# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1213 data_alfadef _audit_creation_method SHELXL-97 _chemical_name_systematic ? # 1. SUBMISSION DETAILS _publ_contact_author ; Toupet Loic G.M.C.M.-UMR6626 Universite de Rennes Campus de Beaulieu 35042 RENNES cedex , FRANCE ; _publ_contact_author_email 'loic.toupet@univ-rennes1.fr' _publ_contact_author_fax '(33) 2 99 28 67 17' _publ_contact_author_phone '(33) 2 99 28 60 65' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H94 F12 N10 O12 Ru' _chemical_formula_weight 1992.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 .8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.199(3) _cell_length_b 16.372(4) _cell_length_c 37.318(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9286(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 8817 _diffrn_reflns_av_R_equivalents 0.2224 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8777 _reflns_number_gt 6156 _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. In this revised version, the F atoms are refined anisotropically. We have mentionned the results of the refinement with all reflections.We have also mentionned the Flack parameter (with TWIN and BASF options) and the residual density, the values of which are slightly diferent due to new calculations. ; _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^)+(0.0663P)^2^+4.8960P] 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 0.00(4) _refine_ls_number_reflns 8777 _refine_ls_number_parameters 1244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.031 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.31540(4) 0.06778(3) 0.867310(15) 0.01761(13) Uani 1 1 d . . . F1 F 0.4533(3) -0.4220(3) 0.80709(12) 0.0484(13) Uani 1 1 d . . . F2 F 0.4306(3) -0.4107(3) 0.86347(13) 0.0438(12) Uani 1 1 d . . . F3 F 0.3493(4) -0.4895(3) 0.83153(14) 0.0509(15) Uani 1 1 d . . . F4 F 0.7861(3) -0.0738(4) 0.80858(14) 0.0592(15) Uani 1 1 d . . . F5 F 0.8486(4) -0.1446(4) 0.85034(16) 0.0626(17) Uani 1 1 d . . . F6 F 0.8263(4) -0.0156(4) 0.85707(17) 0.080(2) Uani 1 1 d . . . F7 F 0.4553(3) 0.3411(3) 1.00697(14) 0.0551(15) Uani 1 1 d . . . F8 F 0.3129(4) 0.3377(3) 1.00567(12) 0.0434(12) Uani 1 1 d . . . F9 F 0.3888(4) 0.2627(3) 0.96934(15) 0.0532(15) Uani 1 1 d . . . F10 F 0.0618(4) 0.5050(3) 0.83480(12) 0.0443(13) Uani 1 1 d . . . F11 F 0.0231(4) 0.4939(3) 0.88991(12) 0.0480(14) Uani 1 1 d . . . F12 F -0.0751(4) 0.4891(3) 0.84810(13) 0.0437(13) Uani 1 1 d . . . O1 O 0.2467(4) -0.3895(3) 0.87550(14) 0.0354(14) Uani 1 1 d . . . O2 O 0.3804(4) -0.2741(3) 0.81832(14) 0.0310(13) Uani 1 1 d . . . O3 O 0.7691(5) -0.1100(5) 0.91807(19) 0.073(3) Uani 1 1 d . . . O4 O 0.6353(4) -0.0506(3) 0.84533(15) 0.0362(14) Uani 1 1 d . . . O5 O 0.5382(4) 0.3935(3) 0.94498(15) 0.0385(14) Uani 1 1 d . . . O6 O 0.3065(4) 0.3857(3) 0.93482(13) 0.0324(13) Uani 1 1 d . . . O7 O -0.0125(4) 0.3890(3) 0.79327(14) 0.0404(15) Uani 1 1 d . . . O8 O 0.0978(4) 0.3501(3) 0.87306(14) 0.0303(13) Uani 1 1 d . . . O9 O 0.0859(4) 0.1708(3) 0.88358(15) 0.0364(15) Uani 1 1 d . . . O10 O 0.0231(3) 0.0739(4) 0.91724(13) 0.0326(13) Uani 1 1 d . . . O11 O 0.2817(4) -0.1165(3) 0.79885(16) 0.0400(16) Uani 1 1 d . . . O12 O 0.2557(4) -0.0378(3) 0.75050(15) 0.0373(14) Uani 1 1 d . . . N1 N 0.3197(4) -0.0337(3) 0.89885(14) 0.0170(12) Uani 1 1 d . . . N2 N 0.4300(4) 0.1065(3) 0.88944(15) 0.0196(14) Uani 1 1 d . . . N3 N 0.3139(4) 0.1688(3) 0.83519(14) 0.0192(12) Uani 1 1 d . . . N4 N 0.2002(4) 0.0299(3) 0.84557(15) 0.0193(14) Uani 1 1 d . . . N5 N 0.2165(4) -0.2631(4) 0.85306(16) 0.0221(15) Uani 1 1 d . . . N6 N 0.6223(4) -0.0802(4) 0.91565(16) 0.0315(16) Uani 1 1 d . . . N7 N 0.4470(4) 0.3810(4) 0.89703(17) 0.0287(15) Uani 1 1 d . . . N8 N 0.0446(4) 0.2667(4) 0.81077(15) 0.0255(15) Uani 1 1 d . . . N9 N 0.2482(4) 0.1354(4) 0.90741(16) 0.0229(15) Uani 1 1 d . . . N10 N 0.3860(4) -0.0012(4) 0.82833(15) 0.0231(14) Uani 1 1 d . . . C1 C 0.2582(5) -0.0966(4) 0.89877(19) 0.0182(16) Uani 1 1 d . . . C2 C 0.2854(5) -0.1574(4) 0.9244(2) 0.0237(18) Uani 1 1 d . . . C3 C 0.3613(5) -0.1331(4) 0.93884(19) 0.0224(17) Uani 1 1 d . . . C4 C 0.3836(5) -0.0545(4) 0.92273(17) 0.0210(16) Uani 1 1 d . . . C5 C 0.4559(5) -0.0077(4) 0.93172(18) 0.0183(16) Uani 1 1 d . . . C6 C 0.4773(5) 0.0688(5) 0.91693(18) 0.0243(16) Uani 1 1 d . . . C7 C 0.5488(5) 0.1198(4) 0.9275(2) 0.0254(18) Uani 1 1 d . . . C8 C 0.5483(5) 0.1859(4) 0.90606(19) 0.0242(17) Uani 1 1 d . . . C9 C 0.4743(5) 0.1782(4) 0.88245(19) 0.0211(16) Uani 1 1 d . . . C10 C 0.4511(5) 0.2337(4) 0.85528(18) 0.0192(16) Uani 1 1 d . . . C11 C 0.3781(5) 0.2288(4) 0.83349(18) 0.0198(16) Uani 1 1 d . . . C12 C 0.3552(5) 0.2859(5) 0.8059(2) 0.0246(18) Uani 1 1 d . . . C13 C 0.2789(5) 0.2614(5) 0.7908(2) 0.0226(18) Uani 1 1 d . . . C14 C 0.2518(5) 0.1877(4) 0.8092(2) 0.0249(17) Uani 1 1 d . . . C15 C 0.1776(6) 0.1428(4) 0.80181(17) 0.0232(16) Uani 1 