Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email SHIGGINS@LIVERPOOL.AC.UK _publ_contact_author_name 'Dr Simon J Higgins' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name S.J.Higgins J.F.Bickley 'A.La Pensee' C.A.Stuart data_cs189 _database_code_CSD 144522 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H64 Cl2 F6 O12 P6 Ru S2' _chemical_formula_weight 1525.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0020 0.0020 '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 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1100 0.1240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.4200 0.8360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1320 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.540(2) _cell_length_b 13.8934(14) _cell_length_c 25.426(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.126(13) _cell_angle_gamma 90.00 _cell_volume 6630.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31220 _diffrn_reflns_av_R_equivalents 0.1586 _diffrn_reflns_av_sigmaI/netI 0.1580 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8644 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00031(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8644 _refine_ls_number_parameters 828 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6355(4) 0.1191(6) 0.1583(3) 0.035(2) Uani 1 d . . . C2 C 0.6480(4) 0.1952(7) 0.1262(3) 0.048(2) Uani 1 d . . . H2 H 0.6371 0.2587 0.1339 0.058 Uiso 1 calc R . . C3 C 0.6761(5) 0.1767(8) 0.0836(4) 0.065(3) Uani 1 d . . . H3 H 0.6826 0.2284 0.0617 0.078 Uiso 1 calc R . . C4 C 0.6951(5) 0.0870(8) 0.0716(4) 0.062(3) Uani 1 d . . . H4 H 0.7162 0.0766 0.0431 0.075 Uiso 1 calc R . . C5 C 0.6818(5) 0.0109(7) 0.1033(4) 0.062(3) Uani 1 d . . . H5 H 0.6928 -0.0523 0.0952 0.074 Uiso 1 calc R . . C6 C 0.6527(5) 0.0267(6) 0.1465(3) 0.046(2) Uani 1 d . . . H6 H 0.6447 -0.0254 0.1676 0.055 Uiso 1 calc R . . C7 C 0.6272(4) 0.0399(5) 0.2591(3) 0.0323(19) Uani 1 d . . . C8 C 0.6912(4) 0.0454(6) 0.3012(3) 0.040(2) Uani 1 d . . . H8 H 0.7175 0.1030 0.3072 0.047 Uiso 1 calc R . . C9 C 0.7155(5) -0.0344(6) 0.3339(3) 0.045(2) Uani 1 d . . . H9 H 0.7585 -0.0302 0.3620 0.054 Uiso 1 calc R . . C10 C 0.6784(5) -0.1187(6) 0.3262(4) 0.050(2) Uani 1 d . . . H10 H 0.6951 -0.1722 0.3487 0.060 Uiso 1 calc R . . C11 C 0.6153(5) -0.1241(6) 0.2843(4) 0.050(2) Uani 1 d . . . H11 H 0.5896 -0.1822 0.2784 0.060 Uiso 1 calc R . . C12 C 0.5896(4) -0.0462(5) 0.2514(3) 0.038(2) Uani 1 d . . . H12 H 0.5465 -0.0513 0.2235 0.045 Uiso 1 calc R . . C13 C 0.6425(4) 0.2446(5) 0.2527(3) 0.0288(18) Uani 1 d . . . C14 C 0.7077(4) 0.2761(6) 0.2558(3) 0.0347(19) Uani 1 d . . . H14A H 0.743(4) 0.232(5) 0.237(3) 0.05(2) Uiso 1 d . . . H14B H 0.727(5) 0.347(7) 0.277(4) 0.07(3) Uiso 1 d . . . C15 C 0.5947(4) 0.4295(5) 0.2742(3) 0.034(2) Uani 1 d . . . C16 C 0.6175(4) 0.4661(6) 0.2315(3) 0.038(2) Uani 1 d . . . H16 H 0.6179 0.4258 0.2019 0.045 Uiso 1 calc R . . C17 C 0.6398(4) 0.5605(6) 0.2309(4) 0.045(2) Uani 1 d . . . H17 H 0.6558 0.5834 0.2016 0.054 Uiso 1 calc R . . C18 C 0.6384(5) 0.6200(6) 0.2732(5) 0.060(3) Uani 1 d . . . H18 H 0.6522 0.6847 0.2725 0.071 Uiso 1 calc R . . C19 C 0.6170(5) 0.5864(6) 0.3169(4) 0.059(3) Uani 1 d . . . H19 H 0.6182 0.6276 0.3465 0.070 Uiso 1 calc R . . C20 C 0.5935(5) 0.4920(5) 0.3180(3) 0.044(2) Uani 1 d . . . H20 H 0.5771 0.4701 0.3473 0.052 Uiso 1 calc R . . C21 C 0.5969(4) 0.2859(5) 0.3508(3) 0.0280(16) Uani 1 d . . . C22 C 0.5474(4) 0.3010(6) 0.3793(3) 0.0349(19) Uani 1 d . . . H22 H 0.4993 0.3105 0.3600 0.042 Uiso 1 calc R . . C23 C 0.5674(4) 0.3025(6) 0.4359(3) 0.043(2) Uani 1 d . . . H23 H 0.5329 0.3138 0.4547 0.051 Uiso 1 calc R . . C24 C 0.6362(5) 0.2877(7) 0.4646(3) 0.052(2) Uani 1 d . . . H24 H 0.6495 0.2892 0.5030 0.062 Uiso 1 calc R . . C25 C 0.6870(5) 0.2704(6) 0.4369(3) 0.049(2) Uani 1 d . . . H25 H 0.7345 0.2587 0.4567 0.059 Uiso 1 calc R . . C26 C 0.6678(4) 0.2703(5) 0.3792(3) 0.038(2) Uani 1 d . . . H26 H 0.7023 0.2599 0.3604 0.045 Uiso 1 calc R . . C27 C 0.4170(4) -0.0345(5) 0.2612(3) 0.0315(19) Uani 1 d . . . C28 C 0.3600(4) -0.0614(6) 0.2159(3) 0.038(2) Uani 1 d . . . H28 H 0.3339 -0.0139 0.1924 0.046 Uiso 1 calc R . . C29 C 0.3426(5) -0.1560(6) 0.2061(4) 0.047(2) Uani 1 d . . . H29 H 0.3044 -0.1730 0.1759 0.056 Uiso 1 calc R . . C30 C 0.3802(5) -0.2268(6) 0.2397(4) 0.049(2) Uani 1 d . . . H30 H 0.3688 -0.2920 0.2323 0.058 Uiso 1 calc R . . C31 C 0.4342(5) -0.2008(6) 0.2841(3) 0.049(2) Uani 1 d . . . H31 H 0.4596 -0.2487 0.3078 0.059 Uiso 1 calc R . . C32 C 0.4524(4) -0.1048(5) 0.2949(3) 0.038(2) Uani 1 d . . . H32 H 0.4896 -0.0883 0.3259 0.045 Uiso 1 calc R . . C33 C 0.4788(4) 0.0933(5) 0.3458(3) 0.0291(18) Uani 1 d . . . C34 C 0.4372(4) 0.1079(5) 0.3811(3) 0.034(2) Uani 1 d . . . H34 H 0.3888 0.1239 0.3668 0.041 Uiso 1 calc R . . C35 C 0.4659(5) 0.0992(6) 0.4374(3) 0.045(2) Uani 1 d . . . H35 H 0.4374 0.1110 0.4610 0.054 Uiso 1 calc R . . C36 C 0.5364(6) 0.0733(6) 0.4583(3) 0.051(3) Uani 1 d . . . H36 H 0.5559 0.0663 0.4963 0.062 Uiso 1 calc R . . C37 C 0.5781(5) 0.0578(6) 0.4236(3) 0.043(2) Uani 1 d . . . H37 H 0.6260 0.0395 0.4381 0.051 Uiso 1 calc R . . C38 C 0.5507(4) 0.0687(5) 0.3680(3) 0.0342(19) Uani 1 d . . . H38 H 0.5801 0.0596 0.3448 0.041 Uiso 1 calc R . . C39 C 0.3560(4) 0.1557(5) 0.2599(3) 0.0300(18) Uani 1 d . . . C40 C 0.2953(5) 0.1219(8) 0.2650(3) 0.036(2) Uani 1 d . . . H40A H 0.253(5) 0.157(5) 0.257(3) 0.04(2) Uiso 1 d . . . H40B H 0.290(5) 0.064(8) 0.276(4) 0.07(4) Uiso 1 d . . . C41 C 0.3799(4) 0.3568(5) 0.2846(3) 0.0307(18) Uani 1 d . . . C42 C 0.4165(4) 0.4443(6) 0.2850(3) 0.042(2) Uani 1 d . . . H42 H 0.4391 0.4572 0.2576 0.051 Uiso 1 calc R . . C43 C 0.4193(5) 0.5117(6) 0.3262(3) 0.046(2) Uani 1 d . . . H43 H 0.4435 0.5703 0.3264 0.056 Uiso 1 calc R . . C44 C 0.3869(5) 0.4929(7) 0.3662(4) 0.053(2) Uani 1 d . . . H44 H 0.3892 0.5384 0.3940 0.064 Uiso 1 calc R . . C45 C 0.3506(4) 0.4070(6) 0.3662(3) 0.047(2) Uani 1 d . . . H45 H 0.3278 0.3937 0.3934 0.056 Uiso 1 calc R . . C46 C 0.3490(4) 0.3415(6) 0.3249(3) 0.036(2) Uani 1 d . . . H46 H 0.3249 0.2830 0.3251 0.044 Uiso 1 calc R . . C47 C 0.2913(4) 0.3044(6) 0.1805(3) 0.0311(18) Uani 1 d . . . C48 C 0.2763(4) 0.4026(6) 0.1711(3) 0.041(2) Uani 1 d . . . H48 H 0.3095 0.4489 0.1895 0.049 Uiso 1 calc R . . C49 C 0.2123(5) 0.4321(7) 0.1346(3) 0.046(2) Uani 1 d . . . H49 H 0.2034 0.4979 0.1269 0.055 Uiso 1 calc R . . C50 C 0.1623(5) 0.3644(7) 0.1099(3) 0.053(3) Uani 1 d . . . H50 H 0.1182 0.3848 0.0870 0.063 Uiso 1 calc R . . C51 C 0.1754(5) 0.2674(7) 0.1182(3) 0.047(2) Uani 1 d . . . H51 H 0.1410 0.2219 0.1007 0.056 Uiso 1 calc R . . C52 C 0.2410(4) 0.2375(6) 0.1531(3) 0.037(2) Uani 1 d . . . H52 H 0.2511 0.1714 0.1580 0.044 Uiso 1 calc R . . C53 C 0.3092(5) 0.1243(9) 0.0536(3) 0.071(3) Uani 1 d . . . H53A H 0.2584 0.1218 0.0494 0.085 Uiso 1 calc R . . H53B H 0.3222 0.0734 0.0320 0.085 Uiso 1 calc R . . H53C H 0.3214 0.1862 0.0410 0.085 Uiso 1 calc R . . C54 C 0.4810(5) 0.0901(6) 0.0454(3) 0.046(2) Uani 1 d . . . H54A H 0.4979 0.1322 0.0213 0.055 Uiso 1 calc R . . H54B H 0.4394 0.0552 0.0244 0.055 Uiso 1 calc R . . H54C H 0.5183 0.0447 0.0626 0.055 Uiso 1 calc R . . C55 C 0.4117(6) -0.0741(7) 0.1096(4) 0.064(3) Uani 1 d . . . H55A H 0.4329 -0.1364 0.1211 0.077 Uiso 1 calc R . . H55B H 0.4107 -0.0628 0.0717 0.077 Uiso 1 calc R . . H55C H 0.3634 -0.0730 0.1129 0.077 Uiso 1 calc R . . C56 C 0.5180(6) 0.3669(8) 0.0602(3) 0.069(3) Uani 1 d . . . H56A H 0.5641 0.3790 0.0541 0.082 Uiso 1 calc R . . H56B H 0.4869 0.4215 0.0473 0.082 Uiso 1 calc R . . H56C H 0.4972 0.3095 0.0404 0.082 Uiso 1 calc R . . C57 C 0.3511(5) 0.3890(6) 0.0649(3) 0.055(3) Uani 1 d . . . H57A H 0.3108 0.3587 0.0390 0.065 Uiso 1 calc R . . H57B H 0.3792 0.4236 0.0451 0.065 Uiso 1 calc R . . H57C H 0.3341 0.4335 0.0878 0.065 Uiso 1 calc R . . C58 C 0.4633(5) 0.5289(6) 0.1522(4) 0.057(3) Uani 1 d . . . H58A H 0.4528 0.5768 0.1766 0.068 Uiso 1 calc R . . H58B H 0.4308 0.5366 0.1159 0.068 Uiso 1 calc R . . H58C H 0.5119 0.5370 0.1505 0.068 Uiso 1 calc R . . C59 C 0.5471(5) 0.7487(7) 0.0985(4) 0.056(3) Uani 1 d . . . C60 C 0.2534(7) -0.3799(7) 0.0124(4) 0.066(3) Uani 1 d . . . C61 C 0.0990(7) -0.1728(9) -0.0227(5) 0.100(4) Uani 1 d . . . H61A H 0.1442 -0.1914 -0.0294 0.120 Uiso 1 calc R . . H61B H 0.1007 -0.1919 0.0148 0.120 Uiso 1 calc R . . P1 P 0.59565(10) 0.14293(14) 0.21473(8) 0.0279(5) Uani 1 d . . . P2 P 0.57266(10) 0.30222(14) 0.27661(7) 0.0261(4) Uani 1 d . . . P3 P 0.44182(10) 0.09417(13) 0.27188(7) 0.0252(4) Uani 1 d . . . P4 P 0.37465(10) 0.26814(13) 0.22986(8) 0.0279(5) Uani 1 d . . . P5 P 0.43256(11) 0.11170(14) 0.13537(8) 0.0303(5) Uani 1 d . . . P6 P 0.46661(11) 0.33176(14) 0.14694(8) 0.0324(5) Uani 1 d . . . S1 S 0.62411(12) 0.69676(18) 0.09000(9) 0.0537(6) Uani 1 d . . . S2 S 0.26094(12) -0.30345(17) 0.07089(9) 0.0488(6) Uani 1 d . . . O1 O 0.3483(3) 0.1113(4) 0.1117(2) 0.0438(15) Uani 1 d . . . O2 O 0.4627(3) 0.1459(4) 0.0864(2) 0.0461(15) Uani 1 d . . . O3 O 0.4539(3) 0.0014(3) 0.1443(2) 0.0350(13) Uani 1 d . . . O4 O 0.5268(3) 0.3530(4) 0.1186(2) 0.0461(15) Uani 1 d . . . O5 O 0.3954(3) 0.3149(4) 0.0993(2) 0.0468(15) Uani 1 d . . . O6 O 0.4546(3) 0.4310(4) 0.1732(2) 0.0369(13) Uani 1 d . . . O7 O 0.6777(3) 0.7196(5) 0.1397(2) 0.0694(19) Uani 1 d . . . O8 O 0.6318(3) 0.7419(5) 0.0405(2) 0.068(2) Uani 1 d . . . O9 O 0.6076(4) 0.5944(5) 0.0846(4) 0.093(2) Uani 1 d . . . O10 O 0.3108(5) -0.3515(6) 0.1145(3) 0.105(3) Uani 1 d . . . O11 O 0.2803(4) -0.2129(5) 0.0525(3) 0.092(2) Uani 1 d . . . O12 O 0.1922(4) -0.3034(6) 0.0766(3) 0.079(2) Uani 1 d . . . F1 F 0.4888(3) 0.7348(5) 0.0589(3) 0.094(2) Uani 1 d . . . F2 F 0.5329(3) 0.7269(4) 0.1453(2) 0.0779(17) Uani 1 d . . . F3 F 0.5543(4) 0.8477(4) 0.1010(3) 0.094(2) Uani 1 d . . . F4 F 0.3169(5) -0.3921(6) 0.0029(3) 0.123(3) Uani 1 d . . . F5 F 0.2310(4) -0.4676(4) 0.0206(2) 0.090(2) Uani 1 d . . . F6 F 0.2110(4) -0.3446(4) -0.0323(2) 0.102(2) Uani 1 d . . . Ru1 Ru 0.47992(3) 0.20780(4) 0.21044(2) 0.02363(17) Uani 1 d . . . Cl1 Cl 0.0306(2) -0.2331(4) -0.06779(14) 0.1462(19) Uani 1 d . . . Cl2 Cl 0.0894(4) -0.0487(3) -0.02856(18) 0.176(2) 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 C1 0.026(5) 0.045(5) 0.030(4) -0.006(4) 0.003(3) -0.002(4) C2 0.051(6) 0.045(5) 0.054(5) 0.000(5) 0.023(4) -0.010(5) C3 0.063(7) 0.091(9) 0.050(6) 0.002(5) 0.030(5) -0.014(6) C4 0.058(7) 0.083(8) 0.057(6) -0.018(6) 0.036(5) -0.001(6) C5 0.063(7) 0.054(6) 0.068(7) -0.027(5) 0.019(6) 0.010(5) C6 0.048(6) 0.044(5) 0.047(5) -0.015(4) 0.015(4) 0.000(4) C7 0.024(5) 0.030(5) 0.044(5) 0.002(4) 0.011(4) 0.009(4) C8 0.033(5) 0.031(5) 0.052(5) 0.014(4) 0.008(4) 0.010(4) C9 0.037(5) 0.047(6) 0.048(5) 0.014(4) 0.008(4) 0.014(4) C10 0.046(6) 0.037(5) 0.069(6) 0.021(4) 0.017(5) 0.018(5) C11 0.049(6) 0.026(5) 0.076(6) 0.009(4) 0.019(5) 0.011(4) C12 0.027(5) 0.036(5) 0.049(5) -0.004(4) 0.009(4) 0.001(4) C13 0.033(5) 0.028(4) 0.024(4) 0.004(3) 0.005(3) 0.002(4) C14 0.025(5) 0.036(5) 0.038(4) 0.007(4) 0.001(3) -0.006(4) C15 0.019(4) 0.034(5) 0.045(5) 0.002(4) 0.000(4) 0.005(4) C16 0.031(5) 0.034(5) 0.046(5) 0.009(4) 0.007(4) 0.000(4) C17 0.035(5) 0.032(5) 0.072(6) 0.009(5) 0.021(4) 0.006(4) C18 0.050(7) 0.017(5) 0.119(9) 0.001(5) 0.036(6) -0.009(4) C19 0.053(6) 0.038(6) 0.087(7) -0.016(5) 0.025(5) -0.012(5) C20 0.050(6) 0.028(5) 0.054(6) -0.004(4) 0.018(4) -0.006(4) C21 0.026(4) 0.029(4) 0.028(4) 0.002(4) 0.007(3) 0.001(4) C22 0.034(5) 0.032(4) 0.031(4) 0.001(4) -0.003(3) -0.003(4) C23 0.045(6) 0.049(5) 0.034(5) 0.000(4) 0.010(4) -0.007(5) C24 0.053(6) 0.073(6) 0.025(4) 0.004(5) 0.003(4) -0.008(6) C25 0.040(5) 0.065(7) 0.033(5) 0.000(4) -0.005(4) -0.009(5) C26 0.031(5) 0.045(5) 0.033(5) 0.001(4) 0.004(4) -0.001(4) C27 0.028(5) 0.036(5) 0.029(4) 0.000(4) 0.006(4) 0.001(4) C28 0.033(5) 0.030(5) 0.047(5) 0.002(4) 0.006(4) -0.002(4) C29 0.040(5) 0.043(5) 0.054(6) -0.006(4) 0.007(4) -0.017(4) C30 0.046(6) 0.034(5) 0.069(6) -0.010(4) 0.023(5) -0.012(4) C31 0.056(6) 0.025(5) 0.062(6) 0.003(5) 0.009(5) 0.004(5) C32 0.032(5) 0.032(5) 0.043(5) 0.005(4) 0.001(4) 0.002(4) C33 0.031(5) 0.028(4) 0.031(4) 0.003(3) 0.012(4) -0.002(4) C34 0.035(5) 0.030(4) 0.033(5) -0.007(4) 0.000(4) -0.010(4) C35 0.046(6) 0.052(5) 