181(3) Uani 1 d . . . Cl4 Cl 0.1700(7) -0.4084(6) 0.1072(6) 0.0919(16) Uiso 0.50 d PD B 1 Cl4A Cl 0.180(3) -0.403(3) 0.141(3) 0.344(17) Uiso 0.50 d PD C 2 Cl5 Cl 0.3175(8) -0.2103(7) 0.1341(6) 0.117(2) Uiso 0.50 d PD B 1 Cl5A Cl 0.2443(13) -0.1754(11) 0.1487(11) 0.173(4) Uiso 0.50 d PD C 2 Cl6 Cl 0.1288(8) -0.2236(7) 0.2380(7) 0.121(2) Uiso 0.50 d PD B 1 Cl6A Cl 0.1156(12) -0.2562(11) 0.2708(10) 0.160(4) Uiso 0.50 d PD C 2 Cl7 Cl 0.8438(8) 0.6579(8) 0.4650(7) 0.125(2) Uiso 0.50 d PD G 1 Cl7A Cl 0.8366(7) 0.7183(7) 0.4932(6) 0.116(2) Uiso 0.50 d PD G 2 Cl8 Cl 0.6066(5) 0.5029(5) 0.3536(5) 0.0801(14) Uiso 0.50 d PD G 1 Cl8A Cl 0.5879(7) 0.5328(6) 0.3807(6) 0.103(2) Uiso 0.50 d PD G 2 Cl9 Cl 0.7401(5) 0.6396(4) 0.2890(3) 0.1322(15) Uani 1 d D . . Cl10 Cl -0.1909(3) 0.2706(4) 0.2041(3) 0.1168(12) Uani 1 d . . . Cl11 Cl -0.0780(4) 0.4405(5) 0.1679(5) 0.169(2) Uani 1 d . . . Cl12 Cl -0.3424(3) 0.3105(4) 0.0925(4) 0.1397(17) Uani 1 d . . . Cl13 Cl 0.8556(4) -0.1543(3) 0.7786(4) 0.1312(15) Uani 1 d . . . Cl14 Cl 0.6738(4) -0.3777(3) 0.6562(4) 0.1250(12) Uani 1 d . . . Cl15 Cl 0.6292(4) -0.2118(4) 0.6458(3) 0.1194(11) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01757(15) 0.01659(15) 0.02888(19) 0.01114(13) 0.00512(12) 0.00599(12) N1 0.024(2) 0.021(2) 0.028(3) 0.0145(19) 0.0027(18) 0.0048(18) N1' 0.028(2) 0.021(2) 0.026(3) 0.0123(19) 0.0075(19) 0.0087(19) N21 0.030(3) 0.022(2) 0.030(3) 0.012(2) 0.008(2) 0.010(2) N21' 0.023(2) 0.026(2) 0.028(3) 0.015(2) 0.006(2) 0.009(2) N41 0.019(2) 0.018(2) 0.033(3) 0.010(2) 0.0015(18) 0.0048(17) N41' 0.024(2) 0.018(2) 0.034(3) 0.009(2) 0.0033(19) 0.0095(19) C2 0.032(2) 0.022(2) 0.031(3) 0.013(2) 0.008(2) 0.014(2) C3 0.037(3) 0.037(3) 0.036(3) 0.022(2) 0.015(2) 0.023(2) C4 0.026(2) 0.021(2) 0.036(3) 0.013(2) 0.006(2) 0.009(2) C5 0.048(3) 0.039(3) 0.029(3) 0.014(3) 0.016(3) 0.025(3) C6 0.040(3) 0.034(3) 0.037(3) 0.006(3) 0.011(3) 0.019(3) C7 0.050(4) 0.053(4) 0.034(3) 0.026(3) 0.017(3) 0.026(3) C8 0.035(3) 0.048(3) 0.036(3) 0.020(3) 0.009(2) 0.022(3) C9 0.029(3) 0.028(3) 0.034(3) 0.017(2) 0.012(2) 0.012(2) C10 0.024(3) 0.023(2) 0.035(3) 0.012(2) 0.006(2) 0.009(2) C11 0.037(3) 0.036(3) 0.034(3) 0.008(3) -0.001(3) 0.008(3) C12 0.054(4) 0.048(4) 0.060(5) 0.033(3) 0.022(3) 0.021(3) C13 0.114(8) 0.108(7) 0.044(5) 0.056(5) 0.033(5) 0.072(7) C2' 0.028(2) 0.026(2) 0.034(3) 0.016(2) 0.007(2) 0.014(2) C3' 0.042(3) 0.047(3) 0.038(3) 0.022(3) 0.009(2) 0.029(3) C4' 0.039(3) 0.048(3) 0.038(3) 0.025(3) 0.006(2) 0.027(3) C5' 0.068(5) 0.076(5) 0.041(4) 0.032(4) 0.011(3) 0.055(4) C6' 0.074(6) 0.087(6) 0.046(4) 0.036(5) 0.004(4) 0.053(5) C7' 0.070(6) 0.091(6) 0.043(4) 0.041(4) 0.018(4) 0.046(5) C8' 0.048(3) 0.050(3) 0.035(3) 0.017(3) 0.002(3) 0.024(3) C9' 0.035(3) 0.028(3) 0.028(3) 0.013(3) 0.004(2) 0.014(3) C10' 0.029(2) 0.030(3) 0.036(3) 0.020(2) 0.009(2) 0.013(2) C11' 0.050(4) 0.079(5) 0.046(4) 0.024(4) -0.008(3) 0.029(4) C13' 0.109(8) 0.070(5) 0.073(6) 0.054(5) 0.031(6) 0.030(5) C12' 0.134(10) 0.129(9) 0.049(5) 0.057(6) 0.033(6) 0.090(9) C22 0.025(2) 0.023(2) 0.029(3) 0.013(2) 0.0040(19) 0.0060(19) C23 0.021(2) 0.031(2) 0.037(3) 0.018(2) 0.006(2) 0.005(2) C24 0.032(3) 0.024(2) 0.039(3) 0.019(2) 0.010(2) 0.009(2) C25 0.024(3) 0.040(3) 0.046(4) 0.029(3) 0.013(2) 0.008(2) C27 0.031(3) 0.058(4) 0.044(4) 0.033(4) 0.009(3) 0.009(3) C26 0.037(3) 0.038(3) 0.042(4) 0.028(3) 0.006(3) 0.010(3) C28 0.029(3) 0.044(3) 0.056(4) 0.036(3) 0.010(3) 0.014(2) C29 0.025(3) 0.026(3) 0.039(3) 0.020(2) 0.009(2) 0.008(2) C30 0.023(2) 0.023(2) 0.036(3) 0.016(2) 0.006(2) 0.009(2) C31 0.044(3) 0.038(3) 0.061(5) 0.033(3) 0.018(3) 0.013(3) C32 0.045(4) 0.075(5) 0.063(5) 0.048(4) 0.005(3) 0.003(4) C33 0.055(4) 0.047(4) 0.044(4) 0.017(3) 0.011(3) 0.008(3) C22' 0.025(2) 0.026(2) 0.032(3) 0.016(2) 0.007(2) 0.005(2) C23' 0.029(3) 0.042(3) 0.044(3) 0.031(3) 0.010(2) 0.010(2) C24' 0.028(3) 0.048(3) 0.042(3) 0.028(3) 0.005(2) 0.010(2) C25' 0.029(3) 0.076(5) 0.065(5) 0.050(4) -0.003(3) 0.008(3) C26' 0.036(3) 0.091(7) 0.069(6) 0.059(5) 0.004(3) 0.022(4) C27' 0.043(4) 0.093(6) 0.052(5) 0.056(5) -0.004(3) 0.008(4) C28' 0.034(3) 0.052(4) 0.057(4) 0.039(3) 0.003(3) 0.009(3) C29' 0.028(3) 0.032(3) 0.037(3) 0.020(3) 0.003(2) 0.009(3) C30' 0.029(3) 0.024(3) 0.035(3) 0.015(2) 0.006(2) 0.008(2) C31' 0.063(5) 0.074(5) 0.079(7) 0.058(5) 0.010(4) 0.032(4) C32' 0.066(5) 0.127(10) 0.092(8) 0.088(8) 0.013(5) 0.022(6) C33' 0.077(6) 0.081(6) 0.042(4) 0.029(4) 0.011(4) 0.026(5) C42 0.030(2) 0.017(2) 0.033(3) 0.009(2) 0.002(2) 0.0071(19) C43 0.040(3) 0.024(2) 0.036(3) 0.011(2) 0.004(2) 0.003(2) C44 0.042(3) 0.020(2) 0.042(3) 0.016(2) 0.006(2) 0.005(2) C45 0.076(5) 0.025(3) 0.045(4) 0.021(3) 0.019(3) 0.003(3) C46 0.088(6) 0.027(3) 0.047(4) 0.026(3) 0.028(4) 0.013(3) C47 0.140(10) 0.038(4) 0.044(5) 0.028(4) 0.030(5) 0.022(5) C48 0.065(4) 0.034(3) 0.061(5) 0.028(3) 0.036(4) 0.019(3) C49 0.032(3) 0.028(3) 0.037(3) 0.020(2) 0.008(3) 0.009(2) C50 0.024(2) 0.020(2) 0.034(3) 0.012(2) 0.002(2) 0.002(2) C51 0.063(5) 0.053(4) 0.085(7) 0.039(5) 0.046(5) 0.014(4) C52 0.216(17) 0.051(5) 0.068(7) 0.024(5) 0.073(9) 0.017(7) C53 0.103(8) 0.058(5) 0.061(6) 0.038(4) -0.005(5) 0.009(5) C42' 0.036(3) 0.022(2) 0.036(3) 0.015(2) 0.013(2) 0.013(2) C43' 0.051(3) 0.014(2) 0.051(4) 0.012(2) 0.018(3) 0.008(2) C44' 0.052(4) 0.025(3) 0.047(4) 0.010(3) 0.022(3) 0.015(3) C45' 0.097(6) 0.017(3) 0.058(5) 0.008(3) 0.044(4) 0.007(3) C46' 0.078(6) 0.034(3) 0.049(4) 0.014(3) 0.039(4) 0.015(4) C47' 0.083(6) 0.045(4) 0.045(4) 0.019(3) 0.030(4) 0.025(4) C48' 0.049(3) 0.029(3) 0.049(4) 0.009(3) 0.028(3) 0.011(3) C49' 0.047(4) 0.028(3) 0.038(4) 0.013(3) 0.019(3) 0.018(3) C50' 0.034(3) 0.025(2) 0.035(3) 0.012(2) 0.013(2) 0.014(2) C51' 0.080(6) 0.051(4) 0.066(6) 0.025(4) 0.052(5) 0.038(4) C52' 0.140(10) 0.055(5) 0.048(5) 0.029(4) 0.033(6) 0.018(6) C53' 0.076(6) 0.081(6) 0.052(5) 0.027(4) 0.010(4) 0.030(5) C54 0.096(8) 0.095(8) 0.121(10) 0.064(8) 0.047(7) 0.036(7) C56 0.073(6) 0.083(7) 0.099(8) 0.047(6) 0.018(6) 0.021(5) C57 0.118(10) 0.167(14) 0.110(10) 0.067(10) 0.050(9) 0.099(11) C58 0.108(9) 0.131(10) 0.077(7) 0.062(7) 0.024(6) 0.057(8) P1 0.0636(11) 0.0400(9) 0.0599(12) 0.0253(8) -0.0017(9) 0.0211(8) P2 0.0540(10) 0.0472(10) 0.0528(11) 0.0241(8) 0.0179(8) 0.0173(8) F1 0.100(5) 0.108(5) 0.081(4) -0.004(4) -0.005(4) 0.006(4) F2 0.104(5) 0.096(4) 0.099(5) 0.003(4) 0.000(4) 0.064(4) F3 0.115(5) 0.088(4) 0.085(4) 0.037(3) 0.019(3) 0.075(4) F4 0.173(8) 0.123(6) 0.214(10) 0.140(7) 0.103(8) 0.085(6) F5 0.043(2) 0.091(4) 0.176(7) 0.091(5) 0.009(3) 0.016(3) F6 0.049(3) 0.094(4) 0.202(8) 0.101(5) 0.020(4) 0.025(3) Cl3 0.212(6) 0.133(4) 0.147(4) 0.024(3) 0.037(4) 0.092(4) Cl9 0.151(4) 0.128(3) 0.115(3) 0.087(3) 0.029(3) 0.025(3) Cl10 0.107(2) 0.178(4) 0.107(2) 0.079(2) 0.0428(19) 0.095(3) Cl11 0.102(3) 0.168(4) 0.191(5) 0.097(4) 0.043(3) 0.005(3) Cl12 0.0731(17) 0.198(4) 0.196(5) 0.147(4) 0.018(2) 0.048(2) Cl13 0.095(2) 0.094(2) 0.147(3) 0.035(2) -0.006(2) 0.0260(19) Cl14 0.113(2) 0.105(2) 0.143(3) 0.073(2) 0.014(2) 0.024(2) Cl15 0.109(2) 0.144(3) 0.124(3) 0.083(3) 0.020(2) 0.055(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.045(5) . ? Ru1 N21 2.049(6) . ? Ru1 N41 2.057(5) . ? Ru1 N21' 2.057(5) . ? Ru1 N1' 2.060(5) . ? Ru1 N41' 2.064(5) . ? N1 C10 1.353(8) . ? N1 C2 1.353(7) . ? N1' C10' 1.330(8) . ? N1' C2' 1.364(7) . ? N21 C30 1.348(8) . ? N21 C22 1.360(8) . ? N21' C30' 1.335(8) . ? N21' C22' 1.367(7) . ? N41 C50 1.325(8) . ? N41 C42 1.370(7) . ? N41' C50' 1.330(8) . ? N41' C42' 1.355(7) . ? C2 C3 1.399(7) . ? C2 C2' 1.459(8) . ? C3 C4 1.365(8) . ? C4 C9 1.406(8) . ? C4 C5 1.517(8) . ? C5 C6 1.531(10) . ? C6 C11 1.551(9) . ? C6 C7 1.564(9) . ? C7 C12 1.493(10) . ? C7 C13 1.533(11) . ? C7 C8 1.590(9) . ? C8 C9 1.491(10) . ? C8 C11 1.588(8) . ? C9 C10 1.375(8) . ? C2' C3' 1.406(7) . ? C3' C4' 1.378(9) . ? C4' C9' 1.398(8) . ? C4' C5' 1.545(8) . ? C5' C6' 1.549(11) . ? C6' C11' 1.543(14) . ? C6' C7' 1.579(13) . ? C7' C13' 1.520(15) . ? C7' C12' 1.540(13) . ? C7' C8' 1.552(13) . ? C8' C9' 1.505(9) . ? C8' C11' 1.552(10) . ? C9' C10' 1.398(8) . ? C22 C23 1.397(7) . ? C22 C22' 1.456(8) . ? C23 C24 1.389(9) . ? C24 C29 1.405(8) . ? C24 C25 1.531(8) . ? C25 C26 1.523(9) . ? C27 C32 1.505(12) . ? C27 C33 1.524(11) . ? C27 C26 1.562(9) . ? C27 C28 1.563(9) . ? C26 C31 1.532(9) . ? C28 C29 1.475(9) . ? C28 C31 1.571(9) . ? C29 C30 1.383(8) . ? C22' C23' 1.386(8) . ? C23' C24' 1.386(9) . ? C24' C29' 1.422(9) . ? C24' C25' 1.523(8) . ? C25' C26' 1.534(12) . ? C26' C27' 1.534(13) . ? C26' C31' 1.543(14) . ? C27' C33' 1.496(15) . ? C27' C32' 1.547(14) . ? C27' C28' 1.565(12) . ? C28' C29' 1.502(10) . ? C28' C31' 1.540(10) . ? C29' C30' 1.385(8) . ? C42 C43 1.375(8) . ? C42 C42' 1.467(8) . ? C43 C44 1.383(9) . ? C44 C49 1.394(8) . ? C44 C45 1.548(8) . ? C45 C46 1.517(11) . ? C46 C51 1.562(14) . ? C46 C47 1.605(12) . ? C47 C53 1.477(17) . ? C47 C52 1.556(14) . ? C47 C48 1.589(14) . ? C48 C49 1.498(9) . ? C48 C51 1.580(11) . ? C49 C50 1.382(8) . ? C42' C43' 1.411(8) . ? C43' C44' 1.377(10) . ? C44' C49' 1.399(9) . ? C44' C45' 1.513(8) . ? C45' C46' 1.538(11) . ? C46' C51' 1.512(14) . ? C46' C47' 1.588(12) . ? C47' C52' 1.497(13) . ? C47' C53' 1.541(13) . ? C47' C48' 1.542(12) . ? C48' C49' 1.477(10) . ? C48' C51' 1.577(9) . ? C49' C50' 1.419(8) . ? C54 Cl2 1.674(13) . ? C54 Cl3 1.715(13) . ? C54 Cl1 1.753(13) . ? C54 Cl1A 1.756(13) . ? C54 Cl2A 1.777(13) . ? C55 Cl6 1.713(15) . ? C55 Cl5 1.732(15) . ? C55 Cl4 1.745(14) . ? C55A Cl5A 1.78(2) . ? C55A Cl6A 1.78(2) . ? C55A Cl4A 1.80(2) . ? C56 Cl8A 1.684(11) . ? C56 Cl7A 1.706(11) . ? C56 Cl9 1.711(11) . ? C56 Cl7 1.776(12) . ? C56 Cl8 1.806(10) . ? C57 Cl11 1.674(17) . ? C57 Cl10 1.758(17) . ? C57 Cl12 1.786(16) . ? C58 Cl15 1.731(13) . ? C58 Cl13 1.737(14) . ? C58 Cl14 1.772(15) . ? P1 F1 1.553(7) . ? P1 F4 1.557(7) . ? P1 F6 1.571(6) . ? P1 F2 1.573(7) . ? P1 F5 1.585(5) . ? P1 F3 1.590(6) . ? P2 F9A 1.506(16) . ? P2 F10 1.529(18) . ? P2 F7A 1.550(18) . ? P2 F11A 1.57(3) . ? P2 F8 1.591(13) . ? P2 F12A 1.60(3) . ? P2 F12 1.602(17) . ? P2 F7 1.612(11) . ? P2 F11 1.612(16) . ? P2 F8A 1.61(2) . ? P2 F9 1.654(15) . ? P2 F10A 1.666(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N21 92.7(2) . . ? N1 Ru1 N41 93.9(2) . . ? N21 Ru1 N41 171.7(2) . . ? N1 Ru1 N21' 95.7(2) . . ? N21 Ru1 N21' 78.8(2) . . ? N41 Ru1 N21' 95.6(2) . . ? N1 Ru1 N1' 78.9(2) . . ? N21 Ru1 N1' 95.6(2) . . ? N41 Ru1 N1' 90.5(2) . . ? N21' Ru1 N1' 172.1(2) . . ? N1 Ru1 N41' 171.2(2) . . ? N21 Ru1 N41' 94.6(2) . . ? N41 Ru1 N41' 79.3(2) . . ? N21' Ru1 N41' 90.6(2) . . ? N1' Ru1 N41' 95.4(2) . . ? C10 N1 C2 117.5(5) . . ? C10 N1 Ru1 125.8(4) . . ? C2 N1 Ru1 116.0(4) . . ? C10' N1' C2' 119.3(5) . . ? C10' N1' Ru1 125.7(4) . . ? C2' N1' Ru1 114.6(4) . . ? C30 N21 C22 118.5(5) . . ? C30 N21 Ru1 124.9(4) . . ? C22 N21 Ru1 115.9(4) . . ? C30' N21' C22' 119.1(5) . . ? C30' N21' Ru1 125.6(4) . . ? C22' N21' Ru1 115.1(4) . . ? C50 N41 C42 118.1(5) . . ? C50 N41 Ru1 126.6(4) . . ? C42 N41 Ru1 115.1(4) . . ? C50' N41' C42' 120.2(5) . . ? C50' N41' Ru1 124.9(4) . . ? C42' N41' Ru1 114.7(4) . . ? N1 C2 C3 121.3(5) . . ? N1 C2 C2' 114.2(4) . . ? C3 C2 C2' 124.4(5) . . ? C4 C3 C2 120.4(5) . . ? C3 C4 C9 118.8(5) . . ? C3 C4 C5 123.9(5) . . ? C9 C4 C5 117.1(6) . . ? C4 C5 C6 111.2(5) . . ? C5 C6 C11 108.0(6) . . ? C5 C6 C7 111.9(5) . . ? C11 C6 C7 88.5(5) . . ? C12 C7 C13 110.5(7) . . ? C12 C7 C6 119.1(6) . . ? C13 C7 C6 111.0(6) . . ? C12 C7 C8 117.9(5) . . ? C13 C7 C8 110.6(7) . . ? C6 C7 C8 85.4(5) . . ? C9 C8 C11 107.2(5) . . ? C9 C8 C7 108.3(5) . . ? C11 C8 C7 86.3(5) . . ? C10 C9 C4 117.8(6) . . ? C10 C9 C8 123.9(5) . . ? C4 C9 C8 118.2(5) . . ? N1 C10 C9 124.1(5) . . ? C6 C11 C8 85.9(4) . . ? N1' C2' C3' 120.6(5) . . ? N1' C2' C2 115.2(4) . . ? C3' C2' C2 124.2(5) . . ? C4' C3' C2' 119.4(5) . . ? C3' C4' C9' 119.7(5) . . ? C3' C4' C5' 122.6(5) . . ? C9' C4' C5' 117.6(6) . . ? C4' C5' C6' 109.0(5) . . ? C11' C6' C5' 109.9(8) . . ? C11' C6' C7' 88.4(7) . . ? C5' C6' C7' 110.0(7) . . ? C13' C7' C12' 108.3(9) . . ? C13' C7' C8' 120.1(7) . . ? C12' C7' C8' 111.5(8) . . ? C13' C7' C6' 120.4(8) . . ? C12' C7' C6' 110.3(8) . . ? C8' C7' C6' 84.6(7) . . ? C9' C8' C11' 106.6(6) . . ? C9' C8' C7' 108.0(6) . . ? C11' C8' C7' 89.1(6) . . ? C10' C9' C4' 117.6(6) . . ? C10' C9' C8' 124.4(5) . . ? C4' C9' C8' 117.8(5) . . ? N1' C10' C9' 123.2(5) . . ? C6' C11' C8' 85.8(6) . . ? N21 C22 C23 120.8(5) . . ? N21 C22 C22' 114.5(5) . . ? C23 C22 C22' 124.6(5) . . ? C24 C23 C22 120.0(5) . . ? C23 C24 C29 119.1(5) . . ? C23 C24 C25 123.7(5) . . ? C29 C24 C25 117.2(5) . . ? C26 C25 C24 110.1(5) . . ? C32 C27 C33 109.1(7) . . ? C32 C27 C26 112.8(6) . . ? C33 C27 C26 118.7(6) . . ? C32 C27 C28 112.1(6) . . ? C33 C27 C28 117.4(6) . . ? C26 C27 C28 85.0(5) . . ? C25 C26 C31 108.7(6) . . ? C25 C26 C27 112.4(5) . . ? C31 C26 C27 88.3(5) . . ? C29 C28 C27 110.2(5) . . ? C29 C28 C31 106.9(5) . . ? C27 C28 C31 86.9(5) . . ? C30 C29 C24 117.5(6) . . ? C30 C29 C28 124.7(5) . . ? C24 C29 C28 117.6(5) . . ? N21 C30 C29 123.9(5) . . ? C26 C31 C28 85.7(5) . . ? N21' C22' C23' 120.7(6) . . ? N21' C22' C22 115.0(5) . . ? C23' C22' C22 124.3(5) . . ? C22' C23' C24' 120.4(5) . . ? C23' C24' C29' 118.5(5) . . ? C23' C24' C25' 123.4(6) . . ? C29' C24' C25' 118.1(6) . . ? C24' C25' C26' 109.5(6) . . ? C25' C26' C27' 113.6(7) . . ? C25' C26' C31' 108.5(8) . . ? C27' C26' C31' 87.2(7) . . ? C33' C27' C26' 118.8(8) . . ? C33' C27' C32' 107.3(9) . . ? C26' C27' C32' 111.7(8) . . ? C33' C27' C28' 118.2(7) . . ? C26' C27' C28' 86.3(7) . . ? C32' C27' C28' 113.6(9) . . ? C29' C28' C31' 106.7(6) . . ? C29' C28' C27' 109.0(6) . . ? C31' C28' C27' 86.2(6) . . ? C30' C29' C24' 117.5(6) . . ? C30' C29' C28' 125.3(5) . . ? C24' C29' C28' 117.0(5) . . ? N21' C30' C29' 123.6(5) . . ? C28' C31' C26' 86.8(6) . . ? N41 C42 C43 121.3(6) . . ? N41 C42 C42' 114.4(5) . . ? C43 C42 C42' 124.3(5) . . ? C42 C43 C44 119.7(5) . . ? C43 C44 C49 119.1(5) . . ? C43 C44 C45 123.5(5) . . ? C49 C44 C45 117.4(6) . . ? C46 C45 C44 109.9(5) . . ? C45 C46 C51 109.0(7) . . ? C45 C46 C47 111.1(7) . . ? C51 C46 C47 88.6(7) . . ? C53 C47 C52 113.4(12) . . ? C53 C47 C48 120.0(8) . . ? C52 C47 C48 108.2(10) . . ? C53 C47 C46 120.1(8) . . ? C52 C47 C46 107.3(9) . . ? C48 C47 C46 84.2(7) . . ? C49 C48 C51 106.6(6) . . ? C49 C48 C47 107.0(6) . . ? C51 C48 C47 88.6(7) . . ? C50 C49 C44 117.6(6) . . ? C50 C49 C48 124.0(5) . . ? C44 C49 C48 118.4(5) . . ? N41 C50 C49 124.0(5) . . ? C46 C51 C48 85.9(7) . . ? N41' C42' C43' 119.9(5) . . ? N41' C42' C42 115.9(5) . . ? C43' C42' C42 124.2(5) . . ? C44' C43' C42' 120.0(5) . . ? C43' C44' C49' 120.0(5) . . ? C43' C44' C45' 123.6(6) . . ? C49' C44' C45' 116.5(6) . . ? C44' C45' C46' 110.3(5) . . ? C51' C46' C45' 108.3(8) . . ? C51' C46' C47' 88.8(6) . . ? C45' C46' C47' 111.4(6) . . ? C52' C47' C53' 108.3(9) . . ? C52' C47' C48' 113.3(8) . . ? C53' C47' C48' 118.5(6) . . ? C52' C47' C46' 110.9(7) . . ? C53' C47' C46' 119.8(8) . . ? C48' C47' C46' 84.4(7) . . ? C49' C48' C47' 108.9(6) . . ? C49' C48' C51' 105.6(6) . . ? C47' C48' C51' 88.1(6) . . ? C44' C49' C50' 116.7(6) . . ? C44' C49' C48' 119.1(6) . . ? C50' C49' C48' 124.0(6) . . ? N41' C50' C49' 123.0(5) . . ? C46' C51' C48' 85.8(6) . . ? Cl2 C54 Cl3 103.8(7) . . ? Cl2 C54 Cl1 119.6(9) . . ? Cl3 C54 Cl1 125.3(8) . . ? Cl2 C54 Cl1A 127.3(9) . . ? Cl3 C54 Cl1A 98.5(7) . . ? Cl1 C54 Cl1A 28.6(5) . . ? Cl2 C54 Cl2A 21.0(4) . . ? Cl3 C54 Cl2A 113.7(8) . . ? Cl1 C54 Cl2A 100.2(8) . . ? Cl1A C54 Cl2A 106.5(8) . . ? Cl6 C55 Cl5 111.8(10) . . ? Cl6 C55 Cl4 113.0(10) . . ? Cl5 C55 Cl4 104.1(9) . . ? Cl5A C55A Cl6A 113.2(18) . . ? Cl5A C55A Cl4A 132(3) . . ? Cl6A C55A Cl4A 95.6(19) . . ? Cl8A C56 Cl7A 121.1(7) . . ? Cl8A C56 Cl9 118.3(6) . . ? Cl7A C56 Cl9 113.6(6) . . ? Cl8A C56 Cl7 106.2(7) . . ? Cl7A C56 Cl7 28.7(4) . . ? Cl9 C56 Cl7 108.1(6) . . ? Cl8A C56 Cl8 19.0(3) . . ? Cl7A C56 Cl8 121.7(7) . . ? Cl9 C56 Cl8 105.5(6) . . ? Cl7 C56 Cl8 99.3(6) . . ? Cl11 C57 Cl10 111.1(7) . . ? Cl11 C57 Cl12 110.9(9) . . ? Cl10 C57 Cl12 107.2(10) . . ? Cl15 C58 Cl13 112.4(8) . . ? Cl15 C58 Cl14 110.0(7) . . ? Cl13 C58 Cl14 110.8(7) . . ? F1 P1 F4 90.1(6) . . ? F1 P1 F6 92.3(6) . . ? F4 P1 F6 177.6(6) . . ? F1 P1 F2 176.2(6) . . ? F4 P1 F2 93.6(6) . . ? F6 P1 F2 84.1(5) . . ? F1 P1 F5 92.2(5) . . ? F4 P1 F5 89.9(4) . . ? F6 P1 F5 90.0(3) . . ? F2 P1 F5 88.9(4) . . ? F1 P1 F3 88.7(4) . . ? F4 P1 F3 91.9(4) . . ? F6 P1 F3 88.1(3) . . ? F2 P1 F3 90.2(3) . . ? F5 P1 F3 178.0(3) . . ? F9A P2 F10 120.5(10) . . ? F9A P2 F7A 96.2(10) . . ? F10 P2 F7A 112.7(11) . . ? F9A P2 F11A 81.8(13) . . ? F10 P2 F11A 52.9(12) . . ? F7A P2 F11A 84.4(13) . . ? F9A P2 F8 82.2(8) . . ? F10 P2 F8 90.6(9) . . ? F7A P2 F8 153.0(10) . . ? F11A P2 F8 121.7(12) . . ? F9A P2 F12A 103.6(16) . . ? F10 P2 F12A 115.0(15) . . ? F7A P2 F12A 106.6(16) . . ? F11A P2 F12A 166.9(16) . . ? F8 P2 F12A 48.7(13) . . ? F9A P2 F12 34.6(7) . . ? F10 P2 F12 87.6(10) . . ? F7A P2 F12 101.4(10) . . ? F11A P2 F12 49.3(12) . . ? F8 P2 F12 92.6(8) . . ? F12A P2 F12 132.2(16) . . ? F9A P2 F7 97.2(7) . . ? F10 P2 F7 90.3(9) . . ? F7A P2 F7 26.3(8) . . ? F11A P2 F7 58.8(11) . . ? F8 P2 F7 179.1(7) . . ? F12A P2 F7 130.9(15) . . ? F12 P2 F7 87.4(8) . . ? F9A P2 F11 134.2(10) . . ? F10 P2 F11 103.0(10) . . ? F7A P2 F11 78.2(10) . . ? F11A P2 F11 141.0(14) . . ? F8 P2 F11 83.7(8) . . ? F12A P2 F11 39.5(13) . . ? F12 P2 F11 168.8(10) . . ? F7 P2 F11 96.2(8) . . ? F9A P2 F8A 91.0(12) . . ? F10 P2 F8A 53.9(11) . . ? F7A P2 F8A 166.6(13) . . ? F11A P2 F8A 85.5(15) . . ? F8 P2 F8A 39.4(10) . . ? F12A P2 F8A 82.6(16) . . ? F12 P2 F8A 78.4(12) . . ? F7 P2 F8A 141.4(12) . . ? F11 P2 F8A 104.7(12) . . ? F9A P2 F9 48.7(8) . . ? F10 P2 F9 169.2(9) . . ? F7A P2 F9 72.4(9) . . ? F11A P2 F9 120.2(12) . . ? F8 P2 F9 87.0(7) . . ? F12A P2 F9 70.9(14) . . ? F12 P2 F9 82.0(8) . . ? F7 P2 F9 92.1(7) . . ? F11 P2 F9 87.3(8) . . ? F8A P2 F9 120.5(12) . . ? F9A P2 F10A 179.0(9) . . ? F10 P2 F10A 58.6(9) . . ? F7A P2 F10A 83.8(8) . . ? F11A P2 F10A 97.2(12) . . ? F8 P2 F10A 98.2(6) . . ? F12A P2 F10A 77.4(15) . . ? F12 P2 F10A 144.4(8) . . ? F7 P2 F10A 82.3(6) . . ? F11 P2 F10A 46.8(7) . . ? F8A P2 F10A 88.8(11) . . ? F9 P2 F10A 132.