1 d . . . C16 C 0.1520(4) 0.0693(5) 0.81888(16) 0.0194(15) Uani 1 1 d . . . C17 C 0.0734(5) 0.0240(5) 0.8114(2) 0.0275(18) Uani 1 1 d . . . C18 C 0.0734(5) -0.0421(4) 0.83274(19) 0.0224(17) Uani 1 1 d . . . C19 C 0.1525(5) -0.0393(4) 0.85395(19) 0.0200(17) Uani 1 1 d . . . C20 C 0.1802(5) -0.0984(4) 0.87868(18) 0.0216(16) Uani 1 1 d . . . C21 C 0.1180(5) -0.1688(4) 0.88471(19) 0.0206(17) Uani 1 1 d . . . C22 C 0.0388(5) -0.1555(4) 0.9018(2) 0.0261(18) Uani 1 1 d . . . C23 C -0.0201(6) -0.2170(5) 0.9069(2) 0.034(2) Uani 1 1 d . . . C24 C -0.0010(6) -0.2951(5) 0.8942(2) 0.033(2) Uani 1 1 d . . . C25 C 0.0784(6) -0.3107(4) 0.8779(2) 0.0268(19) Uani 1 1 d . . . C26 C 0.1377(5) -0.2478(4) 0.87243(19) 0.0220(17) Uani 1 1 d . . . C27 C 0.2601(5) -0.3337(5) 0.8542(2) 0.0260(18) Uani 1 1 d . . . C28 C 0.3293(6) -0.3444(4) 0.8234(2) 0.0281(19) Uani 1 1 d . . . C29 C 0.2789(6) -0.3595(5) 0.7888(2) 0.032(2) Uani 1 1 d . . . C30 C 0.2957(5) -0.3144(4) 0.75811(19) 0.031(2) Uani 1 1 d . . . C31 C 0.2471(6) -0.3277(5) 0.7273(2) 0.041(2) Uani 1 1 d . . . C32 C 0.1810(8) -0.3857(6) 0.7273(2) 0.049(2) Uani 1 1 d . . . C33 C 0.1646(6) -0.4308(6) 0.7575(2) 0.048(2) Uani 1 1 d . . . C34 C 0.2124(6) -0.4177(5) 0.7878(2) 0.041(2) Uani 1 1 d . . . C35 C 0.4265(6) -0.2409(5) 0.8486(2) 0.039(2) Uani 1 1 d . . . C36 C 0.3896(6) -0.4162(5) 0.8315(2) 0.034(2) Uani 1 1 d . . . C37 C 0.5163(5) -0.0397(4) 0.96081(18) 0.0221(17) Uani 1 1 d . . . C38 C 0.4907(6) -0.0351(5) 0.9964(2) 0.035(2) Uani 1 1 d . . . C39 C 0.5455(6) -0.0642(6) 1.0237(2) 0.042(2) Uani 1 1 d . . . C40 C 0.6253(7) -0.0967(5) 1.0151(2) 0.045(3) Uani 1 1 d . . . C41 C 0.6526(6) -0.1010(5) 0.9803(2) 0.043(2) Uani 1 1 d . . . C42 C 0.5989(5) -0.0740(5) 0.95279(18) 0.0268(17) Uani 1 1 d . . . C43 C 0.7021(5) -0.0976(5) 0.9014(2) 0.040(2) Uani 1 1 d . . . C44 C 0.7001(5) -0.1035(5) 0.8601(2) 0.035(2) Uani 1 1 d . . . C45 C 0.6748(6) -0.1890(5) 0.8481(2) 0.034(2) Uani 1 1 d . . . C46 C 0.6823(7) -0.2558(5) 0.8713(2) 0.048(2) Uani 1 1 d . . . C47 C 0.6638(8) -0.3341(6) 0.8586(3) 0.063(3) Uani 1 1 d . . . C48 C 0.6423(8) -0.3466(6) 0.8242(3) 0.060(3) Uani 1 1 d . . . C49 C 0.6364(7) -0.2819(6) 0.8004(2) 0.044(2) Uani 1 1 d . . . C50 C 0.6538(6) -0.2032(5) 0.8124(2) 0.032(2) Uani 1 1 d . . . C51 C 0.6530(8) 0.0347(5) 0.8505(3) 0.055(3) Uani 1 1 d . . . C52 C 0.7904(6) -0.0846(6) 0.8445(3) 0.049(3) Uani 1 1 d . . . C53 C 0.5138(5) 0.3025(4) 0.8490(2) 0.0226(17) Uani 1 1 d . . . C54 C 0.5756(5) 0.2966(5) 0.8212(2) 0.0274(18) Uani 1 1 d . . . C55 C 0.6365(6) 0.3573(5) 0.8160(2) 0.031(2) Uani 1 1 d . . . C56 C 0.6387(6) 0.4238(5) 0.8380(2) 0.037(2) Uani 1 1 d . . . C57 C 0.5767(5) 0.4326(5) 0.8649(2) 0.0339(17) Uani 1 1 d . . . C58 C 0.5137(5) 0.3721(4) 0.8699(2) 0.0227(16) Uani 1 1 d . . . C59 C 0.4649(6) 0.3912(4) 0.9320(2) 0.0301(19) Uani 1 1 d . . . C60 C 0.3836(5) 0.4035(4) 0.9555(2) 0.0252(18) Uani 1 1 d . . . C61 C 0.3852(5) 0.4901(5) 0.9699(2) 0.0280(19) Uani 1 1 d . . . C62 C 0.3938(6) 0.5107(6) 1.0059(2) 0.042(2) Uani 1 1 d . . . C63 C 0.3981(7) 0.5921(6) 1.0160(2) 0.053(3) Uani 1 1 d . . . C64 C 0.3925(7) 0.6521(5) 0.9911(3) 0.052(3) Uani 1 1 d . . . C65 C 0.3811(8) 0.6328(5) 0.9553(3) 0.057(3) Uani 1 1 d . . . C66 C 0.3779(7) 0.5518(5) 0.9449(2) 0.046(2) Uani 1 1 d . . . C67 C 0.2250(5) 0.4241(6) 0.9444(2) 0.041(2) Uani 1 1 d . . . C68 C 0.3859(6) 0.3367(5) 0.9849(2) 0.037(2) Uani 1 1 d . . . C69 C 0.1186(5) 0.1704(4) 0.77174(19) 0.0223(17) Uani 1 1 d . . . C70 C 0.1305(6) 0.1378(5) 0.7373(2) 0.036(2) Uani 1 1 d . . . C71 C 0.0804(7) 0.1623(5) 0.7091(2) 0.047(3) Uani 1 1 d . . . C72 C 0.0142(7) 0.2180(5) 0.7142(2) 0.043(2) Uani 1 1 d . . . C73 C 0.0028(6) 0.2521(5) 0.7477(2) 0.038(2) Uani 1 1 d . . . C74 C 0.0549(5) 0.2303(4) 0.7760(2) 0.0283(19) Uani 1 1 d . . . C75 C 0.0154(6) 0.3425(5) 0.8162(2) 0.0269(19) Uani 1 1 d . . . C76 C 0.0186(5) 0.3718(4) 0.85589(19) 0.0239(18) Uani 1 1 d . . . C77 C -0.0564(5) 0.3359(4) 0.87816(19) 0.0231(17) Uani 1 1 d . . . C78 C -0.1337(6) 0.3107(5) 0.8628(2) 0.039(2) Uani 1 1 d . . . C79 C -0.2024(6) 0.2838(6) 0.8831(2) 0.047(2) Uani 1 1 d . . . C80 C -0.1958(7) 0.2818(6) 0.9201(2) 0.049(3) Uani 1 1 d . . . C81 C -0.1194(6) 0.3077(5) 0.9357(2) 0.041(2) Uani 1 1 d . . . C82 C -0.0494(6) 0.3335(5) 0.9155(2) 0.037(2) Uani 1 1 d . . . C83 C 0.1773(6) 0.3786(5) 0.8572(2) 0.038(2) Uani 1 1 d . . . C84 C 0.0072(6) 0.4664(5) 0.8565(2) 0.033(2) Uani 1 1 d . . . C85 C 0.1732(5) 0.0966(4) 0.92632(19) 0.0237(17) Uani 1 1 d . . . C86 C 0.0896(5) 0.1182(5) 0.9064(2) 0.0265(18) Uani 1 1 d . . . C87 C -0.0601(6) 0.0921(6) 0.9001(3) 0.050(3) Uani 1 1 d . . . C88 C 0.1666(5) 0.1187(5) 0.9660(2) 0.030(2) Uani 1 1 d . . . C89 C 0.2483(6) 0.0900(5) 0.9859(2) 0.042(2) Uani 1 1 d . . . C90 C 0.1489(6) 0.2091(5) 0.9721(2) 0.040(2) Uani 1 1 d . . . C91 C 0.3617(5) 0.0076(4) 0.79049(19) 0.0260(17) Uani 1 1 d . . . C92 C 0.2964(5) -0.0566(5) 