# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1594 data_nrb9939 _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr Neil R Branda' _publ_contact_author_address ; Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; _publ_contact_author_email Neil.Branda@ualberta.ca _publ_contact_author_fax '+1 780 492 8231' _publ_contact_author_phone '+1 780 492 8187' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data which are being submitted in support of an upcoming communication to be published in Chemical Communications (manuscript MS B001259I). Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Chemical Communications' _publ_section_title 'Axially Coordinated Porphyrins as New Rotaxane Stoppers' loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Walsh, M. Catherine' . ; Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; 'Chichak, Kelly' . ; Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; 'Branda, Neil R.' . ; Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; _chemical_formula_sum 'C166.50 H169 F12 N12 O17.50 P2 Ru2' _chemical_formula_weight 3110.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.655(2) _cell_length_b 30.385(5) _cell_length_c 24.340(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.745(3) _cell_angle_gamma 90.00 _cell_volume 8373(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5453 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3236 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5738 _exptl_absorpt_correction_T_max 0.9803 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41325 _diffrn_reflns_av_R_equivalents 0.2291 _diffrn_reflns_av_sigmaI/netI 0.4346 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.52 _reflns_number_total 17184 _reflns_number_gt 4929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0981P)^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 17184 _refine_ls_number_parameters 976 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2872 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2673 _refine_ls_wR_factor_gt 0.2014 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _refine_ls_shift/su_max 0.090 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.06653(7) 0.24090(2) 0.21983(3) 0.0281(2) Uani 1 1 d . . . O1 O -0.0534(7) 0.1610(2) 0.1629(3) 0.064(2) Uani 1 1 d . . . O2 O 0.2541(5) 0.4242(2) 0.4903(3) 0.0411(18) Uani 1 1 d . . . O3 O 0.2345(6) 0.5241(2) 0.4899(3) 0.0482(19) Uani 1 1 d . . . O4 O 0.3125(6) 0.6040(2) 0.4607(3) 0.051(2) Uani 1 1 d . . . O5 O 0.5642(6) 0.6274(2) 0.4846(3) 0.0447(18) Uani 1 1 d . . . N1 N -0.0503(6) 0.2476(2) 0.2707(3) 0.030(2) Uani 1 1 d . . . N2 N -0.0337(6) 0.2841(2) 0.1630(3) 0.0262(19) Uani 1 1 d . . . N3 N 0.1885(6) 0.2379(2) 0.1717(3) 0.0256(18) Uani 1 1 d . . . N4 N 0.1714(6) 0.2013(2) 0.2790(3) 0.0266(19) Uani 1 1 d . . . N5 N 0.1649(6) 0.2975(2) 0.2632(3) 0.0247(18) Uani 1 1 d . . . N6 N 0.4489(7) 0.4734(2) 0.4291(3) 0.0288(19) Uani 1 1 d . . . C1 C -0.0118(8) 0.1916(3) 0.1835(4) 0.034(3) Uani 1 1 d . . . C2 C 0.4996(9) 0.5081(3) 0.4714(3) 0.037(3) Uani 1 1 d . . . H2A H 0.5812 0.5152 0.4689 0.044 Uiso 1 1 calc R . . H2B H 0.4515 0.5352 0.4634 0.044 Uiso 1 1 calc R . . C10 C 0.0487(8) 0.1988(3) 0.3500(4) 0.028(2) Uani 1 1 d . . . C11 C -0.0443(8) 0.2271(3) 0.3212(4) 0.029(2) Uani 1 1 d . . . C12 C -0.1479(8) 0.2382(3) 0.3417(4) 0.033(2) Uani 1 1 d . . . H12 H -0.1665 0.2278 0.3753 0.040 Uiso 1 1 calc R . . C13 C -0.2126(8) 0.2662(3) 0.3038(4) 0.032(2) Uani 1 1 d . . . H13 H -0.2841 0.2799 0.3067 0.038 Uiso 1 1 calc R . . C14 C -0.1553(8) 0.2715(3) 0.2588(4) 0.028(2) Uani 1 1 d . . . C15 C -0.1955(8) 0.2972(3) 0.2091(4) 0.031(2) Uani 1 1 d . . . C16 C -0.1401(8) 0.3024(3) 0.1644(4) 0.030(2) Uani 1 1 d . . . C17 C -0.1845(9) 0.3285(3) 0.1155(5) 0.047(3) Uani 1 1 d . . . H17 H -0.2562 0.3447 0.1069 0.056 Uiso 1 1 calc R . . C18 C -0.1047(9) 0.3254(3) 0.0841(5) 0.046(3) Uani 1 1 d . . . H18 H -0.1108 0.3391 0.0484 0.056 Uiso 1 1 calc R . . C19 C -0.0080(8) 0.2979(3) 0.1131(4) 0.031(2) Uani 1 1 d . . . C20 C 0.0949(9) 0.2876(3) 0.0936(4) 0.035(3) Uani 1 1 d . . . C21 C 0.1846(8) 0.2583(3) 0.1214(4) 0.030(2) Uani 1 1 d . . . C22 C 0.2833(8) 0.2471(3) 0.1004(4) 0.032(2) Uani 1 1 d . . . H22 H 0.3010 0.2574 0.0665 0.039 Uiso 1 1 calc R . . C23 C 0.3469(8) 0.2190(3) 0.1376(4) 0.032(2) Uani 1 1 d . . . H23 H 0.4183 0.2052 0.1344 0.039 Uiso 1 1 calc R . . C24 C 0.2909(8) 0.2130(3) 0.1823(4) 0.031(2) Uani 1 1 d . . . C25 C 0.3306(8) 0.1878(3) 0.2318(4) 0.030(2) Uani 1 1 