0.038(5) -0.005(4) 0.013(4) -0.016(5) C36 0.076(8) 0.052(6) 0.020(4) 0.003(4) 0.004(5) -0.016(5) C37 0.041(5) 0.045(5) 0.031(5) 0.008(4) -0.009(4) -0.001(4) C38 0.033(5) 0.036(4) 0.031(5) 0.001(3) 0.003(4) -0.004(4) C39 0.022(5) 0.030(4) 0.034(4) 0.002(3) 0.001(3) 0.001(4) C40 0.024(5) 0.049(6) 0.035(5) 0.000(4) 0.008(4) 0.002(5) C41 0.029(5) 0.034(5) 0.028(4) -0.001(3) 0.005(3) 0.006(4) C42 0.041(5) 0.048(5) 0.035(5) 0.008(4) 0.005(4) 0.003(4) C43 0.059(6) 0.029(5) 0.048(6) -0.011(4) 0.009(5) -0.003(4) C44 0.068(7) 0.048(6) 0.043(5) -0.021(4) 0.016(5) -0.010(5) C45 0.042(6) 0.056(6) 0.041(5) -0.002(4) 0.010(4) 0.006(5) C46 0.039(5) 0.032(4) 0.041(5) -0.008(4) 0.014(4) -0.001(4) C47 0.028(4) 0.041(5) 0.025(4) 0.005(4) 0.007(3) 0.011(4) C48 0.042(5) 0.039(5) 0.035(5) 0.004(4) 0.002(4) 0.013(4) C49 0.046(6) 0.051(5) 0.043(5) 0.013(4) 0.016(4) 0.021(5) C50 0.035(5) 0.078(7) 0.039(5) 0.003(5) 0.000(4) 0.024(5) C51 0.036(5) 0.067(7) 0.034(5) -0.001(4) 0.002(4) 0.008(4) C52 0.029(5) 0.049(5) 0.029(4) 0.007(4) 0.002(4) 0.008(4) C53 0.041(6) 0.123(9) 0.036(5) -0.007(6) -0.010(4) 0.006(6) C54 0.049(6) 0.054(6) 0.039(5) -0.014(4) 0.018(4) 0.003(5) C55 0.093(8) 0.045(6) 0.055(6) -0.015(5) 0.020(5) -0.018(6) C56 0.098(9) 0.089(8) 0.023(5) 0.013(5) 0.025(5) -0.002(7) C57 0.057(6) 0.054(6) 0.040(5) 0.017(4) -0.008(4) 0.023(5) C58 0.063(7) 0.034(5) 0.076(7) 0.027(5) 0.022(5) 0.012(5) C59 0.051(6) 0.062(7) 0.049(6) 0.002(5) 0.007(5) -0.012(5) C60 0.087(9) 0.051(7) 0.062(7) 0.001(5) 0.027(6) -0.006(6) C61 0.076(9) 0.093(9) 0.111(10) 0.025(7) -0.008(7) 0.016(7) P1 0.0219(11) 0.0277(11) 0.0326(11) -0.0014(9) 0.0050(9) 0.0001(9) P2 0.0234(10) 0.0261(10) 0.0250(10) -0.0002(8) 0.0005(7) -0.0011(9) P3 0.0207(11) 0.0279(11) 0.0251(10) 0.0031(8) 0.0033(8) -0.0007(9) P4 0.0223(11) 0.0298(12) 0.0289(11) 0.0017(8) 0.0027(8) 0.0023(8) P5 0.0262(12) 0.0368(12) 0.0267(11) -0.0020(9) 0.0053(8) 0.0005(9) P6 0.0350(12) 0.0322(11) 0.0270(11) 0.0059(8) 0.0038(9) -0.0031(9) S1 0.0432(14) 0.0618(15) 0.0518(14) 0.0095(13) 0.0061(10) -0.0039(13) S2 0.0432(14) 0.0482(14) 0.0482(12) -0.0068(11) 0.0011(10) 0.0053(12) O1 0.022(3) 0.061(4) 0.041(3) -0.010(3) -0.005(2) 0.000(3) O2 0.058(4) 0.051(4) 0.032(3) 0.004(3) 0.019(3) 0.008(3) O3 0.043(3) 0.025(3) 0.038(3) -0.012(2) 0.012(2) -0.003(2) O4 0.054(4) 0.051(4) 0.037(3) 0.000(3) 0.018(3) -0.010(3) O5 0.048(4) 0.040(3) 0.041(3) 0.007(3) -0.007(3) 0.008(3) O6 0.042(3) 0.028(3) 0.038(3) 0.010(2) 0.008(2) 0.006(3) O7 0.043(4) 0.100(5) 0.052(4) 0.012(4) -0.009(3) -0.014(4) O8 0.052(4) 0.105(6) 0.047(4) 0.028(3) 0.010(3) -0.003(4) O9 0.096(6) 0.060(5) 0.130(7) -0.017(5) 0.042(5) 0.002(4) O10 0.103(7) 0.100(6) 0.076(5) -0.024(5) -0.037(5) 0.046(5) O11 0.102(6) 0.051(4) 0.120(6) -0.004(5) 0.026(5) -0.032(5) O12 0.076(5) 0.100(6) 0.075(5) 0.017(4) 0.043(4) 0.022(5) F1 0.047(4) 0.134(6) 0.090(4) -0.019(4) 0.000(3) 0.001(4) F2 0.081(4) 0.078(4) 0.085(4) 0.022(3) 0.040(3) 0.012(3) F3 0.103(6) 0.061(4) 0.120(6) 0.009(4) 0.036(4) 0.005(4) F4 0.158(8) 0.104(6) 0.142(7) 0.010(5) 0.098(6) 0.035(5) F5 0.139(6) 0.036(3) 0.074(4) -0.003(3) -0.003(4) -0.012(3) F6 0.170(7) 0.072(4) 0.043(3) 0.007(3) -0.003(4) 0.014(4) Ru1 0.0209(3) 0.0246(3) 0.0232(3) 0.0015(3) 0.0024(2) 0.0003(3) Cl1 0.111(3) 0.215(5) 0.083(2) 0.042(3) -0.022(2) -0.055(3) Cl2 0.299(7) 0.112(3) 0.105(3) 0.033(3) 0.036(4) 0.085(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.382(11) . ? C1 C2 1.398(11) . ? C1 P1 1.842(8) . ? C2 C3 1.368(12) . ? C3 C4 1.359(14) . ? C4 C5 1.397(14) . ? C5 C6 1.386(12) . ? C7 C12 1.390(11) . ? C7 C8 1.403(10) . ? C7 P1 1.821(7) . ? C8 C9 1.388(11) . ? C9 C10 1.363(12) . ? C10 C11 1.388(12) . ? C11 C12 1.376(11) . ? C13 C14 1.329(10) . ? C13 P1 1.809(7) . ? C13 P2 1.826(8) . ? C15 C16 1.380(11) . ? C15 C20 1.419(11) . ? C15 P2 1.825(8) . ? C16 C17 1.383(11) . ? C17 C18 1.363(13) . ? C18 C19 1.373(14) . ? C19 C20 1.391(12) . ? C21 C22 1.375(10) . ? C21 C26 1.391(10) . ? C21 P2 1.827(7) . ? C22 C23 1.385(10) . ? C23 C24 1.355(11) . ? C24 C25 1.388(12) . ? C25 C26 1.408(11) . ? C27 C32 1.355(10) . ? C27 C28 1.414(10) . ? C27 P3 1.852(8) . ? C28 C29 1.363(11) . ? C29 C30 1.375(12) . ? C30 C31 1.363(11) . ? C31 C32 1.389(11) . ? C33 C34 1.384(11) . ? C33 C38 1.402(10) . ? C33 P3 1.816(7) . ? C34 C35 1.389(11) . ? C35 C36 1.380(13) . ? C36 C37 1.375(13) . ? C37 C38 1.374(10) . ? C39 C40 1.316(11) . ? C39 P4 1.820(7) . ? C39 P3 1.832(8) . ? C41 C46 1.344(11) . ? C41 C42 1.409(11) . ? C41 P4 1.840(7) . ? C42 C43 1.395(11) . ? C43 C44 1.364(12) . ? C44 C45 1.389(12) . ? C45 C46 1.381(11) . ? C47 C52 1.390(10) . ? C47 C48 1.403(11) . ? C47 P4 1.829(7) . ? C48 C49 1.397(11) . ? C49 C50 1.375(13) . ? C50 C51 1.377(13) . ? C51 C52 1.405(10) . ? C53 O1 1.475(9) . ? C54 O2 1.421(9) . ? C55 O3 1.468(9) . ? C56 O4 1.461(9) . ? C57 O5 1.467(9) . ? C58 O6 1.487(9) . ? C59 F1 1.308(10) . ? C59 F2 1.329(11) . ? C59 F3 1.383(10) . ? C59 S1 1.735(11) . ? C60 F6 1.301(11) . ? C60 F5 1.331(11) . ? C60 F4 1.338(13) . ? C60 S2 1.801(10) . ? C61 Cl1 1.717(12) . ? C61 Cl2 1.735(13) . ? P1 Ru1 2.409(2) . ? P2 Ru1 2.4782(19) . ? P3 Ru1 2.4764(19) . ? P4 Ru1 2.396(2) . ? P5 O3 1.588(5) . ? P5 O1 1.589(5) . ? P5 O2 1.591(6) . ? P5 Ru1 2.303(2) . ? P6 O4 1.568(6) . ? P6 O6 1.577(6) . ? P6 O5 1.588(5) . ? P6 Ru1 2.325(2) . ? S1 O7 1.435(6) . ? S1 O8 1.452(6) . ? S1 O9 1.457(7) . ? S2 O12 1.391(7) . ? S2 O10 1.423(7) . ? S2 O11 1.430(7) . ? F1 F3 2.117(9) . ? F1 F2 2.127(8) . ? F2 F3 2.126(9) . ? F4 F6 2.120(12) . ? F4 F5 2.131(11) . ? F5 F6 2.141(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(8) . . ? C6 C1 P1 121.2(6) . . ? C2 C1 P1 119.9(6) . . ? C3 C2 C1 119.6(9) . . ? C4 C3 C2 123.1(10) . . ? C3 C4 C5 117.2(8) . . ? C6 C5 C4 121.4(9) . . ? C1 C6 C5 119.8(9) . . ? C12 C7 C8 118.7(7) . . ? C12 C7 P1 120.9(6) . . ? C8 C7 P1 120.4(6) . . ? C9 C8 C7 119.8(8) . . ? C10 C9 C8 121.3(8) . . ? C9 C10 C11 118.8(8) . . ? C12 C11 C10 121.3(8) . . ? C11 C12 C7 120.1(8) . . ? C14 C13 P1 128.6(6) . . ? C14 C13 P2 128.9(6) . . ? P1 C13 P2 101.9(4) . . ? C16 C15 C20 118.1(7) . . ? C16 C15 P2 121.0(6) . . ? C20 C15 P2 120.8(6) . . ? C15 C16 C17 122.0(8) . . ? C18 C17 C16 119.4(9) . . ? C17 C18 C19 120.7(8) . . ? C18 C19 C20 120.8(9) . . ? C19 C20 C15 119.0(8) . . ? C22 C21 C26 119.7(6) . . ? C22 C21 P2 120.4(5) . . ? C26 C21 P2 119.4(6) . . ? C21 C22 C23 120.9(7) . . ? C24 C23 C22 120.5(8) . . ? C23 C24 C25 119.8(7) . . ? C24 C25 C26 120.5(7) . . ? C21 C26 C25 118.6(8) . . ? C32 C27 C28 118.2(7) . . ? C32 C27 P3 122.4(6) . . ? C28 C27 P3 119.3(6) . . ? C29 C28 C27 120.3(7) . . ? C28 C29 C30 120.8(8) . . ? C31 C30 C29 118.9(8) . . ? C30 C31 C32 121.0(8) . . ? C27 C32 C31 120.7(7) . . ? C34 C33 C38 118.5(7) . . ? C34 C33 P3 122.2(6) . . ? C38 C33 P3 119.0(6) . . ? C33 C34 C35 120.9(8) . . ? C36 C35 C34 119.7(8) . . ? C37 C36 C35 119.9(8) . . ? C38 C37 C36 120.8(8) . . ? C37 C38 C33 120.2(8) . . ? C40 C39 P4 129.8(7) . . ? C40 C39 P3 128.8(7) . . ? P4 C39 P3 100.9(4) . . ? C46 C41 C42 117.8(7) . . ? C46 C41 P4 121.9(6) . . ? C42 C41 P4 120.3(6) . . ? C43 C42 C41 119.9(8) . . ? C44 C43 C42 120.2(8) . . ? C43 C44 C45 120.4(8) . . ? C46 C45 C44 118.1(8) . . ? C41 C46 C45 123.7(8) . . ? C52 C47 C48 118.7(7) . . ? C52 C47 P4 122.0(6) . . ? C48 C47 P4 119.3(6) . . ? C49 C48 C47 120.3(8) . . ? C50 C49 C48 119.6(8) . . ? C49 C50 C51 121.5(8) . . ? C50 C51 C52 118.9(8) . . ? C47 C52 C51 120.9(8) . . ? F1 C59 F2 107.5(8) . . ? F1 C59 F3 103.7(8) . . ? F2 C59 F3 103.3(8) . . ? F1 C59 S1 116.3(7) . . ? F2 C59 S1 114.9(7) . . ? F3 C59 S1 109.8(7) . . ? F6 C60 F5 108.9(9) . . ? F6 C60 F4 106.9(9) . . ? F5 C60 F4 105.9(9) . . ? F6 C60 S2 112.6(8) . . ? F5 C60 S2 111.4(7) . . ? F4 C60 S2 110.9(8) . . ? Cl1 C61 Cl2 112.5(7) . . ? C13 P1 C7 104.4(3) . . ? C13 P1 C1 107.2(4) . . ? C7 P1 C1 101.4(4) . . ? C13 P1 Ru1 93.5(3) . . ? C7 P1 Ru1 118.3(3) . . ? C1 P1 Ru1 128.8(2) . . ? C15 P2 C13 102.0(3) . . ? C15 P2 C21 99.2(3) . . ? C13 P2 C21 106.7(3) . . ? C15 P2 Ru1 128.7(2) . . ? C13 P2 Ru1 90.8(2) . . ? C21 P2 Ru1 124.5(2) . . ? C33 P3 C39 104.9(3) . . ? C33 P3 C27 99.1(3) . . ? C39 P3 C27 103.7(3) . . ? C33 P3 Ru1 123.6(2) . . ? C39 P3 Ru1 91.1(2) . . ? C27 P3 Ru1 129.4(3) . . ? C39 P4 C47 106.3(3) . . ? C39 P4 C41 103.4(3) . . ? C47 P4 C41 100.8(3) . . ? C39 P4 Ru1 94.0(3) . . ? C47 P4 Ru1 127.3(2) . . ? C41 P4 Ru1 121.3(2) . . ? O3 P5 O1 104.7(3) . . ? O3 P5 O2 105.1(3) . . ? O1 P5 O2 106.0(3) . . ? O3 P5 Ru1 114.4(2) . . ? O1 P5 Ru1 116.8(2) . . ? O2 P5 Ru1 109.0(2) . . ? O4 P6 O6 104.4(3) . . ? O4 P6 O5 106.7(3) . . ? O6 P6 O5 104.5(3) . . ? O4 P6 Ru1 120.3(2) . . ? O6 P6 Ru1 110.8(2) . . ? O5 P6 Ru1 109.0(2) . . ? O7 S1 O8 116.2(4) . . ? O7 S1 O9 112.7(5) . . ? O8 S1 O9 114.5(5) . . ? O7 S1 C59 104.2(4) . . ? O8 S1 C59 103.4(4) . . ? O9 S1 C59 103.9(5) . . ? O12 S2 O10 113.0(5) . . ? O12 S2 O11 112.7(5) . . ? O10 S2 O11 118.8(5) . . ? O12 S2 C60 103.1(5) . . ? O10 S2 C60 104.4(5) . . ? O11 S2 C60 102.5(5) . . ? C53 O1 P5 124.9(6) . . ? C54 O2 P5 129.3(5) . . ? C55 O3 P5 121.5(5) . . ? C56 O4 P6 126.9(6) . . ? C57 O5 P6 126.7(5) . . ? C58 O6 P6 127.0(5) . . ? C59 F1 F3 39.4(5) . . ? C59 F1 F2 36.6(5) . . ? F3 F1 F2 60.1(3) . . ? C59 F2 F3 39.3(5) . . ? C59 F2 F1 35.9(5) . . ? F3 F2 F1 59.7(3) . . ? C59 F3 F1 36.9(5) . . ? C59 F3 F2 37.5(5) . . ? F1 F3 F2 60.2(3) . . ? C60 F4 F6 36.0(5) . . ? C60 F4 F5 36.9(5) . . ? F6 F4 F5 60.5(4) . . ? C60 F5 F4 37.1(6) . . ? C60 F5 F6 35.1(5) . . ? F4 F5 F6 59.5(4) . . ? C60 F6 F4 37.2(6) . . ? C60 F6 F5 36.0(5) . . ? F4 F6 F5 60.0(3) . . ? P5 Ru1 P6 84.96(7) . . ? P5 Ru1 P4 101.73(7) . . ? P6 Ru1 P4 86.97(7) . . ? P5 Ru1 P1 88.66(7) . . ? P6 Ru1 P1 103.36(8) . . ? P4 Ru1 P1 166.05(7) . . ? P5 Ru1 P3 91.79(7) . . ? P6 Ru1 P3 156.19(7) . . ? P4 Ru1 P3 70.57(7) . . ? P1 Ru1 P3 100.13(7) . . ? P5 Ru1 P2 156.85(7) . . ? P6 Ru1 P2 89.94(7) . . ? P4 Ru1 P2 100.52(7) . . ? P1 Ru1 P2 70.55(7) . . ? P3 Ru1 P2 101.57(6) . . ? 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 C6 C1 C2 C3 0.7(12) . . . . ? P1 C1 C2 C3 -178.5(7) . . . . ? C1 C2 C3 C4 -2.2(15) . . . . ? C2 C3 C4 C5 2.9(15) . . . . ? C3 C4 C5 C6 -2.2(15) . . . . ? C2 C1 C6 C5 0.0(12) . . . . ? P1 C1 C6 C5 179.2(7) . . . . ? C4 C5 C6 C1 0.8(14) . . . . ? C12 C7 C8 C9 0.0(12) . . . . ? P1 C7 C8 C9 -178.5(6) . . . . ? C7 C8 C9 C10 -0.1(13) . . . . ? C8 C9 C10 C11 0.4(14) . . . . ? C9 C10 C11 C12 -0.7(14) . . . . ? C10 C11 C12 C7 0.7(13) . . . . ? C8 C7 C12 C11 -0.3(12) . . . . ? P1 C7 C12 C11 178.2(7) . . . . ? C20 C15 C16 C17 0.9(12) . . . . ? P2 C15 C16 C17 -174.8(6) . . . . ? C15 C16 C17 C18 -1.0(12) . . . . ? C16 C17 C18 C19 1.8(14) . . . . ? C17 C18 C19 C20 -2.7(15) . . . . ? C18 C19 C20 C15 2.6(14) . . . . ? C16 C15 C20 C19 -1.7(12) . . . . ? P2 C15 C20 C19 174.1(7) . . . . ? C26 C21 C22 C23 1.1(12) . . . . ? P2 C21 C22 C23 -170.7(6) . . . . ? C21 C22 C23 C24 -0.9(13) . . . . ? C22 C23 C24 C25 -0.4(15) . . . . ? C23 C24 C25 C26 1.5(14) . . . . ? C22 C21 C26 C25 0.0(11) . . . . ? P2 C21 C26 C25 171.8(6) . . . . ? C24 C25 C26 C21 -1.3(13) . . . . ? C32 C27 C28 C29 -1.5(13) . . . . ? P3 C27 C28 C29 177.4(7) . . . . ? C27 C28 C29 C30 -0.3(14) . . . . ? C28 C29 C30 C31 1.7(14) . . . . ? C29 C30 C31 C32 -1.3(14) . . . . ? C28 C27 C32 C31 1.8(12) . . . . ? P3 C27 C32 C31 -177.0(7) . . . . ? C30 C31 C32 C27 -0.5(14) . . . . ? C38 C33 C34 C35 0.6(11) . . . . ? P3 C33 C34 C35 174.8(6) . . . . ? C33 C34 C35 C36 -1.7(12) . . . . ? C34 C35 C36 C37 1.1(13) . . . . ? C35 C36 C37 C38 0.6(13) . . . . ? C36 C37 C38 C33 -1.8(12) . . . . ? C34 C33 C38 C37 1.2(11) . . . . ? P3 C33 C38 C37 -173.3(6) . . . . ? C46 C41 C42 C43 -0.4(11) . . . . ? P4 C41 C42 C43 179.0(6) . . . . ? C41 C42 C43 C44 0.4(13) . . . . ? C42 C43 C44 C45 -0.5(14) . . . . ? C43 C44 C45 C46 0.6(13) . . . . ? C42 C41 C46 C45 0.6(12) . . . . ? P4 C41 C46 C45 -178.8(6) . . . . ? C44 C45 C46 C41 -0.7(13) . . . . ? C52 C47 C48 C49 -0.5(12) . . . . ? P4 C47 C48 C49 -178.5(6) . . . . ? C47 C48 C49 C50 3.3(13) . . . . ? C48 C49 C50 C51 -3.5(14) . . . . ? C49 C50 C51 C52 0.8(14) . . . . ? C48 C47 C52 C51 -2.2(11) . . . . ? P4 C47 C52 C51 175.7(6) . . . . ? C50 C51 C52 C47 2.1(12) . . . . ? C14 C13 P1 C7 83.3(7) . . . . ? P2 C13 P1 C7 -104.8(4) . . . . ? C14 C13 