0.7811(2) 0.0292(19) Uani 1 1 d . . . C93 C 0.1822(7) -0.0883(6) 0.7408(2) 0.052(2) Uani 1 1 d . . . C94 C 0.4404(5) 0.0083(5) 0.7646(2) 0.034(2) Uani 1 1 d . . . C95 C 0.4916(6) -0.0734(8) 0.7666(2) 0.058(3) Uani 1 1 d . . . C96 C 0.5001(7) 0.0819(7) 0.7724(2) 0.064(3) Uani 1 1 d . . . C97 C 0.3600(13) 0.1624(10) 0.5101(5) 0.127(7) Uani 1 1 d . . . C98 C 0.3783(14) 0.0912(14) 0.5263(5) 0.147(9) Uani 1 1 d . . . C99 C 0.3291(10) 0.0458(8) 0.5496(4) 0.083(4) Uani 1 1 d . . . C100 C 0.2098(12) 0.1446(8) 0.5425(4) 0.094(6) Uani 1 1 d . . . C101 C 0.1886(10) 0.0313(10) 0.5817(4) 0.105(5) Uani 1 1 d . . . C102 C 0.2432(11) 0.0695(9) 0.5593(3) 0.092(4) Uani 1 1 d . . . C103 C 0.2657(13) 0.1860(9) 0.5208(5) 0.109(6) Uani 1 1 d . . . H2 H 0.2548 -0.1999 0.9282 0.050 Uiso 1 1 d . . . H3 H 0.3934 -0.1537 0.9545 0.050 Uiso 1 1 d . . . H7 H 0.5823 0.1132 0.9453 0.050 Uiso 1 1 d . . . H8 H 0.5858 0.2339 0.9036 0.050 Uiso 1 1 d . . . H12 H 0.3818 0.3400 0.7998 0.050 Uiso 1 1 d . . . H13 H 0.2500 0.2912 0.7730 0.050 Uiso 1 1 d . . . H17 H 0.0254 0.0446 0.7969 0.050 Uiso 1 1 d . . . H18 H 0.0347 -0.0823 0.8327 0.050 Uiso 1 1 d . . . H22 H 0.0382 -0.0957 0.9116 0.050 Uiso 1 1 d . . . H23 H -0.0705 -0.1951 0.9162 0.050 Uiso 1 1 d . . . H24 H -0.0401 -0.3316 0.8976 0.050 Uiso 1 1 d . . . H25 H 0.0926 -0.3601 0.8689 0.050 Uiso 1 1 d . . . H5A H 0.2335 -0.2178 0.8341 0.050 Uiso 1 1 d . . . H30 H 0.3471 -0.2706 0.7578 0.050 Uiso 1 1 d . . . H31 H 0.2594 -0.2950 0.7044 0.050 Uiso 1 1 d . . . H32 H 0.1507 -0.3834 0.7073 0.050 Uiso 1 1 d . . . H33 H 0.1167 -0.4642 0.7555 0.050 Uiso 1 1 d . . . H34 H 0.1943 -0.4365 0.8071 0.050 Uiso 1 1 d . . . H35A H 0.4538 -0.1918 0.8462 0.050 Uiso 1 1 d . . . H35B H 0.3754 -0.2219 0.8682 0.050 Uiso 1 1 d . . . H35C H 0.4545 -0.2784 0.8626 0.050 Uiso 1 1 d . . . H38 H 0.4245 -0.0022 1.0000 0.050 Uiso 1 1 d . . . H39 H 0.5150 -0.0602 1.0470 0.050 Uiso 1 1 d . . . H40 H 0.6472 -0.1119 1.0332 0.050 Uiso 1 1 d . . . H41 H 0.6993 -0.1220 0.9744 0.050 Uiso 1 1 d . . . H6A H 0.5617 -0.0793 0.8985 0.050 Uiso 1 1 d . . . H46 H 0.6823 -0.2395 0.8959 0.050 Uiso 1 1 d . . . H47 H 0.6775 -0.3746 0.8711 0.050 Uiso 1 1 d . . . H48 H 0.6214 -0.3870 0.8137 0.050 Uiso 1 1 d . . . H49 H 0.6175 -0.2780 0.7769 0.050 Uiso 1 1 d . . . H50 H 0.6468 -0.1498 0.7970 0.050 Uiso 1 1 d . . . H51A H 0.6022 0.0768 0.8425 0.050 Uiso 1 1 d . . . H51B H 0.6484 0.0559 0.8778 0.050 Uiso 1 1 d . . . H51C H 0.7010 0.0616 0.8429 0.050 Uiso 1 1 d . . . H54 H 0.5673 0.2500 0.8074 0.050 Uiso 1 1 d . . . H55 H 0.6721 0.3541 0.7988 0.050 Uiso 1 1 d . . . H56 H 0.6738 0.4736 0.8383 0.050 Uiso 1 1 d . . . H57 H 0.5709 0.4848 0.8812 0.050 Uiso 1 1 d . . . H7A H 0.3838 0.3771 0.8910 0.050 Uiso 1 1 d . . . H62 H 0.3835 0.4758 1.0245 0.050 Uiso 1 1 d . . . H63 H 0.3929 0.6164 1.0381 0.050 Uiso 1 1 d . . . H64 H 0.3921 0.7142 0.9999 0.050 Uiso 1 1 d . . . H65 H 0.3975 0.6838 0.9377 0.050 Uiso 1 1 d . . . H66 H 0.3656 0.5431 0.9198 0.050 Uiso 1 1 d . . . H67A H 0.1808 0.4155 0.9297 0.050 Uiso 1 1 d . . . H67B H 0.2094 0.4137 0.9691 0.050 Uiso 1 1 d . . . H67C H 0.2312 0.4885 0.9456 0.050 Uiso 1 1 d . . . H70 H 0.1804 0.1072 0.7353 0.050 Uiso 1 1 d . . . H71 H 0.0927 0.1416 0.6867 0.050 Uiso 1 1 d . . . H72 H -0.0121 0.2434 0.6937 0.050 Uiso 1 1 d . . . H73 H -0.0329 0.3052 0.7512 0.050 Uiso 1 1 d . . . H8A H 0.0663 0.2436 0.8305 0.050 Uiso 1 1 d . . . H78 H -0.1417 0.3157 0.8362 0.050 Uiso 1 1 d . . . H79 H -0.2504 0.2632 0.8707 0.050 Uiso 1 1 d . . . H80 H -0.2398 0.2671 0.9304 0.050 Uiso 1 1 d . . . H81 H -0.1090 0.3012 0.9598 0.050 Uiso 1 1 d . . . H82 H 0.0043 0.3519 0.9258 0.050 Uiso 1 1 d . . . H83A H 0.2140 0.3966 0.8769 0.050 Uiso 1 1 d . . . H83B H 0.1956 0.3496 0.8419 0.050 Uiso 1 1 d . . . H83C H 0.1606 0.4373 0.8469 0.050 Uiso 1 1 d . . . H9A H 0.2254 0.1888 0.8970 0.050 Uiso 1 1 d . . . H9B H 0.2905 0.1560 0.9249 0.050 Uiso 1 1 d . . . H10A H 0.3824 -0.0488 0.8359 0.050 Uiso 1 1 d . . . H10B H 0.4444 0.0247 0.8316 0.050 Uiso 1 1 d . . . H85 H 0.1956 0.0456 0.9252 0.050 Uiso 1 1 d . . . H87A H -0.0995 0.0560 0.9063 0.050 Uiso 1 1 d . . . H87B H -0.0736 0.1463 0.9008 0.050 Uiso 1 1 d . . . H87C H -0.0479 0.0815 0.8728 0.050 Uiso 1 1 d . . . H88 H 0.1185 0.0936 0.9741 0.050 Uiso 1 1 d . . . H89A H 0.2422 0.1080 1.0091 0.050 Uiso 1 1 d . . . H89B H 0.2566 0.0393 0.9815 0.050 Uiso 1 1 d . . . H89C H 0.2964 0.1248 0.9753 0.050 Uiso 1 1 d . . . H90A H 0.1398 0.2233 0.9960 0.050 Uiso 1 1 d . . . H90B H 0.1939 0.2456 0.9627 0.050 Uiso 1 1 d . . . H90C H 0.0959 0.2277 0.9590 0.050 Uiso 1 1 d . . . H91 H 0.3338 0.0672 0.7865 0.050 Uiso 1 1 d . . . H93A H 0.1561 -0.0758 0.7206 0.050 Uiso 1 1 d . . . H93B H 0.2031 -0.1461 0.7401 0.050 Uiso 1 1 d . . . H93C H 0.1391 -0.0908 0.7606 0.050 Uiso 1 1 d . . . H94 H 0.4127 0.0095 0.7410 0.050 Uiso 1 1 d . . . H95A H 0.5322 -0.0593 0.7490 0.050 Uiso 1 1 d . . . H95B H 0.5096 -0.0690 0.7889 0.050 Uiso 1 1 d . . . H95C H 0.4508 -0.1079 0.7602 0.050 Uiso 1 1 d . . . H96A H 0.5417 0.0864 0.7548 0.050 Uiso 1 1 d . . . H96B H 0.4605 0.1355 0.7658 0.050 Uiso 1 1 d . . . H96C H 0.5133 0.0889 0.7943 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0216(3) 0.0141(2) 0.0171(2) 0.0009(3) 0.0002(3) -0.0006(3) F1 0.054(3) 0.051(3) 0.040(3) 0.004(3) 0.016(3) 0.023(3) F2 0.048(3) 0.044(3) 0.039(3) 0.008(2) 0.003(3) 0.018(2) F3 0.065(4) 0.023(2) 0.065(4) 0.002(2) 0.006(3) 0.012(3) F4 0.063(4) 0.055(3) 0.060(3) 0.007(3) 0.019(3) -0.010(3) F5 0.037(3) 0.080(4) 0.071(4) -0.011(3) 0.005(3) 0.003(3) F6 0.043(4) 0.089(4) 0.108(5) -0.042(4) 0.011(4) -0.030(4) F7 0.039(3) 0.065(3) 0.062(3) 0.035(3) -0.015(3) -0.009(3) F8 0.037(3) 0.055(3) 0.039(3) 0.017(2) -0.007(3) -0.007(3) F9 0.061(4) 0.028(3) 0.071(4) 0.013(3) 0.012(3) 0.000(3) F10 0.068(4) 0.027(2) 0.038(3) 0.003(2) 0.011(3) -0.008(3) F11 0.083(4) 0.031(3) 0.030(3) -0.006(2) -0.001(3) -0.006(3) F12 0.056(3) 0.029(3) 0.046(3) 0.005(2) 0.009(3) 0.014(3) O1 0.037(3) 0.035(3) 0.034(3) 0.015(3) 0.008(3) 0.009(3) O2 0.040(3) 0.023(3) 0.030(3) 0.004(2) 0.004(3) -0.007(3) O3 0.034(4) 0.128(7) 0.057(5) -0.032(5) -0.014(4) 0.026(5) O4 0.038(4) 0.034(3) 0.037(3) 0.002(3) 0.000(3) 0.003(3) O5 0.039(4) 0.036(3) 0.041(3) 0.003(3) 0.004(3) -0.001(3) O6 0.032(3) 0.036(3) 0.029(3) -0.003(2) -0.004(3) -0.003(3) O7 0.068(4) 0.027(3) 0.027(3) 0.004(3) -0.012(3) 0.013(3) O8 0.039(4) 0.030(3) 0.022(3) 0.002(2) -0.001(3) 0.000(3) O9 0.042(4) 0.032(3) 0.036(3) 0.002(3) 0.004(3) 0.010(3) O10 0.031(3) 0.035(3) 0.032(3) -0.002(3) 0.000(2) -0.009(3) O11 0.046(4) 0.027(3) 0.047(4) -0.002(3) 0.011(3) -0.008(3) O12 0.032(3) 0.044(3) 0.036(3) -0.014(3) -0.009(3) 0.007(3) N1 0.022(3) 0.014(3) 0.015(3) -0.002(2) 0.006(3) -0.001(3) N2 0.027(4) 0.013(3) 0.019(3) 0.000(2) 0.006(3) 0.000(3) N3 0.025(3) 0.017(3) 0.016(3) -0.001(2) 0.000(3) 0.007(3) N4 0.018(4) 0.014(3) 0.025(3) -0.001(2) 0.004(3) -0.002(3) N5 0.028(4) 0.018(3) 0.020(3) -0.002(3) 0.006(3) 0.002(3) N6 0.026(4) 0.038(4) 0.030(4) -0.001(3) -0.007(3) 0.005(3) N7 0.030(4) 0.021(3) 0.035(4) -0.005(3) -0.001(3) -0.001(3) N8 0.034(4) 0.027(3) 0.016(3) -0.004(3) -0.005(3) 0.010(3) N9 0.027(4) 0.020(3) 0.021(3) 0.002(3) 0.012(3) 0.000(3) N10 0.030(4) 0.021(3) 0.018(3) 0.003(3) -0.003(3) 0.001(3) C1 0.012(4) 0.021(4) 0.021(4) 0.001(3) 0.000(3) 0.000(3) C2 0.035(5) 0.011(3) 0.025(4) 0.006(3) 0.000(4) -0.008(3) C3 0.030(5) 0.014(4) 0.023(4) 0.007(3) -0.003(4) -0.003(3) C4 0.025(4) 0.021(4) 0.016(3) 0.002(3) 0.002(3) 0.000(3) C5 0.020(4) 0.019(4) 0.016(3) -0.002(3) 0.003(3) 0.002(3) C6 0.020(4) 0.031(4) 0.022(4) -0.001(4) 0.005(3) 0.008(4) C7 0.023(4) 0.020(4) 0.033(4) -0.005(3) -0.007(4) -0.003(3) C8 0.032(5) 0.017(4) 0.024(4) 0.000(3) -0.001(4) -0.001(3) C9 0.016(4) 0.020(4) 0.027(4) -0.002(3) 0.001(3) 0.000(3) C10 0.022(4) 0.017(4) 0.019(4) -0.002(3) 0.003(3) 0.005(3) C11 0.024(4) 0.016(4) 0.020(4) 0.002(3) 0.007(3) 0.002(3) C12 0.028(5) 0.023(4) 0.023(4) 0.003(3) 0.008(4) -0.002(4) C13 0.030(5) 0.022(4) 0.016(4) 0.007(3) 0.002(4) 0.004(4) C14 0.028(4) 0.019(4) 0.027(4) -0.003(3) 0.005(4) 0.004(3) C15 0.030(4) 0.020(3) 0.019(3) 0.000(3) 0.009(4) 0.004(4) C16 0.027(4) 0.018(3) 0.012(3) -0.003(3) 0.002(3) 0.001(4) C17 0.029(5) 0.027(4) 0.026(4) -0.002(4) -0.007(4) 0.005(4) C18 0.021(4) 0.019(4) 0.027(4) -0.002(3) -0.003(3) 0.001(3) C19 0.023(4) 0.013(3) 0.024(4) 0.000(3) 0.001(3) -0.001(3) C20 0.026(4) 0.014(3) 0.025(4) -0.005(3) 0.004(4) -0.005(4) C21 0.024(4) 0.014(3) 0.023(4) 0.002(3) 0.000(3) -0.002(3) C22 0.023(4) 0.017(4) 0.038(5) -0.002(3) 0.002(4) 0.003(3) C23 0.041(6) 0.021(4) 0.040(5) 0.003(4) 0.008(4) 0.004(4) C24 0.035(5) 0.022(4) 0.041(5) 0.001(4) 0.006(4) -0.005(4) C25 0.032(5) 0.017(4) 0.031(5) 0.002(3) 0.003(4) 0.001(4) C26 0.027(4) 0.019(3) 0.021(4) 0.002(3) -0.003(4) 0.003(3) C27 0.030(5) 0.025(4) 0.023(4) -0.001(3) 0.001(4) 0.004(4) C28 0.031(5) 0.027(4) 0.026(4) -0.001(3) 0.006(4) 0.003(4) C29 0.033(5) 0.024(4) 0.039(5) -0.003(4) 0.010(4) 0.009(4) C30 0.044(6) 0.027(4) 0.022(4) 0.000(3) 0.008(4) 0.008(4) C31 0.049(6) 0.042(5) 0.032(5) 0.000(4) 0.008(4) 0.006(5) C32 0.055(6) 0.059(6) 0.034(5) -0.013(4) -0.005(5) 0.010(6) C33 0.048(6) 0.051(5) 0.044(5) -0.010(5) 0.006(4) -0.019(6) C34 0.052(6) 0.042(5) 0.029(4) -0.001(4) 0.014(4) -0.012(5) C35 0.039(5) 0.026(4) 0.050(5) 0.004(4) 0.000(5) 0.004(4) C36 0.043(5) 0.026(5) 0.033(5) 0.003(4) 0.016(4) -0.001(4) C37 0.027(4) 0.021(4) 0.018(4) 0.004(3) -0.003(3) 0.001(3) C38 0.050(6) 0.034(4) 0.022(4) -0.003(4) -0.003(4) -0.005(4) C39 0.056(6) 0.044(5) 0.025(4) 0.001(4) -0.011(4) 0.004(6) C40 0.067(7) 0.036(5) 0.032(5) 0.002(4) -0.025(5) -0.002(5) C41 0.050(6) 0.033(4) 0.047(6) -0.008(4) -0.012(5) 0.007(4) C42 0.031(4) 0.026(4) 0.023(4) 0.001(4) -0.006(3) -0.002(4) C43 0.023(5) 0.049(5) 0.047(5) -0.007(4) -0.008(4) 0.007(4) C44 0.030(5) 