d . . . C26 C 0.2794(8) 0.1829(3) 0.2772(4) 0.030(2) Uani 1 1 d . . . C27 C 0.3243(8) 0.1585(3) 0.3281(4) 0.038(3) Uani 1 1 d . . . H27 H 0.3970 0.1429 0.3375 0.045 Uiso 1 1 calc R . . C28 C 0.2451(9) 0.1614(3) 0.3601(5) 0.042(3) Uani 1 1 d . . . H28 H 0.2515 0.1482 0.3961 0.051 Uiso 1 1 calc R . . C29 C 0.1497(8) 0.1880(3) 0.3302(4) 0.032(2) Uani 1 1 d . . . C31 C 0.0345(8) 0.1774(3) 0.4022(4) 0.036(3) Uani 1 1 d . . . C32 C 0.0368(9) 0.1998(3) 0.4526(5) 0.043(3) Uani 1 1 d . . . H32 H 0.0505 0.2307 0.4542 0.052 Uiso 1 1 calc R . . C33 C 0.0199(9) 0.1786(4) 0.4999(5) 0.055(3) Uani 1 1 d . . . H33 H 0.0220 0.1951 0.5333 0.065 Uiso 1 1 calc R . . C34 C -0.0001(9) 0.1334(4) 0.5001(5) 0.052(3) Uani 1 1 d . . . C35 C 0.0010(10) 0.1112(4) 0.4523(5) 0.058(3) Uani 1 1 d . . . H35 H -0.0101 0.0802 0.4519 0.070 Uiso 1 1 calc R . . C36 C 0.0177(9) 0.1313(4) 0.4040(5) 0.052(3) Uani 1 1 d . . . H36 H 0.0179 0.1140 0.3715 0.062 Uiso 1 1 calc R . . C37 C -0.0191(11) 0.1128(4) 0.5530(5) 0.079(4) Uani 1 1 d . . . H37A H -0.0209 0.0807 0.5489 0.095 Uiso 1 1 calc R . . H37B H -0.0944 0.1230 0.5597 0.095 Uiso 1 1 calc R . . H37C H 0.0454 0.1212 0.5850 0.095 Uiso 1 1 calc R . . C41 C -0.3084(8) 0.3213(3) 0.2058(4) 0.032(2) Uani 1 1 d . . . C42 C -0.3057(9) 0.3654(3) 0.2232(5) 0.050(3) Uani 1 1 d . . . H42 H -0.2322 0.3798 0.2375 0.060 Uiso 1 1 calc R . . C43 C -0.4107(9) 0.3880(3) 0.2194(5) 0.053(3) Uani 1 1 d . . . H43 H -0.4073 0.4178 0.2314 0.064 Uiso 1 1 calc R . . C44 C -0.5190(9) 0.3690(3) 0.1991(4) 0.037(3) Uani 1 1 d . . . C45 C -0.5205(9) 0.3247(3) 0.1833(4) 0.046(3) Uani 1 1 d . . . H45 H -0.5939 0.3099 0.1709 0.055 Uiso 1 1 calc R . . C46 C -0.4162(8) 0.3023(3) 0.1856(4) 0.041(3) Uani 1 1 d . . . H46 H -0.4197 0.2727 0.1726 0.050 Uiso 1 1 calc R . . C47 C -0.6331(9) 0.3942(4) 0.1915(5) 0.059(3) Uani 1 1 d . . . H47A H -0.6493 0.4100 0.1554 0.071 Uiso 1 1 calc R . . H47B H -0.6265 0.4153 0.2225 0.071 Uiso 1 1 calc R . . H47C H -0.6978 0.3736 0.1918 0.071 Uiso 1 1 calc R . . C51 C 0.1086(8) 0.3096(3) 0.0412(4) 0.031(2) Uani 1 1 d . . . C52 C 0.1336(10) 0.3545(4) 0.0419(5) 0.059(3) Uani 1 1 d . . . H52 H 0.1387 0.3710 0.0756 0.071 Uiso 1 1 calc R . . C53 C 0.1510(10) 0.3754(4) -0.0063(5) 0.060(3) Uani 1 1 d . . . H53 H 0.1689 0.4059 -0.0044 0.072 Uiso 1 1 calc R . . C54 C 0.1434(9) 0.3538(4) -0.0561(5) 0.056(3) Uani 1 1 d . . . C55 C 0.1138(10) 0.3097(4) -0.0560(5) 0.064(3) Uani 1 1 d . . . H55 H 0.1044 0.2935 -0.0901 0.076 Uiso 1 1 calc R . . C56 C 0.0975(9) 0.2884(3) -0.0090(4) 0.048(3) Uani 1 1 d . . . H56 H 0.0778 0.2580 -0.0114 0.058 Uiso 1 1 calc R . . C57 C 0.1654(11) 0.3757(4) -0.1084(5) 0.080(4) Uani 1 1 d . . . H57A H 0.1123 0.4010 -0.1185 0.096 Uiso 1 1 calc R . . H57B H 0.1505 0.3546 -0.1398 0.096 Uiso 1 1 calc R . . H57C H 0.2475 0.3858 -0.1009 0.096 Uiso 1 1 calc R . . C61 C 0.4459(8) 0.1639(3) 0.2370(4) 0.031(2) Uani 1 1 d . . . C62 C 0.5521(8) 0.1850(3) 0.2467(5) 0.046(3) Uani 1 1 d . . . H62 H 0.5530 0.2162 0.2495 0.055 Uiso 1 1 calc R . . C63 C 0.6581(9) 0.1632(3) 0.2526(5) 0.051(3) Uani 1 1 d . . . H63 H 0.7302 0.1793 0.2603 0.061 Uiso 1 1 calc R . . C64 C 0.6591(9) 0.1180(4) 0.2473(4) 0.044(3) Uani 1 1 d . . . C65 C 0.5537(9) 0.0953(4) 0.2353(5) 0.052(3) Uani 1 1 d . . . H65 H 0.5534 0.0642 0.2311 0.062 Uiso 1 1 calc R . . C66 C 0.4485(9) 0.1178(3) 0.2294(4) 0.045(3) Uani 1 1 d . . . H66 H 0.3763 0.1019 0.2200 0.053 Uiso 1 1 calc R . . C67 C 0.7761(9) 0.0931(4) 0.2563(5) 0.067(4) Uani 1 1 d . . . H67A H 0.7698 0.0704 0.2270 0.080 Uiso 1 1 calc R . . H67B H 0.7940 0.0791 0.2936 0.080 Uiso 1 1 calc R . . H67C H 0.8394 0.1137 0.2539 0.080 Uiso 1 1 calc R . . C71 C 0.1083(8) 0.3349(3) 0.2701(4) 0.034(3) Uani 1 1 d . . . H71 H 0.0257 0.3370 0.2543 0.041 Uiso 1 1 calc R . . C72 C 0.1654(8) 0.3697(3) 0.2989(4) 0.037(3) Uani 1 1 d . . . H72 H 0.1215 0.3954 0.3026 0.044 Uiso 1 1 calc R . . C73 C 0.2860(8) 0.3693(3) 0.3231(4) 0.028(2) Uani 1 1 d . . . C74 C 0.3436(8) 0.3312(3) 0.3140(4) 0.032(2) Uani 1 1 d . . . H74 H 0.4266 0.3288 0.3283 0.038 Uiso 1 1 calc R . . C75 C 0.2805(8) 0.2963(3) 0.2841(4) 0.032(3) Uani 1 1 d . . . H75 H 0.3223 0.2705 0.2784 0.039 Uiso 1 1 calc R . . C76 C 0.3407(9) 0.4785(3) 0.3952(4) 0.034(2) Uani 1 1 d . . . H76 H 0.2987 0.5051 0.3969 0.041 Uiso 1 1 calc R . . C77 C 0.2903(8) 0.4465(3) 0.3585(4) 0.040(3) Uani 1 1 d . . . H77 H 0.2149 0.4515 0.3339 0.047 Uiso 1 1 calc R . . C78 C 0.3473(8) 0.4063(3) 0.3562(4) 0.025(2) Uani 1 1 d . . . C79 C 0.4603(8) 0.4026(3) 0.3901(4) 