P1 C1 -23.7(8) . . . . ? P2 C13 P1 C1 148.2(3) . . . . ? C14 C13 P1 Ru1 -156.3(7) . . . . ? P2 C13 P1 Ru1 15.6(3) . . . . ? C12 C7 P1 C13 161.9(7) . . . . ? C8 C7 P1 C13 -19.7(7) . . . . ? C12 C7 P1 C1 -86.9(7) . . . . ? C8 C7 P1 C1 91.6(7) . . . . ? C12 C7 P1 Ru1 59.7(7) . . . . ? C8 C7 P1 Ru1 -121.8(6) . . . . ? C6 C1 P1 C13 134.4(6) . . . . ? C2 C1 P1 C13 -46.4(7) . . . . ? C6 C1 P1 C7 25.2(7) . . . . ? C2 C1 P1 C7 -155.6(6) . . . . ? C6 C1 P1 Ru1 -116.3(6) . . . . ? C2 C1 P1 Ru1 62.9(7) . . . . ? C16 C15 P2 C13 40.0(7) . . . . ? C20 C15 P2 C13 -135.6(6) . . . . ? C16 C15 P2 C21 149.3(6) . . . . ? C20 C15 P2 C21 -26.3(7) . . . . ? C16 C15 P2 Ru1 -60.9(7) . . . . ? C20 C15 P2 Ru1 123.4(6) . . . . ? C14 C13 P2 C15 26.8(7) . . . . ? P1 C13 P2 C15 -145.1(3) . . . . ? C14 C13 P2 C21 -76.7(7) . . . . ? P1 C13 P2 C21 111.4(4) . . . . ? C14 C13 P2 Ru1 156.7(7) . . . . ? P1 C13 P2 Ru1 -15.1(3) . . . . ? C22 C21 P2 C15 89.8(7) . . . . ? C26 C21 P2 C15 -82.0(7) . . . . ? C22 C21 P2 C13 -164.7(6) . . . . ? C26 C21 P2 C13 23.6(7) . . . . ? C22 C21 P2 Ru1 -61.7(7) . . . . ? C26 C21 P2 Ru1 126.5(5) . . . . ? C34 C33 P3 C39 18.6(7) . . . . ? C38 C33 P3 C39 -167.2(6) . . . . ? C34 C33 P3 C27 -88.3(7) . . . . ? C38 C33 P3 C27 86.0(6) . . . . ? C34 C33 P3 Ru1 120.2(6) . . . . ? C38 C33 P3 Ru1 -65.5(6) . . . . ? C40 C39 P3 C33 -78.1(8) . . . . ? P4 C39 P3 C33 109.9(4) . . . . ? C40 C39 P3 C27 25.3(8) . . . . ? P4 C39 P3 C27 -146.7(3) . . . . ? C40 C39 P3 Ru1 156.5(7) . . . . ? P4 C39 P3 Ru1 -15.5(3) . . . . ? C32 C27 P3 C33 -28.9(8) . . . . ? C28 C27 P3 C33 152.3(7) . . . . ? C32 C27 P3 C39 -136.8(7) . . . . ? C28 C27 P3 C39 44.3(7) . . . . ? C32 C27 P3 Ru1 120.2(6) . . . . ? C28 C27 P3 Ru1 -58.7(7) . . . . ? C40 C39 P4 C47 -25.0(8) . . . . ? P3 C39 P4 C47 146.9(3) . . . . ? C40 C39 P4 C41 80.7(8) . . . . ? P3 C39 P4 C41 -107.5(4) . . . . ? C40 C39 P4 Ru1 -155.8(7) . . . . ? P3 C39 P4 Ru1 16.0(3) . . . . ? C52 C47 P4 C39 -29.5(7) . . . . ? C48 C47 P4 C39 148.4(6) . . . . ? C52 C47 P4 C41 -137.1(6) . . . . ? C48 C47 P4 C41 40.8(7) . . . . ? C52 C47 P4 Ru1 78.8(7) . . . . ? C48 C47 P4 Ru1 -103.3(6) . . . . ? C46 C41 P4 C39 -22.2(7) . . . . ? C42 C41 P4 C39 158.4(6) . . . . ? C46 C41 P4 C47 87.6(7) . . . . ? C42 C41 P4 C47 -91.8(6) . . . . ? C46 C41 P4 Ru1 -125.5(6) . . . . ? C42 C41 P4 Ru1 55.1(7) . . . . ? F1 C59 S1 O7 -177.5(7) . . . . ? F2 C59 S1 O7 -50.6(8) . . . . ? F3 C59 S1 O7 65.2(7) . . . . ? F1 C59 S1 O8 60.6(8) . . . . ? F2 C59 S1 O8 -172.6(7) . . . . ? F3 C59 S1 O8 -56.7(7) . . . . ? F1 C59 S1 O9 -59.2(9) . . . . ? F2 C59 S1 O9 67.6(8) . . . . ? F3 C59 S1 O9 -176.5(7) . . . . ? F6 C60 S2 O12 63.8(9) . . . . ? F5 C60 S2 O12 -58.8(9) . . . . ? F4 C60 S2 O12 -176.5(7) . . . . ? F6 C60 S2 O10 -177.9(8) . . . . ? F5 C60 S2 O10 59.5(10) . . . . ? F4 C60 S2 O10 -58.2(9) . . . . ? F6 C60 S2 O11 -53.4(9) . . . . ? F5 C60 S2 O11 -176.0(8) . . . . ? F4 C60 S2 O11 66.3(8) . . . . ? O3 P5 O1 C53 -101.5(7) . . . . ? O2 P5 O1 C53 9.3(8) . . . . ? Ru1 P5 O1 C53 130.9(7) . . . . ? O3 P5 O2 C54 21.2(7) . . . . ? O1 P5 O2 C54 -89.3(7) . . . . ? Ru1 P5 O2 C54 144.2(6) . . . . ? O1 P5 O3 C55 30.1(7) . . . . ? O2 P5 O3 C55 -81.3(7) . . . . ? Ru1 P5 O3 C55 159.3(6) . . . . ? O6 P6 O4 C56 -103.2(7) . . . . ? O5 P6 O4 C56 7.1(8) . . . . ? Ru1 P6 O4 C56 131.8(7) . . . . ? O4 P6 O5 C57 -76.0(7) . . . . ? O6 P6 O5 C57 34.2(8) . . . . ? Ru1 P6 O5 C57 152.6(6) . . . . ? O4 P6 O6 C58 31.3(7) . . . . ? O5 P6 O6 C58 -80.6(7) . . . . ? Ru1 P6 O6 C58 162.2(6) . . . . ? F2 C59 F1 F3 109.0(11) . . . . ? S1 C59 F1 F3 -120.6(11) . . . . ? F3 C59 F1 F2 -109.0(11) . . . . ? S1 C59 F1 F2 130.4(11) . . . . ? F1 C59 F2 F3 -109.3(11) . . . . ? S1 C59 F2 F3 119.5(10) . . . . ? F3 C59 F2 F1 109.3(11) . . . . ? S1 C59 F2 F1 -131.2(11) . . . . ? F3 F1 F2 C59 -43.8(8) . . . . ? C59 F1 F2 F3 43.8(8) . . . . ? F2 C59 F3 F1 -112.1(11) . . . . ? S1 C59 F3 F1 124.9(10) . . . . ? F1 C59 F3 F2 112.1(11) . . . . ? S1 C59 F3 F2 -123.0(9) . . . . ? F2 F1 F3 C59 40.5(8) . . . . ? C59 F1 F3 F2 -40.5(8) . . . . ? F1 F2 F3 C59 -39.9(7) . . . . ? C59 F2 F3 F1 39.9(7) . . . . ? F5 C60 F4 F6 116.0(11) . . . . ? S2 C60 F4 F6 -123.1(10) . . . . ? F6 C60 F4 F5 -116.0(11) . . . . ? S2 C60 F4 F5 121.0(11) . . . . ? F6 C60 F5 F4 114.6(12) . . . . ? S2 C60 F5 F4 -120.6(12) . . . . ? F4 C60 F5 F6 -114.6(12) . . . . ? S2 C60 F5 F6 124.7(13) . . . . ? F6 F4 F5 C60 -37.3(8) . . . . ? C60 F4 F5 F6 37.3(8) . . . . ? F5 C60 F6 F4 -114.0(12) . . . . ? S2 C60 F6 F4 122.0(11) . . . . ? F4 C60 F6 F5 114.0(12) . . . . ? S2 C60 F6 F5 -124.0(13) . . . . ? F5 F4 F6 C60 38.3(8) . . . . ? C60 F4 F6 F5 -38.3(8) . . . . ? F4 F5 F6 C60 -39.6(9) . . . . ? C60 F5 F6 F4 39.6(9) . . . . ? O3 P5 Ru1 P6 155.3(2) . . . . ? O1 P5 Ru1 P6 -81.9(3) . . . . ? O2 P5 Ru1 P6 38.1(2) . . . . ? O3 P5 Ru1 P4 -118.9(2) . . . . ? O1 P5 Ru1 P4 3.9(3) . . . . ? O2 P5 Ru1 P4 123.9(2) . . . . ? O3 P5 Ru1 P1 51.8(2) . . . . ? O1 P5 Ru1 P1 174.5(3) . . . . ? O2 P5 Ru1 P1 -65.5(2) . . . . ? O3 P5 Ru1 P3 -48.3(2) . . . . ? O1 P5 Ru1 P3 74.4(3) . . . . ? O2 P5 Ru1 P3 -165.6(2) . . . . ? O3 P5 Ru1 P2 77.3(3) . . . . ? O1 P5 Ru1 P2 -159.9(3) . . . . ? O2 P5 Ru1 P2 -39.9(3) . . . . ? O4 P6 Ru1 P5 -86.9(3) . . . . ? O6 P6 Ru1 P5 151.2(2) . . . . ? O5 P6 Ru1 P5 36.8(3) . . . . ? O4 P6 Ru1 P4 171.1(3) . . . . ? O6 P6 Ru1 P4 49.1(2) . . . . ? O5 P6 Ru1 P4 -65.3(3) . . . . ? O4 P6 Ru1 P1 0.6(3) . . . . ? O6 P6 Ru1 P1 -121.4(2) . . . . ? O5 P6 Ru1 P1 124.2(3) . . . . ? O4 P6 Ru1 P3 -169.8(3) . . . . ? O6 P6 Ru1 P3 68.2(3) . . . . ? O5 P6 Ru1 P3 -46.2(3) . . . . ? O4 P6 Ru1 P2 70.5(3) . . . . ? O6 P6 Ru1 P2 -51.4(2) . . . . ? O5 P6 Ru1 P2 -165.8(3) . . . . ? C39 P4 Ru1 P5 75.5(2) . . . . ? C47 P4 Ru1 P5 -38.5(3) . . . . ? C41 P4 Ru1 P5 -176.2(3) . . . . ? C39 P4 Ru1 P6 159.7(2) . . . . ? C47 P4 Ru1 P6 45.7(3) . . . . ? C41 P4 Ru1 P6 -91.9(3) . . . . ? C39 P4 Ru1 P1 -62.0(4) . . . . ? C47 P4 Ru1 P1 -176.0(4) . . . . ? C41 P4 Ru1 P1 46.4(4) . . . . ? C39 P4 Ru1 P3 -12.3(2) . . . . ? C47 P4 Ru1 P3 -126.3(3) . . . . ? C41 P4 Ru1 P3 96.1(3) . . . . ? C39 P4 Ru1 P2 -110.9(2) . . . . ? C47 P4 Ru1 P2 135.0(3) . . . . ? C41 P4 Ru1 P2 -2.6(3) . . . . ? C13 P1 Ru1 P5 157.7(2) . . . . ? C7 P1 Ru1 P5 -93.8(3) . . . . ? C1 P1 Ru1 P5 42.4(3) . . . . ? C13 P1 Ru1 P6 73.2(2) . . . . ? C7 P1 Ru1 P6 -178.3(3) . . . . ? C1 P1 Ru1 P6 -42.1(3) . . . . ? C13 P1 Ru1 P4 -63.7(4) . . . . ? C7 P1 Ru1 P4 44.8(4) . . . . ? C1 P1 Ru1 P4 -179.1(4) . . . . ? C13 P1 Ru1 P3 -110.7(2) . . . . ? C7 P1 Ru1 P3 -2.2(3) . . . . ? C1 P1 Ru1 P3 133.9(3) . . . . ? C13 P1 Ru1 P2 -11.9(2) . . . . ? C7 P1 Ru1 P2 96.6(3) . . . . ? C1 P1 Ru1 P2 -127.3(3) . . . . ? C33 P3 Ru1 P5 161.5(3) . . . . ? C39 P3 Ru1 P5 -89.7(2) . . . . ? C27 P3 Ru1 P5 19.1(3) . . . . ? C33 P3 Ru1 P6 -116.9(3) . . . . ? C39 P3 Ru1 P6 -8.1(3) . . . . ? C27 P3 Ru1 P6 100.7(4) . . . . ? C33 P3 Ru1 P4 -96.7(3) . . . . ? C39 P3 Ru1 P4 12.2(2) . . . . ? C27 P3 Ru1 P4 120.9(3) . . . . ? C33 P3 Ru1 P1 72.6(3) . . . . ? C39 P3 Ru1 P1 -178.6(2) . . . . ? C27 P3 Ru1 P1 -69.8(3) . . . . ? C33 P3 Ru1 P2 0.5(3) . . . . ? C39 P3 Ru1 P2 109.4(2) . . . . ? C27 P3 Ru1 P2 -141.9(3) . . . . ? C15 P2 Ru1 P5 90.7(4) . . . . ? C13 P2 Ru1 P5 -15.5(3) . . . . ? C21 P2 Ru1 P5 -126.5(3) . . . . ? C15 P2 Ru1 P6 13.7(3) . . . . ? C13 P2 Ru1 P6 -92.5(2) . . . . ? C21 P2 Ru1 P6 156.6(3) . . . . ? C15 P2 Ru1 P4 -73.2(3) . . . . ? C13 P2 Ru1 P4 -179.4(2) . . . . ? C21 P2 Ru1 P4 69.7(3) . . . . ? C15 P2 Ru1 P1 117.9(4) . . . . ? C13 P2 Ru1 P1 11.7(2) . . . . ? C21 P2 Ru1 P1 -99.2(3) . . . . ? C15 P2 Ru1 P3 -145.3(3) . . . . ? C13 P2 Ru1 P3 108.5(2) . . . . ? C21 P2 Ru1 P3 -2.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.697 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.092 data_cs190 _database_code_CSD 207607 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H54 F6 O9 P4 Ru S2' _chemical_formula_weight 1286.07 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' 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' S S 0.1246 0.1234 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 15.043(2) _cell_length_b 23.607(4) _cell_length_c 15.831(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5621.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7364 _exptl_absorpt_correction_T_max 0.8326 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10995 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3832 _reflns_number_gt 2486 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3832 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0081(3) 0.21116(14) 0.0300(2) 0.0195(8) Uani 1 1 d . . . C2 C -0.0324(3) 0.26246(16) -0.0071(3) 0.0271(10) Uani 1 1 d . . . H2 H -0.064(3) 0.2882(16) 0.025(3) 0.032 Uiso 1 1 d . . . C3 C -0.0091(3) 0.27524(18) -0.0892(3) 0.0320(10) Uani 1 1 d . . . H3 H -0.026(3) 0.3091(18) -0.113(3) 0.038 Uiso 1 1 d . . . C4 C 0.0407(3) 0.23749(19) -0.1364(3) 0.0352(11) Uani 1 1 d . . . H4 H 0.058(3) 0.2439(16) -0.199(3) 0.042 Uiso 1 1 d . . . C5 C 0.0640(3) 0.1862(2) -0.1006(3) 0.0376(12) Uani 1 1 d . . . H5 H 0.101(3) 0.1584(17) -0.135(3) 0.045 Uiso 1 1 d . . . C6 C 0.0399(3) 0.17321(18) -0.0189(3) 0.0285(10) Uani 1 1 d . . . H6 H 0.056(3) 0.1405(17) 0.000(3) 0.034 Uiso 1 1 d . . . C7 C -0.0310(3) 0.11871(14) 0.1404(3) 0.0182(9) Uani 1 1 d . . . C8 C 0.0516(3) 0.09340(16) 0.1554(3) 0.0275(11) Uani 1 1 d . . . H8 H 0.101(3) 0.1166(16) 0.170(3) 0.033 Uiso 1 1 d . . . C9 C 0.0627(3) 0.03566(17) 0.1440(3) 0.0354(12) Uani 1 1 d . . . H9 H 0.123(3) 0.0241(17) 0.153(3) 0.042 Uiso 1 1 d . . . C10 C -0.0082(4) 0.00301(17) 0.1187(3) 0.0430(13) Uani 1 1 d . . . H10 H -0.006(3) -0.032(2) 0.111(3) 0.052 Uiso 1 1 d . . . C11 C -0.0907(4) 0.02717(18) 0.1063(3) 0.0423(13) Uani 1 1 d . . . H11 H -0.137(3) 0.0065(19) 0.089(3) 0.051 Uiso 1 1 d . . . C12 C -0.1017(3) 0.08511(17) 0.1165(3) 0.0293(11) Uani 1 1 d . . . H12 H -0.151(3) 0.0999(17) 0.108(3) 0.035 Uiso 1 1 d . . . C13 C 0.1551(3) 0.21513(14) 0.3542(3) 0.0185(9) Uani 1 1 d . . . C14 C 0.2162(3) 0.21520(17) 0.4153(3) 0.0224(10) Uani 1 1 d . . . H14A H 0.273(3) 0.2304(15) 0.408(3) 0.027 Uiso 1 1 d . . . H14B H 0.205(3) 0.1988(15) 0.467(3) 0.027 Uiso 1 1 d . . . C15 C 0.2279(2) 0.31177(14) 0.2555(3) 0.0195(8) Uani 1 1 d . . . C16 C 0.2050(3) 0.35516(16) 0.3113(3) 0.0260(10) Uani 1 1 d . . . H16 H 0.156(3) 0.3514(16) 0.345(3) 0.031 Uiso 1 1 d . . . C17 C 0.2530(3) 0.40550(18) 0.3120(3) 0.0363(12) Uani 1 1 d . . . H17 H 0.236(3) 0.4345(18) 0.354(3) 0.044 Uiso 1 1 d . . . C18 C 0.3234(3) 0.41275(18) 0.2578(4) 0.0387(12) Uani 1 1 d . . . H18 H 0.352(3) 0.4473(18) 0.264(3) 0.046 Uiso 1 1 d . . . C19 C 0.3471(3) 0.3703(2) 0.2037(3) 0.0365(12) Uani 1 1 d . . . H19 H 0.394(3) 0.3686(17) 0.168(3) 0.044 Uiso 1 1 d . . . C20 C 0.3003(3) 0.31974(18) 0.2024(3) 0.0289(10) Uani 1 1 d . . . H20 H 0.315(3) 0.2917(17) 0.167(3) 0.035 Uiso 1 1 d . . . C21 C 0.2190(2) 0.19950(15) 0.1840(3) 0.0203(9) Uani 1 1 d . . . C22 C 0.2706(3) 0.15635(19) 0.2179(3) 0.0324(11) Uani 1 1 d . . . H22 H 0.274(3) 0.1529(18) 0.276(3) 0.039 Uiso 1 1 d . . . C23 C 0.3144(3) 0.11919(19) 0.1644(4) 0.0430(13) Uani 1 1 d . . . H23 H 0.343(3) 0.0918(19) 0.191(4) 0.052 Uiso 1 1 d . . . C24 C 0.3083(3) 0.12460(19) 0.0786(4) 0.0427(13) Uani 1 1 d . . . H24 H 0.341(3) 0.0994(18) 0.035(3) 0.051 Uiso 1 1 d . . . C25 C 0.2579(3) 0.16762(17) 0.0441(3) 0.0314(11) Uani 1 1 d . . . H25 H 0.255(3) 0.1692(16) -0.015(3) 0.038 Uiso 1 1 d . . . C26 C 0.2136(3) 0.20544(17) 0.0966(3) 0.0239(10) Uani 1 1 d . . . H26 H 0.181(3) 0.2357(15) 0.072(3) 0.029 Uiso 1 1 d . . . C27 C 0.4649(4) -0.0052(2) 0.8240(4) 0.0631(17) Uani 1 1 d . . . H27A H 0.4702 -0.0455 0.8128 0.076 Uiso 1 1 calc R . . H27B H 0.4029 0.0044 0.8330 0.076 Uiso 1 1 calc R . . H27C H 0.4989 0.0043 0.8741 0.076 Uiso 1 1 calc R . . C28 C 0.5000 0.0276(2) 0.7500 0.0400(16) Uani 1 2 d S . . C29 C 0.6810(4) 0.0545(2) -0.0425(3) 0.0484(14) Uani 1 1 d . . . P1 P -0.03809(7) 0.19572(4) 0.14015(7) 0.0169(2) Uani 1 1 d . . . P2 P 0.15752(5) 0.24860(3) 0.25090(7) 0.0161(2) Uani 1 1 d . . . F1 F 0.6746(3) 0.00480(11) 0.0039(3) 0.0813(11) Uani 1 1 d . . . F2 F 0.7690(2) 0.06452(12) -0.0445(2) 0.0617(9) Uani 1 1 d . . . F3 F 0.6577(2) 0.04121(13) -0.1212(2) 0.0695(10) Uani 1 1 d . . . S1 S 0.61964(8) 0.10949(4) 0.00362(8) 0.0331(3) Uani 1 1 d . . . O1 O 0.5292(2) 0.08916(12) 0.0002(2) 0.0468(9) Uani 1 1 d . . . O2 O 0.6387(2) 0.15608(11) -0.0526(2) 0.0374(8) Uani 1 1 d . . . O3 O 0.6570(2) 0.11403(12) 0.0872(2) 0.0457(9) Uani 1 1 d . . . O4 O 0.5000 0.07782(15) 0.7500 0.0403(11) Uani 1 2 d S . . O5 O -0.0007(2) 0.32501(11) 0.15875(19) 0.0234(6) Uani 1 1 d . . . H28A H 0.036(3) 0.3261(18) 0.129(3) 0.028 Uiso 1 1 d . . . H28B H -0.005(3) 0.3560(17) 0.181(3) 0.028 Uiso 1 1 d . . . Ru1 Ru 0.0000 0.255739(15) 0.2500 0.01388(13) Uani 1 2 d S . . 