0.040(4) 0.035(5) -0.002(4) -0.004(4) 0.005(4) C45 0.026(5) 0.040(5) 0.037(5) 0.007(4) 0.002(4) 0.002(4) C46 0.063(6) 0.048(5) 0.035(5) 0.007(4) -0.010(6) 0.007(6) C47 0.086(9) 0.032(5) 0.071(8) 0.020(5) -0.003(7) 0.008(5) C48 0.079(8) 0.036(5) 0.064(7) -0.008(5) -0.018(6) -0.002(6) C49 0.054(6) 0.044(5) 0.032(5) 0.004(4) -0.001(5) 0.002(5) C50 0.032(5) 0.034(4) 0.030(5) 0.001(4) 0.008(4) 0.008(4) C51 0.079(8) 0.032(5) 0.053(6) -0.001(4) 0.015(6) -0.009(5) C52 0.031(6) 0.053(6) 0.063(7) -0.015(5) -0.009(5) 0.000(5) C53 0.021(4) 0.020(4) 0.027(4) 0.006(3) -0.005(4) 0.005(3) C54 0.031(5) 0.023(4) 0.029(4) 0.001(3) 0.004(4) 0.002(4) C55 0.024(5) 0.032(5) 0.037(5) 0.008(4) 0.006(4) 0.002(4) C56 0.035(5) 0.021(4) 0.054(5) 0.014(4) 0.004(4) -0.006(4) C57 0.039(4) 0.018(3) 0.045(4) 0.010(4) -0.001(4) -0.004(4) C58 0.020(4) 0.021(4) 0.027(4) 0.003(4) 0.000(4) 0.001(3) C59 0.029(5) 0.016(4) 0.046(5) 0.006(4) 0.000(4) 0.000(4) C60 0.028(5) 0.022(4) 0.025(4) 0.006(3) -0.004(4) 0.001(3) C61 0.027(5) 0.032(4) 0.025(4) -0.003(4) -0.001(4) 0.006(4) C62 0.044(6) 0.053(6) 0.029(5) -0.003(4) 0.002(4) -0.014(5) C63 0.065(7) 0.056(7) 0.039(5) -0.026(5) 0.001(5) -0.006(5) C64 0.059(7) 0.025(5) 0.071(7) -0.021(5) -0.004(6) 0.008(5) C65 0.078(8) 0.024(5) 0.069(7) 0.009(5) -0.008(7) 0.002(5) C66 0.062(6) 0.040(6) 0.036(5) 0.002(4) -0.003(5) 0.017(5) C67 0.032(5) 0.058(6) 0.033(5) -0.001(5) -0.001(4) 0.009(5) C68 0.033(5) 0.037(5) 0.043(5) 0.018(4) -0.003(5) -0.013(4) C69 0.024(4) 0.020(4) 0.023(4) 0.002(3) 0.000(3) 0.000(3) C70 0.043(6) 0.037(5) 0.029(4) -0.005(4) -0.005(4) 0.019(4) C71 0.074(7) 0.039(5) 0.028(5) -0.012(4) -0.014(5) 0.007(5) C72 0.063(7) 0.030(5) 0.036(5) -0.012(4) -0.024(5) 0.013(5) C73 0.039(5) 0.034(5) 0.041(5) -0.008(4) -0.019(4) 0.019(4) C74 0.035(5) 0.024(4) 0.025(4) -0.002(3) -0.013(4) 0.001(4) C75 0.035(5) 0.024(4) 0.022(4) -0.004(3) 0.001(4) 0.005(4) C76 0.033(5) 0.018(4) 0.020(4) -0.004(3) 0.002(3) 0.001(3) C77 0.022(4) 0.024(4) 0.023(4) 0.004(3) 0.002(3) 0.003(3) C78 0.040(6) 0.036(5) 0.042(5) 0.014(4) 0.005(5) 0.007(4) C79 0.035(6) 0.058(6) 0.050(5) 0.020(5) 0.003(5) -0.005(5) C80 0.051(7) 0.054(6) 0.044(5) 0.021(4) 0.018(5) 0.001(6) C81 0.045(6) 0.043(5) 0.035(5) 0.007(4) 0.013(5) 0.005(5) C82 0.042(6) 0.037(5) 0.031(5) 0.013(4) -0.006(4) 0.005(4) C83 0.030(5) 0.048(5) 0.036(5) -0.009(4) -0.001(4) -0.017(5) C84 0.040(6) 0.028(4) 0.031(5) -0.001(4) 0.007(4) -0.001(4) C85 0.029(5) 0.019(3) 0.023(4) -0.001(3) 0.003(4) -0.001(4) C86 0.032(5) 0.020(4) 0.027(4) -0.004(4) 0.005(4) 0.006(4) C87 0.036(6) 0.071(7) 0.042(5) -0.020(5) -0.002(5) -0.002(5) C88 0.030(5) 0.033(4) 0.026(4) -0.003(3) 0.003(4) 0.004(4) C89 0.056(6) 0.051(6) 0.019(4) 0.003(4) -0.004(4) 0.003(5) C90 0.051(6) 0.038(5) 0.031(5) -0.011(4) 0.004(4) -0.003(4) C91 0.029(4) 0.025(4) 0.023(4) -0.005(3) 0.004(4) 0.003(4) C92 0.029(5) 0.031(5) 0.027(4) -0.006(4) 0.009(3) 0.005(4) C93 0.045(5) 0.063(6) 0.048(5) -0.030(4) -0.004(5) 0.003(6) C94 0.024(5) 0.057(6) 0.020(4) 0.001(4) 0.000(4) -0.013(4) C95 0.031(5) 0.110(9) 0.032(5) -0.026(6) -0.006(4) 0.020(7) C96 0.074(7) 0.089(8) 0.029(5) -0.013(5) 0.009(5) -0.039(7) C97 0.153(16) 0.094(11) 0.135(14) -0.020(11) -0.089(13) 0.064(12) C98 0.147(18) 0.19(2) 0.108(14) 0.027(15) -0.039(13) -0.071(17) C99 0.087(10) 0.087(9) 0.076(8) -0.057(7) -0.035(8) 0.046(8) C100 0.159(17) 0.058(8) 0.065(9) -0.010(6) -0.049(10) 0.042(10) C101 0.077(9) 0.120(12) 0.118(12) -0.003(9) 0.019(10) -0.033(10) C102 0.151(14) 0.085(9) 0.041(6) -0.030(7) -0.008(8) -0.011(11) C103 0.143(16) 0.070(9) 0.115(13) -0.040(9) -0.079(12) 0.039(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N4 2.027(6) . ? Ru1 N2 2.030(6) . ? Ru1 N1 2.037(5) . ? Ru1 N3 2.043(5) . ? Ru1 N9 2.123(6) . ? Ru1 N10 2.131(6) . ? F1 C36 1.334(9) . ? F2 C36 1.348(9) . ? F3 C36 1.346(9) . ? F4 C52 1.355(11) . ? F5 C52 1.339(10) . ? F6 C52 1.339(10) . ? F7 C68 1.340(10) . ? F8 C68 1.353(10) . ? F9 C68 1.345(10) . ? F10 C84 1.322(9) . ? F11 C84 1.346(9) . ? F12 C84 1.342(10) . ? O1 C27 1.229(9) . ? O2 C28 1.402(9) . ? O2 C35 1.437(10) . ? O3 C43 1.210(10) . ? O4 C44 1.424(9) . ? O4 C51 1.434(10) . ? O5 C59 1.215(9) . ? O6 C67 1.434(10) . ? O6 C60 1.433(9) . ? O7 C75 1.222(9) . ? O8 C76 1.409(9) . ? O8 C83 1.424(10) . ? O9 C86 1.214(9) . ? O10 C86 1.307(9) . ? O10 C87 1.448(11) . ? O11 C92 1.204(9) . ? O12 C92 1.335(9) . ? O12 C93 1.437(11) . ? N1 C4 1.362(9) . ? N1 C1 1.390(9) . ? N2 C9 1.377(9) . ? N2 C6 1.397(9) . ? N3 C14 1.388(10) . ? N3 C11 1.385(9) . ? N4 C19 1.380(9) . ? N4 C16 1.394(9) . ? N5 C27 1.334(9) . ? N5 C26 1.420(9) . ? N5 H5A 1.0583 . ? N6 C43 1.353(10) . ? N6 C42 1.435(9) . ? N6 H6A 1.1230 . ? N7 C59 1.345(10) . ? N7 C58 1.441(10) . ? N7 H7A 0.9880 . ? N8 C75 1.335(10) . ? N8 C74 1.437(9) . ? N8 H8A 0.8915 . ? N9 C85 1.485(10) . ? N9 H9A 1.0171 . ? N9 H9B 0.9753 . ? N10 C91 1.466(9) . ? N10 H10A 0.8312 . ? N10 H10B 