# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Mike Ward' 'H. Adams' 'Stephen P. Argent' 'Qiao-Hua Wei.' _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Post-coordination functionalisation of pyrazolyl-based ligands as a route to polynuclear complexes based on an inert Ru(II)N6 core ; data_imw930 _database_code_depnum_ccdc_archive 'CCDC 659047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 F12 N12 O2 P2 Ru' _chemical_formula_weight 1043.82 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 C2/c 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' '-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 25.6147(16) _cell_length_b 10.1935(6) _cell_length_c 36.361(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.085(4) _cell_angle_gamma 90.00 _cell_volume 9166.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5304 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 23.15 _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 1.513 _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9012 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 53604 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10549 _reflns_number_gt 7236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0634P)^2^+27.2979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10549 _refine_ls_number_parameters 565 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.606306(12) -0.38194(3) 0.878517(8) 0.03217(10) Uani 1 1 d . . . P1 P 0.12694(5) 0.57958(13) 0.70308(4) 0.0509(3) Uani 1 1 d . . . P2 P 0.89218(5) 0.76967(13) 0.49772(4) 0.0537(3) Uani 1 1 d . . . F1 F 0.08863(13) 0.6318(3) 0.72942(8) 0.0705(8) Uani 1 1 d . . . F2 F 0.13420(15) 0.7239(4) 0.68976(13) 0.1015(13) Uani 1 1 d . . . F3 F 0.07226(12) 0.5669(4) 0.66872(8) 0.0746(9) Uani 1 1 d . . . F4 F 0.16082(14) 0.5218(4) 0.67648(11) 0.0967(12) Uani 1 1 d . . . F5 F 0.11708(14) 0.4337(3) 0.71664(10) 0.0795(9) Uani 1 1 d . . . F6 F 0.17757(15) 0.5925(4) 0.73723(12) 0.1066(13) Uani 1 1 d . . . F7 F 0.90493(13) 0.8334(4) 0.53893(10) 0.0992(13) Uani 1 1 d . A . F8 F 0.95526(13) 0.7523(3) 0.50156(9) 0.0743(9) Uani 1 1 d . A . F9 F 0.8263(2) 0.8086(6) 0.49201(15) 0.0551(13) Uiso 0.592(5) 1 d PU A 1 F10 F 0.8982(2) 0.9257(6) 0.48673(16) 0.0665(15) Uiso 0.592(5) 1 d PU A 1 F11 F 0.8766(3) 0.7374(7) 0.45296(19) 0.0942(19) Uiso 0.592(5) 1 d PU A 1 F12 F 0.8828(3) 0.6314(8) 0.5083(3) 0.109(2) Uiso 0.592(5) 1 d PU A 1 F9' F 0.8340(3) 0.7532(9) 0.5010(2) 0.062(2) Uiso 0.408(5) 1 d PU A 2 F10' F 0.8866(4) 0.8638(10) 0.4683(3) 0.088(2) Uiso 0.408(5) 1 d PU A 2 F11' F 0.8820(4) 0.6405(9) 0.4706(3) 0.085(2) Uiso 0.408(5) 1 d PU A 2 F12' F 0.9046(4) 0.6477(10) 0.5333(3) 0.101(3) Uiso 0.408(5) 1 d PU A 2 O1 O 0.6567(2) -0.5121(5) 0.76849(15) 0.1078(17) Uani 1 1 d . . . O2 O 0.79063(14) 0.4804(3) 0.57932(10) 0.0621(9) Uani 1 1 d . . . N1 N 0.63646(14) -0.1727(4) 0.94675(10) 0.0433(8) Uani 1 1 d . . . H1A H 0.6630 -0.1311 0.9405 0.052 Uiso 1 1 calc R . . N2 N 0.60690(13) -0.2694(3) 0.92621(9) 0.0365(7) Uani 1 1 d . . . N3 N 0.54550(13) -0.4606(3) 0.89726(9) 0.0351(7) Uani 1 1 d . . . N4 N 0.57872(14) -0.5333(3) 0.84019(9) 0.0393(8) Uani 1 1 d . . . N5 N 0.59047(16) -0.5876(4) 0.80957(10) 0.0496(9) Uani 1 1 d . . . H5A H 0.6167 -0.5615 0.7997 0.060 Uiso 1 1 calc R . . N6 N 0.51888(14) -0.1823(4) 0.82936(10) 0.0464(9) Uani 1 1 d . . . H6A H 0.4907 -0.2037 0.8377 0.056 Uiso 1 1 calc R . . N7 N 0.56760(13) -0.2394(3) 0.84068(9) 0.0369(7) Uani 1 1 d . . . N8 N 0.66646(13) -0.3090(3) 0.85823(9) 0.0369(7) Uani 1 1 d . . . N9 N 0.67306(13) -0.4852(3) 0.90886(9) 0.0364(7) Uani 1 1 d . . . N10 N 0.68495(14) -0.5725(4) 0.93754(10) 0.0439(8) Uani 1 1 d . . . H10A H 0.6610 -0.6092 0.9478 0.053 Uiso 1 1 calc R . . N100 N 0.6122(2) 0.1346(6) 0.57633(15) 0.0833(16) Uani 1 1 d . . . N101 N 0.5660(2) -0.2617(7) 0.63749(17) 0.0967(18) Uani 1 1 d . C . C1 C 0.6196(2) -0.1487(5) 0.97803(13) 0.0538(12) Uani 1 1 d . . . H1B H 0.6343 -0.0844 0.9968 0.065 Uiso 1 1 calc R . . C2 C 0.57790(19) -0.2321(5) 0.97860(12) 0.0502(11) Uani 1 1 d . . . H2A H 0.5583 -0.2380 0.9974 0.060 Uiso 1 1 calc R . . C3 C 0.57069(16) -0.3057(4) 0.94564(11) 0.0364(9) Uani 1 1 d . . . C4 C 0.53413(16) -0.4124(4) 0.92876(11) 0.0378(9) Uani 1 1 d . . . C5 C 0.49232(18) -0.4640(5) 0.94203(13) 0.0476(11) Uani 1 1 d . . . H5B H 0.4846 -0.4298 0.9643 0.057 Uiso 1 1 calc R . . C6 C 0.46220(19) -0.5660(5) 0.92219(14) 0.0529(12) Uani 1 1 d . . . H6B H 0.4333 -0.6021 0.9308 0.063 Uiso 1 1 calc R . . C7 C 0.47392(18) -0.6156(5) 0.89012(14) 0.0510(11) Uani 1 1 d . . . H7A H 0.4533 -0.6860 0.8765 0.061 Uiso 1 1 calc R . . C8 C 0.51626(16) -0.5618(4) 0.87769(12) 0.0398(9) Uani 1 1 d . . . C9 C 0.53606(17) -0.6017(4) 0.84552(12) 0.0413(9) Uani 1 1 d . . . C10 C 0.5214(2) -0.7003(5) 0.81828(13) 0.0537(12) Uani 1 1 d . . . H10B H 0.4932 -0.7628 0.8157 0.064 Uiso 1 1 calc R . . C11 C 0.5566(2) -0.6872(5) 0.79619(14) 0.0589(13) Uani 1 1 d . . . H11A H 0.5571 -0.7400 0.7748 0.071 Uiso 1 1 calc R . . C12 C 0.5188(2) -0.0877(5) 0.80349(13) 0.0571(13) Uani 1 1 d . . . H12A H 0.4888 -0.0342 0.7915 0.068 Uiso 1 1 calc R . . C13 C 0.5689(2) -0.0819(5) 0.79758(13) 0.0528(12) Uani 1 1 d . . . H13A H 0.5808 -0.0249 0.7808 0.063 Uiso 1 1 calc R . . C14 C 0.59883(17) -0.1768(4) 0.82119(11) 0.0408(9) Uani 1 1 d . . . C15 C 0.65511(18) -0.2174(4) 0.83054(12) 0.0415(10) Uani 1 1 d . . . C16 C 0.6953(2) -0.1713(5) 0.81415(14) 0.0539(12) Uani 1 1 d . . . H16A H 0.6873 -0.1081 0.7943 0.065 Uiso 1 1 calc R . . C17 C 0.7471(2) -0.2207(6) 0.82775(15) 0.0621(14) Uani 1 1 d . . . H17A H 0.7751 -0.1909 0.8170 0.075 Uiso 1 1 calc R . . C18 C 0.75878(19) -0.3128(5) 0.85674(14) 0.0567(12) Uani 1 1 d . . . H18A H 0.7945 -0.3454 0.8662 0.068 Uiso 1 1 calc R . . C19 C 0.71734(16) -0.3563(4) 0.87165(12) 0.0416(10) Uani 1 1 d . . . C20 C 0.72055(16) -0.4540(4) 0.90157(12) 0.0418(10) Uani 1 1 d . . . C21 C 0.76267(18) -0.5232(5) 0.92598(13) 0.0517(11) Uani 1 1 d . . . H21A H 0.8000 -0.5199 0.9268 0.062 Uiso 1 1 calc R . . C22 C 0.73867(19) -0.5963(5) 0.94837(14) 0.0551(12) Uani 1 1 d . . . H22A H 0.7566 -0.6539 0.9682 0.066 Uiso 1 1 calc R . . C100 C 0.5230(3) 0.0087(10) 0.5713(3) 0.113(3) Uani 1 1 d . . . H1F H 0.5019 0.0536 0.5865 0.11(3) Uiso 1 1 calc R . . H1D H 0.5310 -0.0810 0.5808 0.26(7) Uiso 1 1 calc R . . H1C H 0.5022 0.0061 0.5446 0.41(12) Uiso 1 1 calc R . . C101 C 0.5733(3) 0.0791(6) 0.57445(16) 0.0687(16) Uani 1 1 d . . . C02 C 0.5583(8) -0.4031(17) 0.7330(5) 0.096(4) Uiso 0.462(10) 1 d PU B 1 H02A H 0.5395 -0.3445 0.7124 0.144 