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 0.014(2) 0.0308(19) 0.014(2) -0.0027(15) -0.002(2) 0.0007(17) C2 0.026(2) 0.034(2) 0.021(2) -0.0028(19) 0.003(2) 0.0027(17) C3 0.030(3) 0.047(2) 0.019(2) 0.0070(19) -0.005(2) 0.000(2) C4 0.023(2) 0.066(3) 0.016(3) -0.001(2) 0.002(2) -0.006(2) C5 0.033(3) 0.059(3) 0.021(3) -0.003(2) 0.007(2) 0.012(2) C6 0.029(2) 0.038(2) 0.018(3) -0.0007(19) 0.002(2) 0.0064(19) C7 0.020(2) 0.0228(19) 0.012(2) -0.0031(16) 0.0018(18) -0.0008(16) C8 0.026(3) 0.029(2) 0.027(3) 0.0009(19) 0.000(2) 0.0021(19) C9 0.041(3) 0.032(2) 0.033(3) 0.007(2) 0.000(3) 0.011(2) C10 0.069(4) 0.0194(19) 0.041(3) 0.0016(18) -0.007(3) 0.003(3) C11 0.049(4) 0.030(3) 0.048(4) 0.003(2) -0.014(3) -0.014(2) C12 0.024(3) 0.035(2) 0.029(3) 0.0044(19) -0.007(2) 0.0008(19) C13 0.017(2) 0.0193(18) 0.020(2) 0.0000(16) 0.005(2) 0.0002(15) C14 0.019(3) 0.033(2) 0.014(3) 0.0024(18) -0.002(2) 0.0003(18) C15 0.0110(19) 0.0286(17) 0.019(2) 0.007(2) -0.003(2) -0.0017(14) C16 0.019(2) 0.031(2) 0.028(3) 0.0012(19) 0.000(2) -0.0026(18) C17 0.034(3) 0.033(2) 0.042(3) -0.005(2) -0.011(3) 0.001(2) C18 0.036(3) 0.035(2) 0.045(3) 0.009(3) -0.013(3) -0.013(2) C19 0.029(3) 0.053(3) 0.028(3) 0.014(2) 0.001(2) -0.017(2) C20 0.027(3) 0.042(3) 0.018(3) 0.0059(19) 0.001(2) -0.006(2) C21 0.011(2) 0.029(2) 0.021(2) 0.0013(17) 0.0042(19) -0.0001(16) C22 0.029(3) 0.040(2) 0.028(3) 0.002(2) 0.006(2) 0.007(2) C23 0.040(3) 0.043(3) 0.047(4) 0.008(2) 0.007(3) 0.018(2) C24 0.046(3) 0.038(3) 0.044(4) -0.007(2) 0.015(3) 0.008(2) C25 0.032(3) 0.037(2) 0.025(3) -0.004(2) 0.010(2) -0.003(2) C26 0.020(2) 0.028(2) 0.024(3) 0.0008(19) 0.001(2) 0.0002(17) C27 0.068(4) 0.062(3) 0.059(4) 0.012(3) 0.010(3) -0.006(3) C28 0.034(4) 0.042(4) 0.044(4) 0.000 -0.007(4) 0.000 C29 0.042(4) 0.075(4) 0.028(3) -0.010(3) -0.006(3) -0.024(3) P1 0.0142(5) 0.0232(5) 0.0133(6) -0.0020(4) 0.0005(5) 0.0020(4) P2 0.0115(5) 0.0244(4) 0.0123(5) 0.0012(5) 0.0009(5) -0.0008(3) F1 0.119(3) 0.0368(15) 0.088(3) 0.0107(15) 0.016(3) 0.0126(17) F2 0.050(2) 0.082(2) 0.053(2) 0.0037(16) -0.0065(17) 0.0189(16) F3 0.078(2) 0.086(2) 0.044(2) -0.0258(16) -0.0086(19) 0.0063(17) S1 0.0350(7) 0.0347(6) 0.0295(7) 0.0045(5) -0.0053(6) -0.0031(5) O1 0.032(2) 0.0515(18) 0.057(3) -0.0013(16) -0.0051(18) -0.0120(14) O2 0.0298(19) 0.0401(16) 0.042(2) 0.0206(15) -0.0053(16) -0.0064(13) O3 0.054(2) 0.0538(19) 0.029(2) 0.0002(15) -0.0180(19) 0.0032(16) O4 0.062(3) 0.026(2) 0.033(3) 0.000 -0.009(3) 0.000 O5 0.0246(16) 0.0259(13) 0.0198(17) 0.0011(11) 0.0055(16) 0.0035(15) Ru1 0.0112(2) 0.0202(2) 0.0102(2) 0.000 0.0013(2) 0.000 _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 C6 1.387(6) . ? C1 C2 1.394(5) . ? C1 P1 1.838(4) . ? C2 C3 1.379(6) . ? C3 C4 1.384(7) . ? C4 C5 1.381(7) . ? C5 C6 1.378(6) . ? C7 C12 1.380(6) . ? C7 C8 1.398(6) . ? C7 P1 1.821(3) . ? C8 C9 1.385(6) . ? C9 C10 1.376(7) . ? C10 C11 1.380(7) . ? C11 C12 1.387(6) . ? C13 C14 1.334(6) . ? C13 P2 1.816(4) . ? C13 P1 1.822(4) 7_556 ? C15 C20 1.387(6) . ? C15 C16 1.396(6) . ? C15 P2 1.831(3) . ? C16 C17 1.391(6) . ? C17 C18 1.373(7) . ? C18 C19 1.366(7) . ? C19 C20 1.385(6) . ? C21 C22 1.389(6) . ? C21 C26 1.393(6) . ? C21 P2 1.823(4) . ? C22 C23 1.386(7) . ? C23 C24 1.367(7) . ? C24 C25 1.381(7) . ? C25 C26 1.390(6) . ? C27 C28 1.500(6) . ? C28 O4 1.186(7) . ? C28 C27 1.500(6) 7_657 ? C29 F3 1.332(6) . ? C29 F2 1.345(6) . ? C29 F1 1.388(6) . ? C29 S1 1.752(6) . ? P1 C13 1.822(4) 7_556 ? P1 Ru1 2.3151(11) . ? P2 Ru1 2.3756(9) . ? S1 O3 1.442(3) . ? S1 O1 1.443(3) . ? S1 O2 1.444(3) . ? O5 Ru1 2.182(3) . ? Ru1 O5 2.182(3) 7_556 ? Ru1 P1 2.3151(11) 7_556 ? Ru1 P2 2.3756(9) 7_556 ? 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 C6 C1 C2 117.5(4) . . ? C6 C1 P1 122.0(3) . . ? C2 C1 P1 120.5(3) . . ? C3 C2 C1 121.3(4) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 118.7(4) . . ? C6 C5 C4 120.9(4) . . ? C5 C6 C1 121.1(4) . . ? C12 C7 C8 119.1(4) . . ? C12 C7 P1 121.9(3) . . ? C8 C7 P1 118.6(3) . . ? C9 C8 C7 120.4(4) . . ? C10 C9 C8 119.7(4) . . ? C9 C10 C11 120.5(4) . . ? C10 C11 C12 119.8(4) . . ? C7 C12 C11 120.5(4) . . ? C14 C13 P2 129.7(3) . . ? C14 C13 P1 129.1(3) . 7_556 ? P2 C13 P1 99.9(2) . 7_556 ? C20 C15 C16 118.5(4) . . ? C20 C15 P2 122.7(3) . . ? C16 C15 P2 118.7(3) . . ? C17 C16 C15 120.2(4) . . ? C18 C17 C16 120.1(4) . . ? C19 C18 C17 120.1(4) . . ? C18 C19 C20 120.6(5) . . ? C19 C20 C15 120.5(4) . . ? C22 C21 C26 119.4(4) . . ? C22 C21 P2 121.7(3) . . ? C26 C21 P2 118.9(3) . . ? C23 C22 C21 119.5(5) . . ? C24 C23 C22 121.1(5) . . ? C23 C24 C25 119.9(5) . . ? C24 C25 C26 119.9(5) . . ? C25 C26 C21 120.1(4) . . ? O4 C28 C27 121.1(3) . 7_657 ? O4 C28 C27 121.1(3) . . ? C27 C28 C27 117.9(6) 7_657 . ? F3 C29 F2 106.2(4) . . ? F3 C29 F1 106.1(4) . . ? F2 C29 F1 103.3(4) . . ? F3 C29 S1 115.2(4) . . ? F2 C29 S1 113.5(3) . . ? F1 C29 S1 111.7(4) . . ? C7 P1 C13 107.93(17) . 7_556 ? C7 P1 C1 100.69(16) . . ? C13 P1 C1 103.54(19) 7_556 . ? C7 P1 Ru1 126.49(13) . . ? C13 P1 Ru1 92.78(13) 7_556 . ? C1 P1 Ru1 122.05(12) . . ? C13 P2 C21 104.87(17) . . ? C13 P2 C15 109.28(19) . . ? C21 P2 C15 104.32(17) . . ? C13 P2 Ru1 90.95(13) . . ? C21 P2 Ru1 123.22(13) . . ? C15 P2 Ru1 121.30(11) . . ? O3 S1 O1 115.2(2) . . ? O3 S1 O2 115.62(19) . . ? O1 S1 O2 114.6(2) . . ? O3 S1 C29 103.4(2) . . ? O1 S1 C29 103.6(2) . . ? O2 S1 C29 101.7(2) . . ? O5 Ru1 O5 82.91(16) 7_556 . ? O5 Ru1 P1 163.16(9) 7_556 . ? O5 Ru1 P1 87.72(9) . . ? O5 Ru1 P1 87.72(9) 7_556 7_556 ? O5 Ru1 P1 163.16(9) . 7_556 ? P1 Ru1 P1 104.54(5) . 7_556 ? O5 Ru1 P2 93.55(9) 7_556 7_556 ? O5 Ru1 P2 92.54(9) . 7_556 ? P1 Ru1 P2 72.85(4) . 7_556 ? P1 Ru1 P2 102.00(4) 7_556 7_556 ? O5 Ru1 P2 92.54(9) 7_556 . ? O5 Ru1 P2 93.55(9) . . ? P1 Ru1 P2 102.00(4) . . ? P1 Ru1 P2 72.85(4) 7_556 . ? P2 Ru1 P2 171.86(4) 7_556 . ? 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 C6 C1 C2 C3 -0.4(6) . . . . ? P1 C1 C2 C3 178.8(3) . . . . ? C1 C2 C3 C4 -1.2(7) . . . . ? C2 C3 C4 C5 2.1(7) . . . . ? C3 C4 C5 C6 -1.4(7) . . . . ? C4 C5 C6 C1 -0.3(7) . . . . ? C2 C1 C6 C5 1.2(6) . . . . ? P1 C1 C6 C5 -178.1(4) . . . . ? C12 C7 C8 C9 2.0(6) . . . . ? P1 C7 C8 C9 -170.5(4) . . . . ? C7 C8 C9 C10 -0.9(7) . . . . ? C8 C9 C10 C11 -1.2(8) . . . . ? C9 C10 C11 C12 2.1(8) . . . . ? C8 C7 C12 C11 -1.0(7) . . . . ? P1 C7 C12 C11 171.2(4) . . . . ? C10 C11 C12 C7 -1.0(8) . . . . ? C20 C15 C16 C17 1.3(6) . . . . ? P2 C15 C16 C17 -175.2(3) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C16 C17 C18 C19 -0.8(7) . . . . ? C17 C18 C19 C20 0.5(7) . . . . ? C18 C19 C20 C15 0.7(7) . . . . ? C16 C15 C20 C19 -1.6(6) . . . . ? P2 C15 C20 C19 174.7(3) . . . . ? C26 C21 C22 C23 -1.4(7) . . . . ? P2 C21 C22 C23 178.4(4) . . . . ? C21 C22 C23 C24 0.7(8) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C24 C25 C26 C21 -0.9(7) . . . . ? C22 C21 C26 C25 1.5(6) . . . . ? P2 C21 C26 C25 -178.2(3) . . . . ? C12 C7 P1 C13 21.9(4) . . . 7_556 ? C8 C7 P1 C13 -165.9(3) . . . 7_556 ? C12 C7 P1 C1 -86.3(4) . . . . ? C8 C7 P1 C1 86.0(4) . . . . ? C12 C7 P1 Ru1 129.5(3) . . . . ? C8 C7 P1 Ru1 -58.2(4) . . . . ? C6 C1 P1 C7 -22.1(4) . . . . ? C2 C1 P1 C7 158.7(3) . . . . ? C6 C1 P1 C13 -133.6(4) . . . 7_556 ? C2 C1 P1 C13 47.1(4) . . . 7_556 ? C6 C1 P1 Ru1 124.3(3) . . . . ? C2 C1 P1 Ru1 -55.0(4) . . . . ? C14 C13 P2 C21 83.0(4) . . . . ? P1 C13 P2 C21 -109.32(18) 7_556 . . . ? C14 C13 P2 C15 -28.4(4) . . . . ? P1 C13 P2 C15 139.33(16) 7_556 . . . ? C14 C13 P2 Ru1 -152.2(4) . . . . ? P1 C13 P2 Ru1 15.53(14) 7_556 . . . ? C22 C21 P2 C13 -15.9(4) . . . . ? C26 C21 P2 C13 163.9(3) . . . . ? C22 C21 P2 C15 99.0(4) . . . . ? C26 C21 P2 C15 -81.3(3) . . . . ? C22 C21 P2 Ru1 -117.1(3) . . . . ? C26 C21 P2 Ru1 62.7(3) . . . . ? C20 C15 P2 C13 123.7(4) . . . . ? C16 C15 P2 C13 -60.0(4) . . . . ? C20 C15 P2 C21 12.0(4) . . . . ? C16 C15 P2 C21 -171.7(3) . . . . ? C20 C15 P2 Ru1 -132.8(3) . . . . ? C16 C15 P2 Ru1 43.5(4) . . . . ? F3 C29 S1 O3 178.9(4) . . . . ? F2 C29 S1 O3 -58.4(4) . . . . ? F1 C29 S1 O3 57.9(4) . . . . ? F3 C29 S1 O1 58.4(4) . . . . ? F2 C29 S1 O1 -178.9(4) . . . . ? F1 C29 S1 O1 -62.7(4) . . . . ? F3 C29 S1 O2 -60.8(4) . . . . ? F2 C29 S1 O2 61.9(4) . . . . ? F1 C29 S1 O2 178.1(3) . . . . ? C7 P1 Ru1 O5 -139.6(3) . . . 7_556 ? C13 P1 Ru1 O5 -24.8(3) 7_556 . . 7_556 ? C1 P1 Ru1 O5 83.1(3) . . . 7_556 ? C7 P1 Ru1 O5 164.36(18) . . . . ? C13 P1 Ru1 O5 -80.85(15) 7_556 . . . ? C1 P1 Ru1 O5 27.02(17) . . . . ? C7 P1 Ru1 P1 -3.95(16) . . . 7_556 ? C13 P1 Ru1 P1 110.84(12) 7_556 . . 7_556 ? C1 P1 Ru1 P1 -141.28(16) . . . 7_556 ? C7 P1 Ru1 P2 -102.27(17) . . . 7_556 ? C13 P1 Ru1 P2 12.52(12) 7_556 . . 7_556 ? C1 P1 Ru1 P2 120.39(15) . . . 7_556 ? C7 P1 Ru1 P2 71.21(16) . . . . ? C13 P1 Ru1 P2 -174.00(12) 7_556 . . . ? C1 P1 Ru1 P2 -66.13(15) . . . . ? C13 P2 Ru1 O5 74.28(14) . . . 7_556 ? C21 P2 Ru1 O5 -177.19(17) . . . 7_556 ? C15 P2 Ru1 O5 -39.08(19) . . . 7_556 ? C13 P2 Ru1 O5 157.33(14) . . . . ? C21 P2 Ru1 O5 -94.14(17) . . . . ? C15 P2 Ru1 O5 43.97(19) . . . . ? C13 P2 Ru1 P1 -114.25(12) . . . . ? C21 P2 Ru1 P1 -5.72(16) . . . . ? C15 P2 Ru1 P1 132.39(17) . . . . ? C13 P2 Ru1 P1 -12.54(11) . . . 7_556 ? C21 P2 Ru1 P1 95.99(16) . . . 7_556 ? C15 P2 Ru1 P1 -125.91(18) . . . 7_556 ? C13 P2 Ru1 P2 -64.21(11) . . . 7_556 ? C21 P2 Ru1 P2 44.31(15) . . . 7_556 ? C15 P2 Ru1 P2 -177.58(17) . . . 7_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H28B O4 0.81(4) 1.91(4) 2.711(4) 168(4) 6_566 O5 H28A S1 0.73(5) 2.88(5) 3.504(3) 145(4) 6_565 O5 H28A O2 0.73(5) 2.00(5) 2.723(4) 170(5) 6_565 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.591 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.068 data_cs191 _database_code_CSD 207608 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 F6 O7 P4 Ru S2' _chemical_formula_weight 1185.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.109(3) _cell_length_b 11.4033(12) _cell_length_c 22.700(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.936(15) _cell_angle_gamma 90.00 _cell_volume 5189.