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Ru1 N1 C10 91.3(5) . . . . ? N41 Ru1 N1 C10 -83.7(5) . . . . ? N21' Ru1 N1 C10 12.3(5) . . . . ? N1' Ru1 N1 C10 -173.5(5) . . . . ? N41' Ru1 N1 C10 -123.7(15) . . . . ? N21 Ru1 N1 C2 -98.5(4) . . . . ? N41 Ru1 N1 C2 86.5(4) . . . . ? N21' Ru1 N1 C2 -177.4(4) . . . . ? N1' Ru1 N1 C2 -3.3(4) . . . . ? N41' Ru1 N1 C2 46.6(19) . . . . ? N1 Ru1 N1' C10' -176.1(5) . . . . ? N21 Ru1 N1' C10' -84.4(5) . . . . ? N41 Ru1 N1' C10' 90.0(5) . . . . ? N21' Ru1 N1' C10' -128.6(17) . . . . ? N41' Ru1 N1' C10' 10.7(5) . . . . ? N1 Ru1 N1' C2' -3.6(4) . . . . ? N21 Ru1 N1' C2' 88.0(4) . . . . ? N41 Ru1 N1' C2' -97.6(4) . . . . ? N21' Ru1 N1' C2' 44(2) . . . . ? N41' Ru1 N1' C2' -176.9(4) . . . . ? N1 Ru1 N21 C30 90.5(5) . . . . ? N41 Ru1 N21 C30 -126.4(17) . . . . ? N21' Ru1 N21 C30 -174.1(5) . . . . ? N1' Ru1 N21 C30 11.5(5) . . . . ? N41' Ru1 N21 C30 -84.4(5) . . . . ? N1 Ru1 N21 C22 -98.7(4) . . . . ? N41 Ru1 N21 C22 44(2) . . . . ? N21' Ru1 N21 C22 -3.4(4) . . . . ? N1' Ru1 N21 C22 -177.8(4) . . . . ? N41' Ru1 N21 C22 86.4(4) . . . . ? N1 Ru1 N21' C30' -85.2(5) . . . . ? N21 Ru1 N21' C30' -176.7(5) . . . . ? N41 Ru1 N21' C30' 9.4(5) . . . . ? N1' Ru1 N21' C30' -131.7(17) . . . . ? N41' Ru1 N21' C30' 88.7(5) . . . . ? N1 Ru1 N21' C22' 89.5(4) . . . . ? N21 Ru1 N21' C22' -2.0(4) . . . . ? N41 Ru1 N21' C22' -175.9(4) . . . . ? N1' Ru1 N21' C22' 43(2) . . . . ? N41' Ru1 N21' C22' -96.6(4) . . . . ? N1 Ru1 N41 C50 7.2(5) . . . . ? N21 Ru1 N41 C50 -135.8(16) . . . . ? N21' Ru1 N41 C50 -89.0(5) . . . . ? N1' Ru1 N41 C50 86.1(5) . . . . ? N41' Ru1 N41 C50 -178.5(5) . . . . ? N1 Ru1 N41 C42 -178.9(4) . . . . ? N21 Ru1 N41 C42 38(2) . . . . ? N21' Ru1 N41 C42 84.9(4) . . . . ? N1' Ru1 N41 C42 -100.0(4) . . . . ? N41' Ru1 N41 C42 -4.6(4) . . . . ? N1 Ru1 N41' C50' -134.5(15) . . . . ? N21 Ru1 N41' C50' 10.4(5) . . . . ? N41 Ru1 N41' C50' -175.2(5) . . . . ? N21' Ru1 N41' C50' 89.2(5) . . . . ? N1' Ru1 N41' C50' -85.6(5) . . . . ? N1 Ru1 N41' C42' 40.8(19) . . . . ? N21 Ru1 N41' C42' -174.3(4) . . . . ? N41 Ru1 N41' C42' 0.1(4) . . . . ? N21' Ru1 N41' C42' -95.5(4) . . . . ? N1' Ru1 N41' C42' 89.6(4) . . . . ? C10 N1 C2 C3 3.1(8) . . . . ? Ru1 N1 C2 C3 -168.0(4) . . . . ? C10 N1 C2 C2' -179.7(5) . . . . ? Ru1 N1 C2 C2' 9.2(6) . . . . ? N1 C2 C3 C4 -1.6(8) . . . . ? C2' C2 C3 C4 -178.5(5) . . . . ? C2 C3 C4 C9 -0.2(8) . . . . ? C2 C3 C4 C5 174.9(5) . . . . ? C3 C4 C5 C6 -175.6(5) . . . . ? C9 C4 C5 C6 -0.5(8) . . . . ? C4 C5 C6 C11 -49.1(7) . . . . ? C4 C5 C6 C7 46.7(7) . . . . ? C5 C6 C7 C12 38.6(8) . . . . ? C11 C6 C7 C12 147.4(6) . . . . ? C5 C6 C7 C13 168.6(7) . . . . ? C11 C6 C7 C13 -82.5(7) . . . . ? C5 C6 C7 C8 -81.0(6) . . . . ? C11 C6 C7 C8 27.8(5) . . . . ? C12 C7 C8 C9 -41.0(8) . . . . ? C13 C7 C8 C9 -169.5(6) . . . . ? C6 C7 C8 C9 79.7(5) . . . . ? C12 C7 C8 C11 -147.9(6) . . . . ? C13 C7 C8 C11 83.6(7) . . . . ? C6 C7 C8 C11 -27.2(5) . . . . ? C3 C4 C9 C10 0.4(8) . . . . ? C5 C4 C9 C10 -174.9(5) . . . . ? C3 C4 C9 C8 177.8(5) . . . . ? C5 C4 C9 C8 2.4(8) . . . . ? C11 C8 C9 C10 -139.6(6) . . . . ? C7 C8 C9 C10 128.6(6) . . . . ? C11 C8 C9 C4 43.3(7) . . . . ? C7 C8 C9 C4 -48.6(7) . . . . ? C2 N1 C10 C9 -2.9(8) . . . . ? Ru1 N1 C10 C9 167.3(5) . . . . ? C4 C9 C10 N1 1.1(9) . . . . ? C8 C9 C10 N1 -176.0(6) . . . . ? C5 C6 C11 C8 84.7(5) . . . . ? C7 C6 C11 C8 -27.8(5) . . . . ? C9 C8 C11 C6 -80.6(6) . . . . ? C7 C8 C11 C6 27.4(5) . . . . ? C10' N1' C2' C3' 3.1(8) . . . . ? Ru1 N1' C2' C3' -169.9(5) . . . . ? C10' N1' C2' C2 -177.5(5) . . . . ? Ru1 N1' C2' C2 9.5(6) . . . . ? N1 C2 C2' N1' -12.3(7) . . . . ? C3 C2 C2' N1' 164.8(5) . . . . ? N1 C2 C2' C3' 167.1(6) . . . . ? C3 C2 C2' C3' -15.8(9) . . . . ? N1' C2' C3' C4' -0.4(9) . . . . ? C2 C2' C3' C4' -179.8(6) . . . . ? C2' C3' C4' C9' -3.9(10) . . . . ? C2' C3' C4' C5' 173.5(7) . . . . ? C3' C4' C5' C6' 178.8(7) . . . . ? C9' C4' C5' C6' -3.7(10) . . . . ? C4' C5' C6' C11' -45.6(9) . . . . ? C4' C5' C6' C7' 50.1(10) . . . . ? C11' C6' C7' C13' 147.9(9) . . . . ? C5' C6' C7' C13' 37.2(12) . . . . ? C11' C6' C7' C12' -85.0(9) . . . . ? C5' C6' C7' C12' 164.4(9) . . . . ? C11' C6' C7' C8' 25.9(6) . . . . ? C5' C6' C7' C8' -84.7(8) . . . . ? C13' C7' C8' C9' -40.8(10) . . . . ? C12' C7' C8' C9' -168.9(7) . . . . ? C6' C7' C8' C9' 81.4(6) . . . . ? C13' C7' C8' C11' -147.9(8) . . . . ? C12' C7' C8' C11' 83.9(8) . . . . ? C6' C7' C8' C11' -25.7(6) . . . . ? C3' C4' C9' C10' 5.4(10) . . . . ? C5' C4' C9' C10' -172.1(6) . . . . ? C3' C4' C9' C8' -179.1(6) . . . . ? C5' C4' C9' C8' 3.4(9) . . . . ? C11' C8' C9' C10' -139.6(7) . . . . ? C7' C8' C9' C10' 125.9(7) . . . . ? C11' C8' C9' C4' 45.3(9) . . . . ? C7' C8' C9' C4' -49.2(8) . . . . ? C2' N1' C10' C9' -1.4(9) . . . . ? Ru1 N1' C10' C9' 170.7(5) . . . . ? C4' C9' C10' N1' -2.9(9) . . . . ? C8' C9' C10' N1' -178.0(6) . . . . ? C5' C6' C11' C8' 84.9(7) . . . . ? C7' C6' C11' C8' -25.9(6) . . . . ? C9' C8' C11' C6' -82.1(7) . . . . ? C7' C8' C11' C6' 26.3(6) . . . . ? C30 N21 C22 C23 3.2(8) . . . . ? Ru1 N21 C22 C23 -168.2(4) . . . . ? C30 N21 C22 C22' 179.3(5) . . . . ? Ru1 N21 C22 C22' 7.9(6) . . . . ? N21 C22 C23 C24 -0.1(8) . . . . ? C22' C22 C23 C24 -175.8(5) . . . . ? C22 C23 C24 C29 -2.9(8) . . . . ? C22 C23 C24 C25 174.2(5) . . . . ? C23 C24 C25 C26 -178.4(5) . . . . ? C29 C24 C25 C26 -1.2(7) . . . . ? C24 C25 C26 C31 -48.1(7) . . . . ? C24 C25 C26 C27 47.9(7) . . . . ? C32 C27 C26 C25 166.7(6) . . . . ? C33 C27 C26 C25 37.3(9) . . . . ? C28 C27 C26 C25 -81.4(6) . . . . ? C32 C27 C26 C31 -83.8(7) . . . . ? C33 C27 C26 C31 146.8(7) . . . . ? C28 C27 C26 C31 28.1(5) . . . . ? C32 C27 C28 C29 -167.9(6) . . . . ? C33 C27 C28 C29 -40.4(8) . . . . ? C26 C27 C28 C29 79.5(6) . . . . ? C32 C27 C28 C31 85.2(7) . . . . ? C33 C27 C28 C31 -147.3(6) . . . . ? C26 C27 C28 C31 -27.4(5) . . . . ? C23 C24 C29 C30 2.8(8) . . . . ? C25 C24 C29 C30 -174.5(5) . . . . ? C23 C24 C29 C28 179.0(5) . . . . ? C25 C24 C29 C28 1.7(8) . . . . ? C27 C28 C29 C30 127.9(6) . . . . ? C31 C28 C29 C30 -139.1(6) . . . . ? C27 C28 C29 C24 -47.9(7) . . . . ? C31 C28 C29 C24 45.0(7) . . . . ? C22 N21 C30 C29 -3.4(8) . . . . ? Ru1 N21 C30 C29 167.2(4) . . . . ? C24 C29 C30 N21 0.3(8) . . . . ? C28 C29 C30 N21 -175.6(6) . . . . ? C25 C26 C31 C28 85.1(6) . . . . ? C27 C26 C31 C28 -27.9(5) . . . . ? C29 C28 C31 C26 -82.2(6) . . . . ? C27 C28 C31 C26 28.0(5) . . . . ? C30' N21' C22' C23' 3.5(8) . . . . ? Ru1 N21' C22' C23' -171.6(4) . . . . ? C30' N21' C22' C22 -178.2(5) . . . . ? Ru1 N21' C22' C22 6.8(6) . . . . ? N21 C22 C22' N21' -9.6(7) . . . . ? C23 C22 C22' N21' 166.3(5) . . . . ? N21 C22 C22' C23' 168.7(5) . . . . ? C23 C22 C22' C23' -15.4(8) . . . . ? N21' C22' C23' C24' -1.3(9) . . . . ? C22 C22' C23' C24' -179.4(5) . . . . ? C22' C23' C24' C29' -2.3(9) . . . . ? C22' C23' C24' C25' 175.4(6) . . . . ? C23' C24' C25' C26' -177.7(7) . . . . ? C29' C24' C25' C26' 0.0(10) . . . . ? C24' C25' C26' C27' 46.7(11) . . . . ? C24' C25' C26' C31' -48.4(9) . . . . ? C25' C26' C27' C33' 38.7(11) . . . . ? C31' C26' C27' C33' 147.6(8) . . . . ? C25' C26' C27' C32' 164.4(9) . . . . ? C31' C26' C27' C32' -86.7(9) . . . . ? C25' C26' C27' C28' -81.7(8) . . . . ? C31' C26' C27' C28' 27.3(6) . . . . ? C33' C27' C28' C29' -41.8(10) . . . . ? C26' C27' C28' C29' 79.0(7) . . . . ? C32' C27' C28' C29' -168.9(8) . . . . ? C33' C27' C28' C31' -148.2(8) . . . . ? C26' C27' C28' C31' -27.3(6) . . . . ? C32' C27' C28' C31' 84.7(9) . . . . ? C23' C24' C29' C30' 3.5(9) . . . . ? C25' C24' C29' C30' -174.4(6) . . . . ? C23' C24' C29' C28' 179.5(6) . . . . ? C25' C24' C29' C28' 1.7(9) . . . . ? C31' C28' C29' C30' -140.0(7) . . . . ? C27' C28' C29' C30' 128.3(7) . . . . ? C31' C28' C29' C24' 44.3(9) . . . . ? C27' C28' C29' C24' -47.4(8) . . . . ? C22' N21' C30' C29' -2.2(9) . . . . ? Ru1 N21' C30' C29' 172.3(5) . . . . ? C24' C29' C30' N21' -1.3(9) . . . . ? C28' C29' C30' N21' -177.0(6) . . . . ? C29' C28' C31' C26' -81.5(7) . . . . ? C27' C28' C31' C26' 27.1(6) . . . . ? C25' C26' C31' C28' 86.2(7) . . . . ? C27' C26' C31' C28' -27.7(6) . . . . ? C50 N41 C42 C43 3.9(8) . . . . ? Ru1 N41 C42 C43 -170.6(4) . . . . ? C50 N41 C42 C42' -177.4(5) . . . . ? Ru1 N41 C42 C42' 8.1(6) . . . . ? N41 C42 C43 C44 -0.3(9) . . . . ? C42' C42 C43 C44 -178.9(6) . . . . ? C42 C43 C44 C49 -4.2(9) . . . . ? C42 C43 C44 C45 174.4(6) . . . . ? C43 C44 C45 C46 178.9(7) . . . . ? C49 C44 C45 C46 -2.4(9) . . . . ? C44 C45 C46 C51 -47.6(9) . . . . ? C44 C45 C46 C47 48.5(9) . . . . ? C45 C46 C47 C53 38.0(11) . . . . ? C51 C46 C47 C53 147.8(9) . . . . ? C45 C46 C47 C52 169.3(10) . . . . ? C51 C46 C47 C52 -80.9(10) . . . . ? C45 C46 C47 C48 -83.5(8) . . . . ? C51 C46 C47 C48 26.4(6) . . . . ? C53 C47 C48 C49 -40.6(10) . . . . ? C52 C47 C48 C49 -172.8(8) . . . . ? C46 C47 C48 C49 80.9(7) . . . . ? C53 C47 C48 C51 -147.6(8) . . . . ? C52 C47 C48 C51 80.3(9) . . . . ? C46 C47 C48 C51 -26.0(6) . . . . ? C43 C44 C49 C50 5.2(9) . . . . ? C45 C44 C49 C50 -173.6(6) . . . . ? C43 C44 C49 C48 -177.4(6) . . . . ? C45 C44 C49 C48 3.8(9) . . . . ? C51 C48 C49 C50 -139.5(7) . . . . ? C47 C48 C49 C50 126.8(7) . . . . ? C51 C48 C49 C44 43.2(9) . . . . ? C47 C48 C49 C44 -50.5(9) . . . . ? C42 N41 C50 C49 -2.9(8) . . . . ? Ru1 N41 C50 C49 170.9(5) . . . . ? C44 C49 C50 N41 -1.6(9) . . . . ? C48 C49 C50 N41 -178.9(6) . . . . ? C45 C46 C51 C48 85.4(7) . . . . ? C47 C46 C51 C48 -26.5(6) . . . . ? C49 C48 C51 C46 -80.6(7) . . . . ? C47 C48 C51 C46 26.7(6) . . . . ? C50' N41' C42' C43' 1.8(9) . . . . ? Ru1 N41' C42' C43' -173.7(5) . . . . ? C50' N41' C42' C42 179.7(5) . . . . ? Ru1 N41' C42' C42 4.2(6) . . . . ? N41 C42 C42' N41' -8.2(7) . . . . ? C43 C42 C42' N41' 170.5(6) . . . . ? N41 C42 C42' C43' 169.6(6) . . . . ? C43 C42 C42' C43' -11.7(9) . . . . ? N41' C42' C43' C44' 2.7(10) . . . . ? C42 C42' C43' C44' -175.0(6) . . . . ? C42' C43' C44' C49' -6.3(11) . . . . ? C42' C43' C44' C45' 174.3(7) . . . . ? C43' C44' C45' C46' 179.7(8) . . . . ? C49' C44' C45' C46' 0.3(11) . . . . ? C44' C45' C46' C51' -49.4(10) . . . . ? C44' C45' C46' C47' 46.7(11) . . . . ? C51' C46' C47' C52' -85.7(9) . . . . ? C45' C46' C47' C52' 165.0(9) . . . . ? C51' C46' C47' C53' 146.9(8) . . . . ? C45' C46' C47' C53' 37.7(11) . . . . ? C51' C46' C47' C48' 27.1(5) . . . . ? C45' C46' C47' C48' -82.1(8) . . . . ? C52' C47' C48' C49' -169.7(7) . . . . ? C53' C47' C48' C49' -41.1(10) . . . . ? C46' C47' C48' C49' 79.9(6) . . . . ? C52' C47' C48' C51' 84.4(8) . . . . ? C53' C47' C48' C51' -147.0(8) . . . . ? C46' C47' C48' C51' -25.9(5) . . . . ? C43' C44' C49' C50' 5.3(11) . . . . ? C45' C44' C49' C50' -175.3(7) . . . . ? C43' C44' C49' C48' -179.5(7) . . . . ? C45' C44' C49' C48' -0.1(11) . . . . ? C47' C48' C49' C44' -48.0(9) . . . . ? C51' C48' C49' C44' 45.4(10) . . . . ? C47' C48' C49' C50' 126.8(7) . . . . ? C51' C48' C49' C50' -139.8(7) . . . . ? C42' N41' C50' C49' -2.8(9) . . . . ? Ru1 N41' C50' C49' 172.2(5) . . . . ? C44' C49' C50' N41' -0.7(10) . . . . ? C48' C49' C50' N41' -175.7(7) . . . . ? C45' C46' C51' C48' 85.8(7) . . . . ? C47' C46' C51' C48' -26.4(6) . . . . ? C49' C48' C51' C46' -81.8(7) . . . . ? C47' C48' C51' C46' 27.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.177 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.097 data_2b _database_code_depnum_ccdc_archive 'CCDC 281498' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H78 N6 Ru, 2(P F6), 6(C H Cl3' _chemical_formula_weight 2134.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.9231(10) _cell_length_b 23.3654(14) _cell_length_c 15.2120(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.930(7) _cell_angle_gamma 90.00 _cell_volume 4642.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.00 _exptl_crystal_description bloc _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Stoe IPDS' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34933 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.1670 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.91 _reflns_number_total 17860 _reflns_number_gt 10004 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie Company, Germany)' _computing_cell_refinement 'CELL (Stoe & Cie Company, Germany)' _computing_data_reduction 'XRED (Stoe & Cie Company, Germany)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON97 (Spek, 1997)' _computing_publication_material SHELXL-97 _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 w=1/[\s^2^(Fo^2^)+(0.0562P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 17860 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.44420(3) 0.47764(2) 0.30726(4) 0.01735(11) Uani 1 d . . . C2 C 0.3724(5) 0.5370(3) 0.1158(5) 0.0194(14) Uani 1 d . . . C3 C 0.3674(5) 0.5768(3) 0.0456(5) 0.0274(16) Uani 1 d . . . H3 H 0.3170 0.5731 -0.0221 0.033 Uiso 1 calc R . . C4 C 0.4359(5) 0.6220(3) 0.0743(5) 0.0271(16) Uani 1 d . . . C5 C 0.4366(6) 0.6658(3) 0.0012(6) 0.046(2) Uani 1 d . . . H5 H 0.3898 0.6672 -0.0679 0.055 Uiso 1 calc R . . C6 C 0.5252(5) 0.7072(3) 0.0576(5) 0.0327(17) Uani 1 d . . . H6 H 0.5300 0.7380 0.0154 0.039 Uiso 1 calc R . . C7 C 0.6251(6) 0.6760(3) 0.1222(5) 0.0311(17) Uani 1 d . . . C8 C 0.5870(5) 0.6729(3) 0.2030(5) 0.0245(15) Uani 1 d . . . H8 H 0.6398 0.6756 0.2745 0.029 Uiso 1 calc R . . C9 C 0.5120(5) 0.6259(3) 0.1748(5) 0.0233(15) Uani 1 d . . . C10 C 0.5123(5) 0.5853(3) 0.2414(5) 0.0222(14) Uani 1 d . . . H10 H 0.5619 0.5885 0.3095 0.027 Uiso 1 calc R . . C11 C 0.5254(6) 0.7282(3) 0.1528(6) 0.0366(19) Uani 1 d . . . H11A H 0.4576 0.7298 0.1479 0.044 Uiso 1 calc R . . H11B H 0.5636 0.7638 0.1803 0.044 Uiso 1 calc R . . C12 C 0.6501(7) 0.6213(3) 0.0873(7) 0.048(2) Uani 1 d . . . H12A H 0.7144 0.6063 0.1399 0.073 Uiso 1 calc R . . H12B H 0.6561 0.6287 0.0276 0.073 Uiso 1 calc R . . H12C H 0.5960 0.5937 0.0719 0.073 Uiso 1 calc R . . C13 C 0.7206(6) 0.7160(3) 0.1630(7) 0.049(2) Uani 1 d . . . H13A H 0.7808 0.6950 0.2104 0.073 Uiso 1 calc R . . H13B H 0.7102 0.7487 0.1964 0.073 Uiso 1 calc R . . H13C H 0.7301 0.7291 0.1076 0.073 Uiso 1 calc R . . C2' C 0.3046(4) 0.4871(3) 0.0908(4) 0.0204(15) Uani 1 d . . . C3' C 0.2257(4) 0.4742(4) -0.0039(4) 0.0314(14) Uani 1 d . . . H3' H 0.2121 0.4991 -0.0576 0.038 Uiso 1 calc R . . C4' C 0.1665(5) 0.4259(3) -0.0217(5) 0.0297(17) Uani 1 d . . . C5' C 0.0819(6) 0.4097(4) -0.1215(6) 0.049(2) Uani 1 d . . . H5' H 0.0599 0.4311 -0.1807 0.059 Uiso 1 calc R . . C6' C 0.0350(6) 0.3524(4) -0.1136(6) 0.046(2) Uani 1 d . . . H6' H -0.0204 0.3376 -0.1781 0.056 Uiso 1 calc R . . C7' C 0.0100(5) 0.3521(3) -0.0258(6) 0.0394(19) Uani 1 d . . . C8' C 0.1248(5) 0.3376(3) 0.0386(6) 0.0336(17) Uani 1 d . . . H8' H 0.1423 0.3118 0.0962 0.040 Uiso 1 calc R . . C9' C 0.1891(4) 0.3910(3) 0.0616(5) 0.0234(15) Uani 1 d . . . C10' C 0.2671(5) 0.4046(3) 0.1531(5) 0.0255(15) Uani 1 d . . . H10' H 0.2804 0.3804 0.2074 0.031 Uiso 1 calc R . . C11' C 0.1217(6) 0.3097(3) -0.0547(7) 0.054(3) Uani 1 d . . . H11C H 0.1834 0.3158 -0.0609 0.065 Uiso 1 calc R . . H11D H 0.1006 0.2695 -0.0649 0.065 Uiso 1 calc R . . C12' C -0.0323(6) 0.4066(4) -0.0046(7) 0.056(2) Uani 1 d . . . H12D H -0.0366 0.4018 0.0566 0.083 Uiso 1 calc R . . H12E H -0.1000 0.4143 -0.0602 0.083 Uiso 1 calc R . . H12F H 0.0127 0.4384 0.0032 0.083 Uiso 1 calc R . . C13' C -0.0592(6) 0.3014(4) -0.0324(7) 0.061(3) Uani 1 d . . . H13D H -0.0611 0.2981 0.0303 0.091 Uiso 1 calc R . . H13E H -0.0322 0.2663 -0.0445 0.091 Uiso 1 calc R . . H13F H -0.1280 0.3078 -0.0870 0.091 Uiso 1 calc R . . C22 C 0.6576(5) 0.4492(3) 0.3725(5) 0.0227(14) Uani 1 d . . . C23 C 0.7449(4) 0.4289(3) 0.3708(5) 0.0277(16) Uani 1 d . . . H23 H 0.8103 0.4358 0.4254 0.033 Uiso 1 calc R . . C24 C 0.7344(5) 0.3989(3) 0.2884(5) 0.0255(16) Uani 1 d . . . C25 C 0.8267(6) 0.3762(4) 0.2816(6) 0.046(2) Uani 1 d . . . H25 H 0.8959 0.3819 0.3292 0.055 Uiso 1 calc R . . C26 C 0.7867(5) 0.3425(3) 0.1834(5) 0.0360(19) Uani 1 d . . . H26 H 0.8411 0.3243 0.1735 0.043 Uiso 1 calc R . . C27 C 0.7087(5) 0.3762(3) 0.0927(5) 0.0342(18) Uani 1 d . . . C28 C 0.6286(6) 0.3535(3) 0.1233(5) 0.0313(17) Uani 1 d . . . H28 H 0.5590 0.3451 0.0680 0.038 Uiso 1 calc R . . C29 C 0.6359(5) 0.3888(3) 0.2092(5) 0.0224(14) Uani 1 d . . . C30 C 0.5533(5) 0.4111(3) 0.2151(5) 0.0230(15) Uani 1 d . . . H30 H 0.4877 0.4055 0.1600 0.028 Uiso 1 calc R . . C31 C 0.7012(6) 0.3018(3) 0.1706(6) 0.041(2) Uani 1 d . . . H31A H 0.7064 0.2883 0.2339 0.049 Uiso 1 calc R . . H31B H 0.6893 0.2701 0.1240 0.049 Uiso 1 calc R . . C33 C 0.6883(6) 0.3497(4) -0.0091(6) 0.057(3) Uani 1 d . . . H33A H 0.6252 0.3651 -0.0629 0.085 Uiso 1 calc R . . H33B H 0.6824 0.3084 -0.0065 0.085 Uiso 1 calc R . . H33C H 0.7447 0.3589 -0.0214 0.085 Uiso 1 calc R . . C32 C 0.7221(7) 0.4410(4) 0.0887(7) 0.058(2) Uani 1 d . . . H32A H 0.6608 0.4572 0.0336 0.087 Uiso 1 calc R . . H32B H 0.7803 0.4487 0.0786 0.087 Uiso 1 calc R . . H32C H 0.7336 0.4581 0.1514 0.087 Uiso 1 calc R . . C22' C 0.6615(4) 0.4813(4) 0.4580(4) 0.0218(13) Uani 1 d . . . C23' C 0.7471(5) 0.4863(3) 0.5491(5) 0.0310(18) Uani 1 d . . . H23' H 0.8092 0.4700 0.5597 0.037 Uiso 1 calc R . . C24' C 0.7423(5) 0.5160(3) 0.6281(5) 0.0282(16) Uani 1 d . . . C25' C 0.8330(6) 0.5199(4) 0.7346(5) 0.047(2) Uani 1 d . . . H25' H 0.8978 0.5036 0.7561 0.056 Uiso 1 calc R . . C26' C 0.8020(5) 0.5541(3) 0.7990(5) 0.0368(18) Uani 1 d . . . H26' H 0.8572 0.5599 0.8689 0.044 Uiso 1 calc R . . C27' C 0.6982(5) 0.5347(3) 0.7893(5) 0.0341(18) Uani 1 d . . . C28' C 0.6488(5) 0.5732(3) 0.6915(5) 0.0290(16) Uani 1 d . . . H28' H 0.5844 0.5933 0.6760 0.035 Uiso 1 calc R . . C29' C 0.6506(5) 0.5417(3) 0.6086(5) 0.0267(15) Uani 1 d . . . C30' C 0.5678(5) 0.5342(3) 0.5144(5) 0.0219(15) Uani 1 d . . . H30' H 0.5058 0.5518 0.5011 0.026 Uiso 1 calc R . . C31' C 0.7489(6) 0.6087(4) 0.7443(6) 0.042(2) Uani 1 d . . . H31C H 0.7727 0.6233 0.6988 0.051 Uiso 1 calc R . . H31D H 0.7478 0.6390 0.7883 0.051 Uiso 1 calc R . . C32' C 0.6716(6) 0.4727(4) 0.7777(6) 0.052(2) Uani 1 d . . . H32D H 0.6012 0.4680 0.7634 0.079 Uiso 1 calc R . . H32E H 0.7168 0.4527 0.8393 0.079 Uiso 1 calc R . . H32F H 0.6794 0.4570 0.7228 0.079 Uiso 1 calc R . . C33' C 0.6791(6) 0.5605(4) 0.8719(6) 0.048(2) Uani 1 d . . . H33D H 0.6088 0.5534 0.8558 0.072 Uiso 1 calc R . . H33E H 0.6916 0.6014 0.8760 0.072 Uiso 1 calc R . . H33F H 0.7250 0.5429 0.9359 0.072 Uiso 1 calc R . . C42 C 0.3626(5) 0.4248(3) 0.4284(5) 0.0237(15) Uani 1 d . . . C43 C 0.3491(5) 0.3874(3) 0.4916(5) 0.0280(16) Uani 1 d . . . H43 H 0.3028 0.3960 0.5150 0.034 Uiso 1 calc R . . C44 C 0.4057(5) 0.3365(3) 0.5200(5) 0.0235(15) Uani 1 d . . . C45 C 0.3967(6) 0.2918(3) 0.5877(6) 0.039(2) Uani 1 d . . . H45 H 0.3545 0.2949 0.6175 0.047 Uiso 1 calc R . . C46 C 0.4651(6) 0.2420(3) 0.5998(5) 0.0374(18) Uani 1 d . . . H46 H 0.4604 0.2102 0.6405 0.045 Uiso 1 calc R . . C47 C 0.5764(6) 0.2613(3) 0.6316(5) 0.0357(18) Uani 1 d . . . C48 C 0.5326(5) 0.2703(3) 0.5156(5) 0.0307(17) Uani 1 d . . . H48 H 0.5798 0.2628 0.4884 0.037 Uiso 1 calc R . . C49 C 0.4744(5) 0.3264(3) 0.4860(5) 0.0239(15) Uani 1 d . . . C50 C 0.4846(5) 0.3655(3) 0.4242(5) 0.0217(14) Uani 1 d . . . H50 H 0.5322 0.3580 0.4019 0.026 Uiso 1 calc R . . C51 C 0.4530(6) 0.2237(3) 0.4986(6) 0.041(2) Uani 1 d . . . H51A H 0.3849 0.2309 0.4415 0.049 Uiso 1 calc R . . H51B H 0.4760 0.1846 