Uiso 0.462(10) 1 calc PR B 1 H02B H 0.5557 -0.3675 0.7575 0.144 Uiso 0.462(10) 1 calc PR B 1 H02C H 0.5414 -0.4901 0.7292 0.144 Uiso 0.462(10) 1 calc PR B 1 C03 C 0.6176(9) -0.4143(19) 0.7329(5) 0.093(3) Uiso 0.462(10) 1 d PU B 1 H03A H 0.6335 -0.3252 0.7353 0.112 Uiso 0.462(10) 1 calc PR B 1 H03B H 0.6196 -0.4499 0.7079 0.112 Uiso 0.462(10) 1 calc PR B 1 C04 C 0.7028(7) -0.5340(19) 0.7636(5) 0.087(3) Uiso 0.462(10) 1 d PU B 1 H04A H 0.7252 -0.4536 0.7670 0.105 Uiso 0.462(10) 1 calc PR B 1 H04B H 0.7004 -0.5721 0.7382 0.105 Uiso 0.462(10) 1 calc PR B 1 C05 C 0.7252(7) -0.6372(18) 0.7967(5) 0.089(3) Uiso 0.462(10) 1 d PU B 1 H05A H 0.7620 -0.6630 0.7966 0.133 Uiso 0.462(10) 1 calc PR B 1 H05B H 0.7019 -0.7149 0.7927 0.133 Uiso 0.462(10) 1 calc PR B 1 H05C H 0.7256 -0.5974 0.8213 0.133 Uiso 0.462(10) 1 calc PR B 1 C02' C 0.5875(7) -0.3981(15) 0.7299(4) 0.090(3) Uiso 0.538(10) 1 d PU B 2 H02D H 0.5763 -0.3448 0.7067 0.135 Uiso 0.538(10) 1 calc PR B 2 H02E H 0.5838 -0.3465 0.7518 0.135 Uiso 0.538(10) 1 calc PR B 2 H02F H 0.5646 -0.4763 0.7272 0.135 Uiso 0.538(10) 1 calc PR B 2 C03' C 0.6482(7) -0.4408(16) 0.7361(4) 0.095(3) Uiso 0.538(10) 1 d PU B 2 H03C H 0.6532 -0.4946 0.7146 0.114 Uiso 0.538(10) 1 calc PR B 2 H03D H 0.6726 -0.3638 0.7395 0.114 Uiso 0.538(10) 1 calc PR B 2 C04' C 0.7139(6) -0.5951(16) 0.7765(5) 0.086(3) Uiso 0.538(10) 1 d PU B 2 H04C H 0.7151 -0.6460 0.7536 0.103 Uiso 0.538(10) 1 calc PR B 2 H04D H 0.7449 -0.5339 0.7825 0.103 Uiso 0.538(10) 1 calc PR B 2 C05' C 0.7171(7) -0.6911(17) 0.8112(5) 0.109(4) Uiso 0.538(10) 1 d PU B 2 H05D H 0.7507 -0.7417 0.8162 0.163 Uiso 0.538(10) 1 calc PR B 2 H05E H 0.6862 -0.7511 0.8051 0.163 Uiso 0.538(10) 1 calc PR B 2 H05F H 0.7164 -0.6399 0.8339 0.163 Uiso 0.538(10) 1 calc PR B 2 C106 C 0.7192(3) 0.3632(7) 0.5377(2) 0.102(2) Uani 1 1 d . . . H10C H 0.6801 0.3486 0.5304 0.154 Uiso 1 1 calc R . . H10D H 0.7378 0.2802 0.5463 0.154 Uiso 1 1 calc R . . H10E H 0.7307 0.3964 0.5158 0.154 Uiso 1 1 calc R . . C107 C 0.7331(3) 0.4604(8) 0.5691(2) 0.095(2) Uani 1 1 d . . . H10F H 0.7142 0.5443 0.5607 0.113 Uiso 1 1 calc R . . H10G H 0.7215 0.4278 0.5914 0.113 Uiso 1 1 calc R . . C108 C 0.8071(3) 0.5828(6) 0.60691(19) 0.093(2) Uani 1 1 d . . . H10H H 0.8001 0.5562 0.6314 0.112 Uiso 1 1 calc R . . H10I H 0.7861 0.6635 0.5980 0.112 Uiso 1 1 calc R . . C109 C 0.8653(3) 0.6082(7) 0.61238(19) 0.103(3) Uani 1 1 d . . . H10J H 0.8769 0.6782 0.6312 0.154 Uiso 1 1 calc R . . H10K H 0.8719 0.6351 0.5881 0.154 Uiso 1 1 calc R . . H10L H 0.8858 0.5281 0.6214 0.154 Uiso 1 1 calc R . . C110 C 0.6599(8) -0.262(3) 0.6277(6) 0.130(5) Uiso 0.482(19) 1 d PU C 1 H11B H 0.6673 -0.1698 0.6231 0.194 Uiso 0.482(19) 1 calc PR C 1 H11C H 0.6630 -0.3150 0.6059 0.194 Uiso 0.482(19) 1 calc PR C 1 H11D H 0.6861 -0.2927 0.6508 0.194 Uiso 0.482(19) 1 calc PR C 1 C10' C 0.6528(8) -0.362(3) 0.6306(6) 0.129(5) Uiso 0.518(19) 1 d PU C 2 H10M H 0.6438 -0.4531 0.6353 0.194 Uiso 0.518(19) 1 calc PR C 2 H10N H 0.6854 -0.3354 0.6500 0.194 Uiso 0.518(19) 1 calc PR C 2 H10O H 0.6595 -0.3557 0.6053 0.194 Uiso 0.518(19) 1 calc PR C 2 C111 C 0.6064(3) -0.2737(10) 0.6325(2) 0.113(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03290(16) 0.03463(17) 0.02864(15) -0.00034(14) 0.00739(11) 0.00373(14) P1 0.0465(7) 0.0601(8) 0.0482(7) 0.0103(6) 0.0162(5) 0.0036(6) P2 0.0554(7) 0.0541(8) 0.0558(7) -0.0212(6) 0.0219(6) -0.0149(6) F1 0.081(2) 0.079(2) 0.0552(17) 0.0000(16) 0.0244(15) 0.0175(17) F2 0.080(2) 0.088(3) 0.141(4) 0.024(2) 0.035(2) -0.008(2) F3 0.0641(19) 0.104(3) 0.0545(17) 0.0017(17) 0.0131(15) 0.0015(18) F4 0.082(2) 0.126(3) 0.096(3) 0.024(2) 0.049(2) 0.022(2) F5 0.099(2) 0.070(2) 0.080(2) 0.0145(18) 0.043(2) 0.0153(19) F6 0.073(2) 0.124(3) 0.108(3) -0.013(3) -0.003(2) 0.009(2) F7 0.0549(18) 0.156(4) 0.086(2) -0.063(3) 0.0162(17) -0.008(2) F8 0.069(2) 0.081(2) 0.079(2) 0.0023(17) 0.0293(17) 0.0217(17) O1 0.126(4) 0.117(4) 0.100(4) -0.022(3) 0.065(3) -0.033(3) O2 0.064(2) 0.056(2) 0.064(2) -0.0061(17) 0.0122(18) 0.0057(17) N1 0.0436(19) 0.0396(19) 0.044(2) -0.0086(16) 0.0066(16) -0.0047(16) N2 0.0391(18) 0.0361(18) 0.0327(17) -0.0029(14) 0.0064(14) 0.0032(14) N3 0.0347(17) 0.0372(18) 0.0315(16) 0.0023(14) 0.0052(13) 0.0040(14) N4 0.048(2) 0.0408(19) 0.0280(16) -0.0037(14) 0.0077(15) 0.0069(16) N5 0.058(2) 0.053(2) 0.039(2) -0.0061(17) 0.0137(17) 0.0043(18) N6 0.0410(19) 0.059(2) 0.0388(19) 0.0073(17) 0.0091(15) 0.0158(17) N7 0.0372(18) 0.0407(19) 0.0315(17) -0.0017(14) 0.0071(14) 0.0104(15) N8 0.0384(18) 0.0379(19) 0.0361(17) -0.0024(15) 0.0128(14) 0.0039(15) N9 0.0375(17) 0.0360(18) 0.0354(17) 0.0004(14) 0.0091(14) 0.0020(14) N10 0.045(2) 0.043(2) 0.043(2) 0.0087(16) 0.0085(16) 0.0073(16) N100 0.073(3) 0.107(5) 0.070(3) 0.001(3) 0.021(3) 0.013(3) N101 0.079(4) 0.124(5) 0.093(4) -0.016(4) 0.032(3) 0.002(4) C1 0.063(3) 0.052(3) 0.041(2) -0.015(2) 0.006(2) 0.007(2) C2 0.056(3) 0.061(3) 0.033(2) -0.006(2) 0.012(2) 0.010(2) C3 0.038(2) 0.038(2) 0.033(2) 0.0012(17) 0.0092(16) 0.0085(17) C4 0.039(2) 0.046(2) 0.0290(19) 0.0062(17) 0.0102(16) 0.0084(18) C5 0.047(2) 0.054(3) 0.046(2) 0.008(2) 0.019(2) 0.008(2) C6 0.044(2) 0.058(3) 0.059(3) 0.014(2) 0.018(2) -0.001(2) C7 0.044(2) 0.049(3) 0.058(3) 0.008(2) 0.009(2) -0.005(2) C8 0.039(2) 0.038(2) 0.038(2) 0.0034(18) 0.0024(17) 0.0005(18) C9 0.044(2) 0.036(2) 0.038(2) -0.0014(18) 0.0024(18) -0.0007(18) C10 0.060(3) 0.051(3) 0.046(3) -0.008(2) 0.006(2) -0.006(2) C11 0.075(3) 0.048(3) 0.045(3) -0.014(2) 0.000(2) 0.002(3) C12 0.062(3) 0.066(3) 0.043(3) 0.016(2) 0.013(2) 0.025(2) C13 0.068(3) 0.053(3) 0.041(2) 0.012(2) 0.020(2) 0.017(2) C14 0.050(2) 0.041(2) 0.034(2) 0.0009(18) 0.0157(18) 0.0069(19) C15 0.050(2) 0.040(2) 0.038(2) 0.0034(18) 0.0178(19) 0.0057(19) C16 0.062(3) 0.056(3) 0.051(3) 0.009(2) 0.029(2) 0.005(2) C17 0.055(3) 0.076(4) 0.066(3) 0.012(3) 0.035(3) 0.004(3) C18 0.041(2) 0.074(3) 0.061(3) 0.006(3) 0.022(2) 0.008(2) C19 0.036(2) 0.048(3) 0.042(2) -0.0019(19) 0.0142(17) 0.0078(18) C20 0.037(2) 0.046(2) 0.044(2) -0.0012(19) 0.0123(18) 0.0062(18) C21 0.039(2) 0.063(3) 0.051(3) 0.005(2) 0.009(2) 0.014(2) C22 0.051(3) 0.058(3) 0.051(3) 0.007(2) 0.005(2) 0.018(2) C100 0.094(5) 0.110(7) 0.124(7) -0.003(6) 0.010(5) -0.027(5) C101 0.077(4) 0.074(4) 0.050(3) 0.002(3) 0.007(3) 0.022(3) C106 0.062(4) 0.087(5) 0.140(7) -0.004(5) -0.007(4) -0.006(3) C107 0.066(4) 0.094(5) 0.127(6) 0.016(5) 0.030(4) 0.016(4) C108 0.149(7) 0.051(4) 0.075(4) 0.002(3) 0.020(4) 0.008(4) C109 0.129(6) 0.085(5) 0.073(4) 0.004(4) -0.013(4) -0.041(5) C111 0.071(5) 