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Plae yellow' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27325 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 22.49 _reflns_number_total 6477 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6477 _refine_ls_number_parameters 657 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2419(3) -0.0724(4) -0.0383(2) 0.0308(12) Uani 1 1 d . . . C2 C 0.2175(3) -0.1873(4) -0.0535(3) 0.0505(15) Uani 1 1 d . . . H2 H 0.1750 -0.2066 -0.0563 0.061 Uiso 1 1 calc R . . C3 C 0.2564(4) -0.2719(4) -0.0643(3) 0.0608(18) Uani 1 1 d . . . H3 H 0.2403 -0.3491 -0.0739 0.073 Uiso 1 1 calc R . . C4 C 0.3174(4) -0.2455(5) -0.0614(3) 0.0625(19) Uani 1 1 d . . . H4 H 0.3426 -0.3039 -0.0700 0.075 Uiso 1 1 calc R . . C5 C 0.3429(3) -0.1334(5) -0.0458(3) 0.0633(18) Uani 1 1 d . . . H5 H 0.3857 -0.1156 -0.0425 0.076 Uiso 1 1 calc R . . C6 C 0.3035(3) -0.0462(4) -0.0348(3) 0.0437(14) Uani 1 1 d . . . H6 H 0.3199 0.0308 -0.0251 0.052 Uiso 1 1 calc R . . C7 C 0.1327(2) 0.0768(4) -0.1070(2) 0.0304(11) Uani 1 1 d . . . C8 C 0.0699(3) 0.0224(5) -0.1363(3) 0.0558(16) Uani 1 1 d . . . H8 H 0.0569 -0.0325 -0.1129 0.067 Uiso 1 1 calc R . . C9 C 0.0275(3) 0.0498(6) -0.1993(3) 0.0683(19) Uani 1 1 d . . . H9 H -0.0146 0.0138 -0.2186 0.082 Uiso 1 1 calc R . . C10 C 0.0457(3) 0.1290(5) -0.2344(3) 0.0588(16) Uani 1 1 d . . . H10 H 0.0163 0.1472 -0.2774 0.071 Uiso 1 1 calc R . . C11 C 0.1071(3) 0.1811(4) -0.2064(3) 0.0504(15) Uani 1 1 d . . . H11 H 0.1201 0.2342 -0.2305 0.060 Uiso 1 1 calc R . . C12 C 0.1501(3) 0.1562(4) -0.1428(2) 0.0367(12) Uani 1 1 d . . . H12 H 0.1917 0.1941 -0.1238 0.044 Uiso 1 1 calc R . . C13 C 0.1469(2) -0.0181(4) 0.0190(2) 0.0305(11) Uani 1 1 d . . . H13A H 0.1669 -0.0910 0.0419 0.037 Uiso 1 1 calc R . . H13B H 0.0996 -0.0306 -0.0094 0.037 Uiso 1 1 calc R . . C14 C 0.0779(2) 0.1757(4) 0.0470(2) 0.0278(11) Uani 1 1 d . . . C15 C 0.0484(2) 0.2019(4) 0.0884(3) 0.0384(12) Uani 1 1 d . . . H15 H 0.0709 0.1835 0.1327 0.046 Uiso 1 1 calc R . . C16 C -0.0134(3) 0.2546(4) 0.0656(3) 0.0501(16) Uani 1 1 d . . . H16 H -0.0323 0.2720 0.0947 0.060 Uiso 1 1 calc R . . C17 C -0.0480(3) 0.2825(4) 0.0003(3) 0.0470(15) Uani 1 1 d . . . H17 H -0.0901 0.3185 -0.0150 0.056 Uiso 1 1 calc R . . C18 C -0.0197(2) 0.2564(4) -0.0413(3) 0.0443(14) Uani 1 1 d . . . H18 H -0.0428 0.2740 -0.0857 0.053 Uiso 1 1 calc R . . C19 C 0.0428(2) 0.2042(4) -0.0187(3) 0.0383(12) Uani 1 1 d . . . H19 H 0.0617 0.1878 -0.0479 0.046 Uiso 1 1 calc R . . C20 C 0.1708(2) 0.0438(4) 0.1523(2) 0.0264(11) Uani 1 1 d . . . C21 C 0.1933(2) 0.1118(4) 0.2084(2) 0.0340(12) Uani 1 1 d . . . H21 H 0.2053 0.1904 0.2068 0.041 Uiso 1 1 calc R . . C22 C 0.1983(3) 0.0649(5) 0.2662(3) 0.0468(14) Uani 1 1 d . . . H22 H 0.2137 0.1115 0.3039 0.056 Uiso 1 1 calc R . . C23 C 0.1805(3) -0.0501(5) 0.2689(3) 0.0551(16) Uani 1 1 d . . . H23 H 0.1842 -0.0821 0.3084 0.066 Uiso 1 1 calc R . . C24 C 0.1575(3) -0.1180(5) 0.2139(3) 0.0575(17) Uani 1 1 d . . . H24 H 0.1452 -0.1964 0.2158 0.069 Uiso 1 1 calc R . . C25 C 0.1523(3) -0.0718(4) 0.1555(3) 0.0428(14) Uani 1 1 d . . . H25 H 0.1363 -0.1187 0.1179 0.051 Uiso 1 1 calc R . . C26 C 0.4034(2) 0.0899(4) 0.1241(2) 0.0360(12) Uani 1 1 d . . . C27 C 0.4381(3) 0.1905(5) 0.1231(3) 0.0532(16) Uani 1 1 d . . . H27 H 0.4209 0.2643 0.1263 0.064 Uiso 1 1 calc R . . C28 C 0.4980(3) 0.1834(7) 0.1174(3) 0.080(2) Uani 1 1 d . . . H28 H 0.5209 0.2523 0.1163 0.097 Uiso 1 1 calc R . . C29 C 0.5238(4) 0.0773(9) 0.1134(4) 0.092(3) Uani 1 1 d . . . H29 H 0.5654 0.0727 0.1114 0.110 Uiso 1 1 calc R . . C30 C 0.4894(4) -0.0226(7) 0.1121(4) 0.085(2) Uani 1 1 d . . . H30 H 0.5068 -0.0954 0.1073 0.102 Uiso 1 1 calc R . . C31 C 0.4295(3) -0.0193(5) 0.1177(3) 0.0573(16) Uani 1 1 d . . . H31 H 0.4066 -0.0890 0.1171 0.069 Uiso 1 1 calc R . . C32 C 0.3188(2) -0.0411(4) 0.1668(2) 0.0293(11) Uani 1 1 d . . . C33 C 0.3387(3) -0.0537(4) 0.2329(3) 0.0450(14) Uani 1 1 d . . . H33 H 0.3548 0.0116 0.2604 0.054 Uiso 1 1 calc R . . C34 C 0.3351(3) -0.1635(5) 0.2591(3) 0.0636(19) Uani 1 1 d . . . H34 H 0.3488 -0.1720 0.3041 0.076 Uiso 1 1 calc R . . C35 C 0.3112(3) -0.2594(5) 0.2183(4) 0.068(2) Uani 1 1 d . . . H35 H 0.3078 -0.3326 0.2357 0.082 Uiso 1 1 calc R . . C36 C 0.2926(3) -0.2484(4) 0.1530(4) 0.0607(18) Uani 1 1 d . . . H36 H 0.2771 -0.3144 0.1259 0.073 Uiso 1 1 calc R . . C37 C 0.2963(3) -0.1406(4) 0.1265(3) 0.0420(13) Uani 1 1 d . . . H37 H 0.2838 -0.1338 0.0816 0.050 Uiso 1 1 calc R . . C38 C 0.3389(2) 0.2094(3) 0.1963(2) 0.0278(11) Uani 1 1 d . . . H38A H 0.3861 0.2298 0.2203 0.033 Uiso 1 1 calc R . . H38B H 0.3203 0.1850 0.2267 0.033 Uiso 1 1 calc R . . C39 C 0.3528(2) 0.4386(4) 0.1471(2) 0.0268(11) Uani 1 1 d . . . C40 C 0.4047(3) 0.4639(4) 0.2066(3) 0.0447(14) Uani 1 1 d . . . H40 H 0.4077 0.4250 0.2443 0.054 Uiso 1 1 calc R . . C41 C 0.4523(3) 0.5465(5) 0.2108(3) 0.0585(17) Uani 1 1 d . . . H41 H 0.4876 0.5624 0.2513 0.070 Uiso 1 1 calc R . . C42 C 0.4488(3) 0.6054(5) 0.1569(3) 0.0524(16) Uani 1 1 d . . . H42 H 0.4816 0.6609 0.1603 0.063 Uiso 1 1 calc R . . C43 C 0.3966(3) 0.5823(4) 0.0976(3) 0.0439(14) Uani 1 1 d . . . H43 H 0.3935 0.6230 0.0605 0.053 Uiso 1 1 calc R . . C44 C 0.3485(2) 0.4989(4) 0.0924(2) 0.0324(12) Uani 1 1 d . . . H44 H 0.3131 0.4835 0.0518 0.039 Uiso 1 1 calc R . . C45 C 0.2427(2) 0.4023(3) 0.1798(2) 0.0279(11) Uani 1 1 d . . . C46 C 0.1784(3) 0.4404(4) 0.1409(3) 0.0421(13) Uani 1 1 d . . . H46 H 0.1591 0.4242 0.0961 0.051 Uiso 1 1 calc R . . C47 C 0.1428(3) 0.5026(5) 0.1685(4) 0.065(2) Uani 1 1 d . . . H47 H 0.0994 0.5294 0.1425 0.078 Uiso 1 1 calc R . . C48 C 0.1717(4) 0.5247(5) 0.2347(4) 0.071(2) Uani 1 1 d . . . H48 H 0.1478 0.5670 0.2535 0.085 Uiso 1 1 calc R . . C49 C 0.2346(4) 0.4858(5) 0.2732(3) 0.0619(18) Uani 1 1 d . . . H49 H 0.2534 0.5008 0.3181 0.074 Uiso 1 1 calc R . . C50 C 0.2705(3) 0.4249(4) 0.2464(3) 0.0427(14) Uani 1 1 d . . . H50 H 0.3138 0.3985 0.2730 0.051 Uiso 1 1 calc R . . C72 C 0.0878(3) 0.4629(4) -0.1024(3) 0.0494(15) Uani 1 1 d . . . C75 C 0.4275(5) 0.3862(7) 0.9420(5) 0.097(3) Uani 1 1 d . . . P1 P 0.19315(6) 0.04391(9) -0.02437(6) 0.0266(3) Uani 1 1 d . . . P2 P 0.16031(6) 0.10677(9) 0.07506(6) 0.0245(3) Uani 1 1 d . . . P3 P 0.32506(6) 0.10003(9) 0.13233(6) 0.0247(3) Uani 1 1 d . . . P4 P 0.29010(6) 0.32837(9) 0.14151(6) 0.0237(3) Uani 1 1 d . . . F1 F 0.04368(15) 0.4749(3) -0.07738(18) 0.0644(10) Uani 1 1 d . . . F2 F 0.08800(17) 0.5647(3) -0.13270(17) 0.0713(11) Uani 1 1 d . . . F3 F 0.0666(2) 0.3793(3) -0.14615(19) 0.1033(16) Uani 1 1 d . . . F4 F 0.4161(3) 0.4225(4) 0.9901(3) 0.150(3) Uani 1 1 d . . . F5 F 0.4934(3) 0.3510(6) 0.9665(3) 0.144(2) Uani 1 1 d . . . F6 F 0.4265(4) 0.4723(4) 0.9043(3) 0.166(3) Uani 1 1 d . . . S1 S 0.17134(6) 0.43780(9) -0.03985(6) 0.0288(3) Uani 1 1 d . . . S2 S 0.37879(8) 0.26149(12) 0.90135(8) 0.0494(4) Uani 1 1 d . . . O1 O 0.16439(15) 0.3225(2) -0.01444(15) 0.0345(8) Uani 1 1 d . . . O2 O 0.18130(17) 0.5335(3) 0.00470(16) 0.0408(9) Uani 1 1 d . . . O3 O 0.21339(17) 0.4365(3) -0.07368(16) 0.0396(9) Uani 1 1 d . . . O4 O 0.3912(2) 0.1784(3) 0.9506(2) 0.0738(13) Uani 1 1 d . . . O5 O 0.3994(2) 0.2375(4) 0.8513(2) 0.0719(13) Uani 1 1 d . . . O6 O 0.3118(2) 0.3014(6) 0.8804(3) 0.133(2) Uani 1 1 d . . . O7 O 0.30356(16) 0.2645(3) 0.00609(17) 0.0306(8) Uani 1 1 d D . . H51 H 0.3398(18) 0.230(4) 0.007(3) 0.060(18) Uiso 1 1 d D . . H52 H 0.296(7) 0.331(7) -0.019(6) 0.29(7) Uiso 1 1 d D . . Ru1 Ru 0.240280(17) 0.19713(3) 0.051368(17) 0.01942(12) 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 0.054(3) 0.021(2) 0.023(3) -0.0057(19) 0.022(3) -0.001(2) C2 0.075(4) 0.034(3) 0.052(4) -0.012(3) 0.036(3) -0.011(3) C3 0.110(6) 0.027(3) 0.054(5) -0.009(2) 0.043(4) 0.003(3) C4 0.114(6) 0.040(4) 0.057(5) 0.009(3) 0.059(5) 0.029(4) C5 0.088(5) 0.055(4) 0.074(5) 0.010(3) 0.061(4) 0.016(3) C6 0.066(4) 0.029(3) 0.052(4) 0.000(2) 0.040(3) 0.005(3) C7 0.037(3) 0.033(3) 0.018(3) -0.010(2) 0.008(2) -0.006(2) C8 0.057(4) 0.072(4) 0.030(4) -0.006(3) 0.010(3) -0.033(3) C9 0.044(4) 0.112(5) 0.030(5) -0.016(4) -0.002(3) -0.028(4) C10 0.065(4) 0.072(4) 0.023(4) -0.004(3) 0.003(3) -0.006(3) C11 0.072(4) 0.045(3) 0.027(4) -0.004(3) 0.014(3) -0.013(3) C12 0.046(3) 0.037(3) 0.018(3) -0.005(2) 0.005(3) -0.009(2) C13 0.040(3) 0.028(2) 0.023(3) -0.007(2) 0.013(2) -0.007(2) C14 0.023(2) 0.029(3) 0.030(3) -0.001(2) 0.011(2) -0.0054(19) C15 0.040(3) 0.034(3) 0.043(4) -0.001(2) 0.020(3) 0.000(2) C16 0.042(4) 0.045(3) 0.072(5) -0.006(3) 0.032(4) 0.003(3) C17 0.032(3) 0.030(3) 0.075(5) 0.000(3) 0.017(3) 0.001(2) C18 0.028(3) 0.046(3) 0.047(4) 0.005(3) 0.004(3) -0.004(2) C19 0.027(3) 0.048(3) 0.039(4) -0.002(3) 0.012(3) -0.006(2) C20 0.031(3) 0.026(3) 0.026(3) 0.003(2) 0.016(2) 0.001(2) C21 0.036(3) 0.041(3) 0.027(3) -0.003(2) 0.014(3) -0.001(2) C22 0.048(3) 0.066(4) 0.027(4) -0.003(3) 0.017(3) 0.013(3) C23 0.069(4) 0.063(4) 0.042(4) 0.021(3) 0.033(4) 0.018(3) C24 0.089(5) 0.045(3) 0.055(5) 0.011(3) 0.046(4) 0.002(3) C25 0.066(4) 0.031(3) 0.039(4) -0.003(2) 0.030(3) -0.006(3) C26 0.029(3) 0.047(3) 0.026(3) 0.008(2) 0.006(2) 0.017(2) C27 0.034(3) 0.062(4) 0.062(4) 0.025(3) 0.019(3) 0.009(3) C28 0.040(4) 0.118(6) 0.083(6) 0.052(5) 0.026(4) 0.017(4) C29 0.052(5) 0.152(8) 0.089(6) 0.055(5) 0.048(5) 0.047(5) C30 0.073(5) 0.109(6) 0.094(6) 0.015(5) 0.055(5) 0.050(5) C31 0.056(4) 0.062(4) 0.061(5) -0.004(3) 0.032(4) 0.020(3) C32 0.036(3) 0.023(2) 0.030(3) 0.015(2) 0.015(2) 0.015(2) C33 0.064(4) 0.032(3) 0.043(4) 0.018(2) 0.026(3) 0.020(3) C34 0.097(5) 0.053(4) 0.054(5) 0.031(3) 0.043(4) 0.033(3) C35 0.097(5) 0.033(3) 0.098(6) 0.029(4) 0.064(5) 0.024(3) C36 0.090(5) 0.024(3) 0.086(6) 0.007(3) 0.055(4) 0.010(3) C37 0.060(4) 0.022(3) 0.048(4) 0.003(2) 0.027(3) 0.009(2) C38 0.034(3) 0.025(2) 0.018(3) -0.0014(19) 0.005(2) 0.002(2) C39 0.027(3) 0.023(2) 0.022(3) -0.008(2) 0.003(2) -0.0070(19) C40 0.041(3) 0.052(3) 0.030(4) -0.004(2) 0.004(3) -0.018(3) C41 0.048(4) 0.073(4) 0.034(4) -0.010(3) -0.003(3) -0.029(3) C42 0.042(3) 0.058(4) 0.056(5) -0.015(3) 0.021(3) -0.026(3) C43 0.044(3) 0.042(3) 0.046(4) -0.002(3) 0.020(3) -0.014(3) C44 0.030(3) 0.028(3) 0.031(3) -0.006(2) 0.005(2) -0.003(2) C45 0.044(3) 0.015(2) 0.028(3) 0.0011(19) 0.018(3) 0.001(2) C46 0.051(3) 0.038(3) 0.045(4) 0.009(2) 0.027(3) 0.013(3) C47 0.081(5) 0.055(4) 0.087(6) 0.034(4) 0.061(5) 0.036(3) C48 0.115(7) 0.038(3) 0.103(7) -0.001(4) 0.089(6) 0.008(4) C49 0.101(6) 0.052(4) 0.058(5) -0.022(3) 0.058(5) -0.018(4) C50 0.061(4) 0.033(3) 0.037(4) -0.004(2) 0.024(3) -0.009(3) C72 0.059(4) 0.041(3) 0.037(4) 0.006(3) 0.009(3) 0.021(3) C75 0.135(8) 0.098(6) 0.099(7) -0.038(5) 0.091(7) -0.061(6) P1 0.0351(7) 0.0227(6) 0.0221(8) -0.0050(5) 0.0123(6) -0.0055(5) P2 0.0289(7) 0.0243(6) 0.0200(8) -0.0024(5) 0.0099(6) -0.0020(5) P3 0.0292(7) 0.0205(6) 0.0227(8) 0.0027(5) 0.0094(6) 0.0061(5) P4 0.0264(6) 0.0204(6) 0.0189(7) -0.0011(5) 0.0043(6) 0.0011(5) F1 0.0372(18) 0.056(2) 0.090(3) 0.0145(18) 0.017(2) 0.0132(15) F2 0.074(2) 0.082(2) 0.054(3) 0.0399(19) 0.022(2) 0.0449(19) F3 0.090(3) 0.091(3) 0.060(3) -0.034(2) -0.035(2) 0.040(2) F4 0.241(6) 0.115(4) 0.186(6) -0.103(4) 0.178(6) -0.104(4) F5 0.100(4) 0.235(7) 0.106(4) -0.056(4) 0.054(4) -0.094(4) F6 0.313(9) 0.056(3) 0.201(7) 0.014(3) 0.179(7) -0.023(4) S1 0.0334(7) 0.0270(6) 0.0211(8) 0.0040(5) 0.0068(6) 0.0096(5) S2 0.0528(9) 0.0531(9) 0.0437(11) 0.0041(7) 0.0216(8) 0.0126(7) O1 0.0337(18) 0.0309(18) 0.031(2) 0.0075(14) 0.0061(16) 0.0018(14) O2 0.055(2) 0.0332(18) 0.032(2) -0.0066(15) 0.0153(19) 0.0036(16) O3 0.053(2) 0.0342(18) 0.037(2) 0.0146(15) 0.0235(19) 0.0177(16) O4 0.108(4) 0.059(3) 0.067(3) 0.011(2) 0.049(3) -0.012(2) O5 0.075(3) 0.113(3) 0.039(3) -0.014(2) 0.034(3) -0.007(3) O6 0.046(3) 0.201(6) 0.140(6) 0.005(5) 0.027(3) 0.056(4) O7 0.0268(19) 0.0298(18) 0.035(2) 0.0001(14) 0.0127(17) 0.0018(14) Ru1 0.02202(19) 0.01689(18) 0.0168(2) -0.00034(15) 0.00569(16) 0.00071(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.363(7) . ? C1 C2 1.405(6) . ? C1 P1 1.819(4) . ? C2 C3 1.382(8) . ? C3 C4 1.356(8) . ? C4 C5 1.381(8) . ? C5 C6 1.411(7) . ? C7 C12 1.375(6) . ? C7 C8 1.406(7) . ? C7 P1 1.826(5) . ? C8 C9 1.375(8) . ? C9 C10 1.373(8) . ? C10 C11 1.368(8) . ? C11 C12 1.382(7) . ? C13 P1 1.835(5) . ? C13 P2 1.848(4) . ? C14 C15 1.382(7) . ? C14 C19 1.398(7) . ? C14 P2 1.834(4) . ? C15 C16 1.379(7) . ? C16 C17 1.388(8) . ? C17 C18 1.368(8) . ? C18 C19 1.389(7) . ? C20 C21 1.390(6) . ? C20 C25 1.391(6) . ? C20 P2 1.817(5) . ? C21 C22 1.379(7) . ? C22 C23 1.378(7) . ? C23 C24 1.372(8) . ? C24 C25 1.385(7) . ? C26 C27 1.386(7) . ? C26 C31 1.406(7) . ? C26 P3 1.822(5) . ? C27 C28 1.386(8) . ? C28 C29 1.356(10) . ? C29 C30 1.364(10) . ? C30 C31 1.382(9) . ? C32 C33 1.380(7) . ? C32 C37 1.411(7) . ? C32 P3 1.820(4) . ? C33 C34 1.404(7) . ? C34 C35 1.385(9) . ? C35 C36 1.366(9) . ? C36 C37 1.387(7) . ? C38 P3 1.840(4) . ? C38 P4 1.849(4) . ? C39 C40 1.386(7) . ? C39 C44 1.388(6) . ? C39 P4 1.835(4) . ? C40 C41 1.385(7) . ? C41 C42 1.368(8) . ? C42 C43 1.379(8) . ? C43 C44 1.395(6) . ? C45 C46 1.389(7) . ? C45 C50 1.394(7) . ? C45 P4 1.826(4) . ? C46 C47 1.391(8) . ? C47 C48 1.386(10) . ? C48 C49 1.367(10) . ? C49 C50 1.374(8) . ? C72 F3 1.312(6) . ? C72 F1 1.326(6) . ? C72 F2 1.350(6) . ? C72 S1 1.816(6) . ? C75 F4 1.288(8) . ? C75 F6 1.295(9) . ? C75 F5 1.383(11) . ? C75 S2 1.788(7) . ? P1 Ru1 2.3629(12) . ? P2 Ru1 2.2976(12) . ? P3 Ru1 2.2831(13) . ? P4 Ru1 2.3957(12) . ? S1 O3 1.434(3) . ? S1 O2 1.440(3) . ? S1 O1 1.469(3) . ? S2 O4 1.401(4) . ? S2 O5 1.417(4) . ? S2 O6 1.426(5) . ? O1 Ru1 2.231(3) . ? O7 Ru1 2.194(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 C6 C1 C2 119.3(4) . . ? C6 C1 P1 118.8(3) . . ? C2 C1 P1 121.9(4) . . ? C3 C2 C1 119.4(5) . . ? C4 C3 C2 121.1(5) . . ? C3 C4 C5 120.6(5) . . ? C4 C5 C6 118.8(6) . . ? C1 C6 C5 120.7(5) . . ? C12 C7 C8 118.6(5) . . ? C12 C7 P1 118.4(4) . . ? C8 C7 P1 123.0(4) . . ? C9 C8 