0.9918 . ? C1 C20 1.403(10) . ? C1 C2 1.443(10) . ? C2 C3 1.333(10) . ? C2 H2 0.8495 . ? C3 C4 1.460(9) . ? C3 H3 0.8341 . ? C4 C5 1.380(10) . ? C5 C6 1.407(11) . ? C5 C37 1.515(10) . ? C6 C7 1.426(10) . ? C7 C8 1.347(10) . ? C7 H7 0.8430 . ? C8 C9 1.434(10) . ? C8 H8 0.9751 . ? C9 C10 1.407(9) . ? C10 C11 1.378(10) . ? C10 C53 1.493(10) . ? C11 C12 1.434(10) . ? C12 C13 1.349(11) . ? C12 H12 1.0003 . ? C13 C14 1.449(10) . ? C13 H13 0.9350 . ? C14 C15 1.375(11) . ? C15 C16 1.416(10) . ? C15 C69 1.505(10) . ? C16 C17 1.434(10) . ? C17 C18 1.345(10) . ? C17 H17 0.9678 . ? C18 C19 1.440(10) . ? C18 H18 0.8834 . ? C19 C20 1.402(9) . ? C20 C21 1.508(10) . ? C21 C22 1.381(11) . ? C21 C26 1.404(10) . ? C22 C23 1.360(11) . ? C22 H22 1.0456 . ? C23 C24 1.395(11) . ? C23 H23 0.9126 . ? C24 C25 1.375(11) . ? C24 H24 0.8525 . ? C25 C26 1.384(10) . ? C25 H25 0.9024 . ? C27 C28 1.567(11) . ? C28 C29 1.522(11) . ? C28 C36 1.521(11) . ? C29 C34 1.391(11) . ? C29 C30 1.386(11) . ? C30 C31 1.383(12) . ? C30 H30 1.0613 . ? C31 C32 1.381(14) . ? C31 H31 1.0259 . ? C32 C33 1.372(12) . ? C32 H32 0.8784 . ? C33 C34 1.359(12) . ? C33 H33 0.9126 . ? C34 H34 0.8296 . ? C35 H35A 0.9083 . ? C35 H35B 1.1119 . ? C35 H35C 0.9110 . ? C37 C38 1.386(11) . ? C37 C42 1.408(10) . ? C38 C39 1.400(11) . ? C38 H38 1.1485 . ? C39 C40 1.363(13) . ? C39 H39 0.9878 . ? C40 C41 1.364(13) . ? C40 H40 0.7947 . ? C41 C42 1.384(11) . ? C41 H41 0.8191 . ? C43 C44 1.545(11) . ? C44 C52 1.522(12) . ? C44 C45 1.519(11) . ? C45 C46 1.399(11) . ? C45 C50 1.391(11) . ? C46 C47 1.396(13) . ? C46 H46 0.9550 . ? C47 C48 1.343(14) . ? C47 H47 0.8356 . ? C48 C49 1.384(13) . ? C48 H48 0.8315 . ? C49 C50 1.390(12) . ? C49 H49 0.9257 . ? C50 H50 1.0510 . ? C51 H51A 1.0781 . ? C51 H51B 1.0801 . ? C51 H51C 0.8987 . ? C53 C58 1.380(10) . ? C53 C54 1.405(11) . ? C54 C55 1.372(11) . ? C54 H54 0.9268 . ? C55 C56 1.364(12) . ? C55 H55 0.8413 . ? C56 C57 1.385(11) . ? C56 H56 0.9747 . ? C57 C58 1.391(10) . ? C57 H57 1.0526 . ? C59 C60 1.528(11) . ? C60 C61 1.516(11) . ? C60 C68 1.549(10) . ? C61 C66 1.380(11) . ? C61 C62 1.389(11) . ? C62 C63 1.386(13) . ? C62 H62 0.9143 . ? C63 C64 1.354(14) . ? C63 H63 0.9214 . ? C64 C65 1.387(14) . ? C64 H64 1.0677 . ? C65 C66 1.382(13) . ? C65 H65 1.0903 . ? C66 H66 0.9647 . ? C67 H67A 0.8782 . ? C67 H67B 0.9696 . ? C67 H67C 1.0591 . ? C69 C74 1.388(10) . ? C69 C70 1.402(10) . ? C70 C71 1.359(11) . ? C70 H70 0.9118 . ? C71 C72 1.371(12) . ? C71 H71 0.9223 . ? C72 C73 1.377(12) . ? C72 H72 0.9594 . ? C73 C74 1.368(11) . ? C73 H73 1.0337 . ? C75 C76 1.557(10) . ? C76 C77 1.528(10) . ? C76 C84 1.559(11) . ? C77 C78 1.370(11) . ? C77 C82 1.398(10) . ? C78 C79 1.364(12) . ? C78 H78 1.0050 . ? C79 C80 1.382(12) . ? C79 H79 0.9300 . ? C80 C81 1.366(14) . ? C80 H80 0.8085 . ? C81 C82 1.371(12) . ? C81 H81 0.9198 . ? C82 H82 0.9516 . ? C83 H83A 0.9678 . ? C83 H83B 0.7921 . ? C83 H83C 1.0653 . ? C85 C86 1.513(11) . ? C85 C88 1.529(10) . ? C85 H85 0.9018 . ? C87 H87A 0.8736 . ? C87 H87B 0.9101 . ? C87 H87C 1.0505 . ? C88 C89 1.520(11) . ? C88 C90 1.522(11) . ? C88 H88 0.8901 . ? C89 H89A 0.9219 . ? C89 H89B 0.8552 . ? C89 H89C 1.0070 . ? C90 H90A 0.9302 . ? C90 H90B 0.9737 . ? C90 H90C 0.9904 . ? C91 C92 1.487(11) . ? C91 C94 1.538(11) . ? C91 H91 1.0755 . ? C93 H93A 0.8761 . ? C93 H93B 0.9982 . ? C93 H93C 0.9894 . ? C94 C96 1.536(12) . ? C94 C95 1.551(14) . ? C94 H94 0.9770 . ? C95 H95A 0.9290 . ? C95 H95B 0.8811 . ? C95 H95C 0.8714 . ? C96 H96A 0.9157 . ? C96 H96B 1.0938 . ? C96 H96C 0.8465 . ? C97 C98 1.34(2) . ? C97 C103 1.54(2) . ? C98 C99 1.37(2) . ? C99 C102 1.410(19) . ? C100 C103 1.36(2) . ? C100 C102 1.470(18) . ? C101 C102 1.334(18) . ? 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 N4 Ru1 N2 179.4(3) . . ? N4 Ru1 N1 90.5(2) . . ? N2 Ru1 N1 89.6(2) . . ? N4 Ru1 N3 90.2(2) . . ? N2 Ru1 N3 89.7(2) . . ? N1 Ru1 N3 178.6(3) . . ? N4 Ru1 N9 91.5(2) . . ? N2 Ru1 N9 87.9(2) . . ? N1 Ru1 N9 91.9(2) . . ? N3 Ru1 N9 89.2(2) . . ? N4 Ru1 N10 90.0(2) . . ? N2 Ru1 N10 90.7(2) . . ? N1 Ru1 N10 86.9(2) . . ? N3 Ru1 N10 91.9(2) . . ? N9 Ru1 N10 178.1(3) . . ? C28 O2 C35 118.3(6) . . ? C44 O4 C51 114.2(7) . . ? C67 O6 C60 118.9(6) . . ? C76 O8 C83 116.9(6) . . ? C86 O10 C87 115.1(7) . . ? C92 O12 C93 116.3(7) . . ? C4 N1 C1 107.2(5) . . ? C4 N1 Ru1 127.2(5) . . ? C1 N1 Ru1 125.5(5) . . ? C9 N2 C6 105.3(6) . . ? C9 N2 Ru1 127.5(5) . . ? C6 N2 Ru1 127.0(5) . . ? C14 N3 C11 106.8(6) . . ? C14 N3 Ru1 126.7(5) . . ? C11 N3 Ru1 126.4(5) . . ? C19 N4 C16 105.4(6) . . ? C19 N4 Ru1 127.8(5) . . ? C16 N4 Ru1 126.7(5) . . ? C27 N5 C26 123.7(6) . . ? C27 N5 H5A 120.5 . . ? C26 N5 H5A 115.1 . . ? C43 N6 C42 128.0(7) . . ? C43 N6 H6A 121.0 . . ? C42 N6 H6A 110.3 . . ? C59 N7 C58 123.6(7) . . ? C59 N7 H7A 115.2 . . ? C58 N7 H7A 121.1 . . ? C75 N8 C74 124.0(6) . . ? C75 N8 H8A 113.1 . . ? C74 N8 H8A 122.0 . . ? C85 N9 Ru1 118.7(4) . . ? C85 