0.167(8) 0.108(6) -0.053(6) 0.039(4) 0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8 2.016(3) . ? Ru1 N3 2.021(3) . ? Ru1 N9 2.066(3) . ? Ru1 N7 2.068(3) . ? Ru1 N2 2.076(3) . ? Ru1 N4 2.076(3) . ? P1 F6 1.550(4) . ? P1 F4 1.572(4) . ? P1 F2 1.575(4) . ? P1 F5 1.607(4) . ? P1 F3 1.621(3) . ? P1 F1 1.629(3) . ? P2 F10' 1.416(9) . ? P2 F12 1.497(8) . ? P2 F9' 1.536(8) . ? P2 F7 1.587(3) . ? P2 F8 1.595(3) . ? P2 F11 1.606(7) . ? P2 F11' 1.626(9) . ? P2 F10 1.657(6) . ? P2 F9 1.693(5) . ? P2 F12' 1.762(11) . ? O1 C04 1.259(16) . ? O1 C03' 1.354(15) . ? O1 C04' 1.651(16) . ? O1 C03 1.73(2) . ? O2 C108 1.433(7) . ? O2 C107 1.438(7) . ? N1 C1 1.339(6) . ? N1 N2 1.345(5) . ? N1 H1A 0.8800 . ? N2 C3 1.355(5) . ? N3 C4 1.346(5) . ? N3 C8 1.362(5) . ? N4 N5 1.346(5) . ? N4 C9 1.352(5) . ? N5 C11 1.342(6) . ? N5 H5A 0.8800 . ? N6 N7 1.341(4) . ? N6 C12 1.347(6) . ? N6 H6A 0.8800 . ? N7 C14 1.359(5) . ? N8 C15 1.348(5) . ? N8 C19 1.356(5) . ? N9 N10 1.344(5) . ? N9 C20 1.349(5) . ? N10 C22 1.351(6) . ? N10 H10A 0.8800 . ? N100 C101 1.131(8) . ? N101 C111 1.103(8) . ? C1 C2 1.370(7) . ? C1 H1B 0.9500 . ? C2 C3 1.385(6) . ? C2 H2A 0.9500 . ? C3 C4 1.462(6) . ? C4 C5 1.388(6) . ? C5 C6 1.381(7) . ? C5 H5B 0.9500 . ? C6 C7 1.374(7) . ? C6 H6B 0.9500 . ? C7 C8 1.391(6) . ? C7 H7A 0.9500 . ? C8 C9 1.448(6) . ? C9 C10 1.393(6) . ? C10 C11 1.360(7) . ? C10 H10B 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.355(7) . ? C12 H12A 0.9500 . ? C13 C14 1.385(6) . ? C13 H13A 0.9500 . ? C14 C15 1.453(6) . ? C15 C16 1.398(6) . ? C16 C17 1.385(7) . ? C16 H16A 0.9500 . ? C17 C18 1.385(7) . ? C17 H17A 0.9500 . ? C18 C19 1.384(6) . ? C18 H18A 0.9500 . ? C19 C20 1.461(6) . ? C20 C21 1.397(6) . ? C21 C22 1.363(7) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C100 C101 1.453(10) . ? C100 H1F 0.9800 . ? C100 H1D 0.9800 . ? C100 H1C 0.9800 . ? C02 C03 1.53(2) . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C02 H02C 0.9800 . ? C03 H03A 0.9900 . ? C03 H03B 0.9900 . ? C04 C05 1.59(2) . ? C04 H04A 0.9900 . ? C04 H04B 0.9900 . ? C05 H05A 0.9800 . ? C05 H05B 0.9800 . ? C05 H05C 0.9800 . ? C02' C03' 1.574(18) . ? C02' H02D 0.9800 . ? C02' H02E 0.9800 . ? C02' H02F 0.9800 . ? C03' H03C 0.9900 . ? C03' H03D 0.9900 . ? C04' C05' 1.58(2) . ? C04' H04C 0.9900 . ? C04' H04D 0.9900 . ? C05' H05D 0.9800 . ? C05' H05E 0.9800 . ? C05' H05F 0.9800 . ? C106 C107 1.483(10) . ? C106 H10C 0.9800 . ? C106 H10D 0.9800 . ? C106 H10E 0.9800 . ? C107 H10F 0.9900 . ? C107 H10G 0.9900 . ? C108 C109 1.476(10) . ? C108 H10H 0.9900 . ? C108 H10I 0.9900 . ? C109 H10J 0.9800 . ? C109 H10K 0.9800 . ? C109 H10L 0.9800 . ? C110 C111 1.43(2) . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C110 H11D 0.9800 . ? C10' C111 1.51(2) . ? C10' H10M 0.9800 . ? C10' H10N 0.9800 . ? C10' H10O 0.9800 . ? 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 N8 Ru1 N3 177.74(13) . . ? N8 Ru1 N9 77.19(13) . . ? N3 Ru1 N9 102.77(13) . . ? N8 Ru1 N7 77.13(13) . . ? N3 Ru1 N7 102.99(13) . . ? N9 Ru1 N7 154.20(14) . . ? N8 Ru1 N2 105.19(13) . . ? N3 Ru1 N2 77.07(13) . . ? N9 Ru1 N2 90.60(13) . . ? N7 Ru1 N2 93.77(13) . . ? N8 Ru1 N4 100.80(13) . . ? N3 Ru1 N4 76.94(14) . . ? N9 Ru1 N4 93.98(13) . . ? N7 Ru1 N4 93.15(13) . . ? N2 Ru1 N4 153.98(14) . . ? F6 P1 F4 92.5(2) . . ? F6 P1 F2 91.5(2) . . ? F4 P1 F2 91.9(2) . . ? F6 P1 F5 89.9(2) . . ? F4 P1 F5 89.9(2) . . ? F2 P1 F5 177.7(2) . . ? F6 P1 F3 177.4(2) . . ? F4 P1 F3 90.02(19) . . ? F2 P1 F3 89.2(2) . . ? F5 P1 F3 89.4(2) . . ? F6 P1 F1 90.4(2) . . ? F4 P1 F1 176.0(2) . . ? F2 P1 F1 90.7(2) . . ? F5 P1 F1 87.45(17) . . ? F3 P1 F1 86.99(17) . . ? F10' P2 F12 147.2(6) . . ? F10' P2 F9' 102.9(5) . . ? F12 P2 F9' 69.7(4) . . ? F10' P2 F7 113.0(5) . . ? F12 P2 F7 98.6(4) . . ? F9' P2 F7 86.4(3) . . ? F10' P2 F8 92.4(4) . . ? F12 P2 F8 95.7(3) . . ? F9' P2 F8 164.4(4) . . ? F7 P2 F8 90.46(18) . . ? F10' P2 F11 54.8(5) . . ? F12 P2 F11 93.1(4) . . ? F9' P2 F11 93.8(4) . . ? F7 P2 F11 167.6(3) . . ? F8 P2 F11 92.6(3) . . ? F10' P2 F11' 96.9(5) . . ? F12 P2 F11' 51.9(4) . . ? F9' P2 F11' 87.3(4) . . ? F7 P2 F11' 150.0(4) . . ? F8 P2 F11' 87.8(3) . . ? F11 P2 F11' 42.3(4) . . ? F10' P2 F10 33.4(4) . . ? F12 P2 F10 175.6(4) . . ? F9' P2 F10 106.1(4) . . ? F7 P2 F10 80.0(3) . . ? F8 P2 F10 88.4(2) . . ? F11 P2 F10 88.1(3) . . ? F11' P2 F10 129.9(4) . . ? F10' P2 F9 81.2(4) . . ? F12 P2 F9 91.7(4) . . ? F9' P2 F9 22.8(3) . . ? F7 P2 F9 88.5(2) . . ? F8 P2 F9 172.5(3) . . ? F11 P2 F9 86.9(3) . . ? F11' P2 F9 96.7(4) . . ? F10 P2 F9 84.1(3) . . ? F10' P2 F12' 174.8(5) . . ? F12 P2 F12' 32.5(4) . . ? F9' P2 F12' 81.9(5) . . ? F7 P2 F12' 69.1(4) . . ? F8 P2 F12' 82.7(4) . . ? F11 P2 F12' 123.3(5) . . ? F11' P2 F12' 81.0(5) . . ? F10 P2 F12' 147.6(4) . . ? F9 P2 F12' 103.8(4) . . ? C04 O1 C03' 85.1(10) . . ? C04 O1 C04' 27.4(9) . . ? C03' O1 C04' 111.2(10) . . ? C04 O1 C03 112.1(11) . . ? C03' O1 C03 27.0(8) . . ? C04' O1 C03 137.8(9) . . ? C108 O2 C107 112.3(5) . . ? C1 N1 N2 110.2(4) . . ? C1 N1 H1A 124.9 . . ? N2 N1 H1A 124.9 . . ? N1 N2 C3 105.9(3) . . ? N1 N2 Ru1 138.5(3) . . ? C3 N2 Ru1 115.3(3) . . ? C4 N3 C8 120.7(4) . . ? C4 N3 Ru1 119.9(3) . . ? C8 N3 Ru1 119.4(3) . . ? N5 N4 C9 105.7(3) . . ? N5 N4 Ru1 138.7(3) . . ? C9 N4 Ru1 115.7(3) . . ? C11 N5 N4 110.4(4) . . ? C11 N5 H5A 124.8 . . ? N4 N5 H5A 124.8 . . ? N7 N6 C12 111.0(4) . . ? N7 N6 H6A 124.5 . . ? C12 N6 H6A 124.5 . . ? N6 N7 C14 105.2(3) . . ? N6 N7 Ru1 139.1(3) . . ? C14 N7 Ru1 115.6(3) . . ? C15 N8 C19 121.0(4) . . ? C15 N8 Ru1 119.5(3) . . ? C19 N8 Ru1 119.5(3) . . ? N10 N9 C20 106.0(3) . . ? N10 N9 Ru1 137.8(3) . . ? C20 N9 Ru1 116.0(3) . . ? N9 N10 C22 110.7(4) . . ? N9 N10 H10A 124.7 . . ? C22 N10 H10A 124.7 . . ? N1 C1 C2 108.9(4) . . ? N1 C1 H1B 125.5 . . ? C2 C1 H1B 125.5 . . ? C1 C2 C3 104.6(4) . . ? C1 C2 H2A 127.7 . . ? C3 C2 H2A 127.7 . . ? N2 C3 C2 110.4(4) . . ? N2 C3 C4 115.7(3) . . ? C2 C3 C4 133.9(4) . . ? N3 C4 C5 121.0(4) . . ? N3 C4 C3 111.9(3) . . ? C5 C4 C3 127.2(4) . . ? C6 C5 C4 118.7(4) . . ? C6 C5 H5B 120.6 . . ? C4 C5 H5B 120.6 . . ? C7 C6 C5 120.3(4) . . ? C7 C6 H6B 119.9 . . ? C5 C6 H6B 119.9 . . ? C6 C7 C8 119.5(5) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? N3 C8 C7 119.8(4) . . ? N3 C8 C9 111.9(4) . . ? C7 C8 C9 128.2(4) . . ? N4 C9 C10 110.4(4) . . ? N4 C9 C8 115.9(4) . . ? C10 C9 C8 133.7(4) . . ? C11 C10 C9 104.6(4) . . ? C11 C10 H10B 127.7 . . ? C9 C10 H10B 127.7 . . ? N5 C11 C10 109.0(4) . . ? N5 C11 H11A 125.5 . . ? C10 C11 H11A 125.5 . . ? N6 C12 C13 108.2(4) . . ? N6 C12 H12A 125.9 . . ? C13 C12 H12A 125.9 . . ? C12 C13 C14 105.4(4) . . ? C12 C13 H13A 127.3 . . ? C14 C13 H13A 127.3 . . ? N7 C14 C13 110.2(4) . . ? N7 C14 C15 115.3(4) . . ? C13 C14 C15 134.5(4) . . ? N8 C15 C16 120.7(4) . . ? N8 C15 C14 112.4(4) . . ? C16 C15 C14 126.9(4) . . ? C17 C16 C15 118.0(4) . . ? C17 C16 H16A 121.0 . . ? C15 C16 H16A 121.0 . . ? C18 C17 C16 121.0(4) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? N8 C19 C18 120.5(4) . . ? N8 C19 C20 111.9(3) . . ? C18 C19 C20 127.6(4) . . ? N9 C20 C21 110.1(4) . . ? N9 C20 C19 115.4(3) . . ? C21 C20 C19 134.5(4) . . ? C22 C21 C20 105.2(4) . . ? C22 C21 H21A 127.4 . . ? C20 C21 H21A 127.4 . . ? N10 C22 C21 108.2(4) . . ? N10 C22 H22A 125.9 . . ? C21 C22 H22A 125.9 . . ? C101 C100 H1F 109.5 . . ? C101 C100 H1D 109.5 . . ? H1F C100 H1D 109.5 . . ? C101 C100 H1C 109.5 . . ? H1F C100 H1C 109.5 . . ? H1D C100 H1C 109.5 . . ? N100 C101 C100 179.0(8) . . ? C03 C02 H02A 109.5 . . ? C03 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? C03 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? C02 C03 O1 115.0(12) . . ? C02 C03 H03A 108.5 . . ? O1 C03 H03A 108.5 . . ? C02 C03 H03B 108.5 . . ? O1 C03 H03B 108.5 . . ? H03A C03 H03B 107.5 . . ? O1 C04 C05 100.2(13) . . ? O1 C04 H04A 111.7 . . ? C05 C04 H04A 111.7 . . ? O1 C04 H04B 111.7 . . ? C05 C04 H04B 111.7 . . ? H04A C04 H04B 109.5 . . ? C04 C05 H05A 109.5 . . ? C04 C05 H05B 109.5 . . ? H05A C05 H05B 109.5 . . ? C04 C05 H05C 109.5 . . ? H05A C05 H05C 109.5 . . ? H05B C05 H05C 109.5 . . ? C03' C02' H02D 109.5 . . ? C03' C02' H02E 109.5 . . ? H02D C02' H02E 109.5 . . ? C03' C02' H02F 109.5 . . ? H02D C02' H02F 109.5 . . ? H02E C02' H02F 109.5 . . ? O1 C03' C02' 101.6(11) . . ? O1 C03' H03C 111.4 . . ? C02' C03' H03C 111.4 . . ? O1 C03' H03D 111.4 . . ? C02' C03' H03D 111.4 . . ? H03C C03' H03D 109.3 . . ? C05' C04' O1 108.5(10) . . ? C05' C04' H04C 110.0 . . ? O1 C04' H04C 110.0 . . ? C05' C04' H04D 110.0 . . ? O1 C04' H04D 110.0 . . ? H04C C04' H04D 108.4 . . ? C04' C05' H05D 109.5 . . ? C04' C05' H05E 109.5 . . ? H05D C05' H05E 109.5 . . ? C04' C05' H05F 109.5 . . ? H05D C05' H05F 109.5 . . ? H05E C05' H05F 109.5 . . ? C107 C106 H10C 109.5 . . ? C107 C106 H10D 109.5 . . ? H10C C106 H10D 109.5 . . ? C107 C106 H10E 109.5 . . ? H10C C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? O2 C107 C106 108.5(5) . . ? O2 C107 H10F 110.0 . . ? C106 C107 H10F 110.0 . . ? O2 C107 H10G 110.0 . . ? C106 C107 H10G 110.0 . . ? H10F C107 H10G 108.4 . . ? O2 C108 C109 109.0(6) . . ? O2 C108 H10H 109.9 . . ? C109 C108 H10H 109.9 . . ? O2 C108 H10I 109.9 . . ? C109 C108 H10I 109.9 . . ? H10H C108 H10I 108.3 . . ? C108 C109 H10J 109.5 . . ? C108 C109 H10K 109.5 . . ? H10J C109 H10K 109.5 . . ? C108 C109 H10L 109.5 . . ? H10J C109 H10L 109.5 . . ? H10K C109 H10L 109.5 . . ? C111 C110 H11B 109.5 . . ? C111 C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C111 C110 H11D 109.5 . . ? H11B C110 H11D 109.5 . . ? H11C C110 H11D 109.5 . . ? C111 C10' H10M 109.5 . . ? C111 C10' H10N 109.5 . . ? H10M C10' H10N 109.5 . . ? C111 C10' H10O 109.5 . . ? H10M C10' H10O 109.5 . . ? H10N C10' H10O 109.5 . . ? N101 C111 C110 168.5(15) . . ? N101 C111 C10' 149.2(14) . . ? C110 C111 C10' 41.7(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.830 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.086 #===END data_RuL1 _database_code_depnum_ccdc_archive 'CCDC 659048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H78 N24 O10 Ru' _chemical_formula_weight 1708.79 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 16.7252(5) _cell_length_b 16.7252(5) _cell_length_c 16.1385(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4514.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 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 62954 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 32.68 _reflns_number_total 8235 _reflns_number_gt 7779 _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^)+(0.1162P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 8235 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.0000 1.0000 1.0000 0.02924(8) Uani 1 4 d S . . N11 N 0.1773(4) 0.6507(4) 0.6668(4) 0.1012(14) Uani 1 1 d . . . C12 C 0.2166(3) 0.6175(2) 0.7316(3) 0.0744(12) Uani 1 1 d . . . C13 C 0.2087(4) 0.5387(3) 0.7482(6) 0.105(2) Uani 1 1 d . . . H13 H 0.2360 0.5150 0.7920 0.125 Uiso 1 1 calc R . . C14 C 0.1560(4) 0.4921(4) 0.6950(6) 0.114(3) Uani 1 1 d . . . H14 H 0.1494 0.4376 0.7039 0.137 Uiso 1 1 calc R . . C15 C 0.1183(6) 0.5278(7) 0.6348(7) 0.139(3) Uani 1 1 d . . . H15 H 0.0838 0.4980 0.6017 0.167 Uiso 1 1 calc R . . C16 C 0.1282(9) 0.6117(6) 0.6178(8) 0.171(5) Uani 1 1 d . . . H16 H 0.1014 0.6369 0.5746 0.205 Uiso 1 1 calc R . . N21 N 0.28454(18) 0.74406(17) 0.7510(2) 0.0585(7) Uani 1 1 d . . . N22 N 0.3350(2) 0.7779(2) 0.8081(3) 0.0720(9) Uani 1 1 d . . . C23 C 0.3484(3) 0.7266(5) 0.8730(3) 0.097(2) Uani 1 1 d . . . H23 H 0.3807 0.7370 0.9187 0.116 Uiso 1 1 calc R . . C24 C 0.3091(4) 0.6621(3) 0.8605(3) 0.0875(17) Uani 1 1 d . . . H24 H 0.3066 0.6176 0.8950 0.105 Uiso 1 1 calc R . . C25 C 0.2692(2) 0.6724(2) 0.7815(2) 0.0611(8) Uani 1 1 d . . . C31 C 0.3676(3) 0.8579(3) 0.7931(5) 0.105(2) Uani 1 1 d . . . H31A H 0.3794 0.8636 0.7345 0.126 Uiso 1 1 calc R . . H31B H 0.4175 0.8635 0.8232 0.126 Uiso 1 1 calc R . . C32 C 0.3112(3) 0.9240(3) 0.8192(4) 0.0794(14) Uani 1 1 d . . . C33 C 0.3120(2) 0.9437(3) 0.9081(3) 0.0780(13) Uani 1 1 d . . . H33 H 0.3439 0.9161 0.9456 0.094 Uiso 1 1 calc R . . C34 C 0.2626(2) 1.0057(2) 0.9325(3) 0.0650(9) Uani 1 1 d . . . H34 H 0.2624 1.0208 0.9880 0.078 Uiso 1 1 calc R . . C35 C 0.21309(18) 1.04638(17) 0.87731(19) 0.0487(6) Uani 1 1 d . . . C36 C 0.2119(3) 1.0226(2) 0.7944(2) 0.0649(10) Uani 1 1 d . . . H36 H 0.1780 1.0484 0.7573 0.078 Uiso 1 1 calc R . . C37 C 0.2608(3) 0.9608(3) 0.7665(3) 0.0757(15) Uani 1 1 d . . . H37 H 0.2586 0.9449 0.7113 0.091 Uiso 1 1 calc R . . C38 C 0.16291(19) 1.11764(18) 0.9029(2) 0.0465(6) Uani 1 1 d . . . H38A H 0.1891 1.1664 0.8851 0.056 Uiso 1 1 calc R . . H38B H 0.1113 1.1148 0.8757 0.056 Uiso 1 1 calc R . . N41 N 0.09787(11) 1.07199(11) 1.03014(13) 0.0331(3) Uani 1 1 d . . . N42 N 0.15116(11) 1.12012(11) 0.9920(2) 0.0398(5) Uani 1 1 d . . . C43 C 0.19891(16) 1.15758(17) 1.0481(2) 0.0496(6) Uani 1 1 d . . . H43 H 0.2405 1.1926 1.0358 0.060 Uiso 1 1 calc R . . C44 C 0.17551(17) 1.13513(19) 1.1251(2) 0.0470(6) Uani 1 1 d . . . H44 H 0.1967 1.1516 1.1756 0.056 Uiso 1 1 calc R . . C45 C 0.11173(14) 1.08111(15) 1.11191(15) 