0.4972 0.049 Uiso 1 calc R . . C52 C 0.6543(7) 0.2125(3) 0.6729(6) 0.049(2) Uani 1 d . . . H52A H 0.7198 0.2257 0.6817 0.074 Uiso 1 calc R . . H52B H 0.6304 0.1807 0.6261 0.074 Uiso 1 calc R . . H52C H 0.6621 0.2001 0.7371 0.074 Uiso 1 calc R . . C53 C 0.6219(6) 0.3119(4) 0.7029(6) 0.048(2) Uani 1 d . . . H53A H 0.6867 0.3226 0.7073 0.072 Uiso 1 calc R . . H53B H 0.6327 0.3013 0.7690 0.072 Uiso 1 calc R . . H53C H 0.5751 0.3441 0.6778 0.072 Uiso 1 calc R . . C42' C 0.3005(4) 0.4784(4) 0.3874(4) 0.0232(12) Uani 1 d . . . C43' C 0.2186(5) 0.4925(2) 0.3992(5) 0.0266(17) Uani 1 d . . . H43' H 0.2026 0.4705 0.4416 0.032 Uiso 1 calc R . . C44' C 0.1588(5) 0.5393(3) 0.3486(5) 0.0276(16) Uani 1 d . . . C45' C 0.0613(6) 0.5564(4) 0.3495(7) 0.054(3) Uani 1 d . . . H45' H 0.0349 0.5378 0.3868 0.065 Uiso 1 calc R . . C46' C 0.0130(6) 0.6068(3) 0.2833(7) 0.046(2) Uani 1 d . . . H46' H -0.0506 0.6203 0.2818 0.055 Uiso 1 calc R . . C47' C 0.0038(5) 0.5987(3) 0.1759(5) 0.0316(17) Uani 1 d . . . C48' C 0.1174(5) 0.6207(3) 0.2311(5) 0.0265(16) Uani 1 d . . . H48' H 0.1397 0.6432 0.1901 0.032 Uiso 1 calc R . . C49' C 0.1849(4) 0.5717(3) 0.2892(5) 0.0223(14) Uani 1 d . . . C50' C 0.2734(5) 0.5569(3) 0.2840(5) 0.0246(15) Uani 1 d . . . H50' H 0.2934 0.5801 0.2460 0.030 Uiso 1 calc R . . C51' C 0.0907(7) 0.6544(4) 0.3006(7) 0.045(2) Uani 1 d . . . H51C H 0.0598 0.6919 0.2744 0.054 Uiso 1 calc R . . H51D H 0.1465 0.6572 0.3700 0.054 Uiso 1 calc R . . C52' C -0.0684(5) 0.6425(3) 0.0986(6) 0.045(2) Uani 1 d . . . H52D H -0.0629 0.6396 0.0378 0.068 Uiso 1 calc R . . H52E H -0.0494 0.6808 0.1261 0.068 Uiso 1 calc R . . H52F H -0.1383 0.6347 0.0832 0.068 Uiso 1 calc R . . C53' C -0.0190(6) 0.5392(4) 0.1262(7) 0.052(2) Uani 1 d . . . H53D H -0.0133 0.5408 0.0654 0.078 Uiso 1 calc R . . H53E H -0.0878 0.5277 0.1097 0.078 Uiso 1 calc R . . H53F H 0.0298 0.5117 0.1723 0.078 Uiso 1 calc R . . C54 C 0.0809(12) 0.3084(6) 0.3170(12) 0.107(5) Uani 1 d . . . H54 H 0.0129 0.2905 0.2761 0.160 Uiso 1 calc R . . C55 C 0.6385(8) 0.1218(5) 0.3371(8) 0.087(4) Uani 1 d . . . H55 H 0.5772 0.1425 0.2866 0.130 Uiso 1 calc R . . C56 C 1.018(2) 0.6564(12) 0.823(2) 0.204(13) Uiso 0.75 d PD A 1 H56 H 0.9457 0.6687 0.7859 0.244 Uiso 0.75 calc PR A 1 C56A C 1.0692(17) 0.6459(9) 0.8568(16) 0.013(5) Uiso 0.25 d PD A 2 H56A H 1.0012 0.6647 0.8249 0.016 Uiso 0.25 calc PR A 2 C57 C 0.9154(8) 0.3097(4) 0.5641(8) 0.075(3) Uani 1 d . . . H57 H 0.9328 0.3437 0.5366 0.113 Uiso 1 calc R . . C58 C 0.3638(6) 0.4294(4) -0.1618(6) 0.048(2) Uani 1 d . . . H58 H 0.2958 0.4460 -0.2072 0.072 Uiso 1 calc R . . C59 C 0.8592(7) 0.6114(4) 0.4749(7) 0.062(3) Uani 1 d . . . H59 H 0.8991 0.5841 0.5299 0.092 Uiso 1 calc R . . N1 N 0.4446(4) 0.5410(2) 0.2136(4) 0.0208(12) Uani 1 d . . . N1' N 0.3275(4) 0.4515(2) 0.1707(4) 0.0198(12) Uani 1 d . . . N21 N 0.5606(4) 0.4401(2) 0.2939(4) 0.0212(12) Uani 1 d . . . N21' N 0.5690(4) 0.5032(2) 0.4389(4) 0.0212(12) Uani 1 d . . . N41 N 0.4294(4) 0.4147(2) 0.3936(4) 0.0201(12) Uani 1 d . . . N41' N 0.3311(4) 0.5106(2) 0.3315(4) 0.0207(12) Uani 1 d . . . Cl1 Cl 0.0752(3) 0.37440(17) 0.2705(3) 0.1236(13) Uani 1 d . . . Cl2 Cl 0.1690(4) 0.2666(2) 0.3026(4) 0.177(2) Uani 1 d . . . Cl3 Cl 0.1012(4) 0.3129(3) 0.4407(5) 0.190(3) Uani 1 d . . . Cl4 Cl 0.6565(3) 0.13928(19) 0.4524(2) 0.1156(12) Uani 1 d . . . Cl5 Cl 0.7388(4) 0.1382(2) 0.3168(4) 0.1659(19) Uani 1 d . . . Cl6 Cl 0.6121(3) 0.0474(2) 0.3211(5) 0.181(2) Uani 1 d . . . Cl7 Cl 1.0819(4) 0.5948(2) 0.7759(4) 0.1666(19) Uani 1 d D . . Cl8 Cl 1.0803(8) 0.6240(5) 0.9464(8) 0.206(4) Uiso 0.75 d PD A 1 Cl8A Cl 1.0882(10) 0.5953(6) 0.9648(10) 0.079(4) Uiso 0.25 d PD A 2 Cl9 Cl 1.1336(5) 0.7042(3) 0.8501(6) 0.170(3) Uiso 0.75 d PD A 1 Cl9A Cl 1.1787(12) 0.6947(7) 0.9648(13) 0.129(5) Uiso 0.25 d PD A 2 Cl10 Cl 1.0269(2) 0.28418(12) 0.6650(2) 0.0872(9) Uani 1 d . . . Cl11 Cl 0.8578(3) 0.26001(15) 0.4693(2) 0.1173(12) Uani 1 d . . . Cl12 Cl 0.8260(3) 0.33123(17) 0.6051(3) 0.1081(11) Uani 1 d . . . Cl13 Cl 0.3477(2) 0.37089(12) -0.0990(3) 0.0850(9) Uani 1 d . . . Cl14 Cl 0.4211(2) 0.40752(13) -0.2338(2) 0.0861(9) Uani 1 d . . . Cl15 Cl 0.4383(2) 0.48076(15) -0.0762(2) 0.0872(8) Uani 1 d . . . Cl16 Cl 0.9434(3) 0.66255(15) 0.4764(3) 0.1184(13) Uani 1 d . . . Cl17 Cl 0.7648(2) 0.64168(14) 0.4988(2) 0.0879(9) Uani 1 d . . . Cl18 Cl 0.80435(19) 0.57333(10) 0.36468(19) 0.0636(6) Uani 1 d . . . P1 P 1.07563(16) 0.46435(12) 0.60528(18) 0.0624(8) Uani 1 d D . . P2 P 0.41736(17) 0.24606(8) 0.19189(16) 0.0400(5) Uani 1 d . . . F1 F 1.1364(12) 0.4053(6) 0.6412(11) 0.090(5) Uiso 0.50 d PD B 1 F1A F 1.1056(13) 0.4060(7) 0.6569(13) 0.105(6) Uiso 0.50 d PD B 2 F2 F 1.0102(11) 0.5218(6) 0.5667(11) 0.097(4) Uiso 0.50 d PD B 1 F2A F 1.0683(14) 0.5338(7) 0.5695(13) 0.123(6) Uiso 0.50 d PD B 2 F3 F 1.1397(9) 0.4792(7) 0.7195(9) 0.063(4) Uiso 0.50 d PD B 1 F3A F 1.1497(13) 0.4965(7) 0.7112(13) 0.088(6) Uiso 0.50 d PD B 2 F4 F 1.1597(8) 0.4865(5) 0.5825(8) 0.066(3) Uiso 0.50 d PD B 1 F4A F 1.1701(11) 0.4538(7) 0.5871(12) 0.094(4) Uiso 0.50 d PD B 2 F5 F 1.0100(10) 0.4314(7) 0.4960(10) 0.088(5) Uiso 0.50 d PD B 1 F5A F 0.9989(13) 0.4608(8) 0.4958(12) 0.122(7) Uiso 0.50 d PD B 2 F6 F 0.9890(7) 0.4390(4) 0.6273(7) 0.055(2) Uiso 0.50 d PD B 1 F6A F 0.9866(11) 0.4790(10) 0.6307(12) 0.132(5) Uiso 0.50 d PD B 2 F7 F 0.3148(5) 0.2167(3) 0.1152(4) 0.095(2) Uani 1 d . . . F8 F 0.5195(4) 0.2762(3) 0.2709(4) 0.0837(18) Uani 1 d . . . F9 F 0.3563(5) 0.2824(3) 0.2343(5) 0.0893(19) Uani 1 d . . . F10 F 0.3976(5) 0.2942(2) 0.1110(4) 0.0805(17) Uani 1 d . . . F11 F 0.4797(6) 0.2100(3) 0.1537(4) 0.106(3) Uani 1 d . . . F12 F 0.4365(4) 0.1981(2) 0.2738(3) 0.0576(13) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0180(2) 0.0178(2) 0.0164(2) 0.0024(3) 0.00849(18) 0.0011(3) C2 0.022(3) 0.016(3) 0.015(3) 0.001(3) 0.005(3) -0.003(3) C3 0.033(4) 0.026(4) 0.018(4) 0.002(3) 0.007(3) 0.000(3) C4 0.027(4) 0.030(4) 0.021(4) 0.008(3) 0.009(3) 0.000(3) C5 0.061(5) 0.042(5) 0.027(4) 0.022(4) 0.014(4) -0.017(4) C6 0.053(5) 0.025(4) 0.026(4) 0.002(3) 0.023(4) -0.010(3) C7 0.044(4) 0.025(4) 0.038(4) -0.002(3) 0.030(4) -0.006(3) C8 0.037(4) 0.018(4) 0.025(4) -0.003(3) 0.019(3) -0.007(3) C9 0.032(4) 0.018(3) 0.022(4) 0.003(3) 0.014(3) 0.000(3) C10 0.030(4) 0.022(4) 0.012(3) 0.006(3) 0.008(3) 0.003(3) C11 0.056(5) 0.016(4) 0.049(5) 0.001(3) 0.034(4) -0.002(3) C12 0.068(6) 0.036(5) 0.065(6) -0.004(4) 0.051(5) -0.007(4) C13 0.059(5) 0.038(5) 0.066(6) -0.007(4) 0.044(5) -0.021(4) C2' 0.022(3) 0.017(4) 0.023(3) 0.009(3) 0.011(3) 0.006(3) C3' 0.033(3) 0.032(4) 0.018(3) 0.008(4) 0.003(3) -0.004(5) C4' 0.030(4) 0.037(4) 0.020(4) -0.002(3) 0.010(3) -0.005(3) C5' 0.046(5) 0.063(6) 0.022(4) -0.006(4) 0.002(4) -0.026(4) C6' 0.034(4) 0.058(6) 0.037(5) -0.022(4) 0.009(4) -0.012(4) C7' 0.031(4) 0.043(5) 0.054(5) -0.016(4) 0.029(4) -0.010(3) C8' 0.029(4) 0.022(4) 0.044(5) -0.004(4) 0.013(4) -0.001(3) C9' 0.016(3) 0.023(4) 0.030(4) 0.001(3) 0.010(3) 0.001(3) C10' 0.035(4) 0.017(3) 0.026(4) 0.004(3) 0.016(3) 0.000(3) C11' 0.034(5) 0.027(4) 0.099(8) -0.013(5) 0.030(5) -0.010(4) C12' 0.038(5) 0.053(6) 0.081(7) -0.002(5) 0.032(5) 0.009(4) C13' 0.043(5) 0.068(6) 0.066(6) -0.015(5) 0.022(5) -0.026(5) C22 0.022(3) 0.031(4) 0.019(3) 0.001(3) 0.013(3) 0.001(3) C23 0.012(3) 0.037(4) 0.027(4) -0.015(3) 0.003(3) -0.001(3) C24 0.024(4) 0.032(4) 0.024(4) 0.004(3) 0.014(3) 0.006(3) C25 0.023(4) 0.073(6) 0.040(5) -0.020(4) 0.013(4) 0.010(4) C26 0.021(4) 0.059(5) 0.029(4) -0.011(4) 0.013(3) 0.007(4) C27 0.034(4) 0.042(5) 0.035(4) -0.011(4) 0.023(4) -0.002(3) C28 0.038(4) 0.028(4) 0.030(4) -0.012(3) 0.018(3) 0.000(3) C29 0.021(3) 0.028(4) 0.021(4) 0.000(3) 0.013(3) 0.001(3) C30 0.029(4) 0.024(4) 0.018(4) 0.002(3) 0.013(3) 0.000(3) C31 0.052(5) 0.035(5) 0.041(5) -0.006(4) 0.027(4) 0.011(4) C33 0.053(5) 0.092(7) 0.036(5) -0.024(5) 0.029(4) 0.004(5) C32 0.057(5) 0.073(6) 0.061(6) 0.016(5) 0.042(5) 0.002(5) C22' 0.024(3) 0.022(3) 0.018(3) -0.001(4) 0.009(2) 0.003(4) C23' 0.022(3) 0.038(5) 0.030(3) -0.019(4) 0.011(3) 0.001(4) C24' 0.019(3) 0.037(4) 0.024(4) -0.016(3) 0.007(3) -0.006(3) C25' 0.027(4) 0.081(6) 0.021(4) -0.022(4) 0.002(3) 0.005(4) C26' 0.032(4) 0.051(5) 0.018(4) -0.010(4) 0.005(3) -0.006(4) C27' 0.039(4) 0.050(5) 0.013(4) -0.001(3) 0.013(3) 0.003(4) C28' 0.033(4) 0.032(4) 0.025(4) -0.003(3) 0.016(3) 0.005(3) C29' 0.033(4) 0.029(4) 0.020(4) 0.002(3) 0.014(3) 0.003(3) C30' 0.025(4) 0.025(4) 0.018(4) 0.001(3) 0.013(3) 0.004(3) C31' 0.049(5) 0.052(5) 0.030(4) -0.019(4) 0.022(4) -0.022(4) C32' 0.063(5) 0.054(6) 0.044(4) 0.019(6) 0.029(4) 0.001(6) C33' 0.057(5) 0.064(6) 0.028(5) -0.001(4) 0.025(4) 0.009(4) C42 0.034(4) 0.021(4) 0.022(4) 0.005(3) 0.018(3) 0.005(3) C43 0.035(4) 0.033(4) 0.020(4) 0.012(3) 0.017(3) 0.008(3) C44 0.026(4) 0.025(4) 0.021(4) 0.010(3) 0.012(3) 0.005(3) C45 0.060(5) 0.026(4) 0.048(5) 0.017(4) 0.040(5) 0.012(4) C46 0.061(5) 0.026(4) 0.032(4) 0.012(4) 0.028(4) 0.008(4) C47 0.055(5) 0.028(4) 0.023(4) 0.015(3) 0.018(4) 0.016(4) C48 0.041(4) 0.030(4) 0.030(4) 0.006(3) 0.024(4) 0.017(3) C49 0.030(4) 0.024(4) 0.018(4) 0.005(3) 0.012(3) 0.002(3) C50 0.032(4) 0.014(3) 0.024(4) 0.006(3) 0.017(3) 0.006(3) C51 0.074(6) 0.021(4) 0.037(5) -0.001(4) 0.035(5) 0.005(4) C52 0.068(6) 0.040(5) 0.037(5) 0.018(4) 0.024(4) 0.028(4) C53 0.054(5) 0.057(6) 0.029(5) 0.002(4) 0.018(4) 0.008(4) C42' 0.020(3) 0.025(3) 0.022(3) 0.004(4) 0.008(2) 0.012(4) C43' 0.037(4) 0.023(4) 0.029(4) 0.009(3) 0.024(3) 0.010(3) C44' 0.030(4) 0.030(4) 0.030(4) 0.011(3) 0.021(3) 0.011(3) C45' 0.063(5) 0.063(6) 0.068(6) 0.045(5) 0.057(5) 0.048(5) C46' 0.042(5) 0.035(4) 0.075(6) 0.012(4) 0.040(5) 0.029(4) C47' 0.022(4) 0.032(4) 0.038(4) 0.010(4) 0.012(3) 0.010(3) C48' 0.022(4) 0.017(3) 0.038(4) 0.001(3) 0.013(3) 0.001(3) C49' 0.016(3) 0.022(4) 0.025(4) 0.003(3) 0.006(3) 0.006(3) C50' 0.024(3) 0.028(4) 0.023(4) -0.001(3) 0.013(3) -0.003(3) C51' 0.045(5) 0.039(5) 0.047(5) -0.012(4) 0.018(4) 0.011(4) C52' 0.024(4) 0.050(5) 0.053(5) 0.017(4) 0.012(4) 0.016(4) C53' 0.031(4) 0.046(5) 0.059(6) -0.002(5) 0.006(4) -0.002(4) C54 0.121(11) 0.081(9) 0.113(12) 0.016(8) 0.053(10) 0.009(8) C55 0.069(7) 0.089(8) 0.082(8) -0.032(7) 0.020(6) 0.029(6) C57 0.107(8) 0.049(6) 0.067(7) -0.007(5) 0.039(6) -0.007(6) C58 0.046(5) 0.053(5) 0.045(5) -0.015(4) 0.022(4) 0.001(4) C59 0.066(6) 0.058(6) 0.066(7) 0.009(5) 0.036(5) -0.005(5) N1 0.020(3) 0.022(3) 0.020(3) -0.007(3) 0.010(2) 0.000(2) N1' 0.023(3) 0.015(3) 0.028(3) 0.005(2) 0.017(3) 0.005(2) N21 0.023(3) 0.020(3) 0.017(3) 0.004(3) 0.007(2) -0.003(2) N21' 0.025(3) 0.017(3) 0.025(3) 0.009(2) 0.016(3) 0.007(2) N41 0.021(3) 0.024(3) 0.015(3) 0.002(2) 0.008(2) 0.010(2) N41' 0.028(3) 0.014(3) 0.017(3) 0.004(2) 0.010(3) 0.002(2) Cl1 0.126(3) 0.109(3) 0.131(3) 0.018(3) 0.058(3) 0.002(2) Cl2 0.170(4) 0.168(4) 0.160(4) 0.031(4) 0.053(4) 0.088(4) Cl3 0.131(3) 0.267(7) 0.211(6) 0.117(5) 0.114(4) 0.070(4) Cl4 0.095(2) 0.166(4) 0.066(2) -0.022(2) 0.0237(18) 0.006(2) Cl5 0.180(4) 0.164(4) 0.219(5) -0.001(4) 0.148(4) 0.021(3) Cl6 0.099(3) 0.155(4) 0.252(6) -0.111(4) 0.055(3) -0.002(3) Cl7 0.166(4) 0.199(5) 0.158(4) 0.015(4) 0.096(4) -0.002(4) Cl10 0.093(2) 0.0734(18) 0.097(2) 0.0125(16) 0.0472(18) -0.0048(15) Cl11 0.166(3) 0.088(2) 0.071(2) -0.0122(18) 0.037(2) -0.013(2) Cl12 0.095(2) 0.128(3) 0.097(2) 0.013(2) 0.042(2) 0.014(2) Cl13 0.0734(17) 0.0663(17) 0.124(3) 0.0067(17) 0.0546(18) -0.0004(14) Cl14 0.101(2) 0.096(2) 0.0743(19) -0.0185(17) 0.0529(18) 0.0137(17) Cl15 0.0949(18) 0.0818(18) 0.0907(19) -0.046(2) 0.0496(16) -0.026(2) Cl16 0.139(3) 0.100(2) 0.152(3) -0.048(2) 0.098(3) -0.062(2) Cl17 0.115(2) 0.103(2) 0.0763(19) 0.0075(17) 0.0707(19) 0.0118(18) Cl18 0.0690(16) 0.0619(15) 0.0647(16) 0.0001(13) 0.0360(14) 0.0017(12) P1 0.0367(11) 0.088(3) 0.0516(14) 0.0270(14) 0.0131(10) 0.0006(12) P2 0.0597(14) 0.0284(11) 0.0358(12) 0.0024(10) 0.0263(11) 0.0066(10) F7 0.097(4) 0.074(4) 0.067(4) 0.015(3) 0.001(3) -0.022(3) F8 0.077(4) 0.094(5) 0.068(4) 0.005(3) 0.025(3) -0.022(3) F9 0.124(5) 0.080(4) 0.090(4) 0.011(4) 0.072(4) 0.051(4) F10 0.129(5) 0.050(3) 0.063(4) 0.029(3) 0.047(4) -0.006(3) F11 0.156(6) 0.126(6) 0.074(4) 0.029(4) 0.086(5) 0.082(5) F12 0.078(3) 0.047(3) 0.052(3) 0.025(2) 0.034(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N21 2.042(5) . ? Ru1 N41' 2.045(5) . ? Ru1 N41 2.053(5) . ? Ru1 N1' 2.055(5) . ? Ru1 N21' 2.056(5) . ? Ru1 N1 2.057(5) . ? C2 N1 1.354(8) . ? C2 C3 1.391(9) . ? C2 C2' 1.468(9) . ? C3 C4 1.385(9) . ? C4 C9 1.398(9) . ? C4 C5 1.515(9) . ? C5 C6 1.523(10) . ? C6 C7 1.517(10) . ? C6 C11 1.527(10) . ? C7 C12 1.498(10) . ? C7 C13 1.559(10) . ? C7 C8 1.586(9) . ? C8 C9 1.476(9) . ? C8 C11 1.554(9) . ? C9 C10 1.387(8) . ? C10 N1 1.361(8) . ? C2' N1' 1.374(7) . ? C2' C3' 1.382(8) . ? C3' C4' 1.378(10) . ? C4' C9' 1.404(9) . ? C4' C5' 1.479(10) . ? C5' C6' 1.542(11) . ? C6' C11' 1.532(11) . ? C6' C7' 1.551(11) . ? C7' C12' 1.525(10) . ? C7' C8' 1.543(10) . ? C7' C13' 1.544(10) . ? C8' C9' 1.508(9) . ? C8' C11' 1.542(11) . ? C9' C10' 1.351(9) . ? C10' N1' 1.359(8) . ? C22 N21 1.377(8) . ? C22 C23 1.399(8) . ? C22 C22' 1.479(9) . ? C23 C24 1.378(9) . ? C24 C29 1.398(9) . ? C24 C25 1.526(9) . ? C25 C26 1.531(10) . ? C26 C27 1.524(10) . ? C26 C31 1.527(10) . ? C27 C32 1.532(11) . ? C27 C33 1.556(10) . ? C27 C28 1.570(10) . ? C28 C29 1.503(9) . ? C28 C31 1.548(10) . ? C29 C30 1.379(8) . ? C30 N21 1.336(8) . ? C22' C23' 1.362(8) . ? C22' N21' 1.364(7) . ? C23' C24' 1.420(9) . ? C24' C29' 1.389(9) . ? C24' C25' 1.530(9) . ? C25' C26' 1.499(10) . ? C26' C31' 1.520(11) . ? C26' C27' 1.551(10) . ? C27' C32' 1.490(12) . ? C27' C33' 1.539(9) . ? C27' C28' 1.583(10) . ? C28' C29' 1.472(9) . ? C28' C31' 1.550(10) . ? C29' C30' 1.378(9) . ? C30' N21' 1.366(8) . ? C42 N41 1.357(7) . ? C42 C43 1.383(8) . ? C42 C42' 1.504(9) . ? C43 C44 1.400(9) . ? C44 C49 1.375(8) . ? C44 C45 1.516(9) . ? C45 C46 1.499(10) . ? C46 C51 1.523(10) . ? C46 C47 1.556(11) . ? C47 C53 1.524(10) . ? C47 C52 1.530(10) . ? C47 C48 1.572(9) . ? C48 C49 1.515(9) . ? C48 C51 1.539(10) . ? C49 C50 1.373(8) . ? C50 N41 1.359(8) . ? C42' C43' 1.358(8) . ? C42' N41' 1.369(8) . ? C43' C44' 1.387(9) . ? C44' C49' 1.372(9) . ? C44' C45' 1.516(9) . ? C45' C46' 1.490(10) . ? C46' C51' 1.534(11) . ? C46' C47' 1.583(11) . ? C47' C52' 1.537(9) . ? C47' C53' 1.539(11) . ? C47' C48' 1.569(9) . ? C48' C49' 1.498(8) . ? C48' C51' 1.519(10) . ? C49' C50' 1.404(8) . ? C50' N41' 1.353(8) . ? C54 Cl1 1.683(14) . ? C54 Cl2 1.734(15) . ? C54 Cl3 1.758(15) . ? C55 Cl4 1.691(11) . ? C55 Cl5 1.711(12) . ? C55 Cl6 1.773(12) . ? C56 Cl8 1.82(3) . ? C56 Cl9 1.92(3) . ? C56 Cl7 2.03(3) . ? C56A Cl7 1.79(2) . ? C56A Cl8A 1.93(2) . ? C56A Cl9A 2.02(3) . ? C57 Cl11 1.722(10) . ? C57 Cl10 1.735(11) . ? C57 Cl12 1.795(11) . ? C58 Cl15 1.724(8) . ? C58 Cl13 1.749(9) . ? C58 Cl14 1.759(8) . ? C59 Cl18 1.716(10) . ? C59 Cl16 1.727(9) . ? C59 Cl17 1.765(10) . ? P1 F5A 1.499(17) . ? P1 F1A 1.529(16) . ? P1 F4 1.544(11) . ? P1 F3 1.565(13) . ? P1 F4A 1.581(14) . ? P1 F6A 1.590(15) . ? P1 F1 1.595(15) . ? P1 F2 1.595(14) . ? P1 F6 1.599(9) . ? P1 F3A 1.631(17) . ? P1 F5 1.656(14) . ? P1 F2A 1.698(17) . ? P2 F11 1.561(5) . ? P2 F7 1.564(6) . ? P2 F8 1.579(6) . ? P2 F10 1.586(5) . ? P2 F9 1.592(5) . ? P2 F12 1.595(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Ru1 N41' 174.9(2) . . ? N21 Ru1 N41 96.67(19) . . ? N41' Ru1 N41 78.50(19) . . ? N21 Ru1 N1' 96.7(2) . . ? N41' Ru1 N1' 85.6(2) . . ? N41 Ru1 N1' 97.6(2) . . ? N21 Ru1 N21' 79.0(2) . . ? N41' Ru1 N21' 98.8(2) . . ? N41 Ru1 N21' 85.0(2) . . ? N1' Ru1 N21' 175.3(2) . . ? N21 Ru1 N1 87.28(19) . . ? N41' Ru1 N1 97.64(19) . . ? N41 Ru1 N1 174.7(2) . . ? N1' Ru1 N1 78.4(2) . . ? N21' Ru1 N1 99.2(2) . . ? N1 C2 C3 121.1(6) . . ? N1 C2 C2' 115.0(5) . . ? C3 C2 C2' 123.9(6) . . ? C4 C3 C2 120.6(6) . . ? C3 C4 C9 118.7(6) . . ? C3 C4 C5 123.3(6) . . ? C9 C4 C5 117.9(6) . . ? C4 C5 C6 109.1(6) . . ? C7 C6 C5 111.9(6) . . ? C7 C6 C11 89.4(5) . . ? C5 C6 C11 110.0(6) . . ? C12 C7 C6 121.0(7) . . ? C12 C7 C13 108.4(6) . . ? C6 C7 C13 113.1(6) . . ? C12 C7 C8 118.7(6) . . ? C6 C7 C8 85.1(5) . . ? C13 C7 C8 108.7(6) . . ? C9 C8 C11 107.0(6) . . ? C9 C8 C7 108.4(5) . . ? C11 C8 C7 86.0(5) . . ? C10 C9 C4 117.8(6) . . ? C10 C9 C8 124.3(6) . . ? C4 C9 C8 117.8(6) . . ? N1 C10 C9 123.6(6) . . ? C6 C11 C8 85.9(5) . . ? N1' C2' C3' 120.8(6) . . ? N1' C2' C2 114.0(5) . . ? C3' C2' C2 125.1(6) . . ? C4' C3' C2' 121.6(7) . . ? C3' C4' C9' 116.6(6) . . ? C3' C4' C5' 124.0(7) . . ? C9' C4' C5' 119.4(6) . . ? C4' C5' C6' 109.7(7) . . ? C11' C6' C5' 108.9(6) . . ? C11' C6' C7' 88.8(7) . . ? C5' C6' C7' 112.1(6) . . ? C12' C7' C8' 119.6(6) . . ? C12' C7' C13' 108.8(6) . . ? C8' C7' C13' 112.1(7) . . ? C12' C7' C6' 118.4(7) . . ? C8' C7' C6' 83.9(5) . . ? C13' C7' C6' 112.4(6) . . ? C9' C8' C11' 107.2(6) . . ? C9' C8' C7' 110.7(6) . . ? C11' C8' C7' 88.7(6) . . ? C10' C9' C4' 120.3(6) . . ? C10' C9' C8' 124.6(6) . . ? C4' C9' C8' 115.0(6) . . ? C9' C10' N1' 123.4(6) . . ? C6' C11' C8' 84.5(6) . . ? N21 C22 C23 121.9(6) . . ? N21 C22 C22' 114.8(5) . . ? C23 C22 C22' 123.2(5) . . ? C24 C23 C22 119.5(6) . . ? C23 C24 C29 118.7(6) . . ? C23 C24 C25 122.0(6) . . ? C29 C24 C25 119.4(6) . . ? C24 C25 C26 107.8(6) . . ? C27 C26 C31 88.9(5) . . ? C27 C26 C25 112.6(6) . . ? C31 C26 C25 110.6(6) . . ? C26 C27 C32 119.3(6) . . ? C26 C27 C33 113.0(6) . . ? C32 C27 C33 108.7(7) . . ? C26 C27 C28 85.1(5) . . ? C32 C27 C28 118.6(6) . . ? C33 C27 C28 110.5(6) . . ? C29 C28 C31 106.5(6) . . ? C29 C28 C27 109.1(5) . . ? C31 C28 C27 86.5(5) . . ? C30 C29 C24 118.7(6) . . ? C30 C29 C28 124.9(6) . . ? C24 C29 C28 116.4(6) . . ? N21 C30 C29 124.3(6) . . ? C26 C31 C28 85.8(6) . . ? C23' C22' N21' 122.7(6) . . ? C23' C22' C22 123.8(6) . . ? N21' C22' C22 113.4(5) . . ? C22' C23' C24' 119.7(6) . . ? C29' C24' C23' 118.6(6) . . ? C29' C24' C25' 118.4(6) . . ? C23' C24' C25' 123.0(6) . . ? C26' C25' C24' 109.3(6) . . ? C25' C26' C31' 109.4(6) . . ? C25' C26' C27' 113.1(6) . . ? C31' C26' C27' 87.7(5) . . ? C32' C27' C33' 109.5(6) . . ? C32' C27' C26' 119.5(6) . . ? C33' C27' C26' 112.2(6) . . ? C32' C27' C28' 117.7(6) . . ? C33' C27' C28' 111.0(6) . . ? C26' C27' C28' 85.0(5) . . ? C29' C28' C31' 107.4(6) . . ? C29' C28' C27' 109.1(5) . . ? C31' C28' C27' 85.6(5) . . ? C30' C29' C24' 117.6(6) . . ? C30' C29' C28' 125.2(6) . . ? C24' C29' C28' 117.2(6) . . ? N21' C30' C29' 124.9(6) . . ? C26' C31' C28' 87.2(5) . . ? N41 C42 C43 122.9(6) . . ? N41 C42 C42' 113.8(5) . . ? C43 C42 C42' 123.2(5) . . ? C42 C43 C44 118.9(6) . . ? C49 C44 C43 118.5(6) . . ? C49 C44 C45 117.7(6) . . ? C43 C44 C45 123.9(6) . . ? C46 C45 C44 109.8(6) . . ? C45 C46 C51 110.7(6) . . ? C45 C46 C47 112.0(6) . . ? C51 C46 C47 89.0(6) . . ? C53 C47 C52 107.3(6) . . ? C53 C47 C46 