0.040(3) Uani 1 1 d . . . H79 H 0.5037 0.3764 0.3884 0.048 Uiso 1 1 calc R . . C80 C 0.5123(8) 0.4358(3) 0.4265(4) 0.044(3) Uani 1 1 d . . . H80 H 0.5903 0.4327 0.4493 0.053 Uiso 1 1 calc R . . C81 C 0.2380(10) 0.3808(3) 0.4691(4) 0.039(3) Uani 1 1 d . . . C82 C 0.3357(9) 0.3550(3) 0.4817(4) 0.037(3) Uani 1 1 d . . . C83 C 0.3260(11) 0.3124(4) 0.4606(5) 0.057(3) Uani 1 1 d . . . H83 H 0.3925 0.2934 0.4695 0.068 Uiso 1 1 calc R . . C84 C 0.2205(11) 0.2973(4) 0.4269(5) 0.057(3) Uani 1 1 d . . . H84 H 0.2149 0.2682 0.4121 0.068 Uiso 1 1 calc R . . C85 C 0.1249(11) 0.3244(4) 0.4152(5) 0.057(3) Uani 1 1 d . . . H85 H 0.0520 0.3141 0.3924 0.069 Uiso 1 1 calc R . . C86 C 0.1333(10) 0.3665(3) 0.4360(4) 0.047(3) Uani 1 1 d . . . H86 H 0.0667 0.3855 0.4276 0.057 Uiso 1 1 calc R . . C87 C 0.1479(8) 0.4504(3) 0.4872(5) 0.048(3) Uani 1 1 d . . . H87A H 0.0906 0.4335 0.5030 0.058 Uiso 1 1 calc R . . H87B H 0.1104 0.4574 0.4472 0.058 Uiso 1 1 calc R . . C88 C 0.1816(9) 0.4922(3) 0.5204(4) 0.044(3) Uani 1 1 d . . . H88A H 0.1102 0.5053 0.5293 0.053 Uiso 1 1 calc R . . H88B H 0.2379 0.4852 0.5566 0.053 Uiso 1 1 calc R . . C89 C 0.1524(8) 0.5570(3) 0.4634(4) 0.045(3) Uani 1 1 d . . . H89A H 0.1268 0.5746 0.4926 0.054 Uiso 1 1 calc R . . H89B H 0.0817 0.5428 0.4392 0.054 Uiso 1 1 calc R . . C90 C 0.2085(9) 0.5863(3) 0.4282(5) 0.048(3) Uani 1 1 d . . . H90A H 0.2258 0.5694 0.3964 0.058 Uiso 1 1 calc R . . H90B H 0.1534 0.6104 0.4122 0.058 Uiso 1 1 calc R . . C91 C 0.3675(8) 0.6315(3) 0.4253(5) 0.053(3) Uani 1 1 d . . . H91A H 0.3093 0.6524 0.4032 0.064 Uiso 1 1 calc R . . H91B H 0.3995 0.6132 0.3988 0.064 Uiso 1 1 calc R . . C92 C 0.4645(9) 0.6557(3) 0.4647(5) 0.051(3) Uani 1 1 d . . . H92A H 0.4886 0.6813 0.4449 0.061 Uiso 1 1 calc R . . H92B H 0.4359 0.6668 0.4973 0.061 Uiso 1 1 calc R . . P P 0.3885(3) 0.03165(9) -0.17568(14) 0.0482(8) Uani 1 1 d . . . F1 F 0.5222(6) 0.0164(2) -0.1663(4) 0.101(3) Uani 1 1 d . . . F2 F 0.2574(5) 0.0469(2) -0.1843(3) 0.081(2) Uani 1 1 d . . . F3 F 0.4216(6) 0.0790(2) -0.1958(3) 0.089(2) Uani 1 1 d . . . F4 F 0.3562(6) -0.01524(18) -0.1553(3) 0.073(2) Uani 1 1 d . . . F5 F 0.4136(6) 0.0488(2) -0.1124(3) 0.072(2) Uani 1 1 d . . . F6 F 0.3625(7) 0.0144(2) -0.2386(3) 0.097(2) Uani 1 1 d . . . O1S O 0.6235(7) 0.3104(2) 0.4026(3) 0.061(2) Uani 1 1 d . . . C1S C 0.7639(11) 0.3624(4) 0.3873(6) 0.078(4) Uani 1 1 d . . . H1SA H 0.7035 0.3697 0.3531 0.094 Uiso 1 1 calc R . . H1SB H 0.8382 0.3553 0.3771 0.094 Uiso 1 1 calc R . . H1SC H 0.7761 0.3876 0.4132 0.094 Uiso 1 1 calc R . . C2S C 0.7235(10) 0.3231(3) 0.4160(5) 0.042(3) Uani 1 1 d . . . C3S C 0.8082(10) 0.3029(4) 0.4615(5) 0.072(4) Uani 1 1 d . . . H3SA H 0.8210 0.3218 0.4950 0.087 Uiso 1 1 calc R . . H3SB H 0.8830 0.2989 0.4504 0.087 Uiso 1 1 calc R . . H3SC H 0.7785 0.2742 0.4702 0.087 Uiso 1 1 calc R . . O2S O -0.0125(9) 0.6519(4) 0.4373(5) 0.130(4) Uani 1 1 d . . . C4S C -0.1723(13) 0.7027(4) 0.4178(6) 0.101(5) Uani 1 1 d . . . H4SA H -0.2302 0.7011 0.4410 0.121 Uiso 1 1 calc R . . H4SB H -0.2120 0.7114 0.3792 0.121 Uiso 1 1 calc R . . H4SC H -0.1115 0.7244 0.4339 0.121 Uiso 1 1 calc R . . C5S C -0.1154(12) 0.6581(5) 0.4165(6) 0.068(4) Uani 1 1 d . . . C6S C -0.1923(11) 0.6226(4) 0.3926(5) 0.072(4) Uani 1 1 d . . . H6SA H -0.1456 0.5959 0.3923 0.087 Uiso 1 1 calc R . . H6SB H -0.2338 0.6301 0.3539 0.087 Uiso 1 1 calc R . . H6SC H -0.2499 0.6176 0.4155 0.087 Uiso 1 1 calc R . . O3S O 0.4248(18) 0.5510(4) 0.3378(6) 0.231(9) Uani 1 1 d . . . C7S C 0.5024(14) 0.5082(5) 0.2769(8) 0.136(7) Uani 1 1 d . . . H7SA H 0.5347 0.5159 0.2445 0.163 Uiso 1 1 calc R . . H7SB H 0.4474 0.4835 0.2667 0.163 Uiso 1 1 calc R . . H7SC H 0.5670 0.4997 0.3089 0.163 Uiso 1 1 calc R . . C8S C 0.4390(15) 0.5467(4) 0.2930(8) 0.093(6) Uani 1 1 d . . . C9S C 0.3850(13) 0.5770(5) 0.2469(7) 0.126(7) Uani 1 1 d . . . H9SA H 0.3134 0.5636 0.2235 0.152 Uiso 1 1 calc R . . H9SB H 0.4411 0.5829 0.2235 0.152 Uiso 1 1 calc R . . H9SC H 0.3644 0.6046 0.2629 0.152 Uiso 1 1 calc R . . O4S O 0.1878(15) 0.4797(6) 0.2207(8) 0.142(7) Uani 0.75 1 d P . . C10S C 0.022(2) 0.4347(6) 0.1664(8) 0.113(8) Uani 0.75 1 d P . . H10A H 0.0754 0.4093 0.1741 0.135 Uiso 0.75 1 calc PR . . H10B H -0.0131 0.4366 0.1257 0.135 Uiso 0.75 1 calc PR . . H10C H -0.0407 0.4312 0.1866 0.135 Uiso 0.75 1 calc PR . . C11S C 0.092(2) 0.4769(8) 0.1863(11) 0.110(9) Uani 0.75 1 d P . . C12S C 0.032(2) 0.5169(7) 0.1661(10) 0.155(10) Uani 0.75 1 d P . . H12A H -0.0193 0.5255 0.1908 0.186 Uiso 0.75 1 calc PR . . H12B H -0.0154 0.5126 0.1275 0.186 Uiso 0.75 1 calc PR . . H12C H 0.0906 0.5401 0.1662 0.186 Uiso 0.75 1 calc PR . . 