0.0384(4) Uani 1 1 d . . . N51 N 0.0000 1.0000 1.12606(13) 0.0333(4) Uani 1 2 d S . . C52 C 0.05738(15) 1.03933(16) 1.16782(15) 0.0400(4) Uani 1 1 d . . . C53 C 0.0609(2) 1.0398(2) 1.25416(18) 0.0550(7) Uani 1 1 d . . . H53 H 0.1020 1.0656 1.2823 0.066 Uiso 1 1 calc R . . C54 C 0.0000 1.0000 1.29641(19) 0.0651(11) Uani 1 2 d S . . H54 H 0.0000 1.0000 1.3540 0.078 Uiso 1 2 calc SR . . O100 O 0.3157 1.2810 0.91267(19) 0.134(4) Uiso 0.50 1 d PR . . O101 O 0.0601 0.3515 0.48854(19) 0.347(16) Uiso 0.50 1 d 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 Ru1 0.02989(9) 0.02989(9) 0.02795(12) 0.000 0.000 0.000 N11 0.118(4) 0.098(3) 0.087(3) 0.001(3) -0.005(3) -0.005(3) C12 0.063(2) 0.0603(19) 0.100(3) -0.007(2) 0.035(2) 0.0018(15) C13 0.075(3) 0.056(2) 0.183(7) 0.013(3) 0.033(4) 0.001(2) C14 0.100(4) 0.069(3) 0.173(8) -0.006(4) 0.054(5) -0.010(3) C15 0.110(6) 0.160(9) 0.148(8) -0.022(7) 0.028(6) -0.032(6) C16 0.218(12) 0.113(7) 0.183(11) 0.001(7) -0.086(10) -0.029(7) N21 0.0560(14) 0.0532(13) 0.0663(17) -0.0080(12) 0.0217(12) 0.0078(10) N22 0.0617(17) 0.076(2) 0.078(2) -0.0300(17) 0.0218(15) 0.0068(14) C23 0.071(3) 0.167(6) 0.053(2) -0.028(3) 0.0086(18) 0.007(3) C24 0.110(4) 0.082(3) 0.071(3) 0.023(2) 0.037(3) 0.040(3) C25 0.0624(18) 0.0594(17) 0.0615(18) 0.0000(14) 0.0215(15) 0.0128(14) C31 0.077(3) 0.082(3) 0.156(6) -0.062(3) 0.065(3) -0.021(2) C32 0.062(2) 0.076(2) 0.101(3) -0.041(2) 0.042(2) -0.0145(18) C33 0.0552(18) 0.079(3) 0.100(3) -0.042(2) 0.0011(19) 0.0138(17) C34 0.0544(16) 0.068(2) 0.073(2) -0.0305(18) 0.0062(15) 0.0107(14) C35 0.0501(13) 0.0448(12) 0.0512(14) -0.0093(10) 0.0212(11) -0.0149(10) C36 0.087(2) 0.0564(16) 0.0510(17) -0.0082(13) 0.0302(16) -0.0297(16) C37 0.090(3) 0.073(2) 0.064(2) -0.0225(19) 0.040(2) -0.038(2) C38 0.0501(14) 0.0386(12) 0.0508(15) 0.0023(11) 0.0158(12) -0.0091(10) N41 0.0299(7) 0.0330(7) 0.0364(7) -0.0066(6) 0.0012(6) -0.0001(6) N42 0.0363(7) 0.0338(7) 0.0494(14) -0.0098(10) 0.0047(10) -0.0039(5) C43 0.0355(11) 0.0421(12) 0.0713(19) -0.0161(12) 0.0020(11) -0.0073(9) C44 0.0374(12) 0.0486(14) 0.0550(16) -0.0196(12) -0.0072(11) -0.0010(10) C45 0.0333(9) 0.0437(11) 0.0382(10) -0.0088(9) -0.0046(8) 0.0056(8) N51 0.0359(19) 0.0359(19) 0.0280(8) 0.000 0.000 0.0086(18) C52 0.0375(10) 0.0492(12) 0.0332(10) -0.0056(9) -0.0051(8) 0.0078(9) C53 0.0595(16) 0.0706(19) 0.0350(12) -0.0075(12) -0.0103(11) 0.0039(14) C54 0.086(5) 0.082(5) 0.0266(12) 0.000 0.000 -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N51 2.034(2) 2_467 ? Ru1 N51 2.034(2) . ? Ru1 N41 2.0894(19) . ? Ru1 N41 2.0894(19) 4_667 ? Ru1 N41 2.0894(19) 3_575 ? Ru1 N41 2.0894(19) 2_467 ? N11 C16 1.313(10) . ? N11 C12 1.355(8) . ? C12 C13 1.352(7) . ? C12 C25 1.504(7) . ? C13 C14 1.456(12) . ? C14 C15 1.304(13) . ? C15 C16 1.440(14) . ? N21 C25 1.321(5) . ? N21 N22 1.371(5) . ? N22 C23 1.374(8) . ? N22 C31 1.464(7) . ? C23 C24 1.280(9) . ? C24 C25 1.449(7) . ? C31 C32 1.514(6) . ? C32 C37 1.346(8) . ? C32 C33 1.472(7) . ? C33 C34 1.383(5) . ? C34 C35 1.394(6) . ? C35 C36 1.396(4) . ? C35 C38 1.515(4) . ? C36 C37 1.393(7) . ? C38 N42 1.452(5) . ? N41 C45 1.349(3) . ? N41 N42 1.349(3) . ? N42 C43 1.360(4) . ? C43 C44 1.356(5) . ? C44 C45 1.414(4) . ? C45 C52 1.459(4) . ? N51 C52 1.345(3) . ? N51 C52 1.345(3) 3_575 ? C52 C53 1.395(4) . ? C53 C54 1.395(4) . ? C54 C53 1.395(4) 3_575 ? 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 N51 Ru1 N51 180.0 2_467 . ? N51 Ru1 N41 103.46(6) 2_467 . ? N51 Ru1 N41 76.54(6) . . ? N51 Ru1 N41 76.54(6) 2_467 4_667 ? N51 Ru1 N41 103.46(6) . 4_667 ? N41 Ru1 N41 93.11(3) . 4_667 ? N51 Ru1 N41 103.46(6) 2_467 3_575 ? N51 Ru1 N41 76.54(6) . 3_575 ? N41 Ru1 N41 153.08(11) . 3_575 ? N41 Ru1 N41 93.11(3) 4_667 3_575 ? N51 Ru1 N41 76.54(6) 2_467 2_467 ? N51 Ru1 N41 103.46(6) . 2_467 ? N41 Ru1 N41 93.11(3) . 2_467 ? N41 Ru1 N41 153.08(11) 4_667 2_467 ? N41 Ru1 N41 93.11(3) 3_575 2_467 ? C16 N11 C12 124.4(7) . . ? C13 C12 N11 120.3(6) . . ? C13 C12 C25 123.1(6) . . ? N11 C12 C25 116.6(4) . . ? C12 C13 C14 117.7(8) . . ? C15 C14 C13 119.2(7) . . ? C14 C15 C16 122.1(10) . . ? N11 C16 C15 116.2(10) . . ? C25 N21 N22 104.2(4) . . ? N21 N22 C23 110.8(4) . . ? N21 N22 C31 119.7(5) . . ? C23 N22 C31 129.5(6) . . ? C24 C23 N22 108.8(5) . . ? C23 C24 C25 106.0(4) . . ? N21 C25 C24 110.3(4) . . ? N21 C25 C12 117.9(4) . . ? C24 C25 C12 131.8(4) . . ? N22 C31 C32 112.8(3) . . ? C37 C32 C33 121.3(4) . . ? C37 C32 C31 123.3(5) . . ? C33 C32 C31 115.4(6) . . ? C34 C33 C32 116.1(5) . . ? C33 C34 C35 122.6(4) . . ? C34 C35 C36 118.8(3) . . ? C34 C35 C38 122.6(3) . . ? C36 C35 C38 118.5(4) . . ? C37 C36 C35 120.8(5) . . ? C32 C37 C36 120.2(4) . . ? N42 C38 C35 111.6(3) . . ? C45 N41 N42 105.4(2) . . ? C45 N41 Ru1 115.32(17) . . ? N42 N41 Ru1 139.0(2) . . ? N41 N42 C43 111.1(3) . . ? N41 N42 C38 121.6(2) . . ? C43 N42 C38 126.4(2) . . ? C44 C43 N42 108.2(3) . . ? C43 C44 C45 104.9(3) . . ? N41 C45 C44 110.5(3) . . ? N41 C45 C52 116.4(2) . . ? C44 C45 C52 133.1(3) . . ? C52 N51 C52 119.8(3) . 3_575 ? C52 N51 Ru1 120.08(13) . . ? C52 N51 Ru1 120.08(13) 3_575 . ? N51 C52 C53 122.2(3) . . ? N51 C52 C45 111.7(2) . . ? C53 C52 C45 126.1(3) . . ? C54 C53 C52 117.1(3) . . ? C53 C54 C53 121.5(3) 3_575 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 32.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.026 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.133 #===END data_RuL2 _database_code_depnum_ccdc_archive 'CCDC 659049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H84 F12 N22 P2 Ru' _chemical_formula_weight 2177.06 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 orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 27.3364(11) _cell_length_b 15.9057(6) _cell_length_c 24.5589(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10678.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 0.