N9 H9A 106.7 . . ? Ru1 N9 H9A 110.1 . . ? C85 N9 H9B 109.6 . . ? Ru1 N9 H9B 109.6 . . ? H9A N9 H9B 100.5 . . ? C91 N10 Ru1 118.6(5) . . ? C91 N10 H10A 113.8 . . ? Ru1 N10 H10A 103.4 . . ? C91 N10 H10B 107.6 . . ? Ru1 N10 H10B 98.1 . . ? H10A N10 H10B 114.6 . . ? N1 C1 C20 125.8(6) . . ? N1 C1 C2 108.4(6) . . ? C20 C1 C2 125.7(6) . . ? C3 C2 C1 108.1(6) . . ? C3 C2 H2 130.7 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 107.4(6) . . ? C2 C3 H3 132.0 . . ? C4 C3 H3 120.6 . . ? N1 C4 C5 126.0(6) . . ? N1 C4 C3 108.9(6) . . ? C5 C4 C3 125.0(7) . . ? C4 C5 C6 125.7(7) . . ? C4 C5 C37 117.7(6) . . ? C6 C5 C37 116.6(6) . . ? N2 C6 C5 124.2(7) . . ? N2 C6 C7 109.6(7) . . ? C5 C6 C7 126.1(7) . . ? C8 C7 C6 107.6(7) . . ? C8 C7 H7 125.0 . . ? C6 C7 H7 127.2 . . ? C7 C8 C9 107.4(6) . . ? C7 C8 H8 134.4 . . ? C9 C8 H8 118.2 . . ? N2 C9 C10 124.3(7) . . ? N2 C9 C8 110.0(6) . . ? C10 C9 C8 125.7(7) . . ? C11 C10 C9 126.1(7) . . ? C11 C10 C53 117.8(6) . . ? C9 C10 C53 116.1(6) . . ? C10 C11 N3 125.6(6) . . ? C10 C11 C12 125.5(7) . . ? N3 C11 C12 108.9(6) . . ? C13 C12 C11 108.3(7) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 130.1 . . ? C12 C13 C14 107.1(7) . . ? C12 C13 H13 123.1 . . ? C14 C13 H13 129.6 . . ? N3 C14 C15 125.4(7) . . ? N3 C14 C13 108.8(7) . . ? C15 C14 C13 125.7(7) . . ? C14 C15 C16 126.1(7) . . ? C14 C15 C69 118.6(6) . . ? C16 C15 C69 115.3(7) . . ? N4 C16 C15 124.8(7) . . ? N4 C16 C17 109.8(6) . . ? C15 C16 C17 125.4(7) . . ? C18 C17 C16 107.4(7) . . ? C18 C17 H17 127.7 . . ? C16 C17 H17 123.9 . . ? C17 C18 C19 107.5(7) . . ? C17 C18 H18 126.9 . . ? C19 C18 H18 125.4 . . ? N4 C19 C20 124.0(7) . . ? N4 C19 C18 109.9(6) . . ? C20 C19 C18 126.2(7) . . ? C19 C20 C1 126.2(7) . . ? C19 C20 C21 116.0(7) . . ? C1 C20 C21 117.8(6) . . ? C22 C21 C26 118.8(7) . . ? C22 C21 C20 119.7(6) . . ? C26 C21 C20 121.5(7) . . ? C21 C22 C23 121.5(7) . . ? C21 C22 H22 108.5 . . ? C23 C22 H22 129.7 . . ? C22 C23 C24 119.5(8) . . ? C22 C23 H23 108.4 . . ? C24 C23 H23 131.5 . . ? C25 C24 C23 120.3(7) . . ? C25 C24 H24 123.1 . . ? C23 C24 H24 116.6 . . ? C24 C25 C26 119.9(7) . . ? C24 C25 H25 122.8 . . ? C26 C25 H25 117.1 . . ? C25 C26 N5 119.6(6) . . ? C25 C26 C21 119.8(7) . . ? N5 C26 C21 120.5(6) . . ? O1 C27 N5 125.7(7) . . ? O1 C27 C28 120.1(7) . . ? N5 C27 C28 114.1(6) . . ? O2 C28 C29 107.3(6) . . ? O2 C28 C36 109.2(7) . . ? C29 C28 C36 110.2(6) . . ? O2 C28 C27 112.4(6) . . ? C29 C28 C27 107.6(7) . . ? C36 C28 C27 110.2(6) . . ? C34 C29 C30 118.4(8) . . ? C34 C29 C28 120.1(7) . . ? C30 C29 C28 121.5(7) . . ? C31 C30 C29 120.3(8) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 120.3 . . ? C32 C31 C30 119.8(8) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 120.8 . . ? C33 C32 C31 120.1(8) . . ? C33 C32 H32 128.8 . . ? C31 C32 H32 110.6 . . ? C34 C33 C32 120.1(9) . . ? C34 C33 H33 126.1 . . ? C32 C33 H33 113.6 . . ? C33 C34 C29 121.3(8) . . ? C33 C34 H34 119.1 . . ? C29 C34 H34 118.0 . . ? O2 C35 H35A 118.6 . . ? O2 C35 H35B 106.4 . . ? H35A C35 H35B 97.9 . . ? O2 C35 H35C 115.0 . . ? H35A C35 H35C 116.2 . . ? H35B C35 H35C 97.9 . . ? F1 C36 F2 105.9(7) . . ? F1 C36 F3 105.5(6) . . ? F2 C36 F3 105.7(6) . . ? F1 C36 C28 110.8(6) . . ? F2 C36 C28 113.7(6) . . ? F3 C36 C28 114.5(7) . . ? C38 C37 C42 118.4(7) . . ? C38 C37 C5 119.8(7) . . ? C42 C37 C5 121.7(6) . . ? C37 C38 C39 120.7(8) . . ? C37 C38 H38 112.6 . . ? C39 C38 H38 126.6 . . ? C40 C39 C38 119.4(8) . . ? C40 C39 H39 130.7 . . ? C38 C39 H39 109.7 . . ? C39 C40 C41 121.0(8) . . ? C39 C40 H40 107.1 . . ? C41 C40 H40 131.8 . . ? C40 C41 C42 120.6(9) . . ? C40 C41 H41 122.9 . . ? C42 C41 H41 116.4 . . ? C41 C42 C37 119.7(7) . . ? C41 C42 N6 123.2(7) . . ? C37 C42 N6 117.1(6) . . ? O3 C43 N6 126.0(8) . . ? O3 C43 C44 121.2(8) . . ? N6 C43 C44 112.8(7) . . ? O4 C44 C52 110.7(7) . . ? O4 C44 C45 105.7(6) . . ? C52 C44 C45 107.6(7) . . ? O4 C44 C43 111.2(6) . . ? C52 C44 C43 110.6(7) . . ? C45 C44 C43 110.9(7) . . ? C46 C45 C50 118.8(8) . . ? C46 C45 C44 121.2(7) . . ? C50 C45 C44 119.6(7) . . ? C47 C46 C45 119.5(8) . . ? C47 C46 H46 125.6 . . ? C45 C46 H46 112.1 . . ? C48 C47 C46 120.9(9) . . ? C48 C47 H47 118.2 . . ? C46 C47 H47 119.3 . . ? C47 C48 C49 120.8(9) . . ? C47 C48 H48 131.7 . . ? C49 C48 H48 106.4 . . ? C48 C49 C50 119.4(8) . . ? C48 C49 H49 132.9 . . ? C50 C49 H49 107.4 . . ? C49 C50 C45 120.5(8) . . ? C49 C50 H50 125.2 . . ? C45 C50 H50 114.1 . . ? O4 C51 H51A 116.8 . . ? O4 C51 H51B 115.3 . . ? H51A C51 H51B 90.6 . . ? O4 C51 H51C 125.9 . . ? H51A C51 H51C 100.4 . . ? H51B C51 H51C 101.2 . . ? F5 C52 F4 106.7(8) . . ? F5 C52 F6 107.2(7) . . ? F4 C52 F6 104.8(8) . . ? F5 C52 C44 112.6(8) . . ? F4 C52 C44 111.2(7) . . ? F6 C52 C44 113.9(8) . . ? C58 C53 C54 118.3(7) . . ? C58 C53 C10 122.3(7) . . ? C54 C53 C10 119.4(7) . . ? C55 C54 C53 120.4(7) . . ? C55 C54 H54 127.6 . . ? C53 C54 H54 111.9 . . ? C56 C55 