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 Ru 0.0333(4) 0.0190(4) 0.0322(5) -0.0061(4) 0.0083(3) -0.0022(4) O1 0.073(6) 0.044(5) 0.073(6) -0.031(4) 0.013(5) -0.023(4) O2 0.036(4) 0.034(4) 0.058(5) 0.002(3) 0.021(4) -0.002(3) O3 0.053(5) 0.030(4) 0.068(6) 0.011(4) 0.028(4) 0.007(3) O4 0.045(4) 0.031(5) 0.069(6) 0.009(4) -0.001(4) 0.002(3) O5 0.047(5) 0.029(4) 0.059(5) 0.005(4) 0.014(4) 0.006(3) N1 0.044(5) 0.023(5) 0.019(5) -0.001(3) 0.002(4) -0.012(4) N2 0.030(5) 0.025(5) 0.024(5) -0.005(4) 0.007(4) -0.005(4) N3 0.039(5) 0.016(4) 0.019(5) -0.004(4) 0.001(4) -0.010(4) N4 0.041(5) 0.021(5) 0.019(5) -0.007(3) 0.010(4) -0.006(4) N5 0.028(5) 0.014(4) 0.034(5) -0.003(3) 0.012(4) 0.002(3) N6 0.040(5) 0.017(5) 0.030(5) -0.006(4) 0.008(4) -0.002(4) C1 0.015(5) 0.040(7) 0.046(7) -0.011(5) 0.003(5) 0.004(5) C2 0.045(6) 0.024(6) 0.036(7) -0.014(5) 0.001(6) -0.005(5) C10 0.041(6) 0.023(6) 0.021(6) -0.002(4) 0.012(5) -0.007(4) C11 0.031(6) 0.030(6) 0.027(6) -0.007(5) 0.007(5) -0.009(4) C12 0.054(7) 0.033(6) 0.015(6) -0.007(5) 0.012(5) -0.007(5) C13 0.036(6) 0.018(6) 0.043(7) -0.010(5) 0.012(5) -0.001(4) C14 0.024(5) 0.018(6) 0.041(7) -0.015(4) 0.006(5) -0.006(4) C15 0.030(6) 0.027(6) 0.029(7) -0.011(5) -0.004(5) 0.004(4) C16 0.027(6) 0.037(6) 0.028(7) -0.007(5) 0.012(5) -0.006(5) C17 0.042(7) 0.053(8) 0.045(8) 0.008(6) 0.009(6) 0.015(5) C18 0.045(7) 0.047(7) 0.043(8) 0.021(6) 0.004(6) 0.012(5) C19 0.040(6) 0.031(6) 0.018(6) -0.004(5) -0.003(5) 0.000(5) C20 0.046(7) 0.030(6) 0.031(7) -0.022(5) 0.017(5) -0.013(5) C21 0.035(6) 0.024(5) 0.028(6) -0.012(5) 0.002(5) -0.005(5) C22 0.038(6) 0.036(7) 0.026(6) -0.008(5) 0.014(5) -0.015(5) C23 0.037(6) 0.031(6) 0.034(7) -0.008(5) 0.019(5) -0.008(5) C24 0.030(6) 0.020(6) 0.043(7) -0.007(5) 0.010(5) 0.003(4) C25 0.028(6) 0.021(6) 0.043(7) -0.015(5) 0.015(5) -0.007(4) C26 0.022(6) 0.037(6) 0.029(7) -0.012(5) 0.000(5) -0.005(5) C27 0.031(6) 0.027(6) 0.055(8) 0.005(5) 0.010(6) 0.007(5) C28 0.040(7) 0.033(7) 0.054(8) 0.019(5) 0.012(6) 0.004(5) C29 0.036(6) 0.034(6) 0.029(7) -0.009(5) 0.011(5) -0.006(5) C31 0.045(7) 0.033(7) 0.034(7) -0.003(5) 0.016(5) 0.001(5) C32 0.057(7) 0.031(6) 0.046(8) -0.001(6) 0.019(6) -0.009(5) C33 0.062(8) 0.063(9) 0.041(8) -0.006(6) 0.017(6) -0.012(6) C34 0.059(8) 0.062(9) 0.035(8) 0.015(7) 0.013(6) -0.010(6) C35 0.091(10) 0.038(7) 0.049(9) 0.004(6) 0.022(7) -0.001(6) C36 0.075(8) 0.046(8) 0.038(8) -0.009(6) 0.022(6) -0.011(6) C37 0.115(11) 0.065(9) 0.061(10) 0.019(7) 0.030(8) -0.021(8) C41 0.032(6) 0.040(7) 0.023(6) -0.005(5) 0.006(5) -0.006(5) C42 0.043(7) 0.027(7) 0.073(9) -0.017(6) 0.000(6) -0.005(5) C43 0.053(8) 0.031(7) 0.067(9) -0.020(6) -0.003(7) 0.003(6) C44 0.038(7) 0.045(7) 0.029(7) -0.005(5) 0.010(5) 0.011(5) C45 0.031(6) 0.039(7) 0.068(9) -0.002(6) 0.014(6) -0.003(5) C46 0.039(7) 0.032(6) 0.052(8) -0.009(5) 0.008(6) 0.000(5) C47 0.056(8) 0.058(8) 0.065(9) 0.006(6) 0.018(7) 0.012(6) C51 0.036(6) 0.035(7) 0.025(7) 0.006(5) 0.012(5) -0.004(5) C52 0.090(9) 0.046(8) 0.046(8) -0.007(6) 0.025(7) -0.014(7) C53 0.093(10) 0.039(7) 0.047(9) 0.008(6) 0.017(7) -0.021(6) C54 0.047(7) 0.073(10) 0.054(9) 0.009(7) 0.019(7) 0.000(6) C55 0.084(9) 0.057(9) 0.047(9) -0.009(7) 0.011(7) -0.011(7) C56 0.078(8) 0.040(7) 0.027(7) 0.003(6) 0.015(6) -0.011(6) C57 0.093(10) 0.091(11) 0.064(10) 0.027(8) 0.032(8) -0.008(8) C61 0.042(6) 0.026(6) 0.029(6) -0.010(4) 0.014(5) 0.001(5) C62 0.031(6) 0.028(6) 0.082(9) -0.007(6) 0.020(6) -0.006(5) C63 0.037(7) 0.035(7) 0.081(10) -0.020(6) 0.014(6) -0.003(5) C64 0.042(7) 0.046(8) 0.048(8) -0.008(6) 0.015(6) 0.013(6) C65 0.040(7) 0.038(7) 0.080(10) -0.002(6) 0.020(7) 0.011(6) C66 0.041(7) 0.022(6) 0.071(9) -0.010(5) 0.013(6) -0.004(5) C67 0.051(8) 0.060(9) 0.086(10) -0.005(7) 0.009(7) 0.013(6) C71 0.024(5) 0.030(6) 0.048(7) -0.013(5) 0.009(5) 0.002(4) C72 0.037(6) 0.029(6) 0.039(7) -0.003(5) -0.001(5) 0.006(5) C73 0.039(6) 0.023(6) 0.026(6) -0.008(4) 0.015(5) 0.003(4) C74 0.034(6) 0.017(6) 0.041(7) -0.001(5) 0.003(5) 0.001(4) C75 0.039(7) 0.020(6) 0.042(7) -0.016(5) 0.017(5) 0.005(5) C76 0.050(7) 0.016(6) 0.032(7) 0.000(4) 0.001(5) 0.007(5) C77 0.041(6) 0.034(6) 0.035(7) -0.012(5) -0.007(5) 0.001(5) C78 0.037(6) 0.016(5) 0.019(6) -0.005(4) 0.004(5) -0.002(4) C79 0.049(7) 0.020(6) 0.046(7) -0.019(5) 0.001(6) 0.006(5) C80 0.034(6) 0.026(6) 0.067(8) -0.008(5) 0.001(6) 0.011(5) C81 0.055(8) 0.026(6) 0.041(7) -0.012(5) 