C7 119.7(5) . . ? C10 C9 C8 121.0(6) . . ? C11 C10 C9 119.4(6) . . ? C10 C11 C12 120.6(5) . . ? C7 C12 C11 120.7(5) . . ? P1 C13 P2 96.2(2) . . ? C15 C14 C19 117.7(4) . . ? C15 C14 P2 122.7(4) . . ? C19 C14 P2 119.6(3) . . ? C16 C15 C14 121.1(5) . . ? C15 C16 C17 120.8(5) . . ? C18 C17 C16 118.7(5) . . ? C17 C18 C19 120.8(6) . . ? C18 C19 C14 120.8(5) . . ? C21 C20 C25 118.7(4) . . ? C21 C20 P2 120.9(3) . . ? C25 C20 P2 120.2(4) . . ? C22 C21 C20 120.6(5) . . ? C23 C22 C21 120.0(5) . . ? C24 C23 C22 120.1(5) . . ? C23 C24 C25 120.4(5) . . ? C24 C25 C20 120.1(5) . . ? C27 C26 C31 118.4(5) . . ? C27 C26 P3 120.4(4) . . ? C31 C26 P3 121.1(4) . . ? C26 C27 C28 120.8(6) . . ? C29 C28 C27 120.2(7) . . ? C28 C29 C30 120.0(6) . . ? C29 C30 C31 121.4(7) . . ? C30 C31 C26 119.0(6) . . ? C33 C32 C37 119.0(4) . . ? C33 C32 P3 120.8(4) . . ? C37 C32 P3 120.1(4) . . ? C32 C33 C34 120.3(5) . . ? C35 C34 C33 119.7(6) . . ? C36 C35 C34 120.5(5) . . ? C35 C36 C37 120.5(6) . . ? C36 C37 C32 120.0(5) . . ? P3 C38 P4 96.3(2) . . ? C40 C39 C44 119.1(4) . . ? C40 C39 P4 120.1(4) . . ? C44 C39 P4 120.8(3) . . ? C41 C40 C39 120.1(5) . . ? C42 C41 C40 121.3(5) . . ? C41 C42 C43 119.1(5) . . ? C42 C43 C44 120.5(5) . . ? C39 C44 C43 120.0(5) . . ? C46 C45 C50 119.8(5) . . ? C46 C45 P4 118.7(4) . . ? C50 C45 P4 121.5(4) . . ? C45 C46 C47 119.6(6) . . ? C48 C47 C46 119.5(6) . . ? C49 C48 C47 120.9(6) . . ? C48 C49 C50 120.2(6) . . ? C49 C50 C45 120.0(6) . . ? F3 C72 F1 107.9(5) . . ? F3 C72 F2 108.4(5) . . ? F1 C72 F2 106.9(4) . . ? F3 C72 S1 113.4(4) . . ? F1 C72 S1 111.7(4) . . ? F2 C72 S1 108.2(4) . . ? F4 C75 F6 111.2(7) . . ? F4 C75 F5 107.5(8) . . ? F6 C75 F5 102.0(7) . . ? F4 C75 S2 113.7(5) . . ? F6 C75 S2 115.1(7) . . ? F5 C75 S2 106.3(6) . . ? C1 P1 C7 101.6(2) . . ? C1 P1 C13 108.5(2) . . ? C7 P1 C13 107.4(2) . . ? C1 P1 Ru1 123.62(16) . . ? C7 P1 Ru1 120.22(14) . . ? C13 P1 Ru1 93.96(14) . . ? C20 P2 C14 102.0(2) . . ? C20 P2 C13 106.1(2) . . ? C14 P2 C13 104.1(2) . . ? C20 P2 Ru1 127.24(15) . . ? C14 P2 Ru1 118.44(14) . . ? C13 P2 Ru1 95.76(15) . . ? C32 P3 C26 103.6(2) . . ? C32 P3 C38 106.1(2) . . ? C26 P3 C38 106.0(2) . . ? C32 P3 Ru1 126.14(16) . . ? C26 P3 Ru1 116.21(16) . . ? C38 P3 Ru1 96.52(14) . . ? C45 P4 C39 102.67(19) . . ? C45 P4 C38 107.9(2) . . ? C39 P4 C38 104.2(2) . . ? C45 P4 Ru1 123.08(16) . . ? C39 P4 Ru1 123.28(15) . . ? C38 P4 Ru1 92.54(14) . . ? O3 S1 O2 116.3(2) . . ? O3 S1 O1 113.55(18) . . ? O2 S1 O1 114.4(2) . . ? O3 S1 C72 105.0(3) . . ? O2 S1 C72 103.5(2) . . ? O1 S1 C72 102.0(2) . . ? O4 S2 O5 119.2(3) . . ? O4 S2 O6 107.9(4) . . ? O5 S2 O6 115.7(4) . . ? O4 S2 C75 104.7(4) . . ? O5 S2 C75 103.9(3) . . ? O6 S2 C75 103.5(5) . . ? S1 O1 Ru1 131.50(19) . . ? O7 Ru1 O1 84.84(12) . . ? O7 Ru1 P3 94.45(9) . . ? O1 Ru1 P3 168.59(8) . . ? O7 Ru1 P2 166.42(9) . . ? O1 Ru1 P2 90.49(8) . . ? P3 Ru1 P2 92.62(4) . . ? O7 Ru1 P1 95.20(9) . . ? O1 Ru1 P1 90.59(9) . . ? P3 Ru1 P1 100.81(4) . . ? P2 Ru1 P1 72.06(4) . . ? O7 Ru1 P4 91.56(9) . . ? O1 Ru1 P4 96.70(9) . . ? P3 Ru1 P4 71.92(4) . . ? P2 Ru1 P4 101.67(4) . . ? P1 Ru1 P4 170.48(4) . . ? 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 C6 C1 C2 C3 0.3(8) . . . . ? P1 C1 C2 C3 179.3(4) . . . . ? C1 C2 C3 C4 -0.9(9) . . . . ? C2 C3 C4 C5 1.6(9) . . . . ? C3 C4 C5 C6 -1.8(9) . . . . ? C2 C1 C6 C5 -0.6(8) . . . . ? P1 C1 C6 C5 -179.5(4) . . . . ? C4 C5 C6 C1 1.3(9) . . . . ? C12 C7 C8 C9 -0.2(8) . . . . ? P1 C7 C8 C9 -178.6(5) . . . . ? C7 C8 C9 C10 0.5(10) . . . . ? C8 C9 C10 C11 0.2(10) . . . . ? C9 C10 C11 C12 -1.2(9) . . . . ? C8 C7 C12 C11 -0.8(7) . . . . ? P1 C7 C12 C11 177.7(4) . . . . ? C10 C11 C12 C7 1.5(8) . . . . ? C19 C14 C15 C16 -0.2(7) . . . . ? P2 C14 C15 C16 179.5(4) . . . . ? C14 C15 C16 C17 0.3(8) . . . . ? C15 C16 C17 C18 0.1(8) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C17 C18 C19 C14 0.8(7) . . . . ? C15 C14 C19 C18 -0.4(7) . . . . ? P2 C14 C19 C18 180.0(4) . . . . ? C25 C20 C21 C22 1.0(7) . . . . ? P2 C20 C21 C22 177.0(4) . . . . ? C20 C21 C22 C23 -0.3(8) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C22 C23 C24 C25 0.4(9) . . . . ? C23 C24 C25 C20 0.4(9) . . . . ? C21 C20 C25 C24 -1.1(7) . . . . ? P2 C20 C25 C24 -177.1(4) . . . . ? C31 C26 C27 C28 -1.5(8) . . . . ? P3 C26 C27 C28 179.5(5) . . . . ? C26 C27 C28 C29 -0.6(10) . . . . ? C27 C28 C29 C30 2.8(12) . . . . ? C28 C29 C30 C31 -2.8(12) . . . . ? C29 C30 C31 C26 0.6(11) . . . . ? C27 C26 C31 C30 1.5(8) . . . . ? P3 C26 C31 C30 -179.5(5) . . . . ? C37 C32 C33 C34 -1.4(8) . . . . ? P3 C32 C33 C34 -178.6(4) . . . . ? C32 C33 C34 C35 -0.2(9) . . . . ? C33 C34 C35 C36 1.5(10) . . . . ? C34 C35 C36 C37 -1.1(10) . . . . ? C35 C36 C37 C32 -0.6(9) . . . . ? C33 C32 C37 C36 1.8(7) . . . . ? P3 C32 C37 C36 179.0(4) . . . . ? C44 C39 C40 C41 -1.5(8) . . . . ? P4 C39 C40 C41 179.6(4) . . . . ? C39 C40 C41 C42 0.7(9) . . . . ? C40 C41 C42 C43 0.4(9) . . . . ? C41 C42 C43 C44 -0.8(8) . . . . ? C40 C39 C44 C43 1.1(7) . . . . ? P4 C39 C44 C43 -180.0(4) . . . . ? C42 C43 C44 C39 0.1(7) . . . . ? C50 C45 C46 C47 1.1(7) . . . . ? P4 C45 C46 C47 -176.5(4) . . . . ? C45 C46 C47 C48 -0.6(8) . . . . ? C46 C47 C48 C49 -0.3(9) . . . . ? C47 C48 C49 C50 0.7(9) . . . . ? C48 C49 C50 C45 -0.2(8) . . . . ? C46 C45 C50 C49 -0.7(7) . . . . ? P4 C45 C50 C49 176.8(4) . . . . ? C6 C1 P1 C7 103.3(4) . . . . ? C2 C1 P1 C7 -75.6(4) . . . . ? C6 C1 P1 C13 -143.7(4) . . . . ? C2 C1 P1 C13 37.4(5) . . . . ? C6 C1 P1 Ru1 -35.6(5) . . . . ? C2 C1 P1 Ru1 145.5(4) . . . . ? C12 C7 P1 C1 -86.5(4) . . . . ? C8 C7 P1 C1 91.8(5) . . . . ? C12 C7 P1 C13 159.6(4) . . . . ? C8 C7 P1 C13 -22.0(5) . . . . ? C12 C7 P1 Ru1 54.2(4) . . . . ? C8 C7 P1 Ru1 -127.4(4) . . . . ? P2 C13 P1 C1 139.1(2) . . . . ? P2 C13 P1 C7 -111.8(2) . . . . ? P2 C13 P1 Ru1 11.59(19) . . . . ? C21 C20 P2 C14 -82.6(4) . . . . ? C25 C20 P2 C14 93.3(4) . . . . ? C21 C20 P2 C13 168.7(4) . . . . ? C25 C20 P2 C13 -15.4(4) . . . . ? C21 C20 P2 Ru1 58.1(4) . . . . ? C25 C20 P2 Ru1 -126.0(4) . . . . ? C15 C14 P2 C20 19.1(4) . . . . ? C19 C14 P2 C20 -161.3(4) . . . . ? C15 C14 P2 C13 129.3(4) . . . . ? C19 C14 P2 C13 -51.0(4) . . . . ? C15 C14 P2 Ru1 -125.9(3) . . . . ? C19 C14 P2 Ru1 53.7(4) . . . . ? P1 C13 P2 C20 -143.4(2) . . . . ? P1 C13 P2 C14 109.3(2) . . . . ? P1 C13 P2 Ru1 -12.0(2) . . . . ? C33 C32 P3 C26 97.0(4) . . . . ? C37 C32 P3 C26 -80.1(4) . . . . ? C33 C32 P3 C38 -14.3(4) . . . . ? C37 C32 P3 C38 168.5(4) . . . . ? C33 C32 P3 Ru1 -125.2(4) . . . . ? C37 C32 P3 Ru1 57.6(4) . . . . ? C27 C26 P3 C32 -155.5(4) . . . . ? C31 C26 P3 C32 25.5(5) . . . . ? C27 C26 P3 C38 -44.0(5) . . . . ? C31 C26 P3 C38 137.0(4) . . . . ? C27 C26 P3 Ru1 61.8(5) . . . . ? C31 C26 P3 Ru1 -117.2(4) . . . . ? P4 C38 P3 C32 -144.6(2) . . . . ? P4 C38 P3 C26 105.6(2) . . . . ? P4 C38 P3 Ru1 -14.04(19) . . . . ? C46 C45 P4 C39 108.0(4) . . . . ? C50 C45 P4 C39 -69.5(4) . . . . ? C46 C45 P4 C38 -142.2(4) . . . . ? C50 C45 P4 C38 40.2(4) . . . . ? C46 C45 P4 Ru1 -36.8(4) . . . . ? C50 C45 P4 Ru1 145.6(3) . . . . ? C40 C39 P4 C45 71.7(4) . . . . ? C44 C39 P4 C45 -107.3(4) . . . . ? C40 C39 P4 C38 -40.8(4) . . . . ? C44 C39 P4 C38 140.3(4) . . . . ? C40 C39 P4 Ru1 -143.5(3) . . . . ? C44 C39 P4 Ru1 37.5(4) . . . . ? P3 C38 P4 C45 139.3(2) . . . . ? P3 C38 P4 C39 -112.0(2) . . . . ? P3 C38 P4 Ru1 13.30(18) . . . . ? F3 C72 S1 O3 62.4(5) . . . . ? F1 C72 S1 O3 -175.4(3) . . . . ? F2 C72 S1 O3 -58.0(4) . . . . ? F3 C72 S1 O2 -175.2(4) . . . . ? F1 C72 S1 O2 -53.0(4) . . . . ? F2 C72 S1 O2 64.4(4) . . . . ? F3 C72 S1 O1 -56.2(5) . . . . ? F1 C72 S1 O1 66.0(4) . . . . ? F2 C72 S1 O1 -176.6(4) . . . . ? F4 C75 S2 O4 -54.1(9) . . . . ? F6 C75 S2 O4 176.0(7) . . . . ? F5 C75 S2 O4 64.0(6) . . . . ? F4 C75 S2 O5 -179.9(8) . . . . ? F6 C75 S2 O5 50.2(8) . . . . ? F5 C75 S2 O5 -61.8(6) . . . . ? F4 C75 S2 O6 58.8(9) . . . . ? F6 C75 S2 O6 -71.0(8) . . . . ? F5 C75 S2 O6 176.9(5) . . . . ? O3 S1 O1 Ru1 55.7(3) . . . . ? O2 S1 O1 Ru1 -81.0(3) . . . . ? C72 S1 O1 Ru1 168.0(3) . . . . ? S1 O1 Ru1 O7 -32.3(3) . . . . ? S1 O1 Ru1 P3 54.6(6) . . . . ? S1 O1 Ru1 P2 160.4(2) . . . . ? S1 O1 Ru1 P1 -127.5(2) . . . . ? S1 O1 Ru1 P4 58.6(3) . . . . ? C32 P3 Ru1 O7 -143.1(2) . . . . ? C26 P3 Ru1 O7 -9.9(2) . . . . ? C38 P3 Ru1 O7 101.48(17) . . . . ? C32 P3 Ru1 O1 130.9(5) . . . . ? C26 P3 Ru1 O1 -95.9(5) . . . . ? C38 P3 Ru1 O1 15.5(5) . . . . ? C32 P3 Ru1 P2 25.3(2) . . . . ? C26 P3 Ru1 P2 158.49(19) . . . . ? C38 P3 Ru1 P2 -90.13(15) . . . . ? C32 P3 Ru1 P1 -47.0(2) . . . . ? C26 P3 Ru1 P1 86.26(19) . . . . ? C38 P3 Ru1 P1 -162.35(15) . . . . ? C32 P3 Ru1 P4 126.7(2) . . . . ? C26 P3 Ru1 P4 -100.09(19) . . . . ? C38 P3 Ru1 P4 11.30(15) . . . . ? C20 P2 Ru1 O7 145.8(4) . . . . ? C14 P2 Ru1 O7 -79.0(4) . . . . ? C13 P2 Ru1 O7 30.5(4) . . . . ? C20 P2 Ru1 O1 -144.55(19) . . . . ? C14 P2 Ru1 O1 -9.33(19) . . . . ? C13 P2 Ru1 O1 100.14(18) . . . . ? C20 P2 Ru1 P3 24.47(18) . . . . ? C14 P2 Ru1 P3 159.69(18) . . . . ? C13 P2 Ru1 P3 -90.84(16) . . . . ? C20 P2 Ru1 P1 124.99(18) . . . . ? C14 P2 Ru1 P1 -99.79(18) . . . . ? C13 P2 Ru1 P1 9.68(16) . . . . ? C20 P2 Ru1 P4 -47.61(18) . . . . ? C14 P2 Ru1 P4 87.61(18) . . . . ? C13 P2 Ru1 P4 -162.92(16) . . . . ? C1 P1 Ru1 O7 59.7(2) . . . . ? C7 P1 Ru1 O7 -72.2(2) . . . . ? C13 P1 Ru1 O7 175.08(18) . . . . ? C1 P1 Ru1 O1 144.6(2) . . . . ? C7 P1 Ru1 O1 12.7(2) . . . . ? C13 P1 Ru1 O1 -100.04(18) . . . . ? C1 P1 Ru1 P3 -35.83(19) . . . . ? C7 P1 Ru1 P3 -167.70(18) . . . . ? C13 P1 Ru1 P3 79.54(16) . . . . ? C1 P1 Ru1 P2 -125.09(19) . . . . ? C7 P1 Ru1 P2 103.04(18) . . . . ? C13 P1 Ru1 P2 -9.73(16) . . . . ? C1 P1 Ru1 P4 -75.3(3) . . . . ? C7 P1 Ru1 P4 152.8(3) . . . . ? C13 P1 Ru1 P4 40.0(3) . . . . ? C45 P4 Ru1 O7 141.33(19) . . . . ? C39 P4 Ru1 O7 3.55(19) . . . . ? C38 P4 Ru1 O7 -105.35(17) . . . . ? C45 P4 Ru1 O1 56.35(19) . . . . ? C39 P4 Ru1 O1 -81.44(19) . . . . ? C38 P4 Ru1 O1 169.67(17) . . . . ? C45 P4 Ru1 P3 -124.50(17) . . . . ? C39 P4 Ru1 P3 97.72(18) . . . . ? C38 P4 Ru1 P3 -11.17(15) . . . . ? C45 P4 Ru1 P2 -35.54(17) . . . . ? C39 P4 Ru1 P2 -173.33(17) . . . . ? C38 P4 Ru1 P2 77.78(15) . . . . ? C45 P4 Ru1 P1 -83.4(3) . . . . ? C39 P4 Ru1 P1 138.8(3) . . . . ? C38 P4 Ru1 P1 29.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.747 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.077 data_cs125 _database_code_CSD 212388 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H50 B2 F8 N2 P4 Ru' _chemical_formula_weight 1125.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0140 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.4200 0.8360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.7375(17) _cell_length_b 19.564(2) _cell_length_c 20.201(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.270(14) _cell_angle_gamma 90.00 _cell_volume 5406.