C54 120.6(8) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.7 . . ? C55 C56 C57 120.2(8) . . ? C55 C56 H56 133.6 . . ? C57 C56 H56 105.9 . . ? C56 C57 C58 119.4(8) . . ? C56 C57 H57 124.2 . . ? C58 C57 H57 116.3 . . ? C53 C58 C57 120.9(7) . . ? C53 C58 N7 118.7(6) . . ? C57 C58 N7 120.4(7) . . ? O5 C59 N7 125.1(8) . . ? O5 C59 C60 120.7(7) . . ? N7 C59 C60 114.2(7) . . ? O6 C60 C61 113.2(6) . . ? O6 C60 C59 108.9(6) . . ? C61 C60 C59 108.3(6) . . ? O6 C60 C68 104.9(6) . . ? C61 C60 C68 114.2(7) . . ? C59 C60 C68 107.1(6) . . ? C66 C61 C62 118.9(8) . . ? C66 C61 C60 116.3(7) . . ? C62 C61 C60 124.8(8) . . ? C63 C62 C61 120.0(9) . . ? C63 C62 H62 113.7 . . ? C61 C62 H62 124.6 . . ? C64 C63 C62 120.6(8) . . ? C64 C63 H63 107.2 . . ? C62 C63 H63 131.0 . . ? C63 C64 C65 120.2(8) . . ? C63 C64 H64 118.7 . . ? C65 C64 H64 120.9 . . ? C66 C65 C64 119.6(9) . . ? C66 C65 H65 125.0 . . ? C64 C65 H65 112.2 . . ? C61 C66 C65 120.7(8) . . ? C61 C66 H66 124.3 . . ? C65 C66 H66 114.8 . . ? O6 C67 H67A 115.8 . . ? O6 C67 H67B 111.8 . . ? H67A C67 H67B 112.4 . . ? O6 C67 H67C 111.7 . . ? H67A C67 H67C 104.8 . . ? H67B C67 H67C 98.8 . . ? F7 C68 F9 106.7(7) . . ? F7 C68 F8 107.0(7) . . ? F9 C68 F8 106.6(6) . . ? F7 C68 C60 114.5(7) . . ? F9 C68 C60 109.4(7) . . ? F8 C68 C60 112.2(7) . . ? C74 C69 C70 117.6(7) . . ? C74 C69 C15 122.9(6) . . ? C70 C69 C15 119.5(7) . . ? C71 C70 C69 121.6(8) . . ? C71 C70 H70 124.4 . . ? C69 C70 H70 113.1 . . ? C70 C71 C72 120.0(8) . . ? C70 C71 H71 118.7 . . ? C72 C71 H71 121.3 . . ? C71 C72 C73 119.2(8) . . ? C71 C72 H72 118.9 . . ? C73 C72 H72 119.7 . . ? C74 C73 C72 121.4(8) . . ? C74 C73 H73 115.1 . . ? C72 C73 H73 121.5 . . ? C73 C74 C69 120.0(7) . . ? C73 C74 N8 121.8(7) . . ? C69 C74 N8 118.2(7) . . ? O7 C75 N8 126.1(7) . . ? O7 C75 C76 119.1(7) . . ? N8 C75 C76 114.9(7) . . ? O8 C76 C77 107.1(6) . . ? O8 C76 C75 112.4(6) . . ? C77 C76 C75 112.0(6) . . ? O8 C76 C84 109.8(7) . . ? C77 C76 C84 106.8(6) . . ? C75 C76 C84 108.5(6) . . ? C78 C77 C82 118.3(8) . . ? C78 C77 C76 121.8(7) . . ? C82 C77 C76 119.7(7) . . ? C79 C78 C77 121.3(8) . . ? C79 C78 H78 119.0 . . ? C77 C78 H78 119.5 . . ? C78 C79 C80 120.5(9) . . ? C78 C79 H79 116.1 . . ? C80 C79 H79 123.2 . . ? C81 C80 C79 118.6(9) . . ? C81 C80 H80 126.2 . . ? C79 C80 H80 115.1 . . ? C80 C81 C82 121.4(8) . . ? C80 C81 H81 121.9 . . ? C82 C81 H81 116.1 . . ? C81 C82 C77 119.8(8) . . ? C81 C82 H82 122.7 . . ? C77 C82 H82 117.4 . . ? O8 C83 H83A 105.9 . . ? O8 C83 H83B 113.6 . . ? H83A C83 H83B 121.6 . . ? O8 C83 H83C 104.1 . . ? H83A C83 H83C 97.9 . . ? H83B C83 H83C 111.5 . . ? F12 C84 F10 107.9(7) . . ? F12 C84 F11 107.0(7) . . ? F10 C84 F11 107.1(7) . . ? F12 C84 C76 112.0(7) . . ? F10 C84 C76 113.3(7) . . ? F11 C84 C76 109.1(7) . . ? N9 C85 C86 108.2(6) . . ? N9 C85 C88 114.1(6) . . ? C86 C85 C88 111.4(6) . . ? N9 C85 H85 94.8 . . ? C86 C85 H85 120.7 . . ? C88 C85 H85 106.8 . . ? O9 C86 O10 125.0(8) . . ? O9 C86 C85 123.3(8) . . ? O10 C86 C85 111.6(6) . . ? O10 C87 H87A 110.0 . . ? O10 C87 H87B 112.6 . . ? H87A C87 H87B 119.9 . . ? O10 C87 H87C 103.9 . . ? H87A C87 H87C 105.4 . . ? H87B C87 H87C 103.3 . . ? C89 C88 C90 111.9(7) . . ? C89 C88 C85 110.2(6) . . ? C90 C88 C85 112.8(6) . . ? C89 C88 H88 111.4 . . ? C90 C88 H88 104.6 . . ? C85 C88 H88 105.7 . . ? C88 C89 H89A 106.1 . . ? C88 C89 H89B 109.2 . . ? H89A C89 H89B 120.2 . . ? C88 C89 H89C 103.2 . . ? H89A C89 H89C 105.2 . . ? H89B C89 H89C 111.5 . . ? C88 C90 H90A 114.3 . . ? C88 C90 H90B 114.7 . . ? H90A C90 H90B 107.3 . . ? C88 C90 H90C 111.7 . . ? H90A C90 H90C 106.0 . . ? H90B C90 H90C 101.8 . . ? N10 C91 C92 109.0(6) . . ? N10 C91 C94 114.2(6) . . ? C92 C91 C94 112.1(6) . . ? N10 C91 H91 108.8 . . ? C92 C91 H91 110.3 . . ? C94 C91 H91 102.2 . . ? O11 C92 O12 124.9(8) . . ? O11 C92 C91 124.7(7) . . ? O12 C92 C91 110.3(7) . . ? O12 C93 H93A 115.6 . . ? O12 C93 H93B 107.7 . . ? H93A C93 H93B 110.2 . . ? O12 C93 H93C 110.5 . . ? H93A C93 H93C 110.8 . . ? H93B C93 H93C 101.1 . . ? C91 C94 C96 110.3(7) . . ? C91 C94 C95 110.7(7) . . ? C96 C94 C95 111.8(7) . . ? C91 C94 H94 103.4 . . ? C96 C94 H94 114.3 . . ? C95 C94 H94 106.0 . . ? C94 C95 H95A 94.9 . . ? C94 C95 H95B 97.4 . . ? H95A C95 H95B 116.1 . . ? C94 C95 H95C 100.9 . . ? H95A C95 H95C 116.3 . . ? H95B C95 H95C 122.1 . . ? C94 C96 H96A 109.6 . . ? C94 C96 H96B 105.1 . . ? H96A C96 H96B 98.8 . . ? C94 C96 H96C 115.4 . . ? H96A C96 H96C 121.2 . . ? H96B C96 H96C 103.9 . . ? C98 C97 C103 107(2) . . ? C97 C98 C99 130(2) . . ? C98 C99 C102 121.3(16) . . ? C103 C100 C102 117.1(16) . . ? C101 C102 C99 127.4(17) . . ? C101 C102 C100 116.4(17) . . ? C99 C102 C100 116.3(14) . . ? C100 C103 C97 127.9(15) . . ? _diffrn_measured_fraction_theta_max .983 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full .983 _refine_diff_density_max .566 _refine_diff_density_min -.720 _refine_diff_density_rms .084