0.021(6) -0.013(5) C82 0.042(7) 0.035(7) 0.041(8) 0.004(5) 0.021(6) 0.001(5) C83 0.072(9) 0.045(8) 0.063(9) -0.001(6) 0.035(7) -0.004(6) C84 0.065(9) 0.040(8) 0.069(9) -0.010(6) 0.025(7) -0.017(7) C85 0.062(8) 0.051(9) 0.062(9) -0.010(7) 0.020(7) -0.010(7) C86 0.066(8) 0.036(7) 0.044(8) 0.001(6) 0.022(6) -0.008(6) C87 0.037(6) 0.036(7) 0.076(9) 0.017(6) 0.021(6) 0.000(5) C88 0.045(7) 0.045(8) 0.048(8) 0.003(6) 0.020(6) 0.009(5) C89 0.032(6) 0.039(7) 0.059(8) -0.002(6) -0.001(6) 0.008(5) C90 0.052(7) 0.027(6) 0.059(8) 0.002(6) 0.001(6) 0.013(5) C91 0.035(6) 0.048(8) 0.070(9) 0.031(7) 0.001(6) 0.010(6) C92 0.043(7) 0.040(7) 0.077(9) 0.017(6) 0.029(7) 0.019(6) P 0.049(2) 0.0305(18) 0.064(3) 0.0035(16) 0.0121(17) -0.0030(14) F1 0.055(5) 0.087(6) 0.165(8) 0.013(5) 0.031(5) 0.008(4) F2 0.044(4) 0.049(4) 0.144(7) -0.001(4) 0.011(4) -0.002(3) F3 0.086(5) 0.045(4) 0.138(7) 0.030(4) 0.033(5) -0.015(4) F4 0.111(5) 0.023(4) 0.089(5) 0.008(3) 0.035(4) -0.003(3) F5 0.093(5) 0.051(4) 0.065(5) -0.006(3) 0.004(4) -0.003(4) F6 0.151(7) 0.065(5) 0.072(6) -0.001(4) 0.020(5) -0.004(5) O1S 0.050(5) 0.045(5) 0.092(7) -0.005(4) 0.024(5) 0.001(4) C1S 0.094(10) 0.042(8) 0.114(12) 0.001(7) 0.054(9) -0.014(7) C2S 0.044(7) 0.039(7) 0.047(8) -0.007(6) 0.015(6) 0.002(6) C3S 0.057(8) 0.099(11) 0.058(9) -0.001(8) 0.010(7) 0.015(7) O2S 0.058(7) 0.175(12) 0.148(11) -0.007(8) 0.009(7) 0.008(7) C4S 0.145(14) 0.047(10) 0.124(14) -0.002(8) 0.058(11) -0.041(9) C5S 0.053(9) 0.071(11) 0.091(12) -0.008(8) 0.037(8) -0.016(8) C6S 0.095(10) 0.061(9) 0.067(10) 0.008(7) 0.033(8) 0.028(8) O3S 0.52(3) 0.061(8) 0.182(15) -0.010(8) 0.226(18) -0.053(12) C7S 0.142(15) 0.066(12) 0.22(2) 0.018(12) 0.086(15) 0.029(10) C8S 0.153(14) 0.039(9) 0.128(16) -0.018(9) 0.117(13) -0.024(9) C9S 0.111(13) 0.062(11) 0.186(18) 0.053(12) -0.005(12) 0.000(9) O4S 0.117(14) 0.155(16) 0.143(16) 0.006(12) 0.008(12) 0.038(12) C10S 0.21(2) 0.059(15) 0.078(16) 0.003(11) 0.047(16) 0.028(15) C11S 0.11(2) 0.10(2) 0.13(2) 0.040(17) 0.051(17) 0.075(17) C12S 0.19(3) 0.12(2) 0.16(2) -0.032(18) 0.06(2) 0.05(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 1.865(10) . ? Ru N4 2.045(7) . ? Ru N3 2.048(7) . ? Ru N1 2.057(7) . ? Ru N2 2.057(7) . ? Ru N5 2.194(7) . ? O1 C1 1.111(10) . ? O2 C81 1.413(10) . ? O2 C87 1.458(10) . ? O3 C89 1.428(10) . ? O3 C88 1.444(11) . ? O4 C90 1.388(11) . ? O4 C91 1.454(11) . ? O5 C82 1.366(11) 3_666 ? O5 C92 1.434(10) . ? N1 C11 1.365(11) . ? N1 C14 1.394(10) . ? N2 C16 1.368(10) . ? N2 C19 1.383(11) . ? N3 C21 1.362(11) . ? N3 C24 1.385(10) . ? N4 C26 1.387(10) . ? N4 C29 1.389(11) . ? N5 C75 1.322(10) . ? N5 C71 1.345(10) . ? N6 C76 1.342(11) . ? N6 C80 1.368(10) . ? N6 C2 1.494(10) . ? C2 C2 1.476(17) 3_666 ? C10 C29 1.412(12) . ? C10 C11 1.428(12) . ? C10 C31 1.472(12) . ? C11 C12 1.452(12) . ? C12 C13 1.344(12) . ? C13 C14 1.422(12) . ? C14 C15 1.421(12) . ? C15 C16 1.401(12) . ? C15 C41 1.493(12) . ? C16 C17 1.419(13) . ? C17 C18 1.341(12) . ? C18 C19 1.446(12) . ? C19 C20 1.426(12) . ? C20 C21 1.416(12) . ? C20 C51 1.483(12) . ? C21 C22 1.408(11) . ? C22 C23 1.333(12) . ? C23 C24 1.408(12) . ? C24 C25 1.410(13) . ? C25 C26 1.382(12) . ? C25 C61 1.507(12) . ? C26 C27 1.434(13) . ? C27 C28 1.345(12) . ? C28 C29 1.426(12) . ? C31 C32 1.398(13) . ? C31 C36 1.415(13) . ? C32 C33 1.375(13) . ? C33 C34 1.392(14) . ? C34 C35 1.347(14) . ? C34 C37 1.496(13) . ? C35 C36 1.381(14) . ? C41 C46 1.364(12) . ? C41 C42 1.403(12) . ? C42 C43 1.386(13) . ? C43 C44 1.369(13) . ? C44 C45 1.398(13) . ? C44 C47 1.507(12) . ? C45 C46 1.384(12) . ? C51 C56 1.359(13) . ? C51 C52 1.395(13) . ? C52 C53 1.390(14) . ? C53 C54 1.363(15) . ? C54 C55 1.383(14) . ? C54 C57 1.514(14) . ? C55 C56 1.367(14) . ? C61 C62 1.365(12) . ? C61 C66 1.413(11) . ? C62 C63 1.379(12) . ? C63 C64 1.382(13) . ? C64 C65 1.379(13) . ? C64 C67 1.528(13) . ? C65 C66 1.381(12) . ? C71 C72 1.353(12) . ? C72 C73 1.389(12) . ? C73 C74 1.381(11) . ? C73 C78 1.468(11) . ? C74 C75 1.393(11) . ? C76 C77 1.358(12) . ? C77 C78 1.398(11) . ? C78 C79 1.383(12) . ? C79 C80 1.384(12) . ? C81 C82 1.358(13) . ? C81 C86 1.364(13) . ? C82 O5 1.366(11) 3_666 ? C82 C83 1.385(13) . ? C83 C84 1.385(14) . ? C84 C85 1.360(14) . ? C85 C86 1.370(13) . ? C87 C88 1.509(13) . ? C89 C90 1.491(13) . ? C91 C92 1.491(14) . ? P F2 1.563(6) . ? P F6 1.579(7) . ? P F4 1.584(6) . ? P F5 1.586(7) . ? P F1 1.589(7) . ? P F3 1.595(6) . ? O1S C2S 1.198(11) . ? C1S C2S 1.514(14) . ? C2S C3S 1.433(14) . ? O2S C5S 1.200(14) . ? C4S