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14445 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 22.48 _reflns_number_total 6982 _reflns_number_gt 4445 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 6982 _refine_ls_number_parameters 644 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 0.628 _refine_ls_restrained_S_all 0.648 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6144(6) 0.6076(4) 0.6217(4) 0.061(2) Uani 1 d . . . C2 C 0.6767(7) 0.5841(6) 0.5711(5) 0.111(4) Uani 1 d . . . H2A H 0.7281 0.5559 0.5915 0.167 Uiso 1 calc R . . H2B H 0.7045 0.6229 0.5506 0.167 Uiso 1 calc R . . H2C H 0.6381 0.5582 0.5379 0.167 Uiso 1 calc R . . C3 C 0.3210(5) 0.5507(5) 0.6702(4) 0.068(2) Uani 1 d . . . C4 C 0.2513(7) 0.4977(5) 0.6518(5) 0.122(4) Uani 1 d . . . H4A H 0.2475 0.4670 0.6885 0.183 Uiso 1 calc R . . H4B H 0.2717 0.4729 0.6144 0.183 Uiso 1 calc R . . H4C H 0.1883 0.5177 0.6401 0.183 Uiso 1 calc R . . C5 C 0.4687(4) 0.6430(3) 0.8754(3) 0.0488(18) Uani 1 d . . . H5A H 0.4363 0.6141 0.9057 0.13(3) Uiso 1 calc R . . H5B H 0.5133 0.6741 0.9003 0.05(2) Uiso 1 calc R . . C6 C 0.6540(5) 0.5802(3) 0.8453(3) 0.0483(18) Uani 1 d . . . C7 C 0.6851(5) 0.5869(4) 0.9121(4) 0.073(2) Uani 1 d . . . H7 H 0.6401 0.5979 0.9421 0.088 Uiso 1 calc R . . C8 C 0.7821(7) 0.5776(5) 0.9347(5) 0.092(3) Uani 1 d . . . H8 H 0.8027 0.5834 0.9795 0.111 Uiso 1 calc R . . C9 C 0.8488(7) 0.5593(5) 0.8901(6) 0.108(3) Uani 1 d . . . H9 H 0.9140 0.5522 0.9052 0.129 Uiso 1 calc R . . C10 C 0.8195(6) 0.5519(5) 0.8247(6) 0.102(3) Uani 1 d . . . H10 H 0.8645 0.5402 0.7948 0.122 Uiso 1 calc R . . C11 C 0.7229(5) 0.5618(4) 0.8026(4) 0.070(2) Uani 1 d . . . H11 H 0.7031 0.5560 0.7577 0.084 Uiso 1 calc R . . C12 C 0.4801(4) 0.5078(3) 0.8082(3) 0.0455(16) Uani 1 d . . . C13 C 0.5039(6) 0.4664(4) 0.7564(4) 0.082(3) Uani 1 d . . . H13 H 0.5451 0.4832 0.7262 0.098 Uiso 1 calc R . . C14 C 0.4677(8) 0.4003(4) 0.7486(4) 0.099(3) Uani 1 d . . . H14 H 0.4876 0.3724 0.7150 0.119 Uiso 1 calc R . . C15 C 0.4032(7) 0.3766(4) 0.7902(5) 0.092(3) Uani 1 d . . . H15 H 0.3771 0.3329 0.7848 0.110 Uiso 1 calc R . . C16 C 0.3776(7) 0.4173(5) 0.8392(5) 0.098(3) Uani 1 d . . . H16 H 0.3324 0.4013 0.8670 0.118 Uiso 1 calc R . . C17 C 0.4156(6) 0.4815(4) 0.8498(4) 0.080(3) Uani 1 d . . . H17 H 0.3978 0.5074 0.8853 0.096 Uiso 1 calc R . . C18 C 0.3552(6) 0.7678(4) 0.8556(4) 0.069(2) Uani 1 d . . . C19 C 0.2887(9) 0.8112(5) 0.8215(5) 0.115(4) Uani 1 d . . . H19 H 0.2628 0.7999 0.7787 0.138 Uiso 1 calc R . . C20 C 0.2601(10) 0.8716(6) 0.8505(7) 0.151(5) Uani 1 d . . . H20 H 0.2169 0.9013 0.8268 0.181 Uiso 1 calc R . . C21 C 0.2960(14) 0.8872(6) 0.9141(8) 0.179(8) Uani 1 d . . . H21 H 0.2755 0.9270 0.9338 0.214 Uiso 1 calc R . . C22 C 0.3618(11) 0.8450(6) 0.9494(7) 0.141(6) Uani 1 d . . . H22 H 0.3869 0.8565 0.9922 0.170 Uiso 1 calc R . . C23 C 0.3907(8) 0.7841(5) 0.9197(5) 0.101(3) Uani 1 d . . . H23 H 0.4340 0.7547 0.9436 0.121 Uiso 1 calc R . . C24 C 0.2692(5) 0.6422(4) 0.8188(4) 0.0550(19) Uani 1 d . . . C25 C 0.2455(6) 0.6072(5) 0.8741(5) 0.084(3) Uani 1 d . . . H25 H 0.2904 0.6068 0.9115 0.101 Uiso 1 calc R . . C26 C 0.1588(8) 0.5727(5) 0.8770(7) 0.123(4) Uani 1 d . . . H26 H 0.1433 0.5520 0.9161 0.148 Uiso 1 calc R . . C27 C 0.0952(9) 0.5699(8) 0.8197(9) 0.148(6) Uani 1 d . . . H27 H 0.0415 0.5408 0.8177 0.177 Uiso 1 calc R . . C28 C 0.1109(8) 0.6097(9) 0.7662(7) 0.139(5) Uani 1 d . . . H28 H 0.0626 0.6140 0.7310 0.167 Uiso 1 calc R . . C29 C 0.2009(6) 0.6442(6) 0.7648(4) 0.103(3) Uani 1 d . . . H29 H 0.2141 0.6684 0.7270 0.123 Uiso 1 calc R . . C30 C 0.4817(5) 0.8224(4) 0.7007(4) 0.0598(19) Uani 1 d . . . H30A H 0.5125 0.8553 0.6734 0.042(17) Uiso 1 calc R . . H30B H 0.4412 0.8457 0.7305 0.10(3) Uiso 1 calc R . . C31 C 0.6079(6) 0.8017(4) 0.8240(4) 0.061(2) Uani 1 d . . . C32 C 0.5743(7) 0.8637(4) 0.8441(4) 0.087(3) Uani 1 d . . . H32 H 0.5314 0.8886 0.8151 0.105 Uiso 1 calc R . . C33 C 0.6025(10) 0.8892(5) 0.9054(6) 0.127(4) Uani 1 d . . . H33 H 0.5761 0.9304 0.9183 0.152 Uiso 1 calc R . . C34 C 0.6666(10) 0.8569(6) 0.9474(5) 0.122(5) Uani 1 d . . . H34 H 0.6854 0.8761 0.9887 0.146 Uiso 1 calc R . . C35 C 0.7054(7) 0.7954(6) 0.9305(5) 0.108(3) Uani 1 d . . . H35 H 0.7511 0.7731 0.9597 0.130 Uiso 1 calc R . . C36 C 0.6748(6) 0.7668(5) 0.8681(4) 0.083(2) Uani 1 d . . . H36 H 0.6991 0.7246 0.8562 0.100 Uiso 1 calc R . . C37 C 0.6781(5) 0.7657(4) 0.7005(4) 0.0570(18) Uani 1 d . . . C38 C 0.6928(7) 0.8114(6) 0.6516(5) 0.088(3) Uani 1 d . . . H38 H 0.6477 0.8462 0.6414 0.106 Uiso 1 calc R . . C39 C 0.7754(9) 0.8062(6) 0.6168(5) 0.118(4) Uani 1 d . . . H39 H 0.7853 0.8381 0.5840 0.142 Uiso 1 calc R . . C40 C 0.8414(8) 0.7559(8) 0.6297(7) 0.122(4) Uani 1 d . . . H40 H 0.8931 0.7506 0.6034 0.147 Uiso 1 calc R . . C41 C 0.8314(7) 0.7110(6) 0.6837(6) 0.108(4) Uani 1 d . . . H41 H 0.8795 0.6793 0.6972 0.130 Uiso 1 calc R . . C42 C 0.7485(6) 0.7165(5) 0.7147(4) 0.083(3) Uani 1 d . . . H42 H 0.7385 0.6850 0.7478 0.100 Uiso 1 calc R . . C43 C 0.4588(5) 0.7544(5) 0.5685(3) 0.065(2) Uani 1 d . . . C44 C 0.4589(6) 0.6945(5) 0.5334(4) 0.081(3) Uani 1 d . . . H44 H 0.4379 0.6548 0.5530 0.097 Uiso 1 calc R . . C45 C 0.4884(8) 0.6908(7) 0.4711(5) 0.129(4) Uani 1 d . . . H45 H 0.4840 0.6503 0.4469 0.154 Uiso 1 calc R . . C46 C 0.5251(11) 0.7496(10) 0.4454(6) 0.156(6) Uani 1 d . . . H46 H 0.5536 0.7476 0.4055 0.188 Uiso 1 calc R . . C47 C 0.5205(10) 0.8092(8) 0.4765(6) 0.143(5) Uani 1 d . . . H47 H 0.5385 0.8487 0.4551 0.171 Uiso 1 calc R . . C48 C 0.4902(7) 0.8143(5) 0.5390(4) 0.098(3) Uani 1 d . . . H48 H 0.4904 0.8560 0.5610 0.117 Uiso 1 calc R . . C49 C 0.2895(6) 0.7827(5) 0.6324(4) 0.059(2) Uani 1 d . . . C50 C 0.2205(6) 0.7365(5) 0.6124(3) 0.075(2) Uani 1 d . . . H50 H 0.2376 0.6906 0.6109 0.089 Uiso 1 calc R . . C51 C 0.1225(6) 0.7557(6) 0.5935(5) 0.094(3) Uani 1 d . . . H51 H 0.0757 0.7228 0.5808 0.113 Uiso 1 calc R . . C52 C 0.0980(7) 0.8225(6) 0.5943(5) 0.105(3) Uani 1 d . . . H52 H 0.0343 0.8359 0.5806 0.126 Uiso 1 calc R . . C53 C 0.1665(7) 0.8709(6) 0.6151(5) 0.105(3) Uani 1 d . . . H53 H 0.1489 0.9168 0.6164 0.126 Uiso 1 calc R . . C54 C 0.2641(6) 0.8508(5) 0.6347(4) 0.085(3) Uani 1 d . . . H54 H 0.3107 0.8833 0.6490 0.102 Uiso 1 calc R . . B1 B 0.4392(9) 0.4778(6) 0.5338(5) 0.083(3) Uani 1 d . . . B2 B -0.0418(10) 0.5191(6) 0.6123(8) 0.225(9) Uani 1 d DU . . F1 F 0.4716(5) 0.4758(3) 0.5995(3) 0.130(2) Uani 1 d . . . F2 F 0.5166(5) 0.4803(3) 0.4955(3) 0.138(2) Uani 1 d . . . F3 F 0.3951(5) 0.4174(3) 0.5181(3) 0.130(2) Uani 1 d . . . F4 F 0.3771(6) 0.5290(3) 0.5208(3) 0.166(3) Uani 1 d . . . F5 F 0.0193(5) 0.4745(3) 0.6313(6) 0.239(5) Uani 1 d DU . . F6 F -0.1033(6) 0.5019(5) 0.5666(4) 0.243(4) Uani 1 d DU . . F7 F -0.0976(11) 0.5224(8) 0.6628(7) 0.401(9) Uani 1 d DU . . F8 F -0.0044(8) 0.5786(3) 0.6066(4) 0.222(4) Uani 1 d DU . . N1 N 0.5650(4) 0.6289(3) 0.6600(3) 0.0546(16) Uani 1 d . . . N2 N 0.3744(4) 0.5943(3) 0.6887(3) 0.0527(16) Uani 1 d . . . P1 P 0.52911(12) 0.59301(9) 0.81296(8) 0.0431(5) Uani 1 d . . . P2 P 0.38355(12) 0.68676(10) 0.81676(8) 0.0482(5) Uani 1 d . . . P3 P 0.56977(13) 0.76364(10) 0.74436(9) 0.0519(5) Uani 1 d . . . P4 P 0.41507(13) 0.75557(10) 0.65131(9) 0.0543(5) Uani 1 d . . . Ru1 Ru 0.47242(4) 0.66728(3) 0.72532(3) 0.04073(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 C1 0.055(5) 0.068(6) 0.062(5) 0.003(5) 0.015(4) 0.002(4) C2 0.098(7) 0.135(10) 0.111(8) -0.047(7) 0.059(6) 0.011(7) C3 0.049(5) 0.097(7) 0.056(5) -0.012(5) -0.002(4) 0.001(5) C4 0.110(8) 0.114(9) 0.139(9) -0.049(7) -0.003(7) -0.061(7) C5 0.060(4) 0.050(5) 0.035(4) 0.009(3) -0.003(3) -0.008(3) C6 0.046(4) 0.047(5) 0.050(5) 0.008(4) -0.003(4) -0.003(3) C7 0.057(5) 0.082(6) 0.080(6) 0.013(5) -0.005(4) -0.005(4) C8 0.078(6) 0.112(8) 0.082(6) 0.006(6) -0.019(6) -0.011(5) C9 0.054(6) 0.135(9) 0.127(10) 0.018(8) -0.022(7) 0.001(6) C10 0.057(6) 0.121(9) 0.123(9) 0.015(7) -0.015(6) -0.001(6) C11 0.060(6) 0.077(6) 0.070(5) 0.013(5) -0.005(4) 0.010(4) C12 0.050(4) 0.047(4) 0.040(4) 0.002(4) 0.006(3) -0.007(3) C13 0.125(7) 0.067(6) 0.058(5) -0.015(5) 0.034(5) -0.038(5) C14 0.142(8) 0.064(6) 0.093(8) -0.022(5) 0.014(8) -0.023(6) C15 0.114(8) 0.069(6) 0.092(7) -0.015(6) 0.012(5) -0.047(6) C16 0.124(8) 0.067(6) 0.110(8) 0.010(6) 0.044(6) -0.039(6) C17 0.107(7) 0.063(6) 0.076(6) 0.000(5) 0.038(5) -0.019(5) C18 0.097(6) 0.049(5) 0.066(6) -0.001(5) 0.041(5) 0.004(4) C19 0.200(12) 0.066(7) 0.086(7) 0.010(6) 0.052(7) 0.039(7) C20 0.253(15) 0.085(9) 0.123(10) 0.010(8) 0.067(10) 0.098(9) C21 0.37(2) 0.056(8) 0.137(13) 0.011(9) 0.153(14) 0.022(11) C22 0.251(17) 0.076(9) 0.110(10) -0.040(8) 0.089(10) -0.042(9) C23 0.173(10) 0.067(7) 0.065(7) -0.026(5) 0.023(6) -0.005(6) C24 0.045(4) 0.071(6) 0.051(4) -0.016(4) 0.015(4) 0.002(4) C25 0.066(6) 0.091(7) 0.098(7) 0.003(6) 0.025(5) -0.016(5) C26 0.082(7) 0.124(9) 0.173(12) -0.022(9) 0.060(8) -0.037(7) C27 0.074(9) 0.175(14) 0.202(17) -0.054(13) 0.047(10) -0.044(9) C28 0.049(7) 0.231(17) 0.135(11) -0.060(11) -0.001(7) -0.012(8) C29 0.043(5) 0.176(11) 0.089(7) -0.014(7) 0.011(5) -0.002(6) C30 0.081(5) 0.043(4) 0.059(5) 0.008(4) 0.025(4) 0.003(4) C31 0.070(6) 0.057(6) 0.054(5) 0.004(5) 0.002(4) -0.036(4) C32 0.144(8) 0.041(5) 0.073(6) -0.018(5) -0.007(5) -0.015(5) C33 0.238(14) 0.065(7) 0.076(8) -0.013(7) 0.009(8) -0.019(8) C34 0.212(13) 0.089(9) 0.066(7) -0.037(7) 0.017(8) -0.082(9) C35 0.118(8) 0.127(9) 0.072(7) -0.006(6) -0.042(5) -0.049(7) C36 0.095(6) 0.086(7) 0.066(6) -0.005(6) -0.002(5) -0.022(5) C37 0.056(5) 0.050(5) 0.065(5) -0.005(4) 0.004(4) -0.014(4) C38 0.087(6) 0.105(8) 0.075(6) 0.001(6) 0.019(5) -0.027(5) C39 0.136(9) 0.123(11) 0.107(8) -0.005(8) 0.070(7) -0.042(8) C40 0.096(9) 0.134(11) 0.143(11) -0.061(10) 0.043(8) -0.044(8) C41 0.082(8) 0.092(8) 0.156(11) -0.015(8) 0.041(7) -0.020(6) C42 0.056(5) 0.082(7) 0.114(7) 0.001(6) 0.025(5) -0.019(5) C43 0.074(5) 0.084(6) 0.037(4) 0.018(5) -0.001(4) 0.027(4) C44 0.099(6) 0.102(8) 0.039(5) 0.005(5) -0.005(4) 0.022(5) C45 0.169(10) 0.155(12) 0.063(7) 0.001(8) 0.016(6) 0.045(9) C46 0.209(14) 0.220(18) 0.046(7) 0.022(10) 0.041(8) 0.065(14) C47 0.200(13) 0.158(14) 0.079(9) 0.052(9) 0.062(8) 0.016(11) C48 0.142(8) 0.084(8) 0.070(6) 0.032(6) 0.023(5) -0.001(6) C49 0.062(5) 0.069(6) 0.049(5) 0.006(5) 0.013(4) 0.012(5) C50 0.066(6) 0.098(7) 0.058(5) 0.003(5) -0.004(4) 0.016(5) C51 0.060(6) 0.106(8) 0.111(7) 0.004(6) -0.015(5) 0.005(5) C52 0.096(7) 0.108(9) 0.112(8) 0.009(8) 0.013(6) 0.037(7) C53 0.085(7) 0.097(8) 0.132(9) 0.031(7) 0.007(6) 0.035(6) C54 0.078(6) 0.085(8) 0.091(6) 0.022(5) 0.003(5) 0.008(5) B1 0.119(9) 0.090(9) 0.041(7) 0.006(6) 0.018(6) 0.017(7) B2 0.205(16) 0.116(13) 0.324(19) -0.050(14) -0.139(15) -0.025(12) F1 0.172(6) 0.152(5) 0.063(4) -0.024(4) -0.005(4) 0.065(4) F2 0.147(5) 0.178(7) 0.092(4) -0.007(4) 0.026(4) -0.015(5) F3 0.180(6) 0.123(5) 0.089(4) -0.026(4) 0.019(4) -0.045(4) F4 0.241(8) 0.137(6) 0.120(5) 0.027(4) 0.012(5) 0.099(6) F5 0.123(5) 0.099(6) 0.479(15) 0.056(8) -0.057(7) -0.008(4) F6 0.223(8) 0.263(10) 0.221(8) -0.082(8) -0.097(7) -0.006(7) F7 0.38(2) 0.43(2) 0.38(2) -0.069(18) -0.008(15) -0.026(16) F8 0.350(11) 0.098(5) 0.200(8) 0.019(5) -0.070(7) -0.031(6) N1 0.054(4) 0.049(4) 0.059(4) 0.005(3) 0.001(3) -0.011(3) N2 0.040(4) 0.075(5) 0.043(4) -0.003(3) 0.007(3) 0.007(3) P1 0.0447(11) 0.0409(11) 0.0432(11) 0.0009(9) 0.0006(8) -0.0041(8) P2 0.0520(11) 0.0508(13) 0.0427(11) 0.0009(10) 0.0094(8) 0.0002(9) P3 0.0604(12) 0.0459(12) 0.0494(12) 0.0029(10) 0.0056(10) -0.0071(9) P4 0.0604(12) 0.0560(13) 0.0468(12) 0.0077(10) 0.0067(10) 0.0083(10) Ru1 0.0430(3) 0.0417(3) 0.0379(3) 0.0013(4) 0.00603(19) -0.0018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.152(8) . ? C1 C2 1.466(10) . ? C3 N2 1.164(9) . ? C3 C4 1.437(11) . ? C5 P2 1.803(6) . ? C5 P1 1.851(7) . ? C6 C11 1.384(9) . ? C6 C7 1.384(9) . ? C6 P1 1.797(7) . ? C7 C8 1.381(10) . ? C8 C9 1.390(12) . ? C9 C10 1.353(12) . ? C10 C11 1.375(10) . ? C12 C17 1.376(9) . ? C12 C13 1.387(9) . ? C12 P1 1.797(6) . ? C13 C14 1.389(10) . ? C14 C15 1.358(10) . ? C15 C16 1.343(11) . ? C16 C17 1.369(10) . ? C18 C23 1.379(11) . ? C18 C19 1.385(12) . ? C18 P2 1.827(7) . ? C19 C20 1.392(13) . ? C20 C21 1.368(18) . ? C21 C22 1.375(18) . ? C22 C23 1.405(13) . ? C24 C29 1.372(10) . ? C24 C25 1.376(10) . ? C24 P2 1.801(7) . ? C25 C26 1.374(11) . ? C26 C27 1.386(16) . ? C27 C28 1.365(17) . ? C28 C29 1.412(14) . ? C30 P3 1.835(7) . ? C30 P4 1.836(8) . ? C31 C32 1.371(10) . ? C31 C36 1.398(11) . ? C31 P3 1.807(8) . ? C32 C33 1.360(12) . ? C33 C34 1.325(14) . ? C34 C35 1.372(14) . ? C35 C36 1.407(11) . ? C37 C38 1.361(10) . ? C37 C42 1.376(10) . ? C37 P3 1.801(7) . ? C38 C39 1.392(13) . ? C39 C40 1.348(14) . ? C40 C41 1.416(14) . ? C41 C42 1.353(11) . ? C43 C44 1.368(10) . ? C43 C48 1.401(10) . ? C43 P4 1.829(7) . ? C44 C45 1.360(12) . ? C45 C46 1.377(17) . ? C46 C47 1.328(17) . ? C47 C48 1.368(14) . ? C49 C50 1.345(11) . ? C49 C54 1.379(11) . ? C49 P4 1.811(8) . ? C50 C51 1.416(10) . ? C51 C52 1.350(13) . ? C52 C53 1.374(12) . ? C53 C54 1.419(11) . ? B1 F4 1.325(11) . ? B1 F3 1.353(12) . ? B1 F1 1.362(10) . ? B1 F2 1.372(11) . ? B2 F6 1.239(11) . ? B2 F5 1.246(12) . ? B2 F8 1.282(12) . ? B2 F7 1.333(14) . ? F5 F7 2.012(13) . ? F5 F6 2.104(9) . ? F5 F8 2.114(9) . ? F6 F7 1.980(13) . ? F6 F8 2.132(10) . ? F7 F8 2.099(13) . ? N1 Ru1 2.058(6) . ? N2 Ru1 2.053(7) . ? P1 Ru1 2.3661(18) . ? P2 Ru1 2.3372(18) . ? P3 Ru1 2.3230(19) . ? P4 Ru1 2.371(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 176.9(9) . . ? N2 C3 C4 175.7(9) . . ? P2 C5 P1 96.2(3) . . ? C11 C6 C7 117.7(6) . . ? C11 C6 P1 119.6(5) . . ? C7 C6 P1 122.7(6) . . ? C8 C7 C6 