119.1(6) . . ? C52 C47 C46 113.3(6) . . ? C53 C47 C48 119.7(6) . . ? C52 C47 C48 112.4(6) . . ? C46 C47 C48 83.6(5) . . ? C49 C48 C51 106.0(5) . . ? C49 C48 C47 108.4(5) . . ? C51 C48 C47 87.8(5) . . ? C50 C49 C44 119.6(6) . . ? C50 C49 C48 122.8(6) . . ? C44 C49 C48 117.5(6) . . ? N41 C50 C49 123.3(6) . . ? C46 C51 C48 85.8(5) . . ? C43' C42' N41' 122.7(6) . . ? C43' C42' C42 124.1(6) . . ? N41' C42' C42 113.1(5) . . ? C42' C43' C44' 119.8(6) . . ? C49' C44' C43' 119.3(6) . . ? C49' C44' C45' 116.1(6) . . ? C43' C44' C45' 124.5(6) . . ? C46' C45' C44' 110.8(6) . . ? C45' C46' C51' 112.3(7) . . ? C45' C46' C47' 112.0(6) . . ? C51' C46' C47' 86.9(6) . . ? C52' C47' C53' 108.6(6) . . ? C52' C47' C48' 111.6(6) . . ? C53' C47' C48' 118.8(5) . . ? C52' C47' C46' 112.9(6) . . ? C53' C47' C46' 120.2(6) . . ? C48' C47' C46' 82.9(5) . . ? C49' C48' C51' 108.3(6) . . ? C49' C48' C47' 108.1(5) . . ? C51' C48' C47' 87.9(5) . . ? C44' C49' C50' 118.5(6) . . ? C44' C49' C48' 119.0(5) . . ? C50' C49' C48' 122.5(6) . . ? N41' C50' C49' 122.6(6) . . ? C48' C51' C46' 86.2(6) . . ? Cl1 C54 Cl2 110.5(9) . . ? Cl1 C54 Cl3 110.0(8) . . ? Cl2 C54 Cl3 114.9(8) . . ? Cl4 C55 Cl5 114.8(7) . . ? Cl4 C55 Cl6 107.0(8) . . ? Cl5 C55 Cl6 110.5(6) . . ? Cl8 C56 Cl9 93.6(14) . . ? Cl8 C56 Cl7 88.6(12) . . ? Cl9 C56 Cl7 88.1(11) . . ? Cl7 C56A Cl8A 98.9(11) . . ? Cl7 C56A Cl9A 128.6(13) . . ? Cl8A C56A Cl9A 85.7(11) . . ? Cl11 C57 Cl10 112.7(6) . . ? Cl11 C57 Cl12 109.0(6) . . ? Cl10 C57 Cl12 110.2(6) . . ? Cl15 C58 Cl13 109.9(5) . . ? Cl15 C58 Cl14 110.1(4) . . ? Cl13 C58 Cl14 110.4(5) . . ? Cl18 C59 Cl16 111.8(5) . . ? Cl18 C59 Cl17 111.0(5) . . ? Cl16 C59 Cl17 111.6(5) . . ? C2 N1 C10 118.1(5) . . ? C2 N1 Ru1 116.3(4) . . ? C10 N1 Ru1 125.6(4) . . ? C10' N1' C2' 117.2(5) . . ? C10' N1' Ru1 126.6(4) . . ? C2' N1' Ru1 116.1(4) . . ? C30 N21 C22 116.9(5) . . ? C30 N21 Ru1 127.2(4) . . ? C22 N21 Ru1 115.7(4) . . ? C22' N21' C30' 116.3(5) . . ? C22' N21' Ru1 116.4(4) . . ? C30' N21' Ru1 126.8(4) . . ? C42 N41 C50 116.8(5) . . ? C42 N41 Ru1 117.0(4) . . ? C50 N41 Ru1 126.1(4) . . ? C50' N41' C42' 117.0(5) . . ? C50' N41' Ru1 124.9(4) . . ? C42' N41' Ru1 117.2(4) . . ? C56A Cl7 C56 20.7(11) . . ? F5A P1 F1A 113.4(10) . . ? F5A P1 F4 92.1(8) . . ? F1A P1 F4 110.3(8) . . ? F5A P1 F3 167.1(9) . . ? F1A P1 F3 76.0(9) . . ? F4 P1 F3 92.8(7) . . ? F5A P1 F4A 93.6(9) . . ? F1A P1 F4A 83.5(9) . . ? F4 P1 F4A 28.8(6) . . ? F3 P1 F4A 96.4(7) . . ? F5A P1 F6A 90.2(9) . . ? F1A P1 F6A 97.9(10) . . ? F4 P1 F6A 148.0(10) . . ? F3 P1 F6A 79.4(7) . . ? F4A P1 F6A 175.0(9) . . ? F5A P1 F1 109.5(10) . . ? F1A P1 F1 22.5(7) . . ? F4 P1 F1 88.8(7) . . ? F3 P1 F1 82.6(8) . . ? F4A P1 F1 61.2(8) . . ? F6A P1 F1 120.4(10) . . ? F5A P1 F2 68.6(9) . . ? F1A P1 F2 156.1(9) . . ? F4 P1 F2 93.1(8) . . ? F3 P1 F2 99.1(8) . . ? F4A P1 F2 120.4(9) . . ? F6A P1 F2 58.3(9) . . ? F1 P1 F2 177.4(8) . . ? F5A P1 F6 87.3(7) . . ? F1A P1 F6 68.1(8) . . ? F4 P1 F6 177.8(6) . . ? F3 P1 F6 88.3(6) . . ? F4A P1 F6 149.2(7) . . ? F6A P1 F6 34.2(8) . . ? F1 P1 F6 89.5(7) . . ? F2 P1 F6 88.6(7) . . ? F5A P1 F3A 155.8(10) . . ? F1A P1 F3A 90.8(9) . . ? F4 P1 F3A 80.3(7) . . ? F3 P1 F3A 16.7(9) . . ? F4A P1 F3A 90.5(8) . . ? F6A P1 F3A 84.7(9) . . ? F1 P1 F3A 93.4(8) . . ? F2 P1 F3A 88.7(8) . . ? F6 P1 F3A 101.2(7) . . ? F5A P1 F5 25.3(7) . . ? F1A P1 F5 89.1(9) . . ? F4 P1 F5 94.6(6) . . ? F3 P1 F5 164.9(8) . . ? F4A P1 F5 84.0(8) . . ? F6A P1 F5 100.7(8) . . ? F1 P1 F5 84.4(8) . . ? F2 P1 F5 93.6(7) . . ? F6 P1 F5 83.8(6) . . ? F3A P1 F5 174.5(8) . . ? F5A P1 F2A 78.5(10) . . ? F1A P1 F2A 167.1(9) . . ? F4 P1 F2A 62.7(8) . . ? F3 P1 F2A 93.1(9) . . ? F4A P1 F2A 91.0(9) . . ? F6A P1 F2A 86.6(10) . . ? F1 P1 F2A 151.0(9) . . ? F2 P1 F2A 31.2(6) . . ? F6 P1 F2A 119.2(7) . . ? F3A P1 F2A 77.5(8) . . ? F5 P1 F2A 102.0(9) . . ? F11 P2 F7 91.7(4) . . ? F11 P2 F8 89.6(4) . . ? F7 P2 F8 178.5(4) . . ? F11 P2 F10 90.8(3) . . ? F7 P2 F10 89.1(3) . . ? F8 P2 F10 91.3(3) . . ? F11 P2 F9 178.3(4) . . ? F7 P2 F9 89.5(4) . . ? F8 P2 F9 89.1(4) . . ? F10 P2 F9 90.4(3) . . ? F11 P2 F12 89.9(3) . . ? F7 P2 F12 90.9(3) . . ? F8 P2 F12 88.7(3) . . ? F10 P2 F12 179.3(3) . . ? F9 P2 F12 88.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 C4 -0.5(10) . . . . ? C2' C2 C3 C4 -178.1(6) . . . . ? C2 C3 C4 C9 1.7(10) . . . . ? C2 C3 C4 C5 178.2(7) . . . . ? C3 C4 C5 C6 -177.1(6) . . . . ? C9 C4 C5 C6 -0.5(9) . . . . ? C4 C5 C6 C7 49.6(8) . . . . ? C4 C5 C6 C11 -48.1(8) . . . . ? C5 C6 C7 C12 36.9(9) . . . . ? C11 C6 C7 C12 148.3(6) . . . . ? C5 C6 C7 C13 168.0(6) . . . . ? C11 C6 C7 C13 -80.7(6) . . . . ? C5 C6 C7 C8 -83.8(6) . . . . ? C11 C6 C7 C8 27.6(5) . . . . ? C12 C7 C8 C9 -43.4(9) . . . . ? C6 C7 C8 C9 79.4(6) . . . . ? C13 C7 C8 C9 -167.8(6) . . . . ? C12 C7 C8 C11 -149.9(7) . . . . ? C6 C7 C8 C11 -27.1(5) . . . . ? C13 C7 C8 C11 85.7(6) . . . . ? C3 C4 C9 C10 -2.4(9) . . . . ? C5 C4 C9 C10 -179.1(6) . . . . ? C3 C4 C9 C8 177.4(6) . . . . ? C5 C4 C9 C8 0.8(9) . . . . ? C11 C8 C9 C10 -134.7(6) . . . . ? C7 C8 C9 C10 134.0(6) . . . . ? C11 C8 C9 C4 45.5(8) . . . . ? C7 C8 C9 C4 -45.8(8) . . . . ? C4 C9 C10 N1 2.1(9) . . . . ? C8 C9 C10 N1 -177.7(6) . . . . ? C7 C6 C11 C8 -28.1(5) . . . . ? C5 C6 C11 C8 85.0(6) . . . . ? C9 C8 C11 C6 -81.1(6) . . . . ? C7 C8 C11 C6 26.9(5) . . . . ? N1 C2 C2' N1' -1.8(8) . . . . ? C3 C2 C2' N1' 176.0(6) . . . . ? N1 C2 C2' C3' -179.9(6) . . . . ? C3 C2 C2' C3' -2.2(10) . . . . ? N1' C2' C3' C4' 0.8(10) . . . . ? C2 C2' C3' C4' 178.8(6) . . . . ? C2' C3' C4' C9' 1.1(10) . . . . ? C2' C3' C4' C5' -179.4(7) . . . . ? C3' C4' C5' C6' 178.3(7) . . . . ? C9' C4' C5' C6' -2.3(10) . . . . ? C4' C5' C6' C11' -47.3(9) . . . . ? C4' C5' C6' C7' 49.3(9) . . . . ? C11' C6' C7' C12' 148.3(7) . . . . ? C5' C6' C7' C12' 38.3(9) . . . . ? C11' C6' C7' C8' 27.8(5) . . . . ? C5' C6' C7' C8' -82.2(7) . . . . ? C11' C6' C7' C13' -83.5(7) . . . . ? C5' C6' C7' C13' 166.5(7) . . . . ? C12' C7' C8' C9' -39.0(9) . . . . ? C13' C7' C8' C9' -168.1(6) . . . . ? C6' C7' C8' C9' 80.3(7) . . . . ? C12' C7' C8' C11' -147.0(7) . . . . ? C13' C7' C8' C11' 84.0(7) . . . . ? C6' C7' C8' C11' -27.7(5) . . . . ? C3' C4' C9' C10' -1.5(10) . . . . ? C5' C4' C9' C10' 179.0(6) . . . . ? C3' C4' C9' C8' -178.3(6) . . . . ? C5' C4' C9' C8' 2.2(9) . . . . ? C11' C8' C9' C10' -130.2(7) . . . . ? C7' C8' C9' C10' 134.6(7) . . . . ? C11' C8' C9' C4' 46.5(8) . . . . ? C7' C8' C9' C4' -48.8(8) . . . . ? C4' C9' C10' N1' -0.1(10) . . . . ? C8' C9' C10' N1' 176.4(6) . . . . ? C5' C6' C11' C8' 85.2(7) . . . . ? C7' C6' C11' C8' -27.8(5) . . . . ? C9' C8' C11' C6' -83.3(6) . . . . ? C7' C8' C11' C6' 28.0(5) . . . . ? N21 C22 C23 C24 0.0(10) . . . . ? C22' C22 C23 C24 179.4(7) . . . . ? C22 C23 C24 C29 -1.1(10) . . . . ? C22 C23 C24 C25 179.4(7) . . . . ? C23 C24 C25 C26 177.0(7) . . . . ? C29 C24 C25 C26 -2.5(10) . . . . ? C24 C25 C26 C27 50.8(8) . . . . ? C24 C25 C26 C31 -46.9(8) . . . . ? C31 C26 C27 C32 147.7(6) . . . . ? C25 C26 C27 C32 35.8(8) . . . . ? C31 C26 C27 C33 -82.7(7) . . . . ? C25 C26 C27 C33 165.3(6) . . . . ? C31 C26 C27 C28 27.5(5) . . . . ? C25 C26 C27 C28 -84.4(6) . . . . ? C26 C27 C28 C29 79.1(6) . . . . ? C32 C27 C28 C29 -41.7(9) . . . . ? C33 C27 C28 C29 -168.1(6) . . . . ? C26 C27 C28 C31 -27.2(5) . . . . ? C32 C27 C28 C31 -148.0(7) . . . . ? C33 C27 C28 C31 85.6(7) . . . . ? C23 C24 C29 C30 2.5(10) . . . . ? C25 C24 C29 C30 -178.0(6) . . . . ? C23 C24 C29 C28 -177.3(6) . . . . ? C25 C24 C29 C28 2.2(10) . . . . ? C31 C28 C29 C30 -134.2(7) . . . . ? C27 C28 C29 C30 133.7(7) . . . . ? C31 C28 C29 C24 45.5(8) . . . . ? C27 C28 C29 C24 -46.6(8) . . . . ? C24 C29 C30 N21 -2.9(10) . . . . ? C28 C29 C30 N21 176.8(6) . . . . ? C27 C26 C31 C28 -27.9(5) . . . . ? C25 C26 C31 C28 85.9(6) . . . . ? C29 C28 C31 C26 -81.8(6) . . . . ? C27 C28 C31 C26 27.1(5) . . . . ? N21 C22 C22' C23' 168.2(7) . . . . ? C23 C22 C22' C23' -11.3(11) . . . . ? N21 C22 C22' N21' -8.3(9) . . . . ? C23 C22 C22' N21' 172.2(6) . . . . ? N21' C22' C23' C24' -1.0(12) . . . . ? C22 C22' C23' C24' -177.3(7) . . . . ? C22' C23' C24' C29' -3.0(11) . . . . ? C22' C23' C24' C25' 175.7(7) . . . . ? C29' C24' C25' C26' -1.1(10) . . . . ? C23' C24' C25' C26' -179.9(7) . . . . ? C24' C25' C26' C31' -47.8(8) . . . . ? C24' C25' C26' C27' 48.2(9) . . . . ? C25' C26' C27' C32' 37.1(9) . . . . ? C31' C26' C27' C32' 147.3(6) . . . . ? C25' C26' C27' C33' 167.3(7) . . . . ? C31' C26' C27' C33' -82.5(7) . . . . ? C25' C26' C27' C28' -82.0(7) . . . . ? C31' C26' C27' C28' 28.2(5) . . . . ? C32' C27' C28' C29' -41.5(8) . . . . ? C33' C27' C28' C29' -168.8(6) . . . . ? C26' C27' C28' C29' 79.3(6) . . . . ? C32' C27' C28' C31' -148.4(7) . . . . ? C33' C27' C28' C31' 84.3(7) . . . . ? C26' C27' C28' C31' -27.6(5) . . . . ? C23' C24' C29' C30' 3.4(10) . . . . ? C25' C24' C29' C30' -175.5(6) . . . . ? C23' C24' C29' C28' -178.7(6) . . . . ? C25' C24' C29' C28' 2.5(10) . . . . ? C31' C28' C29' C30' -139.1(7) . . . . ? C27' C28' C29' C30' 129.6(7) . . . . ? C31' C28' C29' C24' 43.2(8) . . . . ? C27' C28' C29' C24' -48.2(8) . . . . ? C24' C29' C30' N21' 0.2(10) . . . . ? C28' C29' C30' N21' -177.5(6) . . . . ? C25' C26' C31' C28' 85.0(6) . . . . ? C27' C26' C31' C28' -28.7(5) . . . . ? C29' C28' C31' C26' -80.5(6) . . . . ? C27' C28' C31' C26' 28.2(5) . . . . ? N41 C42 C43 C44 -0.9(10) . . . . ? C42' C42 C43 C44 175.5(6) . . . . ? C42 C43 C44 C49 1.7(10) . . . . ? C42 C43 C44 C45 -179.2(7) . . . . ? C49 C44 C45 C46 -2.8(9) . . . . ? C43 C44 C45 C46 178.1(7) . . . . ? C44 C45 C46 C51 -46.5(9) . . . . ? C44 C45 C46 C47 51.1(8) . . . . ? C45 C46 C47 C53 36.1(8) . . . . ? C51 C46 C47 C53 148.0(6) . . . . ? C45 C46 C47 C52 163.8(6) . . . . ? C51 C46 C47 C52 -84.3(7) . . . . ? C45 C46 C47 C48 -84.5(6) . . . . ? C51 C46 C47 C48 27.5(5) . . . . ? C53 C47 C48 C49 -41.0(9) . . . . ? C52 C47 C48 C49 -168.3(6) . . . . ? C46 C47 C48 C49 79.0(6) . . . . ? C53 C47 C48 C51 -147.1(7) . . . . ? C52 C47 C48 C51 85.5(7) . . . . ? C46 C47 C48 C51 -27.2(5) . . . . ? C43 C44 C49 C50 -1.1(10) . . . . ? C45 C44 C49 C50 179.7(6) . . . . ? C43 C44 C49 C48 -178.4(6) . . . . ? C45 C44 C49 C48 2.3(9) . . . . ? C51 C48 C49 C50 -131.9(7) . . . . ? C47 C48 C49 C50 135.0(7) . . . . ? C51 C48 C49 C44 45.3(8) . . . . ? C47 C48 C49 C44 -47.8(8) . . . . ? C44 C49 C50 N41 -0.3(10) . . . . ? C48 C49 C50 N41 176.9(6) . . . . ? C45 C46 C51 C48 85.2(7) . . . . ? C47 C46 C51 C48 -28.0(5) . . . . ? C49 C48 C51 C46 -80.9(6) . . . . ? C47 C48 C51 C46 27.7(5) . . . . ? N41 C42 C42' C43' 169.4(6) . . . . ? C43 C42 C42' C43' -7.2(10) . . . . ? N41 C42 C42' N41' -7.0(8) . . . . ? C43 C42 C42' N41' 176.3(6) . . . . ? N41' C42' C43' C44' 3.9(10) . . . . ? C42 C42' C43' C44' -172.2(6) . . . . ? C42' C43' C44' C49' -1.7(10) . . . . ? C42' C43' C44' C45' 175.1(7) . . . . ? C49' C44' C45' C46' -0.1(11) . . . . ? C43' C44' C45' C46' -177.1(7) . . . . ? C44' C45' C46' C51' -47.0(9) . . . . ? C44' C45' C46' C47' 48.9(10) . . . . ? C45' C46' C47' C52' 165.9(7) . . . . ? C51' C46' C47' C52' -81.4(7) . . . . ? C45' C46' C47' C53' 35.6(9) . . . . ? C51' C46' C47' C53' 148.4(6) . . . . ? C45' C46' C47' C48' -83.7(7) . . . . ? C51' C46' C47' C48' 29.1(5) . . . . ? C52' C47' C48' C49' -168.9(6) . . . . ? C53' C47' C48' C49' -41.5(9) . . . . ? C46' C47' C48' C49' 79.2(6) . . . . ? C52' C47' C48' C51' 82.4(7) . . . . ? C53' C47' C48' C51' -150.1(7) . . . . ? C46' C47' C48' C51' -29.4(5) . . . . ? C43' C44' C49' C50' -1.6(10) . . . . ? C45' C44' C49' C50' -178.7(7) . . . . ? C43' C44' C49' C48' 177.3(6) . . . . ? C45' C44' C49' C48' 0.2(10) . . . . ? C51' C48' C49' C44' 45.8(8) . . . . ? C47' C48' C49' C44' -48.0(8) . . . . ? C51' C48' C49' C50' -135.2(7) . . . . ? C47' C48' C49' C50' 130.9(6) . . . . ? C44' C49' C50' N41' 3.1(10) . . . . ? C48' C49' C50' N41' -175.8(6) . . . . ? C49' C48' C51' C46' -78.1(6) . . . . ? C47' C48' C51' C46' 30.2(5) . . . . ? C45' C46' C51' C48' 82.6(7) . . . . ? C47' C46' C51' C48' -30.0(5) . . . . ? C3 C2 N1 C10 0.0(9) . . . . ? C2' C2 N1 C10 177.9(5) . . . . ? C3 C2 N1 Ru1 -178.5(5) . . . . ? C2' C2 N1 Ru1 -0.6(7) . . . . ? C9 C10 N1 C2 -0.9(9) . . . . ? C9 C10 N1 Ru1 177.5(5) . . . . ? N21 Ru1 N1 C2 99.3(4) . . . . ? N41' Ru1 N1 C2 -82.1(4) . . . . ? N41 Ru1 N1 C2 -40(3) . . . . ? N1' Ru1 N1 C2 1.8(4) . . . . ? N21' Ru1 N1 C2 177.7(4) . . . . ? N21 Ru1 N1 C10 -79.1(5) . . . . ? N41' Ru1 N1 C10 99.5(5) . . . . ? N41 Ru1 N1 C10 142(2) . . . . ? N1' Ru1 N1 C10 -176.5(5) . . . . ? N21' Ru1 N1 C10 -0.7(5) . . . . ? C9' C10' N1' C2' 2.0(9) . . . . ? C9' C10' N1' Ru1 177.6(5) . . . . ? C3' C2' N1' C10' -2.3(8) . . . . ? C2 C2' N1' C10' 179.5(5) . . . . ? C3' C2' N1' Ru1 -178.4(5) . . . . ? C2 C2' N1' Ru1 3.4(6) . . . . ? N21 Ru1 N1' C10' 95.6(5) . . . . ? N41' Ru1 N1' C10' -79.8(5) . . . . ? N41 Ru1 N1' C10' -2.1(5) . . . . ? N21' Ru1 N1' C10' 121(2) . . . . ? N1 Ru1 N1' C10' -178.5(5) . . . . ? N21 Ru1 N1' C2' -88.7(4) . . . . ? N41' Ru1 N1' C2' 95.9(4) . . . . ? N41 Ru1 N1' C2' 173.6(4) . . . . ? N21' Ru1 N1' C2' -64(3) . . . . ? N1 Ru1 N1' C2' -2.9(4) . . . . ? C29 C30 N21 C22 1.8(9) . . . . ? C29 C30 N21 Ru1 177.1(5) . . . . ? C23 C22 N21 C30 -0.3(9) . . . . ? C22' C22 N21 C30 -179.8(6) . . . . ? C23 C22 N21 Ru1 -176.1(5) . . . . ? C22' C22 N21 Ru1 4.3(7) . . . . ? N41' Ru1 N21 C30 120(2) . . . . ? N41 Ru1 N21 C30 101.2(5) . . . . ? N1' Ru1 N21 C30 2.7(5) . . . . ? N21' Ru1 N21 C30 -175.3(5) . . . . ? N1 Ru1 N21 C30 -75.4(5) . . . . ? N41' Ru1 N21 C22 -64(3) . . . . ? N41 Ru1 N21 C22 -83.5(4) . . . . ? N1' Ru1 N21 C22 178.0(4) . . . . ? N21' Ru1 N21 C22 0.1(4) . . . . ? N1 Ru1 N21 C22 100.0(4) . . . . ? C23' C22' N21' C30' 4.5(10) . . . . ? C22 C22' N21' C30' -178.9(6) . . . . ? C23' C22' N21' Ru1 -168.1(6) . . . . ? C22 C22' N21' Ru1 8.4(7) . . . . ? C29' C30' N21' C22' -4.1(9) . . . . ? C29' C30' N21' Ru1 167.6(5) . . . . ? N21 Ru1 N21' C22' -4.9(5) . . . . ? N41' Ru1 N21' C22' 170.4(5) . . . . ? N41 Ru1 N21' C22' 92.9(5) . . . . ? N1' Ru1 N21' C22' -30(3) . . . . ? N1 Ru1 N21' C22' -90.3(5) . . . . ? N21 Ru1 N21' C30' -176.6(5) . . . . ? N41' Ru1 N21' C30' -1.3(5) . . . . ? N41 Ru1 N21' C30' -78.8(5) . . . . ? N1' Ru1 N21' C30' 158(2) . . . . ? N1 Ru1 N21' C30' 98.0(5) . . . . ? C43 C42 N41 C50 -0.5(9) . . . . ? C42' C42 N41 C50 -177.1(6) . . . . ? C43 C42 N41 Ru1 -176.5(5) . . . . ? C42' C42 N41 Ru1 6.8(7) . . . . ? C49 C50 N41 C42 1.0(9) . . . . ? C49 C50 N41 Ru1 176.7(5) . . . . ? N21 Ru1 N41 C42 174.7(5) . . . . ? N41' Ru1 N41 C42 -3.6(4) . . . . ? N1' Ru1 N41 C42 -87.6(5) . . . . ? N21' Ru1 N41 C42 96.4(5) . . . . ? N1 Ru1 N41 C42 -47(3) . . . . ? N21 Ru1 N41 C50 -1.0(5) . . . . ? N41' Ru1 N41 C50 -179.3(5) . . . . ? N1' Ru1 N41 C50 96.7(5) . . . . ? N21' Ru1 N41 C50 -79.3(5) . . . . ? N1 Ru1 N41 C50 138(2) . . . . ? C49' C50' N41' C42' -1.1(9) . . . . ? C49' C50' N41' Ru1 168.0(5) . . . . ? C43' C42' N41' C50' -2.5(9) . . . . ? C42 C42' N41' C50' 174.1(5) . . . . ? C43' C42' N41' Ru1 -172.4(5) . . . . ? C42 C42' N41' Ru1 4.2(7) . . . . ? N21 Ru1 N41' C50' 171(2) . . . . ? N41 Ru1 N41' C50' -169.6(5) . . . . ? N1' Ru1 N41' C50' -70.9(5) . . . . ? N21' Ru1 N41' C50' 107.4(5) . . . . ? N1 Ru1 N41' C50' 6.8(5) . . . . ? N21 Ru1 N41' C42' -20(3) . . . . ? N41 Ru1 N41' C42' -0.6(4) . . . . ? N1' Ru1 N41' C42' 98.1(5) . . . . ? N21' Ru1 N41' C42' -83.6(5) . . . . ? N1 Ru1 N41' C42' 175.8(4) . . . . ? Cl8A C56A Cl7 C56 122(4) . . . . ? Cl9A C56A Cl7 C56 -147(4) . . . . ? Cl8 C56 Cl7 C56A -36(3) . . . . ? Cl9 C56 Cl7 C56A 58(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.761 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.092 data_3a _database_code_depnum_ccdc_archive 'CCDC 281499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H84 N6 Os, 2(P F6)' _chemical_formula_sum 'C72 H84 F12 N6 Os P2' _chemical_formula_weight 1513.59 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' F F 0.0171 0.0103 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.5876(7) _cell_length_b 15.6490(11) _cell_length_c 15.6557(12) _cell_angle_alpha 119.681(8) _cell_angle_beta 90.714(8) _cell_angle_gamma 111.307(8) _cell_volume 2232.