C5S 1.511(17) . ? C5S C6S 1.434(15) . ? O3S C8S 1.150(14) . ? C7S C8S 1.485(17) . ? C8S C9S 1.47(2) . ? O4S C11S 1.23(3) . ? C10S C11S 1.53(3) . ? C11S C12S 1.43(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 C1 Ru N4 90.3(4) . . ? C1 Ru N3 91.2(3) . . ? N4 Ru N3 89.8(3) . . ? C1 Ru N1 92.6(3) . . ? N4 Ru N1 90.2(3) . . ? N3 Ru N1 176.2(3) . . ? C1 Ru N2 93.3(4) . . ? N4 Ru N2 176.5(3) . . ? N3 Ru N2 90.2(3) . . ? N1 Ru N2 89.5(3) . . ? C1 Ru N5 177.9(3) . . ? N4 Ru N5 88.1(3) . . ? N3 Ru N5 87.4(3) . . ? N1 Ru N5 88.7(3) . . ? N2 Ru N5 88.4(3) . . ? C81 O2 C87 116.8(7) . . ? C89 O3 C88 112.2(7) . . ? C90 O4 C91 109.4(8) . . ? C82 O5 C92 118.4(8) 3_666 . ? C11 N1 C14 106.3(7) . . ? C11 N1 Ru 126.7(6) . . ? C14 N1 Ru 126.9(6) . . ? C16 N2 C19 106.5(8) . . ? C16 N2 Ru 128.1(6) . . ? C19 N2 Ru 125.3(6) . . ? C21 N3 C24 105.0(7) . . ? C21 N3 Ru 127.9(6) . . ? C24 N3 Ru 127.0(6) . . ? C26 N4 C29 105.8(8) . . ? C26 N4 Ru 127.5(6) . . ? C29 N4 Ru 126.6(6) . . ? C75 N5 C71 117.5(8) . . ? C75 N5 Ru 122.1(6) . . ? C71 N5 Ru 120.5(6) . . ? C76 N6 C80 120.6(8) . . ? C76 N6 C2 120.0(8) . . ? C80 N6 C2 119.4(8) . . ? O1 C1 Ru 176.4(9) . . ? C2 C2 N6 109.1(9) 3_666 . ? C29 C10 C11 124.7(8) . . ? C29 C10 C31 117.7(9) . . ? C11 C10 C31 117.4(8) . . ? N1 C11 C10 125.9(8) . . ? N1 C11 C12 109.5(8) . . ? C10 C11 C12 124.7(9) . . ? C13 C12 C11 106.8(8) . . ? C12 C13 C14 108.2(8) . . ? N1 C14 C15 124.0(8) . . ? N1 C14 C13 109.2(8) . . ? C15 C14 C13 126.8(9) . . ? C16 C15 C14 127.2(9) . . ? C16 C15 C41 117.7(8) . . ? C14 C15 C41 115.0(9) . . ? N2 C16 C15 124.1(9) . . ? N2 C16 C17 111.1(9) . . ? C15 C16 C17 124.8(9) . . ? C18 C17 C16 106.0(9) . . ? C17 C18 C19 109.0(9) . . ? N2 C19 C20 126.9(9) . . ? N2 C19 C18 107.4(8) . . ? C20 C19 C18 125.7(9) . . ? C21 C20 C19 124.2(9) . . ? C21 C20 C51 118.5(8) . . ? C19 C20 C51 117.3(9) . . ? N3 C21 C22 111.1(8) . . ? N3 C21 C20 125.3(8) . . ? C22 C21 C20 123.5(9) . . ? C23 C22 C21 106.2(8) . . ? C22 C23 C24 108.7(9) . . ? N3 C24 C23 108.9(8) . . ? N3 C24 C25 123.3(9) . . ? C23 C24 C25 127.7(9) . . ? C26 C25 C24 128.7(9) . . ? C26 C25 C61 115.3(9) . . ? C24 C25 C61 116.0(8) . . ? C25 C26 N4 123.4(9) . . ? C25 C26 C27 127.5(9) . . ? N4 C26 C27 109.2(8) . . ? C28 C27 C26 107.8(9) . . ? C27 C28 C29 107.6(9) . . ? N4 C29 C10 125.6(9) . . ? N4 C29 C28 109.6(8) . . ? C10 C29 C28 124.8(9) . . ? C32 C31 C36 115.4(9) . . ? C32 C31 C10 124.0(9) . . ? C36 C31 C10 120.6(9) . . ? C33 C32 C31 122.0(10) . . ? C32 C33 C34 121.5(11) . . ? C35 C34 C33 117.2(10) . . ? C35 C34 C37 124.5(12) . . ? C33 C34 C37 118.3(11) . . ? C34 C35 C36 123.0(11) . . ? C35 C36 C31 120.9(10) . . ? C46 C41 C42 117.8(9) . . ? C46 C41 C15 122.4(9) . . ? C42 C41 C15 119.8(8) . . ? C43 C42 C41 119.7(9) . . ? C44 C43 C42 122.7(10) . . ? C43 C44 C45 117.0(9) . . ? C43 C44 C47 122.8(10) . . ? C45 C44 C47 120.1(9) . . ? C46 C45 C44 120.6(9) . . ? C41 C46 C45 122.0(10) . . ? C56 C51 C52 116.8(9) . . ? C56 C51 C20 123.5(9) . . ? C52 C51 C20 119.7(9) . . ? C53 C52 C51 120.5(10) . . ? C54 C53 C52 122.6(11) . . ? C53 C54 C55 115.4(11) . . ? C53 C54 C57 123.2(12) . . ? C55 C54 C57 121.4(12) . . ? C56 C55 C54 122.9(11) . . ? C51 C56 C55 121.7(11) . . ? C62 C61 C66 116.3(9) . . ? C62 C61 C25 122.7(8) . . ? C66 C61 C25 120.9(8) . . ? C61 C62 C63 123.0(10) . . ? C62 C63 C64 119.7(10) . . ? C65 C64 C63 119.4(9) . . ? C65 C64 C67 120.2(10) . . ? C63 C64 C67 120.4(10) . . ? C64 C65 C66 119.9(10) . . ? C65 C66 C61 121.5(9) . . ? N5 C71 C72 122.0(9) . . ? C71 C72 C73 122.3(9) . . ? C74 C73 C72 115.0(8) . . ? C74 C73 C78 122.6(9) . . ? C72 C73 C78 122.5(8) . . ? C73 C74 C75 120.3(9) . . ? N5 C75 C74 122.9(8) . . ? N6 C76 C77 121.2(9) . . ? C76 C77 C78 121.1(9) . . ? C79 C78 C77 116.2(8) . . ? C79 C78 C73 122.5(8) . . ? C77 C78 C73 121.2(8) . . ? C78 C79 C80 122.2(9) . . ? N6 C80 C79 118.5(9) . . ? C82 C81 C86 122.2(10) . . ? C82 C81 O2 115.2(9) . . ? C86 C81 O2 122.5(10) . . ? C81 C82 O5 117.3(9) . 3_666 ? C81 C82 C83 117.8(10) . . ? O5 C82 C83 124.9(10) 3_666 . ? C82 C83 C84 120.8(11) . . ? C85 C84 C83 119.4(11) . . ? C84 C85 C86 120.3(12) . . ? C81 C86 C85 119.5(11) . . ? O2 C87 C88 108.7(8) . . ? O3 C88 C87 112.2(8) . . ? O3 C89 C90 109.9(8) . . ? O4 C90 C89 110.2(9) . . ? O4 C91 C92 106.1(9) . . ? O5 C92 C91 110.6(8) . . ? F2 P F6 90.7(4) . . ? F2 P F4 90.6(4) . . ? F6 P F4 90.0(4) . . ? F2 P F5 88.9(4) . . ? F6 P F5 179.4(5) . . ? F4 P F5 89.6(4) . . ? F2 P F1 179.4(5) . . ? F6 P F1 89.9(5) . . ? F4 P F1 89.4(4) . . ? F5 P F1 90.5(4) . . ? F2 P F3 89.5(4) . . ? F6 P F3 90.4(4) . . ? F4 P F3 179.6(5) . . ? F5 P F3 90.0(4) . . ? F1 P F3 90.4(4) . . ? O1S C2S C3S 121.3(11) . . ? O1S C2S C1S 121.2(11) . . ? C3S C2S C1S 117.5(11) . . ? O2S C5S C6S 121.1(14) . . ? O2S C5S C4S 122.2(14) . . ? C6S C5S C4S 116.6(12) . . ? O3S C8S C9S 121.3(17) . . ? O3S C8S C7S 122.2(18) . . ? C9S C8S C7S 116.2(15) . . ? O4S C11S C12S 118(3) . . ? O4S C11S C10S 127(2) . . ? C12S C11S C10S 115(2) . . ? 