120.8(8) . . ? C7 C8 C9 119.6(9) . . ? C10 C9 C8 120.4(9) . . ? C9 C10 C11 119.5(10) . . ? C10 C11 C6 122.0(8) . . ? C17 C12 C13 116.9(7) . . ? C17 C12 P1 125.0(6) . . ? C13 C12 P1 118.0(5) . . ? C12 C13 C14 121.5(7) . . ? C15 C14 C13 119.7(8) . . ? C16 C15 C14 118.9(8) . . ? C15 C16 C17 122.5(8) . . ? C16 C17 C12 120.3(8) . . ? C23 C18 C19 119.0(8) . . ? C23 C18 P2 122.3(7) . . ? C19 C18 P2 118.4(7) . . ? C18 C19 C20 120.7(10) . . ? C21 C20 C19 119.6(12) . . ? C20 C21 C22 121.1(12) . . ? C21 C22 C23 119.1(12) . . ? C18 C23 C22 120.5(11) . . ? C29 C24 C25 117.7(7) . . ? C29 C24 P2 120.1(7) . . ? C25 C24 P2 122.1(6) . . ? C26 C25 C24 123.3(10) . . ? C25 C26 C27 117.8(12) . . ? C28 C27 C26 120.4(13) . . ? C27 C28 C29 119.4(12) . . ? C24 C29 C28 120.4(10) . . ? P3 C30 P4 95.1(3) . . ? C32 C31 C36 117.6(8) . . ? C32 C31 P3 123.3(7) . . ? C36 C31 P3 119.0(7) . . ? C33 C32 C31 121.3(9) . . ? C34 C33 C32 121.6(11) . . ? C33 C34 C35 120.7(10) . . ? C34 C35 C36 118.7(10) . . ? C31 C36 C35 120.0(9) . . ? C38 C37 C42 117.5(8) . . ? C38 C37 P3 123.8(7) . . ? C42 C37 P3 118.6(6) . . ? C37 C38 C39 120.0(10) . . ? C40 C39 C38 121.4(11) . . ? C39 C40 C41 119.3(11) . . ? C42 C41 C40 116.9(11) . . ? C41 C42 C37 124.4(10) . . ? C44 C43 C48 118.7(8) . . ? C44 C43 P4 120.0(7) . . ? C48 C43 P4 121.2(7) . . ? C45 C44 C43 122.7(10) . . ? C44 C45 C46 117.0(12) . . ? C47 C46 C45 121.4(11) . . ? C46 C47 C48 122.1(12) . . ? C47 C48 C43 117.6(10) . . ? C50 C49 C54 119.0(8) . . ? C50 C49 P4 119.9(7) . . ? C54 C49 P4 121.0(7) . . ? C49 C50 C51 122.0(9) . . ? C52 C51 C50 119.1(9) . . ? C51 C52 C53 120.4(10) . . ? C52 C53 C54 119.8(9) . . ? C49 C54 C53 119.7(9) . . ? F4 B1 F3 110.4(10) . . ? F4 B1 F1 111.1(9) . . ? F3 B1 F1 107.6(9) . . ? F4 B1 F2 112.4(9) . . ? F3 B1 F2 104.6(9) . . ? F1 B1 F2 110.4(9) . . ? F6 B2 F5 115.7(12) . . ? F6 B2 F8 115.4(12) . . ? F5 B2 F8 113.5(11) . . ? F6 B2 F7 100.6(12) . . ? F5 B2 F7 102.5(12) . . ? F8 B2 F7 106.8(12) . . ? B2 F5 F7 40.3(8) . . ? B2 F5 F6 32.0(6) . . ? F7 F5 F6 57.4(4) . . ? B2 F5 F8 33.8(6) . . ? F7 F5 F8 61.1(4) . . ? F6 F5 F8 60.7(3) . . ? B2 F6 F7 41.4(7) . . ? B2 F6 F5 32.2(7) . . ? F7 F6 F5 58.9(4) . . ? B2 F6 F8 32.9(7) . . ? F7 F6 F8 61.3(4) . . ? F5 F6 F8 59.9(3) . . ? B2 F7 F6 38.0(6) . . ? B2 F7 F5 37.2(7) . . ? F6 F7 F5 63.6(5) . . ? B2 F7 F8 35.8(6) . . ? F6 F7 F8 62.9(4) . . ? F5 F7 F8 61.9(4) . . ? B2 F8 F7 37.5(7) . . ? B2 F8 F5 32.7(6) . . ? F7 F8 F5 57.1(4) . . ? B2 F8 F6 31.7(6) . . ? F7 F8 F6 55.8(4) . . ? F5 F8 F6 59.4(3) . . ? C1 N1 Ru1 177.7(6) . . ? C3 N2 Ru1 176.7(6) . . ? C6 P1 C12 103.3(3) . . ? C6 P1 C5 107.4(3) . . ? C12 P1 C5 109.7(3) . . ? C6 P1 Ru1 126.6(2) . . ? C12 P1 Ru1 115.7(2) . . ? C5 P1 Ru1 92.77(19) . . ? C24 P2 C5 105.6(3) . . ? C24 P2 C18 101.0(3) . . ? C5 P2 C18 106.3(4) . . ? C24 P2 Ru1 117.3(2) . . ? C5 P2 Ru1 95.0(2) . . ? C18 P2 Ru1 128.9(2) . . ? C37 P3 C31 104.1(3) . . ? C37 P3 C30 106.7(3) . . ? C31 P3 C30 107.1(4) . . ? C37 P3 Ru1 115.2(2) . . ? C31 P3 Ru1 126.7(2) . . ? C30 P3 Ru1 94.8(2) . . ? C49 P4 C43 101.4(3) . . ? C49 P4 C30 108.9(4) . . ? C43 P4 C30 108.5(4) . . ? C49 P4 Ru1 126.9(3) . . ? C43 P4 Ru1 116.7(2) . . ? C30 P4 Ru1 93.2(2) . . ? N2 Ru1 N1 86.5(2) . . ? N2 Ru1 P3 166.55(16) . . ? N1 Ru1 P3 91.28(16) . . ? N2 Ru1 P2 91.43(16) . . ? N1 Ru1 P2 164.84(16) . . ? P3 Ru1 P2 94.09(7) . . ? N2 Ru1 P1 90.13(16) . . ? N1 Ru1 P1 94.32(16) . . ? P3 Ru1 P1 103.27(6) . . ? P2 Ru1 P1 70.65(6) . . ? N2 Ru1 P4 96.35(16) . . ? N1 Ru1 P4 92.91(16) . . ? P3 Ru1 P4 70.49(7) . . ? P2 Ru1 P4 102.25(7) . . ? P1 Ru1 P4 170.57(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 C11 C6 C7 C8 1.8(11) . . . . ? P1 C6 C7 C8 -179.0(6) . . . . ? C6 C7 C8 C9 -1.7(13) . . . . ? C7 C8 C9 C10 1.2(16) . . . . ? C8 C9 C10 C11 -0.7(16) . . . . ? C9 C10 C11 C6 0.9(14) . . . . ? C7 C6 C11 C10 -1.4(12) . . . . ? P1 C6 C11 C10 179.4(6) . . . . ? C17 C12 C13 C14 -2.7(12) . . . . ? P1 C12 C13 C14 -178.9(7) . . . . ? C12 C13 C14 C15 3.7(14) . . . . ? C13 C14 C15 C16 -1.7(14) . . . . ? C14 C15 C16 C17 -1.3(15) . . . . ? C15 C16 C17 C12 2.3(15) . . . . ? C13 C12 C17 C16 -0.3(12) . . . . ? P1 C12 C17 C16 175.7(7) . . . . ? C23 C18 C19 C20 2.0(15) . . . . ? P2 C18 C19 C20 176.1(9) . . . . ? C18 C19 C20 C21 -2(2) . . . . ? C19 C20 C21 C22 2(2) . . . . ? C20 C21 C22 C23 -1(2) . . . . ? C19 C18 C23 C22 -1.7(14) . . . . ? P2 C18 C23 C22 -175.6(8) . . . . ? C21 C22 C23 C18 1.5(17) . . . . ? C29 C24 C25 C26 2.1(13) . . . . ? P2 C24 C25 C26 -180.0(7) . . . . ? C24 C25 C26 C27 4.1(16) . . . . ? C25 C26 C27 C28 -11(2) . . . . ? C26 C27 C28 C29 12(2) . . . . ? C25 C24 C29 C28 -1.6(14) . . . . ? P2 C24 C29 C28 -179.6(8) . . . . ? C27 C28 C29 C24 -5.1(19) . . . . ? C36 C31 C32 C33 -2.1(13) . . . . ? P3 C31 C32 C33 177.7(8) . . . . ? C31 C32 C33 C34 2.8(17) . . . . ? C32 C33 C34 C35 -1.2(19) . . . . ? C33 C34 C35 C36 -1.0(16) . . . . ? C32 C31 C36 C35 -0.1(11) . . . . ? P3 C31 C36 C35 -179.9(6) . . . . ? C34 C35 C36 C31 1.6(13) . . . . ? C42 C37 C38 C39 1.7(12) . . . . ? P3 C37 C38 C39 -175.2(7) . . . . ? C37 C38 C39 C40 1.0(16) . . . . ? C38 C39 C40 C41 -5.8(17) . . . . ? C39 C40 C41 C42 7.6(15) . . . . ? C40 C41 C42 C37 -5.2(14) . . . . ? C38 C37 C42 C41 0.6(12) . . . . ? P3 C37 C42 C41 177.6(7) . . . . ? C48 C43 C44 C45 0.1(12) . . . . ? P4 C43 C44 C45 178.5(7) . . . . ? C43 C44 C45 C46 4.2(15) . . . . ? C44 C45 C46 C47 -8(2) . . . . ? C45 C46 C47 C48 8(2) . . . . ? C46 C47 C48 C43 -3.2(19) . . . . ? C44 C43 C48 C47 -0.8(13) . . . . ? P4 C43 C48 C47 -179.1(8) . . . . ? C54 C49 C50 C51 0.1(12) . . . . ? P4 C49 C50 C51 -176.4(6) . . . . ? C49 C50 C51 C52 1.4(13) . . . . ? C50 C51 C52 C53 -2.1(15) . . . . ? C51 C52 C53 C54 1.3(15) . . . . ? C50 C49 C54 C53 -0.9(12) . . . . ? P4 C49 C54 C53 175.6(6) . . . . ? C52 C53 C54 C49 0.2(14) . . . . ? F6 B2 F5 F7 -108.4(16) . . . . ? F8 B2 F5 F7 114.7(16) . . . . ? F8 B2 F5 F6 -137(2) . . . . ? F7 B2 F5 F6 108.4(16) . . . . ? F6 B2 F5 F8 137(2) . . . . ? F7 B2 F5 F8 -114.7(16) . . . . ? F5 B2 F6 F7 109.6(16) . . . . ? F8 B2 F6 F7 -114.4(17) . . . . ? F8 B2 F6 F5 136(2) . . . . ? F7 B2 F6 F5 -109.6(16) . . . . ? F5 B2 F6 F8 -136(2) . . . . ? F7 B2 F6 F8 114.4(17) . . . . ? F7 F5 F6 B2 46.7(14) . . . . ? F8 F5 F6 B2 -25.9(14) . . . . ? B2 F5 F6 F7 -46.7(14) . . . . ? F8 F5 F6 F7 -72.6(5) . . . . ? B2 F5 F6 F8 25.9(14) . . . . ? F7 F5 F6 F8 72.6(5) . . . . ? F5 B2 F7 F6 -119.6(13) . . . . ? F8 B2 F7 F6 120.8(14) . . . . ? F6 B2 F7 F5 119.6(13) . . . . ? F8 B2 F7 F5 -119.6(13) . . . . ? F6 B2 F7 F8 -120.8(14) . . . . ? F5 B2 F7 F8 119.6(13) . . . . ? F5 F6 F7 B2 35.9(10) . . . . ? F8 F6 F7 B2 -34.3(10) . . . . ? B2 F6 F7 F5 -35.9(10) . . . . ? F8 F6 F7 F5 -70.3(4) . . . . ? B2 F6 F7 F8 34.3(10) . . . . ? F5 F6 F7 F8 70.3(4) . . . . ? F6 F5 F7 B2 -36.7(9) . . . . ? F8 F5 F7 B2 35.2(9) . . . . ? B2 F5 F7 F6 36.7(9) . . . . ? F8 F5 F7 F6 71.9(5) . . . . ? B2 F5 F7 F8 -35.2(9) . . . . ? F6 F5 F7 F8 -71.9(5) . . . . ? F6 B2 F8 F7 110.9(17) . . . . ? F5 B2 F8 F7 -112.2(17) . . . . ? F6 B2 F8 F5 -137(2) . . . . ? F7 B2 F8 F5 112.2(17) . . . . ? F5 B2 F8 F6 137(2) . . . . ? F7 B2 F8 F6 -110.9(17) . . . . ? F6 F7 F8 B2 -36.4(10) . . . . ? F5 F7 F8 B2 36.6(10) . . . . ? B2 F7 F8 F5 -36.6(10) . . . . ? F6 F7 F8 F5 -73.0(5) . . . . ? B2 F7 F8 F6 36.4(10) . . . . ? F5 F7 F8 F6 73.0(5) . . . . ? F7 F5 F8 B2 -42.1(13) . . . . ? F6 F5 F8 B2 24.6(14) . . . . ? B2 F5 F8 F7 42.1(13) . . . . ? F6 F5 F8 F7 66.7(5) . . . . ? B2 F5 F8 F6 -24.6(14) . . . . ? F7 F5 F8 F6 -66.7(5) . . . . ? F7 F6 F8 B2 43.4(14) . . . . ? F5 F6 F8 B2 -25.4(14) . . . . ? B2 F6 F8 F7 -43.4(14) . . . . ? F5 F6 F8 F7 -68.8(5) . . . . ? B2 F6 F8 F5 25.4(14) . . . . ? F7 F6 F8 F5 68.8(5) . . . . ? C2 C1 N1 Ru1 62(27) . . . . ? C4 C3 N2 Ru1 75(17) . . . . ? C11 C6 P1 C12 82.3(6) . . . . ? C7 C6 P1 C12 -96.8(6) . . . . ? C11 C6 P1 C5 -161.8(6) . . . . ? C7 C6 P1 C5 19.1(7) . . . . ? C11 C6 P1 Ru1 -54.6(7) . . . . ? C7 C6 P1 Ru1 126.3(6) . . . . ? C17 C12 P1 C6 107.5(7) . . . . ? C13 C12 P1 C6 -76.6(6) . . . . ? C17 C12 P1 C5 -6.8(7) . . . . ? C13 C12 P1 C5 169.2(5) . . . . ? C17 C12 P1 Ru1 -110.0(6) . . . . ? C13 C12 P1 Ru1 65.9(6) . . . . ? P2 C5 P1 C6 149.0(3) . . . . ? P2 C5 P1 C12 -99.3(3) . . . . ? P2 C5 P1 Ru1 19.2(3) . . . . ? C29 C24 P2 C5 -155.0(6) . . . . ? C25 C24 P2 C5 27.1(7) . . . . ? C29 C24 P2 C18 94.4(7) . . . . ? C25 C24 P2 C18 -83.5(7) . . . . ? C29 C24 P2 Ru1 -50.8(7) . . . . ? C25 C24 P2 Ru1 131.3(6) . . . . ? P1 C5 P2 C24 100.7(3) . . . . ? P1 C5 P2 C18 -152.6(3) . . . . ? P1 C5 P2 Ru1 -19.5(3) . . . . ? C23 C18 P2 C24 105.6(7) . . . . ? C19 C18 P2 C24 -68.3(7) . . . . ? C23 C18 P2 C5 -4.4(8) . . . . ? C19 C18 P2 C5 -178.4(7) . . . . ? C23 C18 P2 Ru1 -115.1(7) . . . . ? C19 C18 P2 Ru1 70.9(8) . . . . ? C38 C37 P3 C31 -103.6(7) . . . . ? C42 C37 P3 C31 79.6(7) . . . . ? C38 C37 P3 C30 9.5(7) . . . . ? C42 C37 P3 C30 -167.3(6) . . . . ? C38 C37 P3 Ru1 113.3(6) . . . . ? C42 C37 P3 Ru1 -63.5(6) . . . . ? C32 C31 P3 C37 112.2(7) . . . . ? C36 C31 P3 C37 -67.9(7) . . . . ? C32 C31 P3 C30 -0.6(7) . . . . ? C36 C31 P3 C30 179.3(6) . . . . ? C32 C31 P3 Ru1 -110.4(6) . . . . ? C36 C31 P3 Ru1 69.4(7) . . . . ? P4 C30 P3 C37 97.0(3) . . . . ? P4 C30 P3 C31 -152.0(3) . . . . ? P4 C30 P3 Ru1 -21.2(3) . . . . ? C50 C49 P4 C43 83.3(7) . . . . ? C54 C49 P4 C43 -93.2(7) . . . . ? C50 C49 P4 C30 -162.5(6) . . . . ? C54 C49 P4 C30 21.0(8) . . . . ? C50 C49 P4 Ru1 -53.2(8) . . . . ? C54 C49 P4 Ru1 130.3(6) . . . . ? C44 C43 P4 C49 -96.0(6) . . . . ? C48 C43 P4 C49 82.3(7) . . . . ? C44 C43 P4 C30 149.4(6) . . . . ? C48 C43 P4 C30 -32.2(7) . . . . ? C44 C43 P4 Ru1 45.9(6) . . . . ? C48 C43 P4 Ru1 -135.8(6) . . . . ? P3 C30 P4 C49 151.6(3) . . . . ? P3 C30 P4 C43 -98.9(3) . . . . ? P3 C30 P4 Ru1 20.7(2) . . . . ? C3 N2 Ru1 N1 86(11) . . . . ? C3 N2 Ru1 P3 167(10) . . . . ? C3 N2 Ru1 P2 -79(11) . . . . ? C3 N2 Ru1 P1 -8(11) . . . . ? C3 N2 Ru1 P4 179(100) . . . . ? C1 N1 Ru1 N2 53(15) . . . . ? C1 N1 Ru1 P3 -114(15) . . . . ? C1 N1 Ru1 P2 135(15) . . . . ? C1 N1 Ru1 P1 142(15) . . . . ? C1 N1 Ru1 P4 -44(15) . . . . ? C37 P3 Ru1 N2 -81.4(8) . . . . ? C31 P3 Ru1 N2 145.2(8) . . . . ? C30 P3 Ru1 N2 29.6(8) . . . . ? C37 P3 Ru1 N1 -1.2(3) . . . . ? C31 P3 Ru1 N1 -134.6(4) . . . . ? C30 P3 Ru1 N1 109.8(3) . . . . ? C37 P3 Ru1 P2 164.6(3) . . . . ? C31 P3 Ru1 P2 31.2(4) . . . . ? C30 P3 Ru1 P2 -84.4(2) . . . . ? C37 P3 Ru1 P1 93.5(3) . . . . ? C31 P3 Ru1 P1 -39.9(4) . . . . ? C30 P3 Ru1 P1 -155.4(2) . . . . ? C37 P3 Ru1 P4 -93.8(3) . . . . ? C31 P3 Ru1 P4 132.7(4) . . . . ? C30 P3 Ru1 P4 17.2(2) . . . . ? C24 P2 Ru1 N2 -4.9(3) . . . . ? C5 P2 Ru1 N2 105.6(3) . . . . ? C18 P2 Ru1 N2 -138.7(4) . . . . ? C24 P2 Ru1 N1 -86.7(7) . . . . ? C5 P2 Ru1 N1 23.8(7) . . . . ? C18 P2 Ru1 N1 139.5(7) . . . . ? C24 P2 Ru1 P3 162.9(3) . . . . ? C5 P2 Ru1 P3 -86.6(2) . . . . ? C18 P2 Ru1 P3 29.0(4) . . . . ? C24 P2 Ru1 P1 -94.5(3) . . . . ? C5 P2 Ru1 P1 16.0(2) . . . . ? C18 P2 Ru1 P1 131.7(4) . . . . ? C24 P2 Ru1 P4 92.0(3) . . . . ? C5 P2 Ru1 P4 -157.6(2) . . . . ? C18 P2 Ru1 P4 -41.9(4) . . . . ? C6 P1 Ru1 N2 138.9(3) . . . . ? C12 P1 Ru1 N2 6.4(3) . . . . ? C5 P1 Ru1 N2 -107.0(3) . . . . ? C6 P1 Ru1 N1 52.4(3) . . . . ? C12 P1 Ru1 N1 -80.1(3) . . . . ? C5 P1 Ru1 N1 166.5(3) . . . . ? C6 P1 Ru1 P3 -39.9(3) . . . . ? C12 P1 Ru1 P3 -172.4(2) . . . . ? C5 P1 Ru1 P3 74.2(2) . . . . ? C6 P1 Ru1 P2 -129.6(3) . . . . ? C12 P1 Ru1 P2 97.9(2) . . . . ? C5 P1 Ru1 P2 -15.5(2) . . . . ? C6 P1 Ru1 P4 -87.6(5) . . . . ? C12 P1 Ru1 P4 140.0(5) . . . . ? C5 P1 Ru1 P4 26.5(5) . . . . ? C49 P4 Ru1 N2 49.2(4) . . . . ? C43 P4 Ru1 N2 -81.7(3) . . . . ? C30 P4 Ru1 N2 165.8(3) . . . . ? C49 P4 Ru1 N1 136.0(4) . . . . ? C43 P4 Ru1 N1 5.1(3) . . . . ? C30 P4 Ru1 N1 -107.4(3) . . . . ? C49 P4 Ru1 P3 -133.7(4) . . . . ? C43 P4 Ru1 P3 95.4(3) . . . . ? C30 P4 Ru1 P3 -17.1(2) . . . . ? C49 P4 Ru1 P2 -43.7(4) . . . . ? C43 P4 Ru1 P2 -174.5(3) . . . . ? C30 P4 Ru1 P2 72.9(2) . . . . ? C49 P4 Ru1 P1 -84.0(6) . . . . ? C43 P4 Ru1 P1 145.2(5) . . . . ? C30 P4 Ru1 P1 32.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.500 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.500 _refine_diff_density_max 0.357 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.047