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_process_details ? _exptl_special_details ; 'MULscanABS (PLATON99, Spek, 1999)' ; _diffrn_ambient_temperature 153(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17893 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14785 _reflns_number_gt 12830 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie Company, Germany)' _computing_cell_refinement 'CELL (Stoe & Cie Company, Germany)' _computing_data_reduction 'XRED (Stoe & Cie Company, Germany)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1999)' _computing_publication_material SHELXL-97 _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^)+(0.1201P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(12) _refine_ls_number_reflns 14785 _refine_ls_number_parameters 750 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3881(12) 0.5036(8) -0.8309(9) 0.041(2) Uani 1 1 d . . . H1A H 0.3178 0.5180 -0.8407 0.049 Uiso 1 1 calc R . . C2 C 0.4244(17) 0.4380(15) -0.9139(15) 0.045(4) Uani 1 1 d . . . C3 C 0.5275(11) 0.4182(8) -0.8992(8) 0.041(3) Uani 1 1 d . . . C4 C 0.5855(12) 0.4580(9) -0.8024(9) 0.045(3) Uani 1 1 d . . . H4A H 0.6522 0.4404 -0.7911 0.054 Uiso 1 1 calc R . . C5 C 0.5479(11) 0.5239(8) -0.7207(9) 0.042(3) Uani 1 1 d . . . C6 C 0.3638(15) 0.3968(11) -1.0209(10) 0.066(4) Uani 1 1 d D . . H6A H 0.2870 0.4087 -1.0314 0.079 Uiso 1 1 calc R . . C7 C 0.474(2) 0.4271(18) -1.0740(17) 0.071(7) Uani 1 1 d D . . C8 C 0.492(2) 0.3279(15) -1.0871(14) 0.064(5) Uani 1 1 d D . . H8A H 0.5132 0.2840 -1.1521 0.077 Uiso 1 1 calc R . . C9 C 0.3510(16) 0.2780(12) -1.0820(11) 0.064(4) Uani 1 1 d D . . H9A H 0.2889 0.2307 -1.1485 0.077 Uiso 1 1 calc R . . H9B H 0.3374 0.2426 -1.0430 0.077 Uiso 1 1 calc R . . C10 C 0.5749(16) 0.3558(12) -0.9914(11) 0.048(3) Uani 1 1 d . . . H10A H 0.5691 0.2883 -0.9974 0.057 Uiso 1 1 calc R . . H10B H 0.6652 0.4009 -0.9833 0.057 Uiso 1 1 calc R . . C11 C 0.5843(19) 0.5415(13) -1.0115(13) 0.083(5) Uani 1 1 d . . . H11A H 0.6158 0.5566 -0.9449 0.099 Uiso 1 1 calc R . . H11B H 0.5539 0.5954 -1.0031 0.099 Uiso 1 1 calc R . . H11C H 0.6534 0.5452 -1.0468 0.099 Uiso 1 1 calc R . . C12 C 0.418(3) 0.406(2) -1.1733(18) 0.101(9) Uani 1 1 d . . . H12A H 0.3820 0.4573 -1.1612 0.121 Uiso 1 1 calc R . . H12B H 0.3509 0.3314 -1.2138 0.121 Uiso 1 1 calc R . . H12C H 0.4852 0.4143 -1.2098 0.121 Uiso 1 1 calc R . . C13 C 0.6077(11) 0.5758(8) -0.6146(9) 0.043(3) Uani 1 1 d . . . C14 C 0.6914(14) 0.5479(11) -0.5816(10) 0.058(3) Uani 1 1 d . . . H14A H 0.7151 0.4934 -0.6290 0.069 Uiso 1 1 calc R . . C15 C 0.7405(17) 0.6009(13) -0.4778(10) 0.066(4) Uani 1 1 d . . . C16 C 0.7119(19) 0.6827(14) -0.4092(14) 0.048(4) Uani 1 1 d . . . C17 C 0.6217(11) 0.7028(10) -0.4470(9) 0.044(3) Uani 1 1 d . . . H17A H 0.5968 0.7566 -0.4000 0.052 Uiso 1 1 calc R . . C18 C 0.7647(15) 0.7360(12) -0.2997(11) 0.066(4) Uani 1 1 d D . . H18A H 0.7456 0.7984 -0.2519 0.079 Uiso 1 1 calc R . . C19 C 0.742(3) 0.646(2) -0.2754(18) 0.104(11) Uani 1 1 d D . . C20 C 0.858(3) 0.637(2) -0.3210(17) 0.125(14) Uani 1 1 d D . . H20A H 0.9151 0.6221 -0.2868 0.150 Uiso 1 1 calc R . . C21 C 0.905(2) 0.756(2) -0.2891(15) 0.095(8) Uani 1 1 d D . . H21A H 0.9581 0.8094 -0.2192 0.114 Uiso 1 1 calc R . . H21B H 0.9450 0.7722 -0.3379 0.114 Uiso 1 1 calc R . . C22 C 0.823(2) 0.566(2) -0.4365(13) 0.096(7) Uani 1 1 d D . . H22A H 0.7751 0.4882 -0.4592 0.115 Uiso 1 1 calc R . . H22B H 0.9013 0.5738 -0.4622 0.115 Uiso 1 1 calc R . . C23 C 0.618(2) 0.5435(17) -0.3267(16) 0.112(8) Uani 1 1 d D . . H23A H 0.5905 0.5215 -0.3967 0.134 Uiso 1 1 calc R . . H23B H 0.5528 0.5571 -0.2901 0.134 Uiso 1 1 calc R . . H23C H 0.6323 0.4854 -0.3265 0.134 Uiso 1 1 calc R . . C24 C 0.779(3) 0.695(2) -0.1609(17) 0.117(11) Uani 1 1 d D . . H24A H 0.7679 0.7630 -0.1241 0.140 Uiso 1 1 calc R . . H24B H 0.8681 0.7110 -0.1409 0.140 Uiso 1 1 calc R . . H24C H 0.7240 0.6437 -0.1445 0.140 Uiso 1 1 calc R . . C25 C 0.5070(13) 0.8929(9) -0.4526(9) 0.048(3) Uani 1 1 d . . . C26 C 0.5307(14) 0.9850(9) -0.3570(9) 0.055(3) Uani 1 1 d . . . H26A H 0.5894 1.0547 -0.3412 0.066 Uiso 1 1 calc R . . C27 C 0.4697(14) 0.9746(9) -0.2867(9) 0.056(3) Uani 1 1 d . . . C28 C 0.3782(19) 0.8722(14) -0.3132(14) 0.046(5) Uani 1 1 d . . . C29 C 0.3629(13) 0.7855(9) -0.4050(9) 0.046(3) Uani 1 1 d . . . H29A H 0.3054 0.7155 -0.4208 0.055 Uiso 1 1 calc R . . C30 C 0.3093(15) 0.8650(10) -0.2348(10) 0.065(4) Uani 1 1 d . . . H30A H 0.2400 0.7927 -0.2556 0.078 Uiso 1 1 calc R . . C31 C 0.415(3) 0.9247(18) -0.1345(14) 0.073(7) Uani 1 1 d D . . C32 C 0.418(3) 1.0320(16) -0.1186(16) 0.093(9) Uani 1 1 d . . . H32A H 0.4277 1.0894 -0.0470 0.111 Uiso 1 1 calc R . . C33 C 0.278(2) 0.9613(14) -0.1848(15) 0.075(6) Uani 1 1 d . . . H33A H 0.2121 0.9550 -0.1455 0.090 Uiso 1 1 calc R . . H33B H 0.2568 0.9823 -0.2310 0.090 Uiso 1 1 calc R . . C34 C 0.505(2) 1.0715(11) -0.1774(11) 0.077(5) Uani 1 1 d . . . H34A H 0.4923 1.1312 -0.1765 0.093 Uiso 1 1 calc R . . H34B H 0.5954 1.0989 -0.1458 0.093 Uiso 1 1 calc R . . C35 C 0.357(3) 0.904(2) -0.0560(16) 0.113(11) Uani 1 1 d D . . H35A H 0.3540 0.8358 -0.0676 0.136 Uiso 1 1 calc R . . H35B H 0.2703 0.8995 -0.0619 0.136 Uiso 1 1 calc R . . H35C H 0.4091 0.9641 0.0120 0.136 Uiso 1 1 calc R . . C36 C 0.536(2) 0.9071(16) -0.1400(14) 0.104(7) Uani 1 1 d . . . H36A H 0.5719 0.9164 -0.1927 0.124 Uiso 1 1 calc R . . H36B H 0.5155 0.8334 -0.1564 0.124 Uiso 1 1 calc R . . H36C H 0.5976 0.9601 -0.0746 0.124 Uiso 1 1 calc R . . C37 C 0.5675(12) 0.8925(9) -0.5352(8) 0.045(3) Uani 1 1 d . . . C38 C 0.6341(14) 0.9849(9) -0.5374(10) 0.059(3) Uani 1 1 d . . . H38A H 0.6439 1.0543 -0.4836 0.071 Uiso 1 1 calc R . . C39 C 0.6848(14) 0.9745(10) -0.6177(11) 0.060(4) Uani 1 1 d . . . C40 C 0.672(2) 0.8734(16) -0.6946(17) 0.058(6) Uani 1 1 d . . . C41 C 0.6066(12) 0.7867(9) -0.6875(9) 0.044(3) Uani 1 1 d . . . H41A H 0.6011 0.7179 -0.7389 0.053 Uiso 1 1 calc R . . C42 C 0.7345(15) 0.8647(10) -0.7814(11) 0.063(4) Uani 1 1 d D . . H42A H 0.7309 0.7922 -0.8329 0.075 Uiso 1 1 calc R . . C43 C 0.690(3) 0.9262(18) -0.8217(15) 0.072(7) Uani 1 1 d D . . C44 C 0.792(2) 1.0313(14) -0.7288(14) 0.080(8) Uani 1 1 d D . . H44A H 0.8387 1.0896 -0.7419 0.096 Uiso 1 1 calc R . . C45 C 0.8654(17) 0.9628(13) -0.7330(16) 0.067(5) Uani 1 1 d D . . H45A H 0.9251 0.9580 -0.7782 0.081 Uiso 1 1 calc R . . H45B H 0.9067 0.9832 -0.6659 0.081 Uiso 1 1 calc R . . C46 C 0.745(2) 1.0710(12) -0.6314(13) 0.086(7) Uani 1 1 d . . . H46A H 0.6806 1.0974 -0.6361 0.103 Uiso 1 1 calc R . . H46B H 0.8168 1.1314 -0.5730 0.103 Uiso 1 1 calc R . . C47 C 0.557(2) 0.9084(17) -0.8303(15) 0.100(7) Uani 1 1 d . . . H47A H 0.5323 0.9169 -0.7677 0.120 Uiso 1 1 calc R . . H47B H 0.5029 0.8347 -0.8874 0.120 Uiso 1 1 calc R . . H47C H 0.5452 0.9614 -0.8414 0.120 Uiso 1 1 calc R . . C48 C 0.730(3) 0.903(2) -0.9207(16) 0.108(10) Uani 1 1 d D . . H48A H 0.6624 0.8369 -0.9777 0.130 Uiso 1 1 calc R . . H48B H 0.8086 0.8928 -0.9194 0.130 Uiso 1 1 calc R . . H48C H 0.7454 0.9644 -0.9284 0.130 Uiso 1 1 calc R . . C49 C 0.1574(11) 0.5240(8) -0.6360(8) 0.037(2) Uani 1 1 d . . . C50 C 0.0544(11) 0.4586(9) -0.6194(8) 0.043(3) Uani 1 1 d . . . H50A H -0.0299 0.4417 -0.6474 0.052 Uiso 1 1 calc R . . C51 C 0.0732(12) 0.4179(9) -0.5626(9) 0.044(3) Uani 1 1 d . . . C52 C 0.194(2) 0.4393(17) -0.5281(16) 0.050(5) Uani 1 1 d . . . C53 C 0.2943(12) 0.5027(8) -0.5441(9) 0.042(3) Uani 1 1 d . . . H53A H 0.3785 0.5170 -0.5188 0.050 Uiso 1 1 calc R . . C54 C 0.2125(13) 0.3956(11) -0.4644(13) 0.067(4) Uani 1 1 d D . . H54A H 0.3015 0.4081 -0.4420 0.080 Uiso 1 1 calc R . . C55 C 0.1354(19) 0.4267(14) -0.3810(14) 0.067(6) Uani 1 1 d D . . C56 C 0.0153(16) 0.3260(15) -0.4657(13) 0.059(5) Uani 1 1 d D . . H56A H -0.0487 0.2830 -0.4434 0.071 Uiso 1 1 calc R . . C57 C 0.1089(14) 0.2769(12) -0.5203(17) 0.067(5) Uani 1 1 d D . . H57A H 0.1255 0.2310 -0.5000 0.080 Uiso 1 1 calc R . . H57B H 0.0867 0.2403 -0.5949 0.080 Uiso 1 1 calc R . . C58 C -0.0389(14) 0.3568(12) -0.5319(11) 0.050(3) Uani 1 1 d . . . H58A H -0.0815 0.4038 -0.4934 0.060 Uiso 1 1 calc R . . H58B H -0.1024 0.2904 -0.5931 0.060 Uiso 1 1 calc R . . C59 C 0.1382(16) 0.5395(12) -0.3278(12) 0.077(5) Uani 1 1 d D . . H59A H 0.1167 0.5542 -0.3784 0.092 Uiso 1 1 calc R . . H59B H 0.2237 0.5937 -0.2850 0.092 Uiso 1 1 calc R . . H59C H 0.0760 0.5432 -0.2858 0.092 Uiso 1 1 calc R . . C60 C 0.167(2) 0.405(2) -0.299(2) 0.099(9) Uani 1 1 d . . . H60A H 0.2557 0.4546 -0.2606 0.119 Uiso 1 1 calc R . . H60B H 0.1558 0.3300 -0.3316 0.119 Uiso 1 1 calc R . . H60C H 0.1099 0.4180 -0.2532 0.119 Uiso 1 1 calc R . . C61 C 0.1483(11) 0.5757(9) -0.6915(8) 0.041(2) Uani 1 1 d . . . C62 C 0.0380(12) 0.5478(11) -0.7504(10) 0.058(3) Uani 1 1 d . . . H62A H -0.0397 0.4937 -0.7563 0.070 Uiso 1 1 calc R . . C63 C 0.0399(14) 0.5987(13) -0.8019(12) 0.068(4) Uani 1 1 d . . . C64 C 0.1559(19) 0.6824(14) -0.7883(13) 0.047(4) Uani 1 1 d . . . C65 C 0.2628(12) 0.7035(10) -0.7288(9) 0.042(3) Uani 1 1 d . . . H65A H 0.3418 0.7584 -0.7200 0.051 Uiso 1 1 calc R . . C66 C 0.1527(14) 0.7357(13) -0.8443(12) 0.065(4) Uani 1 1 d . . . H66A H 0.2341 0.7969 -0.8319 0.078 Uiso 1 1 calc R . . C67 C 0.081(3) 0.649(3) -0.955(2) 0.098(10) Uani 1 1 d D . . C68 C -0.036(3) 0.638(2) -0.920(2) 0.131(15) Uani 1 1 d D . . H68A H -0.1077 0.6239 -0.9685 0.157 Uiso 1 1 calc R . . C69 C 0.033(2) 0.758(2) -0.832(2) 0.098(8) Uani 1 1 d D . . H69A H 0.0093 0.7741 -0.7671 0.118 Uiso 1 1 calc R . . H69B H 0.0322 0.8113 -0.8490 0.118 Uiso 1 1 calc R . . C70 C -0.0750(17) 0.5638(19) -0.8780(17) 0.091(7) Uani 1 1 d D . . H70B H -0.1463 0.5707 -0.8451 0.109 Uiso 1 1 calc R . . H70A H -0.1030 0.4870 -0.9336 0.109 Uiso 1 1 calc R . . C71 C 0.110(3) 0.5458(19) -1.0087(15) 0.117(8) Uani 1 1 d . . . H71A H 0.1011 0.5150 -0.9666 0.141 Uiso 1 1 calc R . . H71B H 0.1969 0.5665 -1.0184 0.141 Uiso 1 1 calc R . . H71C H 0.0492 0.4917 -1.0746 0.141 Uiso 1 1 calc R . . C72 C 0.101(3) 0.695(3) -1.024(2) 0.126(13) Uani 1 1 d D . . H72C H 0.0280 0.7100 -1.0330 0.151 Uiso 1 1 calc R . . H72B H 0.1063 0.6411 -1.0898 0.151 Uiso 1 1 calc R . . H72A H 0.1793 0.7619 -0.9927 0.151 Uiso 1 1 calc R . . F1 F -0.308(2) 0.1496(16) -0.9372(14) 0.191(8) Uiso 1 1 d D . . F2 F -0.221(2) 0.3214(16) -0.8494(16) 0.184(7) Uiso 1 1 d D . . F3 F -0.275(2) 0.3228(15) -0.7087(13) 0.175(7) Uiso 1 1 d D . . F4 F -0.359(2) 0.1506(17) -0.7912(17) 0.196(8) Uiso 1 1 d D . . F5 F -0.4272(12) 0.2358(10) -0.8414(9) 0.109(3) Uiso 1 1 d D . . F6 F -0.1552(12) 0.2360(10) -0.8021(9) 0.110(3) Uiso 1 1 d D . . F7A F 0.672(2) 0.2433(17) -1.2568(18) 0.208(9) Uiso 1 1 d D . . F8A F 0.745(2) 0.2484(15) -1.3828(13) 0.181(7) Uiso 1 1 d D . . F9A F 0.856(2) 0.4245(18) -1.2831(19) 0.216(9) Uiso 1 1 d D . . F10A F 0.758(2) 0.4215(18) -1.1644(16) 0.210(9) Uiso 1 1 d D . . F11A F 0.638(3) 0.338(3) -1.314(3) 0.322(17) Uiso 1 1 d D . . F12A F 0.877(3) 0.329(4) -1.229(3) 0.343(19) Uiso 1 1 d D . . N1 N 0.4518(10) 0.5464(9) -0.7377(9) 0.0399(9) Uani 1 1 d . . . N2 N 0.5665(11) 0.6492(7) -0.5486(8) 0.0399(9) Uani 1 1 d . . . N3 N 0.4243(10) 0.7922(9) -0.4757(9) 0.0399(9) Uani 1 1 d . . . N4 N 0.5477(12) 0.7920(9) -0.6111(9) 0.0399(9) Uani 1 1 d . . . N5 N 0.2752(12) 0.5449(9) -0.5948(9) 0.0399(9) Uani 1 1 d . . . N6 N 0.2618(11) 0.6499(7) -0.6818(8) 0.0399(9) Uani 1 1 d . . . Os1 Os 0.42241(3) 0.66331(3) -0.60812(3) 0.03600(13) Uani 1 1 d . . . P1 P -0.2924(5) 0.2341(3) -0.8226(3) 0.0740(11) Uiso 1 1 d D . . P2 P 0.7563(4) 0.3317(3) -1.2740(3) 0.0671(10) Uiso 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 C1 0.028(6) 0.037(5) 0.057(7) 0.024(5) 0.001(5) 0.015(5) C2 0.033(9) 0.040(8) 0.048(8) 0.013(6) 0.003(6) 0.016(7) C3 0.040(7) 0.032(5) 0.042(6) 0.012(4) 0.007(5) 0.016(5) C4 0.041(7) 0.046(6) 0.055(7) 0.026(5) 0.014(5) 0.027(5) C5 0.035(6) 0.038(5) 0.059(7) 0.028(5) 0.017(5) 0.016(4) C6 0.069(10) 0.064(8) 0.043(7) 0.008(6) 0.004(7) 0.039(7) C7 0.085(16) 0.094(16) 0.061(11) 0.039(11) 0.026(10) 0.067(14) C8 0.088(15) 0.074(13) 0.048(9) 0.028(9) 0.022(9) 0.057(11) C9 0.073(11) 0.069(10) 0.033(7) 0.008(7) 0.017(7) 0.042(9) C10 0.055(8) 0.053(7) 0.053(9) 0.033(7) 0.020(7) 0.035(6) C11 0.106(14) 0.065(9) 0.087(11) 0.045(9) 0.018(10) 0.039(9) C12 0.14(2) 0.14(2) 0.075(13) 0.055(14) 0.030(14) 0.11(2) C13 0.039(6) 0.040(5) 0.053(6) 0.027(5) 0.014(5) 0.018(5) C14 0.066(9) 0.071(8) 0.058(7) 0.034(6) 0.020(7) 0.051(7) C15 0.084(11) 0.085(10) 0.051(7) 0.040(7) 0.018(8) 0.053(9) C16 0.045(11) 0.054(10) 0.056(9) 0.033(8) 0.013(7) 0.027(8) C17 0.032(6) 0.045(7) 0.053(7) 0.027(6) 0.009(5) 0.016(5) C18 0.062(10) 0.082(10) 0.062(8) 0.033(7) 0.008(7) 0.047(8) C19 0.14(3) 0.13(2) 0.066(13) 0.061(14) 0.016(15) 0.08(2) C20 0.19(4) 0.19(3) 0.084(17) 0.09(2) 0.04(2) 0.15(3) C21 0.058(12) 0.17(2) 0.063(11) 0.061(14) 0.003(9) 0.063(15) C22 0.129(19) 0.153(19) 0.069(11) 0.066(12) 0.033(11) 0.112(16) C23 0.18(3) 0.110(16) 0.088(13) 0.071(13) 0.043(15) 0.073(17) C24 0.16(3) 0.18(3) 0.097(17) 0.10(2) 0.062(18) 0.12(3) C25 0.057(8) 0.040(6) 0.048(6) 0.022(5) 0.005(5) 0.024(5) C26 0.067(9) 0.026(5) 0.050(7) 0.013(5) 0.001(6) 0.008(5) C27 0.075(10) 0.034(6) 0.043(6) 0.011(5) 0.012(6) 0.022(6) C28 0.053(12) 0.035(7) 0.046(8) 0.017(6) 0.011(8) 0.021(8) C29 0.041(8) 0.036(6) 0.062(7) 0.030(5) 0.015(6) 0.013(5) C30 0.072(10) 0.046(7) 0.049(7) 0.016(6) 0.019(7) 0.010(6) C31 0.108(19) 0.062(9) 0.035(8) 0.024(7) 0.016(10) 0.026(11) C32 0.17(3) 0.054(10) 0.058(11) 0.025(9) 0.076(16) 0.055(14) C33 0.099(15) 0.055(9) 0.055(11) 0.019(8) 0.032(11) 0.030(9) C34 0.116(15) 0.044(7) 0.048(8) 0.018(7) 0.025(9) 0.020(8) C35 0.17(3) 0.078(12) 0.062(12) 0.038(10) 0.025(16) 0.023(17) C36 0.121(18) 0.085(12) 0.068(10) 0.039(9) -0.012(11) 0.012(12) C37 0.046(7) 0.040(6) 0.043(6) 0.018(5) 0.006(5) 0.017(5) C38 0.069(9) 0.031(5) 0.059(7) 0.017(5) 0.011(7) 0.015(5) C39 0.067(9) 0.042(7) 0.063(8) 0.031(6) 0.010(7) 0.012(6) C40 0.068(15) 0.030(8) 0.051(9) 0.019(7) 0.011(9) 0.002(8) C41 0.043(7) 0.035(6) 0.047(6) 0.018(5) 0.008(5) 0.015(5) C42 0.076(10) 0.050(7) 0.070(8) 0.039(6) 0.034(7) 0.024(7) C43 0.101(18) 0.064(10) 0.067(10) 0.045(8) 0.032(11) 0.035(10) C44 0.097(18) 0.045(9) 0.067(10) 0.029(8) 0.036(11) 0.001(10) C45 0.060(11) 0.062(9) 0.083(12) 0.049(10) 0.020(10) 0.015(8) C46 0.130(17) 0.043(7) 0.062(9) 0.030(7) 0.031(11) 0.011(8) C47 0.15(2) 0.099(13) 0.090(12) 0.064(11) 0.029(13) 0.065(14) C48 0.18(3) 0.080(12) 0.066(11) 0.045(10) 0.031(16) 0.049(17) C49 0.039(6) 0.038(5) 0.043(5) 0.023(4) 0.009(5) 0.024(4) C50 0.026(6) 0.049(6) 0.047(6) 0.024(5) 0.007(4) 0.011(5) C51 0.036(7) 0.034(5) 0.058(7) 0.028(5) 0.011(6) 0.006(5) C52 0.049(10) 0.045(10) 0.049(9) 0.026(8) 0.009(7) 0.013(7) C53 0.033(6) 0.037(5) 0.061(7) 0.027(5) 0.012(5) 0.018(5) C54 0.040(8) 0.070(9) 0.120(13) 0.074(9) 0.013(8) 0.018(6) C55 0.054(11) 0.077(13) 0.080(12) 0.055(11) 0.010(9) 0.020(9) C56 0.048(10) 0.075(12) 0.068(11) 0.052(10) 0.014(8) 0.019(8) C57 0.052(10) 0.062(9) 0.111(15) 0.062(11) 0.041(10) 0.027(7) C58 0.045(8) 0.055(7) 0.051(8) 0.034(7) 0.006(6) 0.014(6) C59 0.068(10) 0.077(10) 0.065(9) 0.035(8) -0.002(7) 0.014(8) C60 0.070(13) 0.12(2) 0.117(18) 0.089(17) 0.002(11) 0.018(12) C61 0.033(6) 0.046(6) 0.047(6) 0.028(5) 0.009(5) 0.014(5) C62 0.039(7) 0.069(8) 0.066(8) 0.046(7) 0.005(6) 0.007(6) C63 0.043(8) 0.084(10) 0.076(9) 0.051(8) 0.004(7) 0.015(7) C64 0.041(9) 0.058(10) 0.040(8) 0.029(8) 0.007(6) 0.016(8) C65 0.042(7) 0.046(7) 0.051(6) 0.030(5) 0.015(5) 0.024(5) C66 0.044(8) 0.086(10) 0.080(10) 0.057(8) 0.007(7) 0.025(7) C67 0.069(14) 0.14(2) 0.108(19) 0.100(18) 0.005(13) 0.021(14) C68 0.081(17) 0.18(3) 0.15(3) 0.14(3) -0.021(17) 0.01(2) C69 0.083(15) 0.17(2) 0.12(2) 0.12(2) 0.037(15) 0.075(16) C70 0.056(10) 0.147(17) 0.096(14) 0.097(14) 0.004(10) 0.022(10) C71 0.14(2) 0.107(16) 0.067(11) 0.049(11) 0.005(12) 0.017(15) C72 0.098(17) 0.19(3) 0.094(17) 0.11(2) 0.006(13) 0.014(19) N1 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) N2 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) N3 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) N4 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) N5 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) N6 0.035(2) 0.0323(18) 0.0431(18) 0.0162(15) 0.0113(16) 0.0113(17) Os1 0.03129(19) 0.02600(16) 0.0447(2) 0.01512(13) 0.00825(13) 0.01193(12) _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 C1 N1 1.330(18) . ? C1 C2 1.39(2) . ? C1 H1A 0.9500 . ? C2 C3 1.38(2) . ? C2 C6 1.51(2) . ? C3 C4 1.368(17) . ? C3 C10 1.534(18) . ? C4 C5 1.388(16) . ? C4 H4A 0.9500 . ? C5 N1 1.343(18) . ? C5 C13 1.457(17) . ? C6 C9 1.558(17) . ? C6 C7 1.59(2) . ? C6 H6A 1.0000 . ? C7 C12 1.50(3) . ? C7 C11 1.54(3) . ? C7 C8 1.56(2) . ? C8 C10 1.54(2) . ? C8 C9 1.56(2) . ? C8 H8A 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.361(16) . ? C13 C14 1.384(18) . ? C14 C15 1.40(2) . ? C14 H14A 0.9500 . ? C15 C16 1.36(2) . ? C15 C22 1.54(2) . ? C16 C17 1.40(2) . ? C16 C18 1.48(2) . ? C17 N2 1.381(17) . ? C17 H17A 0.9500 . ? C18 C21 1.53(2) . ? C18 C19 1.56(2) . ? C18 H18A 1.0000 . ? C19 C23 1.52(2) . ? C19 C24 1.54(2) . ? C19 C20 1.55(3) . ? C20 C22 1.53(2) . ? C20 C21 1.54(2) . ? C20 H20A 1.0000 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.364(16) . ? C25 C26 1.399(16) . ? C25 C37 1.477(17) . ? C26 C27 1.361(19) . ? C26 H26A 0.9500 . ? C27 C28 1.40(2) . ? C27 C34 1.535(18) . ? C28 C29 1.35(2) . ? C28 C30 1.50(2) . ? C29 N3 1.350(17) . ? C29 H29A 0.9500 . ? C30 C33 1.50(2) . ? C30 C31 1.59(3) . ? C30 H30A 1.0000 . ? C31 C36 1.51(4) . ? C31 C35 1.52(2) . ? C31 C32 1.56(3) . ? C32 C34 1.54(2) . ? C32 C33 1.56(4) . ? C32 H32A 1.0000 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N4 1.348(15) . ? C37 C38 1.389(17) . ? C38 C39 1.36(2) . ? C38 H38A 0.9500 . ? C39 C40 1.38(2) . ? C39 C46 1.539(19) . ? C40 C41 1.35(2) . ? C40 C42 1.52(3) . ? C41 N4 1.366(17) . ? C41 H41A 0.9500 . ? C42 C45 1.54(2) . ? C42 C43 1.60(2) . ? C42 H42A 1.0000 . ? C43 C47 1.45(3) . ? C43 C48 1.53(2) . ? C43 C44 1.55(3) . ? C44 C46 1.53(2) . ? C44 C45 1.58(2) . ? C44 H44A 1.0000 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N5 1.353(17) . ? C49 C50 1.387(15) . ? C49 C61 1.475(15) . ? C50 C51 1.379(17) . ? C50 H50A 0.9500 . ? C51 C52 1.35(3) . ? C51 C58 1.549(18) . ? C52 C53 1.35(2) . ? C52 C54 1.51(3) . ? C53 N5 1.318(18) . ? C53 H53A 0.9500 . ? C54 C57 1.549(17) . ? C54 C55 1.57(2) . ? C54 H54A 1.0000 . ? C55 C59 1.52(2) . ? C55 C60 1.55(3) . ? C55 C56 1.57(2) . ? C56 C58 1.55(2) . ? C56 C57 1.574(19) . ? C56 H56A 1.0000 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 N6 1.346(15) . ? C61 C62 1.357(18) . ? C62 C63 1.38(2) . ? C62 H62A 0.9500 . ? C63 C64 1.42(2) . ? C63 C70 1.51(2) . ? C64 C65 1.37(2) . ? C64 C66 1.49(2) . ? C65 N6 1.360(17) . ? C65 H65A 0.9500 . ? C66 C67 1.53(4) . ? C66 C69 1.54(3) . ? C66 H66A 1.0000 . ? C67 C68 1.45(4) . ? C67 C72 1.54(2) . ? C67 C71 1.58(4) . ? C68 C70 1.54(2) . ? C68 C69 1.54(3) . ? C68 H68A 1.0000 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70B 0.9900 . ? C70 H70A 0.9900 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72C 0.9800 . ? C72 H72B 0.9800 . ? C72 H72A 0.9800 . ? F1 P1 1.571(18) . ? F2 P1 1.575(18) . ? F3 P1 1.576(17) . ? F4 P1 1.566(18) . ? F5 P1 1.599(13) . ? F6 P1 1.604(13) . ? F7A P2 1.527(19) . ? F8A P2 1.513(17) . ? F9A P2 1.57(2) . ? F10A P2 1.586(19) . ? F11A P2 1.56(2) . ? F12A P2 1.58(3) . ? N1 Os1 2.091(12) . ? N2 Os1 2.034(13) . ? N3 Os1 2.048(12) . ? N4 Os1 2.033(12) . ? N5 Os1 2.116(12) . ? N6 Os1 2.064(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 120.0(14) . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 119.7(16) . . ? C3 C2 C6 118.0(16) . . ? C1 C2 C6 122.0(17) . . ? C4 C3 C2 118.5(12) . . ? C4 C3 C10 122.6(12) . . ? C2 C3 C10 118.9(13) . . ? C3 C4 C5 120.5(12) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? N1 C5 C4 119.2(12) . . ? N1 C5 C13 115.6(10) . . ? C4 C5 C13 125.2(11) . . ? C2 C6 C9 103.1(14) . . ? C2 C6 C7 108.4(15) . . ? C9 C6 C7 88.1(13) . . ? C2 C6 H6A 117.6 . . ? C9 C6 H6A 117.6 . . ? C7 C6 H6A 117.6 . . ? C12 C7 C11 110.2(19) . . ? C12 C7 C8 111.7(18) . . ? C11 C7 C8 119.7(18) . . ? C12 C7 C6 110(2) . . ? C11 C7 C6 117.4(16) . . ? C8 C7 C6 85.5(14) . . ? C10 C8 C7 112.6(16) . . ? C10 C8 C9 106.1(14) . . ? C7 C8 C9 89.0(14) . . ? C10 C8 H8A 115.3 . . ? C7 C8 H8A 115.3 . . ? C9 C8 H8A 115.3 . . ? C6 C9 C8 86.4(13) . . ? C6 C9 H9A 114.3 . . ? C8 C9 H9A 114.3 . . ? C6 C9 H9B 114.3 . . ? C8 C9 H9B 114.3 . . ? H9A C9 H9B 111.4 . . ? C3 C10 C8 109.0(12) . . ? C3 C10 H10A 109.9 . . ? C8 C10 H10A 109.9 . . ? C3 C10 H10B 109.9 . . ? C8 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 121.8(12) . . ? N2 C13 C5 114.1(11) . . ? C14 C13 C5 123.9(11) . . ? C13 C14 C15 119.2(12) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 121.0(15) . . ? C16 C15 C22 117.5(15) . . ? C14 C15 C22 121.4(13) . . ? C15 C16 C17 116.8(16) . . ? C15 C16 C18 119.3(17) . . ? C17 C16 C18 123.5(16) . . ? N2 C17 C16 124.0(13) . . ? N2 C17 H17A 118.0 . . ? C16 C17 H17A 118.0 . . ? C16 C18 C21 105.5(15) . . ? C16 C18 C19 108.8(14) . . ? C21 C18 C19 87.7(16) . . ? C16 C18 H18A 116.9 . . ? C21 C18 H18A 116.9 . . ? C19 C18 H18A 116.9 . . ? C23 C19 C24 112(2) . . ? C23 C19 C20 116(2) . . ? C24 C19 C20 109(2) . . ? C23 C19 C18 120.4(19) . . ? C24 C19 C18 112(2) . . ? C20 C19 C18 84.9(16) . . ? C22 C20 C21 108.4(19) . . ? C22 C20 C19 113(2) . . ? C21 C20 C19 87.7(18) . . ? C22 C20 H20A 114.8 . . ? C21 C20 H20A 114.8 . . ? C19 C20 H20A 114.8 . . ? C18 C21 C20 86.4(17) . . ? C18 C21 H21A 114.3 . . ? C20 C21 H21A 114.3 . . ? C18 C21 H21B 114.3 . . ? C20 C21 H21B 114.3 . . ? H21A C21 H21B 111.4 . . ? C20 C22 C15 108.6(15) . . ? C20 C22 H22A 110.0 . . ? C15 C22 H22A 110.0 . . ? C20 C22 H22B 110.0 . . ? C15 C22 H22B 110.0 . . ? H22A C22 H22B 108.3 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 120.6(12) . . ? N3 C25 C37 113.9(10) . . ? C26 C25 C37 125.5(11) . . ? C27 C26 C25 119.9(11) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 119.2(12) . . ? C26 C27 C34 121.2(12) . . ? C28 C27 C34 119.5(14) . . ? C29 C28 C27 118.2(16) . . ? C29 C28 C30 124.1(15) . . ? C27 C28 C30 117.5(14) . . ? N3 C29 C28 124.0(13) . . ? N3 C29 H29A 118.0 . . ? C28 C29 H29A 118.0 . . ? C28 C30 C33 106.7(14) . . ? C28 C30 C31 106.6(14) . . ? C33 C30 C31 87.6(15) . . ? C28 C30 H30A 117.2 . . ? C33 C30 H30A 117.2 . . ? C31 C30 H30A 117.2 . . ? C36 C31 C35 109(2) . . ? C36 C31 C32 120(2) . . ? C35 C31 C32 110.0(19) . . ? C36 C31 C30 120.0(16) . . ? C35 C31 C30 110.5(19) . . ? C32 C31 C30 85.5(18) . . ? C34 C32 C31 111.9(17) . . ? C34 C32 C33 109.1(18) . . ? C31 C32 C33 86.4(18) . . ? C34 C32 H32A 115.3 . . ? C31 C32 H32A 115.3 . . ? C33 C32 H32A 115.3 . . ? C30 C33 C32 88.3(16) . . ? C30 C33 H33A 113.9 . . ? C32 C33 H33A 113.9 . . ? C30 C33 H33B 113.9 . . ? C32 C33 H33B 113.9 . . ? H33A C33 H33B 111.1 . . ? C27 C34 C32 107.8(13) . . ? C27 C34 H34A 110.2 . . ? C32 C34 H34A 110.2 . . ? C27 C34 H34B 110.2 . . ? C32 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 C38 122.8(12) . . ? N4 C37 C25 113.1(10) . . ? C38 C37 C25 124.0(10) . . ? C39 C38 C37 118.8(11) . . ? C39 C38 H38A 120.6 . . ? C37 C38 H38A 120.6 . . ? C38 C39 C40 120.1(13) . . ? C38 C39 C46 121.4(13) . . ? C40 C39 C46 118.3(15) . . ? C41 C40 C39 118.0(18) . . ? C41 C40 C42 123.0(17) . . ? C39 C40 C42 119.0(16) . . ? C40 C41 N4 124.1(14) . . ? C40 C41 H41A 117.9 . . ? N4 C41 H41A 117.9 . . ? C40 C42 C45 105.7(14) . . ? C40 C42 C43 106.2(15) . . ? C45 C42 C43 87.6(14) . . ? C40 C42 H42A 117.6 . . ? C45 C42 H42A 117.6 . . ? C43 C42 H42A 117.6 . . ? C47 C43 C48 112(2) . . ? C47 C43 C44 119.1(18) . . ? C48 C43 C44 112(2) . . ? C47 C43 C42 117.3(16) . . ? C48 C43 C42 108.3(17) . . ? C44 C43 C42 85.1(15) . . ? C46 C44 C43 113.8(16) . . ? C46 C44 C45 110.0(17) . . ? C43 C44 C45 88.0(15) . . ? C46 C44 H44A 114.1 . . ? C43 C44 H44A 114.1 . . ? C45 C44 H44A 114.1 . . ? C42 C45 C44 86.1(13) . . ? C42 C45 H45A 114.3 . . ? C44 C45 H45A 114.3 . . ? C42 C45 H45B 114.3 . . ? C44 C45 H45B 114.3 . . ? H45A C45 H45B 111.4 . . ? C44 C46 C39 107.7(13) . . ? C44 C46 H46A 110.2 . . ? C39 C46 H46A 110.2 . . ? C44 C46 H46B 110.2 . . ? C39 C46 H46B 110.2 . . ? H46A C46 H46B 108.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C50 117.2(11) . . ? N5 C49 C61 117.7(10) . . ? C50 C49 C61 125.0(11) . . ? C51 C50 C49 120.6(11) . . ? C51 C50 H50A 119.7 . . ? C49 C50 H50A 119.7 . . ? C52 C51 C50 118.0(13) . . ? C52 C51 C58 120.4(14) . . ? C50 C51 C58 121.5(12) . . ? C53 C52 C51 121.5(18) . . ? C53 C52 C54 121.2(19) . . ? C51 C52 C54 117.1(16) . . ? N5 C53 C52 119.7(15) . . ? N5 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? C52 C54 C57 105.4(15) . . ? C52 C54 C55 107.9(14) . . ? C57 C54 C55 88.6(12) . . ? C52 C54 H54A 117.0 . . ? C57 C54 H54A 117.0 . . ? C55 C54 H54A 117.0 . . ? C59 C55 C60 108.0(17) . . ? C59 C55 C54 118.9(15) . . ? C60 C55 C54 112.5(18) . . ? C59 C55 C56 120.0(17) . . ? C60 C55 C56 110.1(16) . . ? C54 C55 C56 86.0(12) . . ? C58 C56 C55 110.5(14) . . ? C58 C56 C57 107.0(14) . . ? C55 C56 C57 87.6(14) . . ? C58 C56 H56A 116.0 . . ? C55 C56 H56A 116.0 . . ? C57 C56 H56A 116.0 . . ? C54 C57 C56 86.5(12) . . ? C54 C57 H57A 114.2 . . ? C56 C57 H57A 114.2 . . ? C54 C57 H57B 114.2 . . ? C56 C57 H57B 114.2 . . ? H57A C57 H57B 111.4 . . ? C56 C58 C51 108.3(12) . . ? C56 C58 H58A 110.0 . . ? C51 C58 H58A 110.0 . . ? C56 C58 H58B 110.0 . . ? C51 C58 H58B 110.0 . . ? H58A C58 H58B 108.4 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N6 C61 C62 123.2(11) . . ? N6 C61 C49 113.1(11) . . ? C62 C61 C49 123.6(10) . . ? C61 C62 C63 119.3(12) . . ? C61 C62 H62A 120.3 . . ? C63 C62 H62A 120.3 . . ? C62 C63 C64 119.2(15) . . ? C62 C63 C70 122.7(13) . . ? C64 C63 C70 118.0(15) . . ? C65 C64 C63 117.2(16) . . ? C65 C64 C66 125.5(15) . . ? C63 C64 C66 117.2(16) . . ? N6 C65 C64 123.4(13) . . ? N6 C65 H65A 118.3 . . ? C64 C65 H65A 118.3 . . ? C64 C66 C67 109.9(16) . . ? C64 C66 C69 106.8(15) . . ? C67 C66 C69 86.0(18) . . ? C64 C66 H66A 116.7 . . ? C67 C66 H66A 116.7 . . ? C69 C66 H66A 116.7 . . ? C68 C67 C66 87(2) . . ? C68 C67 C72 115(3) . . ? C66 C67 C72 113(2) . . ? C68 C67 C71 117(2) . . ? C66 C67 C71 117(2) . . ? C72 C67 C71 106(3) . . ? C67 C68 C70 115(3) . . ? C67 C68 C69 89(2) . . ? C70 C68 C69 110(2) . . ? C67 C68 H68A 113.5 . . ? C70 C68 H68A 113.5 . . ? C69 C68 H68A 113.5 . . ? C68 C69 C66 83.5(19) . . ? C68 C69 H69A 114.7 . . ? C66 C69 H69A 114.7 . . ? C68 C69 H69B 114.7 . . ? C66 C69 H69B 114.7 . . ? H69A C69 H69B 111.8 . . ? C63 C70 C68 107.6(17) . . ? C63 C70 H70B 110.2 . . ? C68 C70 H70B 110.2 . . ? C63 C70 H70A 110.2 . . ? C68 C70 H70A 110.2 . . ? H70B C70 H70A 108.5 . . ? C67 C71 H71A 109.5 . . ? C67 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C67 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C67 C72 H72C 109.5 . . ? C67 C72 H72B 109.5 . . ? H72C C72 H72B 109.5 . . ? C67 C72 H72A 109.5 . . ? H72C C72 H72A 109.5 . . ? H72B C72 H72A 109.5 . . ? C1 N1 C5 121.8(12) . . ? C1 N1 Os1 123.1(10) . . ? C5 N1 Os1 114.9(9) . . ? C13 N2 C17 116.8(12) . . ? C13 N2 Os1 117.0(9) . . ? C17 N2 Os1 126.1(9) . . ? C29 N3 C25 117.8(11) . . ? C29 N3 Os1 125.6(9) . . ? C25 N3 Os1 116.1(8) . . ? C37 N4 C41 115.9(11) . . ? C37 N4 Os1 117.8(9) . . ? C41 N4 Os1 126.1(8) . . ? C53 N5 C49 122.8(11) . . ? C53 N5 Os1 124.1(10) . . ? C49 N5 Os1 112.8(9) . . ? C61 N6 C65 117.5(12) . . ? C61 N6 Os1 117.4(9) . . ? C65 N6 Os1 124.9(9) . . ? N4 Os1 N2 91.6(5) . . ? N4 Os1 N3 78.1(4) . . ? N2 Os1 N3 96.2(5) . . ? N4 Os1 N6 95.9(5) . . ? N2 Os1 N6 170.5(4) . . ? N3 Os1 N6 91.0(5) . . ? N4 Os1 N1 94.9(4) . . ? N2 Os1 N1 78.0(5) . . ? N3 Os1 N1 170.9(4) . . ? N6 Os1 N1 95.6(5) . . ? N4 Os1 N5 170.7(5) . . ? N2 Os1 N5 94.8(5) . . ? N3 Os1 N5 94.5(4) . . ? N6 Os1 N5 78.3(5) . . ? N1 Os1 N5 93.0(4) . . ? F4 P1 F1 97.6(12) . . ? F4 P1 F2 177.3(12) . . ? F1 P1 F2 84.4(11) . . ? F4 P1 F3 84.8(11) . . ? F1 P1 F3 177.5(12) . . ? F2 P1 F3 93.2(11) . . ? F4 P1 F5 87.9(10) . . ? F1 P1 F5 93.9(10) . . ? F2 P1 F5 93.7(10) . . ? F3 P1 F5 85.5(9) . . ? F4 P1 F6 93.3(10) . . ? F1 P1 F6 87.0(10) . . ? F2 P1 F6 85.0(10) . . ? F3 P1 F6 93.5(9) . . ? F5 P1 F6 178.4(7) . . ? F8A P2 F7A 91.7(12) . . ? F8A P2 F11A 86.8(16) . . ? F7A P2 F11A 91.5(17) . . ? F8A P2 F9A 90.7(12) . . ? F7A P2 F9A 173.4(13) . . ? F11A P2 F9A 94.8(17) . . ? F8A P2 F12A 95.3(17) . . ? F7A P2 F12A 88.6(18) . . ? F11A P2 F12A 178(2) . . ? F9A P2 F12A 85.1(18) . . ? F8A P2 F10A 174.0(13) . . ? F7A P2 F10A 89.6(13) . . ? F11A P2 F10A 87.2(16) . . ? F9A P2 F10A 88.6(13) . . ? F12A P2 F10A 90.7(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1(2) . . . . ? N1 C1 C2 C6 -173.7(14) . . . . ? C1 C2 C3 C4 5(2) . . . . ? C6 C2 C3 C4 178.0(13) . . . . ? C1 C2 C3 C10 -173.5(14) . . . . ? C6 C2 C3 C10 0(2) . . . . ? C2 C3 C4 C5 -5.0(18) . . . . ? C10 C3 C4 C5 173.1(11) . . . . ? C3 C4 C5 N1 1.3(16) . . . . ? C3 C4 C5 C13 -176.2(10) . . . . ? C3 C2 C6 C9 46(2) . . . . ? C1 C2 C6 C9 -140.4(16) . . . . ? C3 C2 C6 C7 -46(2) . . . . ? C1 C2 C6 C7 127.2(17) . . . . ? C2 C6 C7 C12 -170.0(17) . . . . ? C9 C6 C7 C12 86.7(18) . . . . ? C2 C6 C7 C11 -43(2) . . . . ? C9 C6 C7 C11 -146.0(17) . . . . ? C2 C6 C7 C8 78.5(16) . . . . ? C9 C6 C7 C8 -24.7(14) . . . . ? C12 C7 C8 C10 167.6(19) . . . . ? C11 C7 C8 C10 37(2) . . . . ? C6 C7 C8 C10 -82.4(16) . . . . ? C12 C7 C8 C9 -85(2) . . . . ? C11 C7 C8 C9 143.8(17) . . . . ? C6 C7 C8 C9 24.7(13) . . . . ? C2 C6 C9 C8 -83.8(15) . . . . ? C7 C6 C9 C8 24.7(14) . . . . ? C10 C8 C9 C6 88.1(14) . . . . ? C7 C8 C9 C6 -25.1(14) . . . . ? C4 C3 C10 C8 -177.3(12) . . . . ? C2 C3 C10 C8 0.7(18) . . . . ? C7 C8 C10 C3 47.4(19) . . . . ? C9 C8 C10 C3 -48.4(15) . . . . ? N1 C5 C13 N2 -7.0(14) . . . . ? C4 C5 C13 N2 170.6(10) . . . . ? N1 C5 C13 C14 167.9(12) . . . . ? C4 C5 C13 C14 -14.5(18) . . . . ? N2 C13 C14 C15 -4(2) . . . . ? C5 C13 C14 C15 -178.2(13) . . . . ? C13 C14 C15 C16 -3(2) . . . . ? C13 C14 C15 C22 173.8(17) . . . . ? C14 C15 C16 C17 6(3) . . . . ? C22 C15 C16 C17 -170.6(18) . . . . ? C14 C15 C16 C18 179.3(15) . . . . ? C22 C15 C16 C18 2(3) . . . . ? C15 C16 C17 N2 -4(2) . . . . ? C18 C16 C17 N2 -176.2(14) . . . . ? C15 C16 C18 C21 45(2) . . . . ? C17 C16 C18 C21 -142.9(19) . . . . ? C15 C16 C18 C19 -48(2) . . . . ? C17 C16 C18 C19 124.3(19) . . . . ? C16 C18 C19 C23 -39(3) . . . . ? C21 C18 C19 C23 -144(2) . . . . ? C16 C18 C19 C24 -173(2) . . . . ? C21 C18 C19 C24 82(2) . . . . ? C16 C18 C19 C20 78.4(18) . . . . ? C21 C18 C19 C20 -27.2(15) . . . . ? C23 C19 C20 C22 39(3) . . . . ? C24 C19 C20 C22 167(2) . . . . ? C18 C19 C20 C22 -82(2) . . . . ? C23 C19 C20 C21 148.3(19) . . . . ? C24 C19 C20 C21 -84(2) . . . . ? C18 C19 C20 C21 26.9(15) . . . . ? C16 C18 C21 C20 -81.6(16) . . . . ? C19 C18 C21 C20 27.3(15) . . . . ? C22 C20 C21 C18 86(2) . . . . ? C19 C20 C21 C18 -27.5(15) . . . . ? C21 C20 C22 C15 -47(3) . . . . ? C19 C20 C22 C15 48(3) . . . . ? C16 C15 C22 C20 -1(3) . . . . ? C14 C15 C22 C20 -178(2) . . . . ? N3 C25 C26 C27 -1(2) . . . . ? C37 C25 C26 C27 -179.2(13) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C25 C26 C27 C34 172.7(15) . . . . ? C26 C27 C28 C29 6(3) . . . . ? C34 C27 C28 C29 -170.1(17) . . . . ? C26 C27 C28 C30 -177.6(15) . . . . ? C34 C27 C28 C30 6(3) . . . . ? C27 C28 C29 N3 -5(3) . . . . ? C30 C28 C29 N3 179.5(16) . . . . ? C29 C28 C30 C33 -142(2) . . . . ? C27 C28 C30 C33 42(2) . . . . ? C29 C28 C30 C31 126(2) . . . . ? C27 C28 C30 C31 -50(2) . . . . ? C28 C30 C31 C36 -42(2) . . . . ? C33 C30 C31 C36 -148.9(19) . . . . ? C28 C30 C31 C35 -169.7(19) . . . . ? C33 C30 C31 C35 83(2) . . . . ? C28 C30 C31 C32 80.5(16) . . . . ? C33 C30 C31 C32 -26.2(14) . . . . ? C36 C31 C32 C34 38(3) . . . . ? C35 C31 C32 C34 166(2) . . . . ? C30 C31 C32 C34 -84(2) . . . . ? C36 C31 C32 C33 147.5(18) . . . . ? C35 C31 C32 C33 -85(2) . . . . ? C30 C31 C32 C33 25.1(13) . . . . ? C28 C30 C33 C32 -80.6(16) . . . . ? C31 C30 C33 C32 26.1(14) . . . . ? C34 C32 C33 C30 85.4(16) . . . . ? C31 C32 C33 C30 -26.6(13) . . . . ? C26 C27 C34 C32 179.7(18) . . . . ? C28 C27 C34 C32 -4(3) . . . . ? C31 C32 C34 C27 49(3) . . . . ? C33 C32 C34 C27 -45(2) . . . . ? N3 C25 C37 N4 -11.1(17) . . . . ? C26 C25 C37 N4 167.3(13) . . . . ? N3 C25 C37 C38 166.5(13) . . . . ? C26 C25 C37 C38 -15(2) . . . . ? N4 C37 C38 C39 -2(2) . . . . ? C25 C37 C38 C39 -179.4(13) . . . . ? C37 C38 C39 C40 -1(3) . . . . ? C37 C38 C39 C46 172.2(16) . . . . ? C38 C39 C40 C41 1(3) . . . . ? C46 C39 C40 C41 -172.6(19) . . . . ? C38 C39 C40 C42 -177.5(17) . . . . ? C46 C39 C40 C42 9(3) . . . . ? C39 C40 C41 N4 3(3) . . . . ? C42 C40 C41 N4 -178.8(17) . . . . ? C41 C40 C42 C45 -138(2) . . . . ? C39 C40 C42 C45 41(3) . . . . ? C41 C40 C42 C43 130(2) . . . . ? C39 C40 C42 C43 -51(3) . . . . ? C40 C42 C43 C47 -42(2) . . . . ? C45 C42 C43 C47 -147.7(18) . . . . ? C40 C42 C43 C48 -170.2(19) . . . . ? C45 C42 C43 C48 84(2) . . . . ? C40 C42 C43 C44 78.3(16) . . . . ? C45 C42 C43 C44 -27.3(13) . . . . ? C47 C43 C44 C46 34(3) . . . . ? C48 C43 C44 C46 167.8(19) . . . . ? C42 C43 C44 C46 -84.4(19) . . . . ? C47 C43 C44 C45 145.2(17) . . . . ? C48 C43 C44 C45 -81.2(19) . . . . ? C42 C43 C44 C45 26.6(12) . . . . ? C40 C42 C45 C44 -79.4(16) . . . . ? C43 C42 C45 C44 26.7(13) . . . . ? C46 C44 C45 C42 87.0(15) . . . . ? C43 C44 C45 C42 -27.7(13) . . . . ? C43 C44 C46 C39 51(2) . . . . ? C45 C44 C46 C39 -46(2) . . . . ? C38 C39 C46 C44 -179.8(17) . . . . ? C40 C39 C46 C44 -6(3) . . . . ? N5 C49 C50 C51 0.3(16) . . . . ? C61 C49 C50 C51 -177.0(10) . . . . ? C49 C50 C51 C52 -3.1(19) . . . . ? C49 C50 C51 C58 172.3(11) . . . . ? C50 C51 C52 C53 3(3) . . . . ? C58 C51 C52 C53 -172.4(15) . . . . ? C50 C51 C52 C54 178.9(13) . . . . ? C58 C51 C52 C54 3(2) . . . . ? C51 C52 C53 N5 0(3) . . . . ? C54 C52 C53 N5 -175.9(14) . . . . ? C53 C52 C54 C57 -139.4(17) . . . . ? C51 C52 C54 C57 45(2) . . . . ? C53 C52 C54 C55 127.0(18) . . . . ? C51 C52 C54 C55 -49(2) . . . . ? C52 C54 C55 C59 -42(2) . . . . ? C57 C54 C55 C59 -147.4(17) . . . . ? C52 C54 C55 C60 -169.3(17) . . . . ? C57 C54 C55 C60 85.0(17) . . . . ? C52 C54 C55 C56 80.6(15) . . . . ? C57 C54 C55 C56 -25.1(13) . . . . ? C59 C55 C56 C58 39(2) . . . . ? C60 C55 C56 C58 165.0(17) . . . . ? C54 C55 C56 C58 -82.5(15) . . . . ? C59 C55 C56 C57 146.0(17) . . . . ? C60 C55 C56 C57 -87.7(18) . . . . ? C54 C55 C56 C57 24.7(13) . . . . ? C52 C54 C57 C56 -83.1(16) . . . . ? C55 C54 C57 C56 25.1(14) . . . . ? C58 C56 C57 C54 85.7(14) . . . . ? C55 C56 C57 C54 -25.0(13) . . . . ? C55 C56 C58 C51 47.9(17) . . . . ? C57 C56 C58 C51 -46.0(16) . . . . ? C52 C51 C58 C56 -2.5(19) . . . . ? C50 C51 C58 C56 -177.9(12) . . . . ? N5 C49 C61 N6 -8.4(15) . . . . ? C50 C49 C61 N6 169.0(10) . . . . ? N5 C49 C61 C62 168.4(12) . . . . ? C50 C49 C61 C62 -14.3(18) . . . . ? N6 C61 C62 C63 -2(2) . . . . ? C49 C61 C62 C63 -178.0(13) . . . . ? C61 C62 C63 C64 -3(2) . . . . ? C61 C62 C63 C70 172.9(17) . . . . ? C62 C63 C64 C65 4(3) . . . . ? C70 C63 C64 C65 -171.8(17) . . . . ? C62 C63 C64 C66 -179.3(15) . . . . ? C70 C63 C64 C66 5(3) . . . . ? C63 C64 C65 N6 -1(2) . . . . ? C66 C64 C65 N6 -177.6(15) . . . . ? C65 C64 C66 C67 129(2) . . . . ? C63 C64 C66 C67 -47(2) . . . . ? C65 C64 C66 C69 -138.9(19) . . . . ? C63 C64 C66 C69 45(2) . . . . ? C64 C66 C67 C68 77(2) . . . . ? C69 C66 C67 C68 -29.1(17) . . . . ? C64 C66 C67 C72 -166(2) . . . . ? C69 C66 C67 C72 87(3) . . . . ? C64 C66 C67 C71 -42(3) . . . . ? C69 C66 C67 C71 -148(2) . . . . ? C66 C67 C68 C70 -83(3) . . . . ? C72 C67 C68 C70 163(3) . . . . ? C71 C67 C68 C70 36(3) . . . . ? C66 C67 C68 C69 29.0(17) . . . . ? C72 C67 C68 C69 -85(3) . . . . ? C71 C67 C68 C69 148(2) . . . . ? C67 C68 C69 C66 -28.9(16) . . . . ? C70 C68 C69 C66 88(2) . . . . ? C64 C66 C69 C68 -82.1(17) . . . . ? C67 C66 C69 C68 27.4(15) . . . . ? C62 C63 C70 C68 -179(2) . . . . ? C64 C63 C70 C68 -4(3) . . . . ? C67 C68 C70 C63 50(3) . . . . ? C69 C68 C70 C63 -48(3) . . . . ? C2 C1 N1 C5 -3.2(19) . . . . ? C2 C1 N1 Os1 171.0(11) . . . . ? C4 C5 N1 C1 2.9(17) . . . . ? C13 C5 N1 C1 -179.4(10) . . . . ? C4 C5 N1 Os1 -171.8(8) . . . . ? C13 C5 N1 Os1 6.0(12) . . . . ? C14 C13 N2 C17 6.3(17) . . . . ? C5 C13 N2 C17 -178.7(10) . . . . ? C14 C13 N2 Os1 -170.3(10) . . . . ? C5 C13 N2 Os1 4.8(12) . . . . ? C16 C17 N2 C13 -2.7(18) . . . . ? C16 C17 N2 Os1 173.5(12) . . . . ? C28 C29 N3 C25 0(2) . . . . ? C28 C29 N3 Os1 171.7(14) . . . . ? C26 C25 N3 C29 3(2) . . . . ? C37 C25 N3 C29 -178.8(12) . . . . ? C26 C25 N3 Os1 -169.7(10) . . . . ? C37 C25 N3 Os1 8.8(15) . . . . ? C38 C37 N4 C41 5(2) . . . . ? C25 C37 N4 C41 -176.9(12) . . . . ? C38 C37 N4 Os1 -169.2(11) . . . . ? C25 C37 N4 Os1 8.4(15) . . . . ? C40 C41 N4 C37 -6(2) . . . . ? C40 C41 N4 Os1 168.4(16) . . . . ? C52 C53 N5 C49 -3(2) . . . . ? C52 C53 N5 Os1 170.9(12) . . . . ? C50 C49 N5 C53 2.6(16) . . . . ? C61 C49 N5 C53 -179.8(10) . . . . ? C50 C49 N5 Os1 -171.6(8) . . . . ? C61 C49 N5 Os1 6.0(12) . . . . ? C62 C61 N6 C65 4.4(18) . . . . ? C49 C61 N6 C65 -178.8(10) . . . . ? C62 C61 N6 Os1 -170.1(10) . . . . ? C49 C61 N6 Os1 6.6(13) . . . . ? C64 C65 N6 C61 -2.9(19) . . . . ? C64 C65 N6 Os1 171.2(12) . . . . ? C37 N4 Os1 N2 -99.0(11) . . . . ? C41 N4 Os1 N2 87.0(12) . . . . ? C37 N4 Os1 N3 -3.0(10) . . . . ? C41 N4 Os1 N3 -177.1(14) . . . . ? C37 N4 Os1 N6 86.7(11) . . . . ? C41 N4 Os1 N6 -87.3(12) . . . . ? C37 N4 Os1 N1 -177.1(11) . . . . ? C41 N4 Os1 N1 8.8(13) . . . . ? C37 N4 Os1 N5 35(5) . . . . ? C41 N4 Os1 N5 -139(4) . . . . ? C13 N2 Os1 N4 -96.0(9) . . . . ? C17 N2 Os1 N4 87.8(10) . . . . ? C13 N2 Os1 N3 -174.2(9) . . . . ? C17 N2 Os1 N3 9.6(10) . . . . ? C13 N2 Os1 N6 47(4) . . . . ? C17 N2 Os1 N6 -129(3) . . . . ? C13 N2 Os1 N1 -1.3(8) . . . . ? C17 N2 Os1 N1 -177.5(11) . . . . ? C13 N2 Os1 N5 90.7(9) . . . . ? C17 N2 Os1 N5 -85.5(10) . . . . ? C29 N3 Os1 N4 -175.2(13) . . . . ? C25 N3 Os1 N4 -3.5(10) . . . . ? C29 N3 Os1 N2 -84.8(12) . . . . ? C25 N3 Os1 N2 86.9(10) . . . . ? C29 N3 Os1 N6 88.9(12) . . . . ? C25 N3 Os1 N6 -99.4(10) . . . . ? C29 N3 Os1 N1 -135(4) . . . . ? C25 N3 Os1 N1 37(5) . . . . ? C29 N3 Os1 N5 10.5(13) . . . . ? C25 N3 Os1 N5 -177.7(11) . . . . ? C61 N6 Os1 N4 -175.4(9) . . . . ? C65 N6 Os1 N4 10.5(10) . . . . ? C61 N6 Os1 N2 42(4) . . . . ? C65 N6 Os1 N2 -132(3) . . . . ? C61 N6 Os1 N3 -97.3(9) . . . . ? C65 N6 Os1 N3 88.6(10) . . . . ? C61 N6 Os1 N1 89.1(9) . . . . ? C65 N6 Os1 N1 -85.0(10) . . . . ? C61 N6 Os1 N5 -2.9(8) . . . . ? C65 N6 Os1 N5 -176.9(10) . . . . ? C1 N1 Os1 N4 -86.6(10) . . . . ? C5 N1 Os1 N4 88.0(9) . . . . ? C1 N1 Os1 N2 -177.3(11) . . . . ? C5 N1 Os1 N2 -2.7(8) . . . . ? C1 N1 Os1 N3 -126(4) . . . . ? C5 N1 Os1 N3 49(5) . . . . ? C1 N1 Os1 N6 9.9(10) . . . . ? C5 N1 Os1 N6 -175.5(9) . . . . ? C1 N1 Os1 N5 88.4(10) . . . . ? C5 N1 Os1 N5 -97.0(9) . . . . ? C53 N5 Os1 N4 -123(4) . . . . ? C49 N5 Os1 N4 51(5) . . . . ? C53 N5 Os1 N2 10.7(10) . . . . ? C49 N5 Os1 N2 -175.1(8) . . . . ? C53 N5 Os1 N3 -85.9(10) . . . . ? C49 N5 Os1 N3 88.3(9) . . . . ? C53 N5 Os1 N6 -176.0(11) . . . . ? C49 N5 Os1 N6 -1.8(7) . . . . ? C53 N5 Os1 N1 89.0(10) . . . . ? C49 N5 Os1 N1 -96.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.603 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.182 data_3b _database_code_depnum_ccdc_archive 'CCDC 281500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H84 N6 Os, 2(C F3 O3 S), 4(C3 H6 O)' _chemical_formula_sum 'C86 H108 F6 N6 O10 Os S2' _chemical_formula_weight 1754.10 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.8936(13) _cell_length_b 21.6543(12) _cell_length_c 15.3712(12) _cell_angle_alpha 90.00 _cell_angle_beta 118.321(6) _cell_angle_gamma 90.00 _cell_volume 4364.