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 C1 Ru N1 C11 86.2(7) . . . . ? N4 Ru N1 C11 -4.0(7) . . . . ? N3 Ru N1 C11 -95(5) . . . . ? N2 Ru N1 C11 179.5(7) . . . . ? N5 Ru N1 C11 -92.1(7) . . . . ? C1 Ru N1 C14 -89.1(7) . . . . ? N4 Ru N1 C14 -179.3(7) . . . . ? N3 Ru N1 C14 90(5) . . . . ? N2 Ru N1 C14 4.2(7) . . . . ? N5 Ru N1 C14 92.6(7) . . . . ? C1 Ru N2 C16 87.1(8) . . . . ? N4 Ru N2 C16 -91(5) . . . . ? N3 Ru N2 C16 178.3(7) . . . . ? N1 Ru N2 C16 -5.5(7) . . . . ? N5 Ru N2 C16 -94.2(7) . . . . ? C1 Ru N2 C19 -88.5(7) . . . . ? N4 Ru N2 C19 93(5) . . . . ? N3 Ru N2 C19 2.7(7) . . . . ? N1 Ru N2 C19 178.9(7) . . . . ? N5 Ru N2 C19 90.1(7) . . . . ? C1 Ru N3 C21 91.3(8) . . . . ? N4 Ru N3 C21 -178.5(7) . . . . ? N1 Ru N3 C21 -87(5) . . . . ? N2 Ru N3 C21 -2.0(7) . . . . ? N5 Ru N3 C21 -90.4(7) . . . . ? C1 Ru N3 C24 -85.6(7) . . . . ? N4 Ru N3 C24 4.6(7) . . . . ? N1 Ru N3 C24 96(5) . . . . ? N2 Ru N3 C24 -178.9(7) . . . . ? N5 Ru N3 C24 92.7(7) . . . . ? C1 Ru N4 C26 90.4(7) . . . . ? N3 Ru N4 C26 -0.8(7) . . . . ? N1 Ru N4 C26 -177.0(7) . . . . ? N2 Ru N4 C26 -91(5) . . . . ? N5 Ru N4 C26 -88.3(7) . . . . ? C1 Ru N4 C29 -91.3(7) . . . . ? N3 Ru N4 C29 177.5(7) . . . . ? N1 Ru N4 C29 1.3(7) . . . . ? N2 Ru N4 C29 87(5) . . . . ? N5 Ru N4 C29 90.1(7) . . . . ? C1 Ru N5 C75 0(10) . . . . ? N4 Ru N5 C75 39.5(7) . . . . ? N3 Ru N5 C75 -50.4(7) . . . . ? N1 Ru N5 C75 129.8(7) . . . . ? N2 Ru N5 C75 -140.7(7) . . . . ? C1 Ru N5 C71 -179(100) . . . . ? N4 Ru N5 C71 -139.5(7) . . . . ? N3 Ru N5 C71 130.5(7) . . . . ? N1 Ru N5 C71 -49.3(7) . . . . ? N2 Ru N5 C71 40.3(7) . . . . ? N4 Ru C1 O1 -26(16) . . . . ? N3 Ru C1 O1 63(16) . . . . ? N1 Ru C1 O1 -117(16) . . . . ? N2 Ru C1 O1 154(16) . . . . ? N5 Ru C1 O1 13(24) . . . . ? C76 N6 C2 C2 107.8(11) . . . 3_666 ? C80 N6 C2 C2 -70.4(13) . . . 3_666 ? C14 N1 C11 C10 -180.0(8) . . . . ? Ru N1 C11 C10 3.9(12) . . . . ? C14 N1 C11 C12 0.1(9) . . . . ? Ru N1 C11 C12 -176.0(5) . . . . ? C29 C10 C11 N1 0.2(14) . . . . ? C31 C10 C11 N1 -175.8(8) . . . . ? C29 C10 C11 C12 -179.8(8) . . . . ? C31 C10 C11 C12 4.2(13) . . . . ? N1 C11 C12 C13 -1.6(10) . . . . ? C10 C11 C12 C13 178.5(8) . . . . ? C11 C12 C13 C14 2.4(10) . . . . ? C11 N1 C14 C15 -178.9(8) . . . . ? Ru N1 C14 C15 -2.8(12) . . . . ? C11 N1 C14 C13 1.4(9) . . . . ? Ru N1 C14 C13 177.5(5) . . . . ? C12 C13 C14 N1 -2.4(10) . . . . ? C12 C13 C14 C15 177.9(9) . . . . ? N1 C14 C15 C16 0.8(14) . . . . ? C13 C14 C15 C16 -179.5(8) . . . . ? N1 C14 C15 C41 -178.1(7) . . . . ? C13 C14 C15 C41 1.5(13) . . . . ? C19 N2 C16 C15 -178.3(8) . . . . ? Ru N2 C16 C15 5.4(13) . . . . ? C19 N2 C16 C17 -0.1(10) . . . . ? Ru N2 C16 C17 -176.4(6) . . . . ? C14 C15 C16 N2 -2.1(15) . . . . ? C41 C15 C16 N2 176.8(8) . . . . ? C14 C15 C16 C17 179.9(9) . . . . ? C41 C15 C16 C17 -1.2(14) . . . . ? N2 C16 C17 C18 0.6(12) . . . . ? C15 C16 C17 C18 178.8(9) . . . . ? C16 C17 C18 C19 -0.8(12) . . . . ? C16 N2 C19 C20 179.1(8) . . . . ? Ru N2 C19 C20 -4.5(12) . . . . ? C16 N2 C19 C18 -0.4(10) . . . . ? Ru N2 C19 C18 176.0(6) . . . . ? C17 C18 C19 N2 0.8(11) . . . . ? C17 C18 C19 C20 -178.7(9) . . . . ? N2 C19 C20 C21 4.6(14) . . . . ? C18 C19 C20 C21 -175.9(9) . . . . ? N2 C19 C20 C51 -174.5(8) . . . . ? C18 C19 C20 C51 5.0(13) . . . . ? C24 N3 C21 C22 -0.7(9) . . . . ? Ru N3 C21 C22 -178.1(5) . . . . ? C24 N3 C21 C20 -179.8(8) . . . . ? Ru N3 C21 C20 2.8(13) . . . . ? C19 C20 C21 N3 -3.7(14) . . . . ? C51 C20 C21 N3 175.4(8) . . . . ? C19 C20 C21 C22 177.3(8) . . . . ? C51 C20 C21 C22 -3.6(13) . . . . ? N3 C21 C22 C23 1.1(10) . . . . ? C20 C21 C22 C23 -179.7(9) . . . . ? C21 C22 C23 C24 -1.1(10) . . . . ? C21 N3 C24 C23 -0.1(9) . . . . ? Ru N3 C24 C23 177.4(5) . . . . ? C21 N3 C24 C25 177.5(8) . . . . ? Ru N3 C24 C25 -5.0(12) . . . . ? C22 C23 C24 N3 0.8(10) . . . . ? C22 C23 C24 C25 -176.7(9) . . . . ? N3 C24 C25 C26 0.1(15) . . . . ? C23 C24 C25 C26 177.2(9) . . . . ? N3 C24 C25 C61 -178.2(8) . . . . ? C23 C24 C25 C61 -1.1(14) . . . . ? C24 C25 C26 N4 4.1(15) . . . . ? C61 C25 C26 