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9150 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 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 175242 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9418 _reflns_number_gt 7566 _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^)+(0.1131P)^2^+11.5267P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9418 _refine_ls_number_parameters 723 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1837 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.2500 0.0000 0.467101(15) 0.03041(15) Uani 1 2 d S . . N11 N -0.07766(12) 0.3146(2) 0.40343(13) 0.0493(8) Uani 1 1 d . . . C12 C -0.08411(11) 0.2569(2) 0.36477(13) 0.0330(7) Uani 1 1 d . . . C13 C -0.11690(12) 0.2684(2) 0.32204(13) 0.0354(8) Uani 1 1 d . . . H13A H -0.1210 0.2259 0.2953 0.042 Uiso 1 1 calc R . . C14 C -0.14327(13) 0.3420(2) 0.31891(14) 0.0388(8) Uani 1 1 d . . . H14A H -0.1660 0.3505 0.2902 0.047 Uiso 1 1 calc R . . C15 C -0.13633(14) 0.4029(2) 0.35785(16) 0.0472(9) Uani 1 1 d . . . H15A H -0.1536 0.4547 0.3565 0.057 Uiso 1 1 calc R . . C16 C -0.10318(17) 0.3861(3) 0.39922(18) 0.0588(12) Uani 1 1 d . . . H16A H -0.0983 0.4279 0.4263 0.071 Uiso 1 1 calc R . . N21 N -0.06318(10) 0.11892(17) 0.33237(11) 0.0333(6) Uani 1 1 d . . . C22 C -0.03503(12) 0.0497(2) 0.33354(13) 0.0341(7) Uani 1 1 d . . . C23 C 0.00184(12) 0.0381(2) 0.37124(14) 0.0366(8) Uani 1 1 d . . . H23A H 0.0212 -0.0115 0.3703 0.044 Uiso 1 1 calc R . . C24 C 0.01056(12) 0.0992(2) 0.41046(14) 0.0358(8) Uani 1 1 d . . . C25 C -0.01785(12) 0.1714(2) 0.40829(13) 0.0353(7) Uani 1 1 d . . . H25A H -0.0127 0.2154 0.4339 0.042 Uiso 1 1 calc R . . C26 C -0.05384(11) 0.1793(2) 0.36857(13) 0.0326(7) Uani 1 1 d . . . N31 N -0.00847(10) -0.07287(19) 0.28497(12) 0.0394(7) Uani 1 1 d . . . C32 C -0.04471(12) -0.0170(2) 0.29265(13) 0.0328(7) Uani 1 1 d . . . C33 C -0.08906(13) -0.0227(2) 0.26542(14) 0.0374(8) Uani 1 1 d . . . H33A H -0.1136 0.0188 0.2706 0.045 Uiso 1 1 calc R . . C34 C -0.09686(13) -0.0892(2) 0.23090(14) 0.0405(8) Uani 1 1 d . . . H34A H -0.1272 -0.0948 0.2124 0.049 Uiso 1 1 calc R . . C35 C -0.06063(14) -0.1473(2) 0.22345(14) 0.0402(8) Uani 1 1 d . . . H35A H -0.0654 -0.1944 0.2003 0.048 Uiso 1 1 calc R . . C36 C -0.01693(14) -0.1355(2) 0.25055(15) 0.0426(8) Uani 1 1 d . . . H36A H 0.0087 -0.1747 0.2442 0.051 Uiso 1 1 calc R . . C41 C 0.07444(13) 0.1517(2) 0.47497(14) 0.0390(8) Uani 1 1 d . . . H41A H 0.0678 0.2075 0.4634 0.047 Uiso 1 1 calc R . . C42 C 0.04816(12) 0.0847(2) 0.45301(14) 0.0366(8) Uani 1 1 d . . . C43 C 0.05808(14) 0.0039(2) 0.47158(15) 0.0399(8) Uani 1 1 d . . . H43A H 0.0402 -0.0423 0.4572 0.048 Uiso 1 1 calc R . . C44 C 0.09350(13) -0.0102(2) 0.51067(15) 0.0398(8) Uani 1 1 d . . . H44A H 0.0997 -0.0658 0.5230 0.048 Uiso 1 1 calc R . . C45 C 0.12005(11) 0.0563(2) 0.53207(12) 0.0328(7) Uani 1 1 d . . . C46 C 0.11050(13) 0.1367(2) 0.51379(15) 0.0401(8) Uani 1 1 d . . . H46A H 0.1288 0.1825 0.5279 0.048 Uiso 1 1 calc R . . C47 C 0.15873(12) 0.0429(2) 0.57558(13) 0.0345(7) Uani 1 1 d . . . H47A H 0.1843 0.0865 0.5719 0.041 Uiso 1 1 calc R . . H47B H 0.1436 0.0491 0.6120 0.041 Uiso 1 1 calc R . . N51 N 0.21111(9) -0.05973(18) 0.52957(10) 0.0315(6) Uani 1 1 d . . . N52 N 0.18116(9) -0.03969(18) 0.57144(10) 0.0308(6) Uani 1 1 d . . . C53 C 0.17331(12) -0.1071(2) 0.60354(13) 0.0353(8) Uani 1 1 d . . . H53A H 0.1533 -0.1080 0.6352 0.042 Uiso 1 1 calc R . . C54 C 0.19867(12) -0.1736(2) 0.58319(14) 0.0357(7) Uani 1 1 d . . . H54A H 0.1998 -0.2293 0.5971 0.043 Uiso 1 1 calc R . . C55 C 0.22273(12) -0.1418(2) 0.53715(13) 0.0323(7) Uani 1 1 d . . . N61 N 0.27502(10) -0.11979(18) 0.46399(11) 0.0341(6) Uani 1 1 d . . . C62 C 0.25696(12) -0.1780(2) 0.49845(15) 0.0369(8) Uani 1 1 d . . . C63 C 0.27030(16) -0.2616(2) 0.49383(17) 0.0484(9) Uani 1 1 d . . . H63A H 0.2582 -0.3022 0.5188 0.058 Uiso 1 1 calc R . . C64 C 0.30175(17) -0.2852(3) 0.45206(19) 0.0582(11) Uani 1 1 d . . . H64A H 0.3107 -0.3425 0.4478 0.070 Uiso 1 1 calc R . . C65 C 0.31987(16) -0.2256(3) 0.41680(17) 0.0526(10) Uani 1 1 d . . . H65A H 0.3414 -0.2412 0.3881 0.063 Uiso 1 1 calc R . . C66 C 0.30620(13) -0.1424(2) 0.42386(14) 0.0401(8) Uani 1 1 d . . . N71 N 0.30293(12) 0.00490(18) 0.40509(12) 0.0388(7) Uani 1 1 d . . . N72 N 0.32150(14) 0.0584(2) 0.36792(13) 0.0531(9) Uani 1 1 d . . . C73 C 0.3504(2) 0.0173(3) 0.3325(2) 0.0795(18) Uani 1 1 d . . . H73A H 0.3677 0.0422 0.3030 0.095 Uiso 1 1 calc R . . C74 C 0.35089(19) -0.0644(3) 0.34561(19) 0.0686(14) Uani 1 1 d . . . H74A H 0.3680 -0.1084 0.3276 0.082 Uiso 1 1 calc R . . C75 C 0.32121(14) -0.0711(2) 0.39100(15) 0.0441(9) Uani 1 1 d . . . C81 C 0.31642(16) 0.1504(2) 0.37253(17) 0.0503(10) Uani 1 1 d . . . H81A H 0.2903 0.1638 0.3990 0.060 Uiso 1 1 calc R . . H81B H 0.3068 0.1740 0.3368 0.060 Uiso 1 1 calc R . . C82 C 0.36333(15) 0.1901(2) 0.39066(15) 0.0450(9) Uani 1 1 d . . . C83 C 0.40074(17) 0.2056(3) 0.35317(17) 0.0612(12) Uani 1 1 d . . . H83A H 0.3957 0.1933 0.3157 0.073 Uiso 1 1 calc R . . C84 C 0.44432(16) 0.2381(3) 0.36984(16) 0.0585(11) Uani 1 1 d . . . H84A H 0.4694 0.2469 0.3437 0.070 Uiso 1 1 calc R . . C85 C 0.45317(14) 0.2591(2) 0.42440(15) 0.0441(9) Uani 1 1 d . . . C86 C 0.41554(14) 0.2453(2) 0.46145(15) 0.0443(9) Uani 1 1 d . . . H86A H 0.4200 0.2593 0.4987 0.053 Uiso 1 1 calc R . . C87 C 0.37161(15) 0.2113(2) 0.44433(15) 0.0457(9) Uani 1 1 d . . . H87A H 0.3464 0.2023 0.4703 0.055 Uiso 1 1 calc R . . N91 N 0.63119(11) 0.2373(2) 0.36152(12) 0.0446(7) Uani 1 1 d . . . C92 C 0.63125(13) 0.3056(2) 0.39393(14) 0.0416(8) Uani 1 1 d . . . C93 C 0.67064(14) 0.3599(3) 0.39676(15) 0.0470(9) Uani 1 1 d . . . H93A H 0.6701 0.4068 0.4207 0.056 Uiso 1 1 calc R . . C94 C 0.71082(14) 0.3445(3) 0.36407(16) 0.0513(10) Uani 1 1 d . . . H94A H 0.7380 0.3817 0.3645 0.062 Uiso 1 1 calc R . . C95 C 0.71096(14) 0.2749(3) 0.33086(15) 0.0501(10) Uani 1 1 d . . . H95A H 0.7383 0.2631 0.3083 0.060 Uiso 1 1 calc R . . C96 C 0.67123(14) 0.2231(3) 0.33085(15) 0.0486(10) Uani 1 1 d . . . H96A H 0.6718 0.1748 0.3082 0.058 Uiso 1 1 calc R . . N101 N 0.58925(11) 0.3744(2) 0.46848(12) 0.0430(7) Uani 1 1 d . . . C102 C 0.54832(14) 0.3876(2) 0.49830(15) 0.0433(9) Uani 1 1 d . . . C103 C 0.50361(13) 0.3514(2) 0.48536(15) 0.0437(9) Uani 1 1 d . . . H10B H 0.4755 0.3638 0.5066 0.052 Uiso 1 1 calc R . . C104 C 0.50013(14) 0.2968(2) 0.44104(14) 0.0425(9) Uani 1 1 d . . . C105 C 0.54282(13) 0.2802(2) 0.41238(14) 0.0425(9) Uani 1 1 d . . . H10A H 0.5425 0.2411 0.3832 0.051 Uiso 1 1 calc R . . C106 C 0.58589(13) 0.3206(2) 0.42625(14) 0.0409(8) Uani 1 1 d . . . N111 N 0.51206(14) 0.4555(2) 0.57550(15) 0.0596(9) Uani 1 1 d . . . C112 C 0.55319(16) 0.4422(3) 0.54695(17) 0.0522(10) Uani 1 1 d . . . C113 C 0.5969(2) 0.4771(4) 0.5615(2) 0.0859(18) Uani 1 1 d . . . H11A H 0.6251 0.4687 0.5396 0.103 Uiso 1 1 calc R . . C114 C 0.5996(3) 0.5247(5) 0.6083(3) 0.111(2) Uani 1 1 d . . . H11D H 0.6297 0.5499 0.6188 0.133 Uiso 1 1 calc R . . C115 C 0.5586(2) 0.5352(4) 0.6394(2) 0.0884(17) Uani 1 1 d . . . H11C H 0.5599 0.5651 0.6728 0.106 Uiso 1 1 calc R . . C116 C 0.5157(2) 0.5014(3) 0.6210(2) 0.0715(15) Uani 1 1 d . . . H11B H 0.4869 0.5110 0.6417 0.086 Uiso 1 1 calc R . . P1 P 0.26872(13) 0.1429(2) 0.20151(13) 0.0817(8) Uani 0.50 1 d P . . P2 P 0.2500 0.0000 0.73121(5) 0.0335(3) Uani 1 2 d S . . F1 F 0.2923(3) 0.1646(5) 0.1449(3) 0.0946(19) Uani 0.50 1 d P . . F2 F 0.2940(3) 0.0621(8) 0.2038(4) 0.163(5) Uani 0.50 1 d P . . F3 F 0.2453(3) 0.2350(5) 0.2045(3) 0.105(2) Uani 0.50 1 d P . . F4 F 0.2198(3) 0.1115(4) 0.1739(3) 0.098(2) Uani 0.50 1 d P . . F5 F 0.2468(3) 0.1212(6) 0.2572(3) 0.126(3) Uani 0.50 1 d P . . F6 F 0.3210(2) 0.1675(4) 0.2281(2) 0.0785(17) Uani 0.50 1 d P . . F7 F 0.21046(16) 0.01644(19) 0.68677(17) 0.1162(16) Uani 1 1 d . . . F8 F 0.28884(13) -0.0137(2) 0.77787(16) 0.0990(12) Uani 1 1 d . . . F9 F 0.26326(9) 0.09790(14) 0.73140(9) 0.0551(6) Uani 1 1 d . . . C201 C 0.0236(4) 0.2500 0.2500 0.133(4) Uani 1 2 d SD . . H201 H -0.0112 0.2500 0.2500 0.159 Uiso 1 2 calc SR . . C202 C 0.0470(3) 0.3070(6) 0.2852(4) 0.147(3) Uani 1 1 d D . . H202 H 0.0289 0.3458 0.3066 0.177 Uiso 1 1 calc R . . C203 C 0.0974(4) 0.3039(6) 0.2873(5) 0.178(6) Uani 1 1 d D . . H203 H 0.1153 0.3367 0.3127 0.213 Uiso 1 1 calc R . . C204 C 0.1216(6) 0.2500 0.2500 0.231(15) Uani 1 2 d SD . . H204 H 0.1563 0.2500 0.2500 0.278 Uiso 1 2 calc SR . . 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 0.0341(2) 0.0288(2) 0.0283(2) 0.000 0.000 0.00238(15) N11 0.058(2) 0.0430(18) 0.0474(18) -0.0133(15) -0.0222(15) 0.0142(16) C12 0.0334(17) 0.0356(18) 0.0299(16) 0.0002(14) -0.0037(13) 0.0047(14) C13 0.0422(19) 0.0386(19) 0.0254(16) -0.0002(14) -0.0028(13) 0.0076(15) C14 0.0421(19) 0.045(2) 0.0292(17) 0.0032(15) -0.0032(14) 0.0094(16) C15 0.053(2) 0.039(2) 0.049(2) -0.0023(17) -0.0102(18) 0.0152(18) C16 0.072(3) 0.047(2) 0.058(2) -0.019(2) -0.025(2) 0.020(2) N21 0.0333(14) 0.0362(15) 0.0303(14) -0.0033(12) -0.0068(11) 0.0042(12) C22 0.0317(16) 0.0372(19) 0.0333(17) -0.0024(14) -0.0025(13) 0.0036(15) C23 0.0326(17) 0.0374(19) 0.0397(19) -0.0062(15) -0.0078(14) 0.0067(15) C24 0.0323(17) 0.0382(19) 0.0369(18) -0.0028(15) -0.0082(14) 0.0057(15) C25 0.0361(17) 0.0384(19) 0.0314(17) -0.0039(14) -0.0085(14) 0.0042(15) C26 0.0315(16) 0.0377(18) 0.0284(16) -0.0026(14) -0.0030(13) 0.0035(14) N31 0.0377(15) 0.0413(17) 0.0393(16) -0.0073(13) -0.0035(12) 0.0061(13) C32 0.0322(17) 0.0368(18) 0.0294(16) -0.0005(14) -0.0020(13) 0.0024(14) C33 0.0343(18) 0.045(2) 0.0327(17) -0.0041(15) -0.0051(14) 0.0073(15) C34 0.0406(19) 0.048(2) 0.0329(18) -0.0059(16) -0.0041(14) -0.0026(16) C35 0.054(2) 0.0362(19) 0.0303(17) -0.0033(15) -0.0032(15) -0.0007(17) C36 0.051(2) 0.0374(19) 0.0392(19) -0.0056(16) -0.0032(17) 0.0116(17) C41 0.0378(18) 0.0363(19) 0.0429(19) -0.0081(15) -0.0137(15) 0.0103(15) C42 0.0334(17) 0.0400(19) 0.0364(18) -0.0054(15) -0.0090(14) 0.0078(15) C43 0.0377(19) 0.037(2) 0.045(2) -0.0026(15) -0.0151(16) 0.0003(15) C44 0.0379(19) 0.042(2) 0.040(2) -0.0005(15) -0.0102(16) 0.0024(15) C45 0.0281(16) 0.0402(19) 0.0299(17) -0.0075(14) -0.0040(13) 0.0066(14) C46 0.0362(18) 0.0369(19) 0.047(2) -0.0140(16) -0.0128(16) 0.0053(15) C47 0.0313(16) 0.042(2) 0.0306(17) -0.0051(15) -0.0060(13) 0.0069(15) N51 0.0288(13) 0.0351(15) 0.0305(14) 0.0018(12) -0.0019(11) 0.0038(12) N52 0.0238(12) 0.0414(16) 0.0272(14) -0.0021(12) -0.0038(10) 0.0036(12) C53 0.0308(17) 0.049(2) 0.0262(16) 0.0036(15) -0.0059(13) -0.0026(15) C54 0.0345(17) 0.0379(19) 0.0346(17) 0.0048(15) -0.0049(14) 0.0003(15) C55 0.0297(16) 0.0337(18) 0.0335(17) 0.0024(14) -0.0050(13) -0.0004(14) N61 0.0359(15) 0.0331(15) 0.0332(15) -0.0006(12) 0.0019(12) 0.0025(13) C62 0.0400(18) 0.0337(18) 0.0370(18) 0.0012(15) 0.0026(14) 0.0034(15) C63 0.061(2) 0.034(2) 0.050(2) 0.0041(17) 0.0099(19) 0.0019(18) C64 0.074(3) 0.035(2) 0.065(3) -0.0028(19) 0.018(2) 0.013(2) C65 0.062(3) 0.042(2) 0.053(2) -0.0057(19) 0.017(2) 0.0089(19) C66 0.0435(19) 0.039(2) 0.0382(19) -0.0037(16) 0.0064(15) 0.0015(16) N71 0.0458(17) 0.0355(17) 0.0352(16) -0.0009(13) 0.0033(13) -0.0047(13) N72 0.075(2) 0.0424(18) 0.0414(18) 0.0037(15) 0.0207(17) -0.0077(17) C73 0.123(5) 0.052(3) 0.063(3) -0.002(2) 0.060(3) -0.009(3) C74 0.094(4) 0.051(3) 0.060(3) -0.009(2) 0.042(3) -0.005(2) C75 0.052(2) 0.040(2) 0.0400(19) -0.0081(16) 0.0119(17) -0.0001(17) C81 0.067(3) 0.038(2) 0.046(2) 0.0052(17) 0.0051(19) -0.0055(19) C82 0.058(2) 0.038(2) 0.0398(19) 0.0094(16) 0.0088(17) 0.0011(17) C83 0.069(3) 0.076(3) 0.038(2) 0.004(2) 0.006(2) -0.017(2) C84 0.058(3) 0.079(3) 0.039(2) 0.006(2) 0.0121(18) -0.010(2) C85 0.048(2) 0.046(2) 0.0379(19) 0.0084(16) 0.0088(16) 0.0008(17) C86 0.053(2) 0.045(2) 0.0351(18) 0.0064(16) 0.0092(16) 0.0073(18) C87 0.054(2) 0.042(2) 0.041(2) 0.0054(17) 0.0134(17) 0.0022(18) N91 0.0495(18) 0.0495(19) 0.0350(16) 0.0082(14) 0.0117(13) 0.0103(15) C92 0.045(2) 0.046(2) 0.0335(18) 0.0139(16) 0.0049(15) 0.0076(17) C93 0.046(2) 0.055(2) 0.040(2) 0.0070(17) -0.0007(16) 0.0086(18) C94 0.0377(19) 0.073(3) 0.044(2) 0.016(2) 0.0003(16) 0.0039(19) C95 0.044(2) 0.069(3) 0.037(2) 0.0099(19) 0.0088(16) 0.018(2) C96 0.053(2) 0.054(2) 0.039(2) 0.0084(18) 0.0113(17) 0.0135(19) N101 0.0439(17) 0.0435(18) 0.0415(17) 0.0057(14) 0.0064(13) 0.0078(14) C102 0.049(2) 0.040(2) 0.0414(19) 0.0053(16) 0.0068(16) 0.0087(17) C103 0.046(2) 0.044(2) 0.0407(19) 0.0111(17) 0.0140(16) 0.0118(17) C104 0.048(2) 0.046(2) 0.0328(18) 0.0093(16) 0.0097(15) 0.0063(17) C105 0.048(2) 0.046(2) 0.0338(18) 0.0050(16) 0.0081(16) 0.0079(17) C106 0.047(2) 0.043(2) 0.0326(18) 0.0099(16) 0.0064(15) 0.0103(17) N111 0.071(2) 0.053(2) 0.055(2) -0.0038(17) 0.0191(18) 0.0092(18) C112 0.057(2) 0.048(2) 0.052(2) -0.0036(19) 0.0095(19) 0.013(2) C113 0.059(3) 0.113(4) 0.086(4) -0.050(4) 0.012(3) 0.004(3) C114 0.082(4) 0.138(6) 0.111(5) -0.071(5) 0.000(4) -0.003(4) C115 0.098(4) 0.094(4) 0.073(4) -0.037(3) 0.008(3) 0.016(4) C116 0.089(4) 0.063(3) 0.063(3) -0.010(2) 0.028(3) 0.016(3) P1 0.101(2) 0.0645(18) 0.0798(19) -0.0031(15) 0.0160(17) -0.0138(17) P2 0.0275(6) 0.0390(7) 0.0338(6) 0.000 0.000 0.0025(5) F1 0.105(5) 0.095(5) 0.084(4) -0.009(4) 0.014(4) -0.008(4) F2 0.082(5) 0.237(12) 0.172(9) 0.135(9) -0.011(5) 0.025(6) F3 0.108(5) 0.113(6) 0.096(5) -0.017(5) 0.008(4) -0.014(4) F4 0.106(5) 0.085(4) 0.103(5) 0.015(4) -0.018(4) -0.005(4) F5 0.126(6) 0.170(8) 0.083(5) 0.032(5) -0.017(4) -0.074(6) F6 0.079(4) 0.101(4) 0.056(3) 0.028(3) -0.001(3) -0.044(3) F7 0.155(3) 0.0598(18) 0.133(3) -0.0013(18) -0.114(3) -0.0028(19) F8 0.090(2) 0.085(2) 0.122(3) 0.0436(19) -0.062(2) -0.0225(17) F9 0.0687(14) 0.0424(13) 0.0543(14) 0.0016(11) -0.0198(11) -0.0077(11) C201 0.094(7) 0.146(11) 0.158(11) 0.007(9) 0.000 0.000 C202 0.127(7) 0.139(8) 