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20228 _cell_measurement_theta_min 0.14 _cell_measurement_theta_max 24.90 _exptl_crystal_description tube _exptl_crystal_colour blue _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.580 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details ? _exptl_special_details ; 'MULscanABS (PLATON03, Spek, 2003)' ; _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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32416 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1418 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.17 _reflns_number_total 14480 _reflns_number_gt 8432 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON03 (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1212P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.040(16) _refine_ls_number_reflns 14480 _refine_ls_number_parameters 292 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max <0.0011 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 C1 C -0.0138(11) 0.1777(6) 0.7712(10) 0.0710(10) Uani 1 1 d . . . H1A H 0.0407 0.2040 0.7793 0.085 Uiso 1 1 calc R . . C2 C -0.1069(11) 0.1858(6) 0.6902(10) 0.0710(10) Uani 1 1 d . . . C3 C -0.1889(11) 0.1472(6) 0.6825(10) 0.0710(10) Uani 1 1 d . . . C4 C -0.1678(9) 0.1021(6) 0.7514(8) 0.0710(10) Uani 1 1 d . . . H4A H -0.2197 0.0740 0.7447 0.085 Uiso 1 1 calc R . . C5 C -0.0747(10) 0.0974(5) 0.8280(9) 0.0710(10) Uani 1 1 d . . . C6 C -0.1310(13) 0.2330(7) 0.6094(12) 0.0924(12) Uani 1 1 d . . . H6 H -0.0738 0.2607 0.6175 0.111 Uiso 1 1 calc R . . C7 C -0.1911(14) 0.2006(7) 0.5076(13) 0.0924(12) Uani 1 1 d . . . C8 C -0.2906(14) 0.2084(7) 0.5266(13) 0.0924(12) Uani 1 1 d . . . H8 H -0.3569 0.2181 0.4670 0.111 Uiso 1 1 calc R . . C9 C -0.2928(13) 0.1579(7) 0.5888(12) 0.0924(12) Uani 1 1 d . . . H9A H -0.3132 0.1194 0.5493 0.111 Uiso 1 1 calc R . . H9B H -0.3452 0.1670 0.6093 0.111 Uiso 1 1 calc R . . C10 C -0.2309(13) 0.2650(7) 0.5921(13) 0.0924(12) Uani 1 1 d . . . H10A H -0.2446 0.3044 0.5553 0.111 Uiso 1 1 calc R . . H10B H -0.2377 0.2699 0.6528 0.111 Uiso 1 1 calc R . . C11 C -0.2008(13) 0.2418(7) 0.4208(12) 0.0924(12) Uani 1 1 d . . . H11A H -0.2052 0.2853 0.4362 0.139 Uiso 1 1 calc R . . H11B H -0.2625 0.2303 0.3602 0.139 Uiso 1 1 calc R . . H11C H -0.1409 0.2358 0.4112 0.139 Uiso 1 1 calc R . . C12 C -0.1578(13) 0.1348(6) 0.4990(13) 0.0924(12) Uani 1 1 d . . . H12A H -0.1066 0.1366 0.4761 0.139 Uiso 1 1 calc R . . H12B H -0.2171 0.1113 0.4515 0.139 Uiso 1 1 calc R . . H12C H -0.1284 0.1146 0.5637 0.139 Uiso 1 1 calc R . . C13 C -0.0430(11) 0.0498(6) 0.9040(10) 0.0710(10) Uani 1 1 d . . . C14 C -0.1168(11) 0.0073(6) 0.9064(10) 0.0710(10) Uani 1 1 d . . . H14A H -0.1875 0.0103 0.8611 0.085 Uiso 1 1 calc R . . C15 C -0.0774(11) -0.0390(6) 0.9806(10) 0.0710(10) Uani 1 1 d . . . C16 C 0.0196(11) -0.0403(6) 1.0421(10) 0.0710(10) Uani 1 1 d . . . C17 C 0.0837(11) -0.0006(6) 1.0323(10) 0.0710(10) Uani 1 1 d . . . H17A H 0.1546 -0.0046 1.0761 0.085 Uiso 1 1 calc R . . C18 C 0.0548(14) -0.0907(7) 1.1215(13) 0.0924(12) Uani 1 1 d . . . H18 H 0.1287 -0.0941 1.1708 0.111 Uiso 1 1 calc R . . C19 C -0.0294(14) -0.0920(8) 1.1591(13) 0.0924(12) Uani 1 1 d . . . C20 C -0.0816(14) -0.1283(7) 1.0787(13) 0.0924(12) Uani 1 1 d . . . H20 H -0.1203 -0.1618 1.0911 0.111 Uiso 1 1 calc R . . C21 C -0.1566(13) -0.0846(7) 0.9820(13) 0.0924(12) Uani 1 1 d . . . H21A H -0.1901 -0.1091 0.9204 0.111 Uiso 1 1 calc R . . H21B H -0.2091 -0.0630 0.9927 0.111 Uiso 1 1 calc R . . C22 C -0.0056(13) -0.1505(7) 1.0635(13) 0.0924(12) Uani 1 1 d . . . H22A H -0.0213 -0.1519 0.9933 0.111 Uiso 1 1 calc R . . H22B H 0.0240 -0.1900 1.0977 0.111 Uiso 1 1 calc R . . C23 C 0.0304(13) -0.1319(7) 1.2607(12) 0.0924(12) Uani 1 1 d . . . H23A H -0.0192 -0.1551 1.2726 0.139 Uiso 1 1 calc R . . H23B H 0.0687 -0.1039 1.3162 0.139 Uiso 1 1 calc R . . H23C H 0.0776 -0.1607 1.2542 0.139 Uiso 1 1 calc R . . C24 C -0.0515(14) -0.0265(7) 1.1981(14) 0.0924(12) Uani 1 1 d . . . H24A H -0.1195 -0.0115 1.1509 0.139 Uiso 1 1 calc R . . H24B H -0.0002 0.0040 1.2040 0.139 Uiso 1 1 calc R . . H24C H -0.0481 -0.0325 1.2628 0.139 Uiso 1 1 calc R . . C25 C 0.0507(14) 0.1890(7) 1.0506(12) 0.0915(13) Uani 1 1 d . . . H25A H -0.0018 0.1971 0.9854 0.110 Uiso 1 1 calc R . . C26 C 0.0417(14) 0.2155(7) 1.1357(12) 0.0915(13) Uani 1 1 d . . . C27 C 0.1215(14) 0.2095(7) 1.2215(12) 0.0915(13) Uani 1 1 d . . . C28 C 0.2101(14) 0.1755(7) 1.2463(12) 0.0915(13) Uani 1 1 d . . . H28A H 0.2633 0.1700 1.3120 0.110 Uiso 1 1 calc R . . C29 C 0.2113(14) 0.1490(7) 1.1580(11) 0.0915(13) Uani 1 1 d . . . C30 C -0.0460(19) 0.2496(10) 1.1172(17) 0.1301(18) Uani 1 1 d . . . H30 H -0.0969 0.2583 1.0470 0.156 Uiso 1 1 calc R . . C31 C -0.090(2) 0.2245(11) 1.1957(17) 0.1301(18) Uani 1 1 d . . . C32 C 0.0164(19) 0.2608(10) 1.2664(18) 0.1301(18) Uani 1 1 d . . . H32 H 0.0078 0.2826 1.3193 0.156 Uiso 1 1 calc R . . C33 C 0.1155(18) 0.2329(10) 1.3112(16) 0.1301(18) Uani 1 1 d . . . H33A H 0.1201 0.1986 1.3557 0.156 Uiso 1 1 calc R . . H33B H 0.1697 0.2634 1.3484 0.156 Uiso 1 1 calc R . . C34 C 0.0041(19) 0.3069(11) 1.1903(16) 0.1301(18) Uani 1 1 d . . . H34A H 0.0687 0.3222 1.1945 0.156 Uiso 1 1 calc R . . H34B H -0.0436 0.3410 1.1817 0.156 Uiso 1 1 calc R . . C35 C -0.1908(17) 0.2525(10) 1.1633(16) 0.1301(18) Uani 1 1 d . . . H35A H -0.2208 0.2360 1.2031 0.195 Uiso 1 1 calc R . . H35B H -0.2353 0.2428 1.0935 0.195 Uiso 1 1 calc R . . H35C H -0.1836 0.2974 1.1717 0.195 Uiso 1 1 calc R . . C36 C -0.0840(18) 0.1557(9) 1.2109(16) 0.1301(18) Uani 1 1 d . . . H36A H -0.0612 0.1466 1.2807 0.195 Uiso 1 1 calc R . . H36B H -0.0354 0.1382 1.1915 0.195 Uiso 1 1 calc R . . H36C H -0.1515 0.1375 1.1704 0.195 Uiso 1 1 calc R . . C37 C 0.2938(11) 0.1181(9) 1.1637(9) 0.0915(13) Uani 1 1 d . . . C38 C 0.3847(11) 0.1039(8) 1.2496(10) 0.0915(13) Uani 1 1 d . . . H38A H 0.3923 0.1186 1.3110 0.110 Uiso 1 1 calc R . . C39 C 0.4641(14) 0.0698(7) 1.2506(12) 0.0915(13) Uani 1 1 d . . . C40 C 0.4458(14) 0.0479(7) 1.1630(12) 0.0915(13) Uani 1 1 d . . . C41 C 0.3544(13) 0.0544(7) 1.0768(12) 0.0915(13) Uani 1 1 d . . . H41A H 0.3446 0.0364 1.0165 0.110 Uiso 1 1 calc R . . C42 C 0.5288(18) 0.0119(10) 1.1628(17) 0.1301(18) Uani 1 1 d . . . H42 H 0.5157 -0.0061 1.0979 0.156 Uiso 1 1 calc R . . C43 C 0.6276(18) 0.0470(10) 1.2193(17) 0.1301(18) Uani 1 1 d . . . C44 C 0.6300(19) 0.0290(10) 1.3217(17) 0.1301(18) Uani 1 1 d . . . H44 H 0.6997 0.0219 1.3783 0.156 Uiso 1 1 calc R . . C45 C 0.5650(17) 0.0653(10) 1.3444(16) 0.1301(18) Uani 1 1 d . . . H45A H 0.5946 0.1069 1.3668 0.156 Uiso 1 1 calc R . . H45B H 0.5555 0.0456 1.3976 0.156 Uiso 1 1 calc R . . C46 C 0.5741(18) -0.0335(10) 1.2545(16) 0.1301(18) Uani 1 1 d . . . H46A H 0.6221 -0.0647 1.2532 0.156 Uiso 1 1 calc R . . H46B H 0.5224 -0.0526 1.2691 0.156 Uiso 1 1 calc R . . C47 C 0.7256(17) 0.0187(10) 1.2176(16) 0.1301(18) Uani 1 1 d . . . H47A H 0.7326 -0.0249 1.2368 0.195 Uiso 1 1 calc R . . H47B H 0.7865 0.0414 1.2642 0.195 Uiso 1 1 calc R . . H47C H 0.7179 0.0223 1.1509 0.195 Uiso 1 1 calc R . . C48 C 0.6290(14) 0.1171(13) 1.2078(13) 0.1301(18) Uani 1 1 d . . . H48A H 0.6305 0.1269 1.1463 0.195 Uiso 1 1 calc R . . H48B H 0.6897 0.1343 1.2640 0.195 Uiso 1 1 calc R . . H48C H 0.5677 0.1350 1.2060 0.195 Uiso 1 1 calc R . . C49 C 0.1293(12) 0.0192(6) 0.8012(12) 0.0843(11) Uani 1 1 d . . . H49A H 0.0817 -0.0004 0.8168 0.101 Uiso 1 1 calc R . . C50 C 0.1464(11) -0.0096(6) 0.7285(13) 0.0843(11) Uani 1 1 d . . . C51 C 0.2182(12) 0.0205(6) 0.7049(13) 0.0843(11) Uani 1 1 d . . . C52 C 0.2672(11) 0.0735(6) 0.7597(12) 0.0843(11) Uani 1 1 d . . . H52A H 0.3180 0.0925 0.7480 0.101 Uiso 1 1 calc R . . C53 C 0.2457(10) 0.0995(6) 0.8293(11) 0.0843(11) Uani 1 1 d . . . C54 C 0.1091(18) -0.0574(9) 0.6819(19) 0.131(2) Uani 1 1 d . . . H54 H 0.0608 -0.0766 0.7022 0.158 Uiso 1 1 calc R . . C55 C 0.0624(18) -0.0574(9) 0.5646(19) 0.131(2) Uani 1 1 d . . . C56 C 0.1824(17) -0.0674(9) 0.5990(19) 0.131(2) Uani 1 1 d . . . H56 H 0.1949 -0.0904 0.5494 0.158 Uiso 1 1 calc R . . C57 C 0.2310(18) -0.0083(9) 0.6237(18) 0.131(2) Uani 1 1 d . . . H57A H 0.2008 0.0188 0.5648 0.158 Uiso 1 1 calc R . . H57B H 0.3045 -0.0131 0.6445 0.158 Uiso 1 1 calc R . . C58 C 0.1859(17) -0.1075(9) 0.6785(18) 0.131(2) Uani 1 1 d . . . H58A H 0.2531 -0.1093 0.7387 0.158 Uiso 1 1 calc R . . H58B H 0.1562 -0.1491 0.6567 0.158 Uiso 1 1 calc R . . C59 C 0.0157(17) 0.0088(9) 0.5108(18) 0.131(2) Uani 1 1 d . . . H59A H 0.0038 0.0075 0.4425 0.197 Uiso 1 1 calc R . . H59B H 0.0641 0.0419 0.5467 0.197 Uiso 1 1 calc R . . H59C H -0.0490 0.0167 0.5112 0.197 Uiso 1 1 calc R . . C60 C -0.0038(18) -0.1106(8) 0.5046(19) 0.131(2) Uani 1 1 d . . . H60A H -0.0468 -0.1244 0.5333 0.197 Uiso 1 1 calc R . . H60B H 0.0396 -0.1449 0.5053 0.197 Uiso 1 1 calc R . . H60C H -0.0472 -0.0971 0.4363 0.197 Uiso 1 1 calc R . . C61 C 0.2808(12) 0.1570(6) 0.8745(13) 0.0843(11) Uani 1 1 d . . . C62 C 0.3534(11) 0.1950(6) 0.8738(12) 0.0843(11) Uani 1 1 d . . . H62A H 0.3856 0.1838 0.8355 0.101 Uiso 1 1 calc R . . C63 C 0.3820(12) 0.2503(6) 0.9283(13) 0.0843(11) Uani 1 1 d . . . C64 C 0.3390(12) 0.2678(6) 0.9757(13) 0.0843(11) Uani 1 1 d . . . C65 C 0.2666(11) 0.2299(6) 0.9818(12) 0.0843(11) Uani 1 1 d . . . H65A H 0.2370 0.2430 1.0215 0.101 Uiso 1 1 calc R . . C66 C 0.3638(16) 0.3318(10) 1.0298(17) 0.131(2) Uani 1 1 d . . . H66 H 0.3383 0.3448 1.0766 0.158 Uiso 1 1 calc R . . C67 C 0.4835(19) 0.3425(9) 1.051(2) 0.131(2) Uani 1 1 d . . . C68 C 0.4724(18) 0.3507(10) 0.9659(18) 0.131(2) Uani 1 1 d . . . H68 H 0.5188 0.3825 0.9617 0.158 Uiso 1 1 calc R . . C69 C 0.4565(18) 0.2906(9) 0.8991(19) 0.131(2) Uani 1 1 d . . . H69A H 0.5217 0.2690 0.9176 0.158 Uiso 1 1 calc R . . H69B H 0.4229 0.3008 0.8278 0.158 Uiso 1 1 calc R . . C70 C 0.3495(17) 0.3761(9) 0.9278(18) 0.131(2) Uani 1 1 d . . . H70A H 0.2979 0.3603 0.8626 0.158 Uiso 1 1 calc R . . H70B H 0.3427 0.4211 0.9343 0.158 Uiso 1 1 calc R . . C71 C 0.5164(17) 0.3978(9) 1.1222(18) 0.131(2) Uani 1 1 d . . . H71A H 0.5827 0.4131 1.1327 0.197 Uiso 1 1 calc R . . H71B H 0.5217 0.3847 1.1855 0.197 Uiso 1 1 calc R . . H71C H 0.4656 0.4308 1.0939 0.197 Uiso 1 1 calc R . . C72 C 0.5525(17) 0.2856(9) 1.1021(18) 0.131(2) Uani 1 1 d . . . H72A H 0.5227 0.2486 1.0619 0.197 Uiso 1 1 calc R . . H72B H 0.5575 0.2799 1.1675 0.197 Uiso 1 1 calc R . . H72C H 0.6207 0.2927 1.1092 0.197 Uiso 1 1 calc R . . N1 N 0.0041(9) 0.1348(4) 0.8387(8) 0.0710(10) Uani 1 1 d . . . N2 N 0.0533(9) 0.0443(5) 0.9643(8) 0.0710(10) Uani 1 1 d . . . N3 N 0.1310(11) 0.1540(6) 1.0632(9) 0.0915(13) Uani 1 1 d . . . N4 N 0.2824(11) 0.0861(5) 1.0812(9) 0.0915(13) Uani 1 1 d . . . N5 N 0.1721(9) 0.0710(5) 0.8508(10) 0.0843(11) Uani 1 1 d . . . N6 N 0.2367(9) 0.1756(5) 0.9339(10) 0.0843(11) Uani 1 1 d . . . Os1 Os 0.14633(4) 0.11151(4) 0.95394(3) 0.06971(18) 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 C1 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C2 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C3 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C4 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C5 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C6 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C7 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C8 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C9 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C10 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C11 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C12 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C13 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C14 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C15 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C16 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C17 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) C18 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C19 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C20 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C21 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C22 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C23 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C24 0.103(3) 0.087(3) 0.099(3) 0.007(2) 0.058(3) 0.002(2) C25 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C26 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C27 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C28 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C29 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C30 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C31 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C32 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C33 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C34 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C35 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C36 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C37 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C38 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C39 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C40 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C41 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) C42 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C43 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C44 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C45 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C46 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C47 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C48 0.150(5) 0.117(4) 0.124(4) -0.011(3) 0.066(4) -0.011(4) C49 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C50 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C51 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C52 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C53 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C54 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C55 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C56 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C57 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C58 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C59 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C60 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C61 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C62 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C63 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C64 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C65 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) C66 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C67 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C68 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C69 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C70 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C71 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) C72 0.136(5) 0.094(4) 0.169(6) -0.005(4) 0.077(5) -0.002(3) N1 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) N2 0.084(3) 0.066(2) 0.073(2) -0.0019(17) 0.045(2) -0.0043(19) N3 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) N4 0.113(4) 0.079(3) 0.075(3) -0.003(2) 0.039(3) -0.019(2) N5 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) N6 0.079(3) 0.066(2) 0.115(3) 0.007(2) 0.053(3) -0.005(2) Os1 0.0943(3) 0.0537(2) 0.0635(2) 0.0001(5) 0.0394(2) -0.0124(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.321(15) . ? C1 C2 1.366(19) . ? C1 H1A 0.9500 . ? C2 C3 1.437(18) . ? C2 C6 1.51(2) . ? C3 C4 1.364(17) . ? C3 C9 1.55(2) . ? C4 C5 1.331(16) . ? C4 H4A 0.9500 . ? C5 N1 1.370(14) . ? C5 C13 1.458(17) . ? C6 C10 1.55(2) . ? C6 C7 1.55(2) . ? C6 H6 1.0000 . ? C7 C12 1.53(2) . ? C7 C11 1.55(2) . ? C7 C8 1.65(2) . ? C8 C9 1.46(2) . ? C8 C10 1.57(2) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.292(17) . ? C13 C14 1.447(18) . ? C14 C15 1.420(18) . ? C14 H14A 0.9500 . ? C15 C16 1.298(19) . ? C15 C21 1.55(2) . ? C16 C17 1.347(17) . ? C16 C18 1.53(2) . ? C17 N2 1.339(16) . ? C17 H17A 0.9500 . ? C18 C22 1.59(2) . ? C18 C19 1.61(2) . ? C18 H18 1.0000 . ? C19 C20 1.36(2) . ? C19 C23 1.63(2) . ? C19 C24 1.63(2) . ? C20 C22 1.35(2) . ? C20 C21 1.67(2) . ? C20 H20 1.0000 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.35(2) . ? C25 C26 1.49(2) . ? C25 H25A 0.9500 . ? C26 C27 1.30(2) . ? C26 C30 1.41(3) . ? C27 C28 1.40(2) . ? C27 C33 1.51(2) . ? C28 C29 1.48(2) . ? C28 H28A 0.9500 . ? C29 C37 1.37(2) . ? C29 N3 1.38(2) . ? C30 C34 1.60(3) . ? C30 C31 1.71(3) . ? C30 C32 2.04(3) . ? C30 H30 1.0000 . ? C31 C35 1.47(3) . ? C31 C36 1.50(3) . ? C31 C32 1.64(3) . ? C32 C33 1.43(3) . ? C32 C34 1.48(3) . ? C32 H32 1.0000 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N4 1.383(18) . ? C37 C38 1.406(19) . ? C38 C39 1.39(2) . ? C38 H38A 0.9500 . ? C39 C40 1.33(2) . ? C39 C45 1.51(3) . ? C40 C41 1.39(2) . ? C40 C42 1.46(3) . ? C41 N4 1.30(2) . ? C41 H41A 0.9500 . ? C42 C43 1.51(3) . ? C42 C46 1.58(3) . ? C42 H42 1.0000 . ? C43 C48 1.53(4) . ? C43 C47 1.59(3) . ? C43 C44 1.61(3) . ? C44 C45 1.41(3) . ? C44 C46 1.67(3) . ? C44 H44 1.0000 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N5 1.337(18) . ? C49 C50 1.40(2) . ? C49 H49A 0.9500 . ? C50 C54 1.23(2) . ? C50 C51 1.439(19) . ? C51 C52 1.41(2) . ? C51 C57 1.49(3) . ? C52 C53 1.374(19) . ? C52 H52A 0.9500 . ? C53 C61 1.40(2) . ? C53 N5 1.426(16) . ? C54 C55 1.60(3) . ? C54 C58 1.59(3) . ? C54 H54 1.0000 . ? C55 C60 1.51(3) . ? C55 C56 1.62(3) . ? C55 C59 1.64(3) . ? C56 C57 1.43(3) . ? C56 C58 1.48(3) . ? C56 H56 1.0000 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.363(19) . ? C61 N6 1.412(19) . ? C62 C63 1.41(2) . ? C62 H62A 0.9500 . ? C63 C64 1.24(2) . ? C63 C69 1.63(2) . ? C64 C65 1.394(19) . ? C64 C66 1.57(3) . ? C65 N6 1.347(18) . ? C65 H65A 0.9500 . ? C66 C67 1.67(3) . ? C66 C70 1.76(3) . ? C66 H66 1.0000 . ? C67 C68 1.24(3) . ? C67 C71 1.54(3) . ? C67 C72 1.56(3) . ? C68 C69 1.60(3) . ? C68 C70 1.73(3) . ? C68 H68 1.0000 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N1 Os1 2.079(11) . ? N2 Os1 2.066(10) . ? N3 Os1 2.020(13) . ? N4 Os1 2.115(13) . ? N5 Os1 2.002(13) . ? N6 Os1 2.056(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.0(13) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 117.1(12) . . ? C1 C2 C6 125.3(13) . . ? C3 C2 C6 117.6(13) . . ? C4 C3 C2 118.6(13) . . ? C4 C3 C9 126.0(12) . . ? C2 C3 C9 115.1(11) . . ? C5 C4 C3 120.1(12) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 122.3(11) . . ? C4 C5 C13 124.7(11) . . ? N1 C5 C13 112.9(11) . . ? C2 C6 C10 106.1(12) . . ? C2 C6 C7 108.7(13) . . ? C10 C6 C7 88.9(13) . . ? C2 C6 H6 116.5 . . ? C10 C6 H6 116.5 . . ? C7 C6 H6 116.5 . . ? C12 C7 C6 116.8(15) . . ? C12 C7 C11 111.1(13) . . ? C6 C7 C11 112.3(13) . . ? C12 C7 C8 117.7(13) . . ? C6 C7 C8 85.0(12) . . ? C11 C7 C8 111.6(13) . . ? C9 C8 C10 110.3(14) . . ? C9 C8 C7 109.8(13) . . ? C10 C8 C7 84.8(12) . . ? C9 C8 H8 115.9 . . ? C10 C8 H8 115.9 . . ? C7 C8 H8 115.9 . . ? C8 C9 C3 113.3(14) . . ? C8 C9 H9A 108.9 . . ? C3 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C3 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C6 C10 C8 