N4 -177.6(8) . . . . ? C24 C25 C26 C27 -177.3(9) . . . . ? C61 C25 C26 C27 1.0(13) . . . . ? C29 N4 C26 C25 178.5(8) . . . . ? Ru N4 C26 C25 -2.9(12) . . . . ? C29 N4 C26 C27 -0.3(9) . . . . ? Ru N4 C26 C27 178.3(6) . . . . ? C25 C26 C27 C28 -178.2(9) . . . . ? N4 C26 C27 C28 0.5(11) . . . . ? C26 C27 C28 C29 -0.5(11) . . . . ? C26 N4 C29 C10 -179.6(8) . . . . ? Ru N4 C29 C10 1.8(12) . . . . ? C26 N4 C29 C28 0.0(10) . . . . ? Ru N4 C29 C28 -178.6(6) . . . . ? C11 C10 C29 N4 -3.3(14) . . . . ? C31 C10 C29 N4 172.7(8) . . . . ? C11 C10 C29 C28 177.1(9) . . . . ? C31 C10 C29 C28 -6.8(14) . . . . ? C27 C28 C29 N4 0.3(11) . . . . ? C27 C28 C29 C10 179.9(9) . . . . ? C29 C10 C31 C32 114.8(11) . . . . ? C11 C10 C31 C32 -68.8(13) . . . . ? C29 C10 C31 C36 -64.9(12) . . . . ? C11 C10 C31 C36 111.5(10) . . . . ? C36 C31 C32 C33 -2.1(15) . . . . ? C10 C31 C32 C33 178.2(10) . . . . ? C31 C32 C33 C34 0.2(16) . . . . ? C32 C33 C34 C35 1.8(16) . . . . ? C32 C33 C34 C37 -179.3(11) . . . . ? C33 C34 C35 C36 -1.9(18) . . . . ? C37 C34 C35 C36 179.4(11) . . . . ? C34 C35 C36 C31 -0.1(18) . . . . ? C32 C31 C36 C35 2.1(15) . . . . ? C10 C31 C36 C35 -178.2(10) . . . . ? C16 C15 C41 C46 95.6(11) . . . . ? C14 C15 C41 C46 -85.3(11) . . . . ? C16 C15 C41 C42 -83.4(11) . . . . ? C14 C15 C41 C42 95.6(11) . . . . ? C46 C41 C42 C43 0.1(16) . . . . ? C15 C41 C42 C43 179.2(10) . . . . ? C41 C42 C43 C44 -0.1(18) . . . . ? C42 C43 C44 C45 1.8(17) . . . . ? C42 C43 C44 C47 -176.1(10) . . . . ? C43 C44 C45 C46 -3.4(15) . . . . ? C47 C44 C45 C46 174.5(10) . . . . ? C42 C41 C46 C45 -1.8(15) . . . . ? C15 C41 C46 C45 179.2(10) . . . . ? C44 C45 C46 C41 3.5(16) . . . . ? C21 C20 C51 C56 71.8(13) . . . . ? C19 C20 C51 C56 -109.0(11) . . . . ? C21 C20 C51 C52 -108.7(11) . . . . ? C19 C20 C51 C52 70.5(12) . . . . ? C56 C51 C52 C53 -2.8(16) . . . . ? C20 C51 C52 C53 177.7(10) . . . . ? C51 C52 C53 C54 0.8(19) . . . . ? C52 C53 C54 C55 1.7(18) . . . . ? C52 C53 C54 C57 -178.3(11) . . . . ? C53 C54 C55 C56 -2.4(18) . . . . ? C57 C54 C55 C56 177.6(11) . . . . ? C52 C51 C56 C55 2.2(16) . . . . ? C20 C51 C56 C55 -178.3(10) . . . . ? C54 C55 C56 C51 0.5(18) . . . . ? C26 C25 C61 C62 -107.3(11) . . . . ? C24 C25 C61 C62 71.1(12) . . . . ? C26 C25 C61 C66 75.4(11) . . . . ? C24 C25 C61 C66 -106.1(10) . . . . ? C66 C61 C62 C63 -4.0(16) . . . . ? C25 C61 C62 C63 178.6(10) . . . . ? C61 C62 C63 C64 1.6(17) . . . . ? C62 C63 C64 C65 0.9(16) . . . . ? C62 C63 C64 C67 -177.3(10) . . . . ? C63 C64 C65 C66 -0.8(16) . . . . ? C67 C64 C65 C66 177.5(10) . . . . ? C64 C65 C66 C61 -1.8(16) . . . . ? C62 C61 C66 C65 4.1(15) . . . . ? C25 C61 C66 C65 -178.5(10) . . . . ? C75 N5 C71 C72 -2.2(14) . . . . ? Ru N5 C71 C72 176.9(7) . . . . ? N5 C71 C72 C73 0.1(15) . . . . ? C71 C72 C73 C74 2.0(14) . . . . ? C71 C72 C73 C78 -177.5(9) . . . . ? C72 C73 C74 C75 -1.9(13) . . . . ? C78 C73 C74 C75 177.6(9) . . . . ? C71 N5 C75 C74 2.2(14) . . . . ? Ru N5 C75 C74 -176.9(7) . . . . ? C73 C74 C75 N5 -0.1(15) . . . . ? C80 N6 C76 C77 1.5(14) . . . . ? C2 N6 C76 C77 -176.7(8) . . . . ? N6 C76 C77 C78 2.4(15) . . . . ? C76 C77 C78 C79 -4.6(14) . . . . ? C76 C77 C78 C73 170.5(9) . . . . ? C74 C73 C78 C79 -13.7(14) . . . . ? C72 C73 C78 C79 165.8(9) . . . . ? C74 C73 C78 C77 171.6(9) . . . . ? C72 C73 C78 C77 -9.0(14) . . . . ? C77 C78 C79 C80 3.2(15) . . . . ? C73 C78 C79 C80 -171.8(9) . . . . ? C76 N6 C80 C79 -2.9(14) . . . . ? C2 N6 C80 C79 175.2(9) . . . . ? C78 C79 C80 N6 0.5(15) . . . . ? C87 O2 C81 C82 -168.7(9) . . . . ? C87 O2 C81 C86 14.2(13) . . . . ? C86 C81 C82 O5 -179.5(9) . . . 3_666 ? O2 C81 C82 O5 3.3(13) . . . 3_666 ? C86 C81 C82 C83 -1.2(15) . . . . ? O2 C81 C82 C83 -178.3(8) . . . . ? C81 C82 C83 C84 1.3(15) . . . . ? O5 C82 C83 C84 179.6(9) 3_666 . . . ? C82 C83 C84 C85 -1.1(16) . . . . ? C83 C84 C85 C86 0.6(17) . . . . ? C82 C81 C86 C85 0.7(16) . . . . ? O2 C81 C86 C85 177.7(9) . . . . ? C84 C85 C86 C81 -0.5(16) . . . . ? C81 O2 C87 C88 170.6(8) . . . . ? C89 O3 C88 C87 99.7(10) . . . . ? O2 C87 C88 O3 77.4(10) . . . . ? C88 O3 C89 C90 -174.7(8) . . . . ? C91 O4 C90 C89 178.4(8) . . . . ? O3 C89 C90 O4 -55.0(11) . . . . ? C90 O4 C91 C92 169.5(8) . . . . ? C82 O5 C92 C91 175.9(8) 3_666 . . . ? O4 C91 C92 O5 76.8(10) . . . . ? N6 C2 C2 N6 180.000(2) . . 3_666 3_666 ? C92 O5 C82 C81 -172.1(9) . . 3_666 3_666 ? C92 O5 C82 C83 6.1(14) . . 3_666 3_666 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.418 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.166