88.1(12) . . ? C6 C10 H10A 114.0 . . ? C8 C10 H10A 114.0 . . ? C6 C10 H10B 114.0 . . ? C8 C10 H10B 114.0 . . ? H10A C10 H10B 111.2 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 121.5(12) . . ? N2 C13 C5 117.8(12) . . ? C14 C13 C5 120.5(13) . . ? C15 C14 C13 116.1(13) . . ? C15 C14 H14A 121.9 . . ? C13 C14 H14A 121.9 . . ? C16 C15 C14 119.6(12) . . ? C16 C15 C21 124.6(13) . . ? C14 C15 C21 115.8(13) . . ? C15 C16 C17 120.5(13) . . ? C15 C16 C18 116.0(12) . . ? C17 C16 C18 123.5(14) . . ? N2 C17 C16 123.8(14) . . ? N2 C17 H17A 118.1 . . ? C16 C17 H17A 118.1 . . ? C16 C18 C22 104.2(13) . . ? C16 C18 C19 105.5(13) . . ? C22 C18 C19 81.8(11) . . ? C16 C18 H18 119.5 . . ? C22 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 83.7(13) . . ? C20 C19 C23 112.4(15) . . ? C18 C19 C23 100.8(13) . . ? C20 C19 C24 135.2(17) . . ? C18 C19 C24 116.4(13) . . ? C23 C19 C24 102.9(13) . . ? C22 C20 C19 101.4(16) . . ? C22 C20 C21 108.1(13) . . ? C19 C20 C21 109.6(14) . . ? C22 C20 H20 112.4 . . ? C19 C20 H20 112.4 . . ? C21 C20 H20 112.4 . . ? C15 C21 C20 100.5(13) . . ? C15 C21 H21A 111.7 . . ? C20 C21 H21A 111.7 . . ? C15 C21 H21B 111.7 . . ? C20 C21 H21B 111.7 . . ? H21A C21 H21B 109.4 . . ? C20 C22 C18 84.9(13) . . ? C20 C22 H22A 114.5 . . ? C18 C22 H22A 114.5 . . ? C20 C22 H22B 114.5 . . ? C18 C22 H22B 114.5 . . ? H22A C22 H22B 111.6 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 122.1(15) . . ? N3 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? C27 C26 C30 124.9(17) . . ? C27 C26 C25 115.7(17) . . ? C30 C26 C25 119.0(17) . . ? C26 C27 C28 128.4(16) . . ? C26 C27 C33 118.2(18) . . ? C28 C27 C33 112.6(16) . . ? C27 C28 C29 112.0(15) . . ? C27 C28 H28A 124.0 . . ? C29 C28 H28A 124.0 . . ? C37 C29 N3 114.1(14) . . ? C37 C29 C28 122.2(15) . . ? N3 C29 C28 123.7(16) . . ? C26 C30 C34 100.7(18) . . ? C26 C30 C31 108.7(18) . . ? C34 C30 C31 87.6(16) . . ? C26 C30 C32 87.2(16) . . ? C34 C30 C32 46.1(11) . . ? C31 C30 C32 50.8(12) . . ? C26 C30 H30 118.2 . . ? C34 C30 H30 118.2 . . ? C31 C30 H30 118.2 . . ? C32 C30 H30 154.1 . . ? C35 C31 C36 116(2) . . ? C35 C31 C32 122.6(19) . . ? C36 C31 C32 114(2) . . ? C35 C31 C30 107.6(19) . . ? C36 C31 C30 114.1(18) . . ? C32 C31 C30 75.0(15) . . ? C33 C32 C34 112(2) . . ? C33 C32 C31 125(2) . . ? C34 C32 C31 95(2) . . ? C33 C32 C30 107.8(17) . . ? C34 C32 C30 51.1(13) . . ? C31 C32 C30 54.2(13) . . ? C33 C32 H32 108.0 . . ? C34 C32 H32 108.0 . . ? C31 C32 H32 108.0 . . ? C30 C32 H32 143.6 . . ? C32 C33 C27 101.3(19) . . ? C32 C33 H33A 111.5 . . ? C27 C33 H33A 111.5 . . ? C32 C33 H33B 111.5 . . ? C27 C33 H33B 111.5 . . ? H33A C33 H33B 109.3 . . ? C32 C34 C30 82.8(17) . . ? C32 C34 H34A 114.8 . . ? C30 C34 H34A 114.8 . . ? C32 C34 H34B 114.8 . . ? C30 C34 H34B 114.8 . . ? H34A C34 H34B 111.9 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C29 C37 N4 118.2(13) . . ? C29 C37 C38 127.1(14) . . ? N4 C37 C38 113.4(16) . . ? C39 C38 C37 124.2(14) . . ? C39 C38 H38A 117.9 . . ? C37 C38 H38A 117.9 . . ? C40 C39 C38 114.5(16) . . ? C40 C39 C45 125.2(18) . . ? C38 C39 C45 120.0(14) . . ? C39 C40 C41 124.7(18) . . ? C39 C40 C42 115.2(17) . . ? C41 C40 C42 120.0(16) . . ? N4 C41 C40 117.6(16) . . ? N4 C41 H41A 121.2 . . ? C40 C41 H41A 121.2 . . ? C40 C42 C43 109.0(17) . . ? C40 C42 C46 109.4(18) . . ? C43 C42 C46 85.0(17) . . ? C40 C42 H42 116.4 . . ? C43 C42 H42 116.4 . . ? C46 C42 H42 116.4 . . ? C42 C43 C48 120(2) . . ? C42 C43 C47 116.6(18) . . ? C48 C43 C47 108.5(17) . . ? C42 C43 C44 90.2(17) . . ? C48 C43 C44 111.0(17) . . ? C47 C43 C44 109.1(19) . . ? C45 C44 C43 114(2) . . ? C45 C44 C46 114(2) . . ? C43 C44 C46 79.4(15) . . ? C45 C44 H44 114.9 . . ? C43 C44 H44 114.9 . . ? C46 C44 H44 114.9 . . ? C44 C45 C39 106.7(19) . . ? C44 C45 H45A 110.4 . . ? C39 C45 H45A 110.4 . . ? C44 C45 H45B 110.4 . . ? C39 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C42 C46 C44 85.6(16) . . ? C42 C46 H46A 114.4 . . ? C44 C46 H46A 114.4 . . ? C42 C46 H46B 114.4 . . ? C44 C46 H46B 114.4 . . ? H46A C46 H46B 111.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C50 127.6(13) . . ? N5 C49 H49A 116.2 . . ? C50 C49 H49A 116.2 . . ? C54 C50 C49 129.4(17) . . ? C54 C50 C51 114.8(18) . . ? C49 C50 C51 115.9(14) . . ? C52 C51 C50 117.1(14) . . ? C52 C51 C57 127.6(14) . . ? C50 C51 C57 115.3(15) . . ? C53 C52 C51 123.7(13) . . ? C53 C52 H52A 118.1 . . ? C51 C52 H52A 118.1 . . ? C52 C53 C61 125.5(12) . . ? C52 C53 N5 119.5(13) . . ? C61 C53 N5 114.6(12) . . ? C50 C54 C55 120(2) . . ? C50 C54 C58 117(2) . . ? C55 C54 C58 84.1(16) . . ? C50 C54 H54 111.1 . . ? C55 C54 H54 111.1 . . ? C58 C54 H54 111.1 . . ? C60 C55 C54 119.8(19) . . ? C60 C55 C56 113.4(17) . . ? C54 C55 C56 79.0(17) . . ? C60 C55 C59 111(2) . . ? C54 C55 C59 115.0(17) . . ? C56 C55 C59 115.0(17) . . ? C57 C56 C58 119(2) . . ? C57 C56 C55 108.0(17) . . ? C58 C56 C55 87.1(16) . . ? C57 C56 H56 113.1 . . ? C58 C56 H56 113.1 . . ? C55 C56 H56 113.1 . . ? C56 C57 C51 110.4(18) . . ? C56 C57 H57A 109.6 . . ? C51 C57 H57A 109.6 . . ? C56 C57 H57B 109.6 . . ? C51 C57 H57B 109.6 . . ? H57A C57 H57B 108.1 . . ? C56 C58 C54 83.3(16) . . ? C56 C58 H58A 114.8 . . ? C54 C58 H58A 114.8 . . ? C56 C58 H58B 114.8 . . ? C54 C58 H58B 114.8 . . ? H58A C58 H58B 111.8 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C53 130.0(14) . . ? C62 C61 N6 116.6(14) . . ? C53 C61 N6 113.3(12) . . ? C61 C62 C63 121.7(14) . . ? C61 C62 H62A 119.1 . . ? C63 C62 H62A 119.1 . . ? C64 C63 C62 121.2(14) . . ? C64 C63 C69 127.3(14) . . ? C62 C63 C69 110.1(14) . . ? C63 C64 C65 119.4(15) . . ? C63 C64 C66 121.9(14) . . ? C65 C64 C66 118.7(15) . . ? N6 C65 C64 122.9(14) . . ? N6 C65 H65A 118.5 . . ? C64 C65 H65A 118.5 . . ? C64 C66 C67 100.7(15) . . ? C64 C66 C70 96.3(15) . . ? C67 C66 C70 76.3(15) . . ? C64 C66 H66 123.9 . . ? C67 C66 H66 123.9 . . ? C70 C66 H66 123.9 . . ? C68 C67 C71 118(2) . . ? C68 C67 C72 112(2) . . ? C71 C67 C72 110(2) . . ? C68 C67 C66 103(2) . . ? C71 C67 C66 101.1(17) . . ? C72 C67 C66 112.0(17) . . ? C67 C68 C69 117(2) . . ? C67 C68 C70 89.7(19) . . ? C69 C68 C70 103.4(17) . . ? C67 C68 H68 114.4 . . ? C69 C68 H68 114.4 . . ? C70 C68 H68 114.4 . . ? C68 C69 C63 99.8(16) . . ? C68 C69 H69A 111.8 . . ? C63 C69 H69A 111.8 . . ? C68 C69 H69B 111.8 . . ? C63 C69 H69B 111.8 . . ? H69A C69 H69B 109.5 . . ? C68 C70 C66 82.1(15) . . ? C68 C70 H70A 114.9 . . ? C66 C70 H70A 114.9 . . ? C68 C70 H70B 114.9 . . ? C66 C70 H70B 114.9 . . ? H70A C70 H70B 112.0 . . ? C67 C71 H71A 109.5 . . ? C67 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C67 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C67 C72 H72A 109.5 . . ? C67 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C67 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C1 N1 C5 118.7(11) . . ? C1 N1 Os1 125.7(9) . . ? C5 N1 Os1 115.3(8) . . ? C13 N2 C17 118.4(12) . . ? C13 N2 Os1 115.9(9) . . ? C17 N2 Os1 125.5(10) . . ? C25 N3 C29 117.4(14) . . ? C25 N3 Os1 125.3(11) . . ? C29 N3 Os1 117.3(12) . . ? C41 N4 C37 124.5(14) . . ? C41 N4 Os1 122.7(11) . . ? C37 N4 Os1 111.3(11) . . ? C49 N5 C53 116.2(12) . . ? C49 N5 Os1 126.9(10) . . ? C53 N5 Os1 116.8(9) . . ? C65 N6 C61 117.9(12) . . ? C65 N6 Os1 125.3(10) . . ? C61 N6 Os1 116.3(9) . . ? N5 Os1 N3 175.9(6) . . ? N5 Os1 N6 78.0(5) . . ? N3 Os1 N6 99.1(5) . . ? N5 Os1 N2 98.1(4) . . ? N3 Os1 N2 85.0(4) . . ? N6 Os1 N2 175.8(5) . . ? N5 Os1 N1 86.1(5) . . ? N3 Os1 N1 97.3(5) . . ? N6 Os1 N1 100.6(5) . . ? N2 Os1 N1 77.7(4) . . ? N5 Os1 N4 99.1(5) . . ? N3 Os1 N4 77.7(5) . . ? N6 Os1 N4 84.6(5) . . ? N2 Os1 N4 97.4(5) . . ? N1 Os1 N4 173.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.9(19) . . . . ? N1 C1 C2 C6 -178.4(12) . . . . ? C1 C2 C3 C4 -4.8(17) . . . . ? C6 C2 C3 C4 176.4(12) . . . . ? C1 C2 C3 C9 -179.5(12) . . . . ? C6 C2 C3 C9 1.7(17) . . . . ? C2 C3 C4 C5 5.0(17) . . . . ? C9 C3 C4 C5 179.0(12) . . . . ? C3 C4 C5 N1 -3.2(17) . . . . ? C3 C4 C5 C13 -177.8(11) . . . . ? C1 C2 C6 C10 -132.8(14) . . . . ? C3 C2 C6 C10 46.0(16) . . . . ? C1 C2 C6 C7 132.7(14) . . . . ? C3 C2 C6 C7 -48.5(16) . . . . ? C2 C6 C7 C12 -38.7(18) . . . . ? C10 C6 C7 C12 -145.4(13) . . . . ? C2 C6 C7 C11 -168.8(13) . . . . ? C10 C6 C7 C11 84.5(14) . . . . ? C2 C6 C7 C8 79.9(13) . . . . ? C10 C6 C7 C8 -26.8(11) . . . . ? C12 C7 C8 C9 34(2) . . . . ? C6 C7 C8 C9 -83.3(15) . . . . ? C11 C7 C8 C9 164.7(14) . . . . ? C12 C7 C8 C10 144.2(16) . . . . ? C6 C7 C8 C10 26.5(11) . . . . ? C11 C7 C8 C10 -85.6(15) . . . . ? C10 C8 C9 C3 -43.1(17) . . . . ? C7 C8 C9 C3 48.7(18) . . . . ? C4 C3 C9 C8 -177.5(13) . . . . ? C2 C3 C9 C8 -3.2(18) . . . . ? C2 C6 C10 C8 -81.0(13) . . . . ? C7 C6 C10 C8 28.2(11) . . . . ? C9 C8 C10 C6 82.8(14) . . . . ? C7 C8 C10 C6 -26.5(11) . . . . ? C4 C5 C13 N2 168.4(12) . . . . ? N1 C5 C13 N2 -6.7(16) . . . . ? C4 C5 C13 C14 -7.0(18) . . . . ? N1 C5 C13 C14 177.9(10) . . . . ? N2 C13 C14 C15 1.9(18) . . . . ? C5 C13 C14 C15 177.2(11) . . . . ? C13 C14 C15 C16 1.5(18) . . . . ? C13 C14 C15 C21 -179.5(11) . . . . ? C14 C15 C16 C17 -4.2(19) . . . . ? C21 C15 C16 C17 176.8(12) . . . . ? C14 C15 C16 C18 178.2(11) . . . . ? C21 C15 C16 C18 -0.8(19) . . . . ? C15 C16 C17 N2 4(2) . . . . ? C18 C16 C17 N2 -178.7(12) . . . . ? C15 C16 C18 C22 43.0(16) . . . . ? C17 C16 C18 C22 -134.5(13) . . . . ? C15 C16 C18 C19 -42.2(17) . . . . ? C17 C16 C18 C19 140.3(14) . . . . ? C16 C18 C19 C20 83.1(14) . . . . ? C22 C18 C19 C20 -19.4(12) . . . . ? C16 C18 C19 C23 -165.2(12) . . . . ? C22 C18 C19 C23 92.3(13) . . . . ? C16 C18 C19 C24 -54.9(19) . . . . ? C22 C18 C19 C24 -157.4(15) . . . . ? C18 C19 C20 C22 23.3(14) . . . . ? C23 C19 C20 C22 -75.9(17) . . . . ? C24 C19 C20 C22 144.9(18) . . . . ? C18 C19 C20 C21 -90.9(13) . . . . ? C23 C19 C20 C21 170.0(12) . . . . ? C24 C19 C20 C21 31(3) . . . . ? C16 C15 C21 C20 0.6(18) . . . . ? C14 C15 C21 C20 -178.3(11) . . . . ? C22 C20 C21 C15 -54.6(16) . . . . ? C19 C20 C21 C15 55.1(16) . . . . ? C19 C20 C22 C18 -23.6(14) . . . . ? C21 C20 C22 C18 91.6(14) . . . . ? C16 C18 C22 C20 -84.5(14) . . . . ? C19 C18 C22 C20 19.5(12) . . . . ? N3 C25 C26 C27 9(2) . . . . ? N3 C25 C26 C30 -177.5(15) . . . . ? C30 C26 C27 C28 178.3(17) . . . . ? C25 C26 C27 C28 -8(2) . . . . ? C30 C26 C27 C33 9(3) . . . . ? C25 C26 C27 C33 -177.3(15) . . . . ? C26 C27 C28 C29 6(2) . . . . ? C33 C27 C28 C29 175.7(14) . . . . ? C27 C28 C29 C37 174.8(15) . . . . ? C27 C28 C29 N3 -4(2) . . . . ? C27 C26 C30 C34 37(2) . . . . ? C25 C26 C30 C34 -135.9(16) . . . . ? C27 C26 C30 C31 -54(2) . . . . ? C25 C26 C30 C31 133.0(16) . . . . ? C27 C26 C30 C32 -7(2) . . . . ? C25 C26 C30 C32 179.8(14) . . . . ? C26 C30 C31 C35 -170.0(17) . . . . ? C34 C30 C31 C35 90(2) . . . . ? C32 C30 C31 C35 120(2) . . . . ? C26 C30 C31 C36 -40(3) . . . . ? C34 C30 C31 C36 -140(2) . . . . ? C32 C30 C31 C36 -110(2) . . . . ? C26 C30 C31 C32 70.0(18) . . . . ? C34 C30 C31 C32 -30.6(16) . . . . ? C35 C31 C32 C33 171(2) . . . . ? C36 C31 C32 C33 22(3) . . . . ? C30 C31 C32 C33 -88(2) . . . . ? C35 C31 C32 C34 -68(3) . . . . ? C36 C31 C32 C34 143.6(19) . . . . ? C30 C31 C32 C34 33.4(16) . . . . ? C35 C31 C32 C30 -102(2) . . . . ? C36 C31 C32 C30 110(2) . . . . ? C26 C30 C32 C33 3.3(19) . . . . ? C34 C30 C32 C33 -105(2) . . . . ? C31 C30 C32 C33 120(2) . . . . ? C26 C30 C32 C34 108(2) . . . . ? C31 C30 C32 C34 -135(2) . . . . ? C26 C30 C32 C31 -117.0(18) . . . . ? C34 C30 C32 C31 135(2) . . . . ? C34 C32 C33 C27 -54(2) . . . . ? C31 C32 C33 C27 59(3) . . . . ? C30 C32 C33 C27 0(2) . . . . ? C26 C27 C33 C32 -5(2) . . . . ? C28 C27 C33 C32 -175.4(16) . . . . ? C33 C32 C34 C30 95(2) . . . . ? C31 C32 C34 C30 -35.0(17) . . . . ? C26 C30 C34 C32 -75.4(19) . . . . ? C31 C30 C34 C32 33.1(17) . . . . ? N3 C29 C37 N4 -12(2) . . . . ? C28 C29 C37 N4 169.4(13) . . . . ? N3 C29 C37 C38 -177.6(16) . . . . ? C28 C29 C37 C38 3(3) . . . . ? C29 C37 C38 C39 177.1(17) . . . . ? N4 C37 C38 C39 11(2) . . . . ? C37 C38 C39 C40 -4(2) . . . . ? C37 C38 C39 C45 170.7(17) . . . . ? C38 C39 C40 C41 -3(2) . . . . ? C45 C39 C40 C41 -177.3(16) . . . . ? C38 C39 C40 C42 179.9(15) . . . . ? C45 C39 C40 C42 6(2) . . . . ? C39 C40 C41 N4 2(2) . . . . ? C42 C40 C41 N4 179.1(15) . . . . ? C39 C40 C42 C43 -48(2) . . . . ? C41 C40 C42 C43 135.4(18) . . . . ? C39 C40 C42 C46 44(2) . . . . ? C41 C40 C42 C46 -133.3(17) . . . . ? C40 C42 C43 C48 -40(3) . . . . ? C46 C42 C43 C48 -148.6(19) . . . . ? C40 C42 C43 C47 -173.6(17) . . . . ? C46 C42 C43 C47 78(2) . . . . ? C40 C42 C43 C44 74.7(19) . . . . ? C46 C42 C43 C44 -34.1(16) . . . . ? C42 C43 C44 C45 -79(2) . . . . ? C48 C43 C44 C45 43(3) . . . . ? C47 C43 C44 C45 162.7(19) . . . . ? C42 C43 C44 C46 32.7(16) . . . . ? C48 C43 C44 C46 155(2) . . . . ? C47 C43 C44 C46 -85.7(18) . . . . ? C43 C44 C45 C39 45(2) . . . . ? C46 C44 C45 C39 -44(2) . . . . ? C40 C39 C45 C44 -5(3) . . . . ? C38 C39 C45 C44 -179.0(16) . . . . ? C40 C42 C46 C44 -75.6(18) . . . . ? C43 C42 C46 C44 32.8(16) . . . . ? C45 C44 C46 C42 81(2) . . . . ? C43 C44 C46 C42 -31.1(16) . . . . ? N5 C49 C50 C54 179(2) . . . . ? N5 C49 C50 C51 0(2) . . . . ? C54 C50 C51 C52 -176.7(17) . . . . ? C49 C50 C51 C52 3(2) . . . . ? C54 C50 C51 C57 4(2) . . . . ? C49 C50 C51 C57 -176.4(16) . . . . ? C50 C51 C52 C53 -4(2) . . . . ? C57 C51 C52 C53 175.4(17) . . . . ? C51 C52 C53 C61 -169.7(15) . . . . ? C51 C52 C53 N5 2(2) . . . . ? C49 C50 C54 C55 131(2) . . . . ? C51 C50 C54 C55 -49(3) . . . . ? C49 C50 C54 C58 -130(2) . . . . ? C51 C50 C54 C58 50(3) . . . . ? C50 C54 C55 C60 -166(2) . . . . ? C58 C54 C55 C60 76(2) . . . . ? C50 C54 C55 C56 83(2) . . . . ? C58 C54 C55 C56 -35.3(13) . . . . ? C50 C54 C55 C59 -30(3) . . . . ? C58 C54 C55 C59 -147.8(18) . . . . ? C60 C55 C56 C57 160(2) . . . . ? C54 C55 C56 C57 -82(2) . . . . ? C59 C55 C56 C57 31(3) . . . . ? C60 C55 C56 C58 -80(2) . . . . ? C54 C55 C56 C58 38.3(14) . . . . ? C59 C55 C56 C58 151.0(19) . . . . ? C58 C56 C57 C51 -37(3) . . . . ? C55 C56 C57 C51 60(2) . . . . ? C52 C51 C57 C56 169.5(17) . . . . ? C50 C51 C57 C56 -11(3) . . . . ? C57 C56 C58 C54 71(2) . . . . ? C55 C56 C58 C54 -37.8(15) . . . . ? C50 C54 C58 C56 -82(2) . . . . ? C55 C54 C58 C56 38.7(15) . . . . ? C52 C53 C61 C62 -11(3) . . . . ? N5 C53 C61 C62 176.6(16) . . . . ? C52 C53 C61 N6 172.5(14) . . . . ? N5 C53 C61 N6 0.5(19) . . . . ? C53 C61 C62 C63 -176.9(16) . . . . ? N6 C61 C62 C63 -1(2) . . . . ? C61 C62 C63 C64 -3(3) . . . . ? C61 C62 C63 C69 -171.1(16) . . . . ? C62 C63 C64 C65 5(3) . . . . ? C69 C63 C64 C65 170.9(17) . . . . ? C62 C63 C64 C66 -175.1(16) . . . . ? C69 C63 C64 C66 -9(3) . . . . ? C63 C64 C65 N6 -3(3) . . . . ? C66 C64 C65 N6 176.7(15) . . . . ? C63 C64 C66 C67 -27(2) . . . . ? C65 C64 C66 C67 153.2(17) . . . . ? C63 C64 C66 C70 51(2) . . . . ? C65 C64 C66 C70 -129.7(16) . . . . ? C64 C66 C67 C68 69(2) . . . . ? C70 C66 C67 C68 -25.5(18) . . . . ? C64 C66 C67 C71 -168.7(17) . . . . ? C70 C66 C67 C71 97.3(17) . . . . ? C64 C66 C67 C72 -52(2) . . . . ? C70 C66 C67 C72 -146(2) . . . . ? C71 C67 C68 C69 170.1(19) . . . . ? C72 C67 C68 C69 41(3) . . . . ? C66 C67 C68 C69 -80(2) . . . . ? C71 C67 C68 C70 -85(2) . . . . ? C72 C67 C68 C70 145.5(17) . . . . ? C66 C67 C68 C70 25.2(17) . . . . ? C67 C68 C69 C63 40(3) . . . . ? C70 C68 C69 C63 -57(2) . . . . ? C64 C63 C69 C68 10(3) . . . . ? C62 C63 C69 C68 177.4(16) . . . . ? C67 C68 C70 C66 -23.5(18) . . . . ? C69 C68 C70 C66 94.7(18) . . . . ? C64 C66 C70 C68 -81.7(14) . . . . ? C67 C66 C70 C68 17.8(13) . . . . ? C2 C1 N1 C5 -1.0(17) . . . . ? C2 C1 N1 Os1 171.7(9) . . . . ? C4 C5 N1 C1 1.1(16) . . . . ? C13 C5 N1 C1 176.3(11) . . . . ? C4 C5 N1 Os1 -172.4(9) . . . . ? C13 C5 N1 Os1 2.8(12) . . . . ? C14 C13 N2 C17 -2.3(18) . . . . ? C5 C13 N2 C17 -177.8(11) . . . . ? C14 C13 N2 Os1 -177.4(9) . . . . ? C5 C13 N2 Os1 7.2(15) . . . . ? C16 C17 N2 C13 -0.5(19) . . . . ? C16 C17 N2 Os1 174.0(9) . . . . ? C26 C25 N3 C29 -7(2) . . . . ? C26 C25 N3 Os1 175.9(10) . . . . ? C37 C29 N3 C25 -173.8(14) . . . . ? C28 C29 N3 C25 5(2) . . . . ? C37 C29 N3 Os1 3.4(18) . . . . ? C28 C29 N3 Os1 -177.7(11) . . . . ? C40 C41 N4 C37 6(2) . . . . ? C40 C41 N4 Os1 171.1(10) . . . . ? C29 C37 N4 C41 -179.5(15) . . . . ? C38 C37 N4 C41 -12(2) . . . . ? C29 C37 N4 Os1 13.8(18) . . . . ? C38 C37 N4 Os1 -178.3(11) . . . . ? C50 C49 N5 C53 -2(2) . . . . ? C50 C49 N5 Os1 179.9(12) . . . . ? C52 C53 N5 C49 1(2) . . . . ? C61 C53 N5 C49 173.5(14) . . . . ? C52 C53 N5 Os1 179.5(11) . . . . ? C61 C53 N5 Os1 -8.0(17) . . . . ? C64 C65 N6 C61 0(2) . . . . ? C64 C65 N6 Os1 170.9(12) . . . . ? C62 C61 N6 C65 2(2) . . . . ? C53 C61 N6 C65 179.1(13) . . . . ? C62 C61 N6 Os1 -169.7(11) . . . . ? C53 C61 N6 Os1 7.0(17) . . . . ? C49 N5 Os1 N3 143(7) . . . . ? C53 N5 Os1 N3 -35(8) . . . . ? C49 N5 Os1 N6 -172.7(13) . . . . ? C53 N5 Os1 N6 8.9(10) . . . . ? C49 N5 Os1 N2 5.9(14) . . . . ? C53 N5 Os1 N2 -172.4(10) . . . . ? C49 N5 Os1 N1 -71.0(13) . . . . ? C53 N5 Os1 N1 110.6(10) . . . . ? C49 N5 Os1 N4 104.8(13) . . . . ? C53 N5 Os1 N4 -73.5(10) . . . . ? C25 N3 Os1 N5 141(7) . . . . ? C29 N3 Os1 N5 -36(8) . . . . ? C25 N3 Os1 N6 97.5(12) . . . . ? C29 N3 Os1 N6 -79.4(11) . . . . ? C25 N3 Os1 N2 -81.3(12) . . . . ? C29 N3 Os1 N2 101.8(11) . . . . ? C25 N3 Os1 N1 -4.4(12) . . . . ? C29 N3 Os1 N1 178.7(10) . . . . ? C25 N3 Os1 N4 179.9(13) . . . . ? C29 N3 Os1 N4 3.0(10) . . . . ? C65 N6 Os1 N5 179.9(13) . . . . ? C61 N6 Os1 N5 -8.7(11) . . . . ? C65 N6 Os1 N3 -3.0(13) . . . . ? C61 N6 Os1 N3 168.5(11) . . . . ? C65 N6 Os1 N2 161(6) . . . . ? C61 N6 Os1 N2 -27(7) . . . . ? C65 N6 Os1 N1 96.2(13) . . . . ? C61 N6 Os1 N1 -92.3(11) . . . . ? C65 N6 Os1 N4 -79.5(13) . . . . ? C61 N6 Os1 N4 91.9(11) . . . . ? C13 N2 Os1 N5 -88.4(10) . . . . ? C17 N2 Os1 N5 97.0(11) . . . . ? C13 N2 Os1 N3 94.4(10) . . . . ? C17 N2 Os1 N3 -80.2(11) . . . . ? C13 N2 Os1 N6 -70(7) . . . . ? C17 N2 Os1 N6 115(7) . . . . ? C13 N2 Os1 N1 -4.2(9) . . . . ? C17 N2 Os1 N1 -178.8(11) . . . . ? C13 N2 Os1 N4 171.2(9) . . . . ? C17 N2 Os1 N4 -3.4(11) . . . . ? C1 N1 Os1 N5 -73.4(10) . . . . ? C5 N1 Os1 N5 99.6(8) . . . . ? C1 N1 Os1 N3 104.3(10) . . . . ? C5 N1 Os1 N3 -82.7(8) . . . . ? C1 N1 Os1 N6 3.6(10) . . . . ? C5 N1 Os1 N6 176.6(8) . . . . ? C1 N1 Os1 N2 -172.5(10) . . . . ? C5 N1 Os1 N2 0.5(7) . . . . ? C1 N1 Os1 N4 144(3) . . . . ? C5 N1 Os1 N4 -43(4) . . . . ? C41 N4 Os1 N5 1.7(12) . . . . ? C37 N4 Os1 N5 168.7(10) . . . . ? C41 N4 Os1 N3 -175.7(12) . . . . ? C37 N4 Os1 N3 -8.7(10) . . . . ? C41 N4 Os1 N6 -75.1(12) . . . . ? C37 N4 Os1 N6 91.9(10) . . . . ? C41 N4 Os1 N2 101.2(12) . . . . ? C37 N4 Os1 N2 -91.8(10) . . . . ? C41 N4 Os1 N1 144(3) . . . . ? C37 N4 Os1 N1 -49(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.017 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.110