0.176(9) -0.033(7) 0.004(7) -0.023(6) C203 0.188(12) 0.123(9) 0.222(14) 0.020(8) -0.075(11) -0.059(9) C204 0.114(10) 0.27(3) 0.31(3) 0.25(3) 0.000 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 Ru1 N61 2.026(3) . ? Ru1 N61 2.026(3) 2 ? Ru1 N51 2.094(3) 2 ? Ru1 N51 2.094(3) . ? Ru1 N71 2.102(3) 2 ? Ru1 N71 2.102(3) . ? N11 C12 1.332(4) . ? N11 C16 1.337(5) . ? C12 C13 1.392(4) . ? C12 C26 1.489(5) . ? C13 C14 1.376(5) . ? C13 H13A 0.9500 . ? C14 C15 1.375(5) . ? C14 H14A 0.9500 . ? C15 C16 1.388(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? N21 C26 1.333(4) . ? N21 C22 1.344(4) . ? C22 C23 1.381(5) . ? C22 C32 1.485(5) . ? C23 C24 1.388(5) . ? C23 H23A 0.9500 . ? C24 C25 1.388(5) . ? C24 C42 1.483(4) . ? C25 C26 1.391(4) . ? C25 H25A 0.9500 . ? N31 C36 1.327(5) . ? N31 C32 1.344(4) . ? C32 C33 1.387(5) . ? C33 C34 1.373(5) . ? C33 H33A 0.9500 . ? C34 C35 1.367(5) . ? C34 H34A 0.9500 . ? C35 C36 1.380(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.392(5) . ? C41 C42 1.393(5) . ? C41 H41A 0.9500 . ? C42 C43 1.391(5) . ? C43 C44 1.382(5) . ? C43 H43A 0.9500 . ? C44 C45 1.386(5) . ? C44 H44A 0.9500 . ? C45 C46 1.380(5) . ? C45 C47 1.519(4) . ? C46 H46A 0.9500 . ? C47 N52 1.453(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N51 N52 1.353(4) . ? N51 C55 1.356(4) . ? N52 C53 1.348(4) . ? C53 C54 1.360(5) . ? C53 H53A 0.9500 . ? C54 C55 1.402(5) . ? C54 H54A 0.9500 . ? C55 C62 1.453(5) . ? N61 C62 1.349(5) . ? N61 C66 1.352(4) . ? C62 C63 1.383(5) . ? C63 C64 1.390(6) . ? C63 H63A 0.9500 . ? C64 C65 1.376(6) . ? C64 H64A 0.9500 . ? C65 C66 1.385(5) . ? C65 H65A 0.9500 . ? C66 C75 1.451(5) . ? N71 N72 1.347(4) . ? N71 C75 1.354(5) . ? N72 C73 1.345(6) . ? N72 C81 1.475(5) . ? C73 C74 1.340(7) . ? C73 H73A 0.9500 . ? C74 C75 1.383(5) . ? C74 H74A 0.9500 . ? C81 C82 1.497(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C87 1.379(5) . ? C82 C83 1.398(6) . ? C83 C84 1.362(6) . ? C83 H83A 0.9500 . ? C84 C85 1.402(6) . ? C84 H84A 0.9500 . ? C85 C86 1.391(5) . ? C85 C104 1.475(5) . ? C86 C87 1.383(6) . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? N91 C92 1.347(5) . ? N91 C96 1.348(5) . ? C92 C93 1.382(6) . ? C92 C106 1.491(5) . ? C93 C94 1.382(5) . ? C93 H93A 0.9500 . ? C94 C95 1.375(6) . ? C94 H94A 0.9500 . ? C95 C96 1.363(6) . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? N101 C106 1.348(5) . ? N101 C102 1.354(5) . ? C102 C103 1.388(5) . ? C102 C112 1.483(6) . ? C103 C104 1.396(6) . ? C103 H10B 0.9500 . ? C104 C105 1.388(5) . ? C105 C106 1.383(5) . ? C105 H10A 0.9500 . ? N111 C116 1.339(6) . ? N111 C112 1.342(5) . ? C112 C113 1.365(7) . ? C113 C114 1.377(8) . ? C113 H11A 0.9500 . ? C114 C115 1.367(9) . ? C114 H11D 0.9500 . ? C115 C116 1.367(8) . ? C115 H11C 0.9500 . ? C116 H11B 0.9500 . ? P1 F2 1.459(11) . ? P1 F5 1.532(8) . ? P1 F1 1.571(7) . ? P1 F4 1.580(8) . ? P1 F3 1.601(9) . ? P1 F6 1.620(6) . ? P2 F7 1.558(3) . ? P2 F7 1.558(3) 2 ? P2 F8 1.577(3) 2 ? P2 F8 1.577(3) . ? P2 F9 1.599(2) 2 ? P2 F9 1.599(2) . ? C201 C202 1.407(7) 4 ? C201 C202 1.407(7) . ? C201 H201 0.9500 . ? C202 C203 1.380(8) . ? C202 H202 0.9500 . ? C203 C204 1.417(8) . ? C203 H203 0.9500 . ? C204 C203 1.417(8) 4 ? C204 H204 0.9500 . ? 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 N61 Ru1 N61 175.67(15) . 2 ? N61 Ru1 N51 106.43(11) . 2 ? N61 Ru1 N51 76.84(11) 2 2 ? N61 Ru1 N51 76.84(11) . . ? N61 Ru1 N51 106.43(11) 2 . ? N51 Ru1 N51 85.80(15) 2 . ? N61 Ru1 N71 99.80(11) . 2 ? N61 Ru1 N71 77.00(11) 2 2 ? N51 Ru1 N71 153.75(11) 2 2 ? N51 Ru1 N71 99.47(11) . 2 ? N61 Ru1 N71 77.00(11) . . ? N61 Ru1 N71 99.80(11) 2 . ? N51 Ru1 N71 99.47(11) 2 . ? N51 Ru1 N71 153.75(11) . . ? N71 Ru1 N71 87.15(17) 2 . ? C12 N11 C16 117.5(3) . . ? N11 C12 C13 122.1(3) . . ? N11 C12 C26 116.9(3) . . ? C13 C12 C26 120.9(3) . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 117.6(3) . . ? C14 C15 H15A 121.2 . . ? C16 C15 H15A 121.2 . . ? N11 C16 C15 124.2(4) . . ? N11 C16 H16A 117.9 . . ? C15 C16 H16A 117.9 . . ? C26 N21 C22 117.8(3) . . ? N21 C22 C23 122.8(3) . . ? N21 C22 C32 118.0(3) . . ? C23 C22 C32 119.2(3) . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C23 C24 C25 117.1(3) . . ? C23 C24 C42 120.0(3) . . ? C25 C24 C42 122.9(3) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? N21 C26 C25 122.6(3) . . ? N21 C26 C12 116.7(3) . . ? C25 C26 C12 120.8(3) . . ? C36 N31 C32 117.2(3) . . ? N31 C32 C33 122.2(3) . . ? N31 C32 C22 115.9(3) . . ? C33 C32 C22 121.9(3) . . ? C34 C33 C32 118.9(3) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C35 C34 C33 119.4(3) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 118.1(3) . . ? C34 C35 H35A 121.0 . . ? C36 C35 H35A 121.0 . . ? N31 C36 C35 124.0(3) . . ? N31 C36 H36A 118.0 . . ? C35 C36 H36A 118.0 . . ? C46 C41 C42 120.0(3) . . ? C46 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C43 C42 C41 118.6(3) . . ? C43 C42 C24 120.6(3) . . ? C41 C42 C24 120.8(3) . . ? C44 C43 C42 120.9(3) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 120.4(3) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C46 C45 C44 119.0(3) . . ? C46 C45 C47 119.4(3) . . ? C44 C45 C47 121.6(3) . . ? C45 C46 C41 121.0(3) . . ? C45 C46 H46A 119.5 . . ? C41 C46 H46A 119.5 . . ? N52 C47 C45 111.8(3) . . ? N52 C47 H47A 109.3 . . ? C45 C47 H47A 109.3 . . ? N52 C47 H47B 109.3 . . ? C45 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? N52 N51 C55 105.3(3) . . ? N52 N51 Ru1 139.2(2) . . ? C55 N51 Ru1 114.7(2) . . ? C53 N52 N51 110.7(3) . . ? C53 N52 C47 127.7(3) . . ? N51 N52 C47 121.4(3) . . ? N52 C53 C54 108.8(3) . . ? N52 C53 H53A 125.6 . . ? C54 C53 H53A 125.6 . . ? C53 C54 C55 104.8(3) . . ? C53 C54 H54A 127.6 . . ? C55 C54 H54A 127.6 . . ? N51 C55 C54 110.4(3) . . ? N51 C55 C62 116.3(3) . . ? C54 C55 C62 133.3(3) . . ? C62 N61 C66 120.3(3) . . ? C62 N61 Ru1 119.9(2) . . ? C66 N61 Ru1 119.4(2) . . ? N61 C62 C63 120.8(3) . . ? N61 C62 C55 111.9(3) . . ? C63 C62 C55 127.2(3) . . ? C62 C63 C64 118.9(4) . . ? C62 C63 H63A 120.5 . . ? C64 C63 H63A 120.5 . . ? C65 C64 C63 120.0(4) . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C66 118.8(4) . . ? C64 C65 H65A 120.6 . . ? C66 C65 H65A 120.6 . . ? N61 C66 C65 121.1(3) . . ? N61 C66 C75 112.0(3) . . ? C65 C66 C75 126.9(3) . . ? N72 N71 C75 104.6(3) . . ? N72 N71 Ru1 140.7(2) . . ? C75 N71 Ru1 114.0(2) . . ? C73 N72 N71 110.7(3) . . ? C73 N72 C81 125.9(3) . . ? N71 N72 C81 122.6(3) . . ? C74 C73 N72 108.7(4) . . ? C74 C73 H73A 125.7 . . ? N72 C73 H73A 125.7 . . ? C73 C74 C75 105.3(4) . . ? C73 C74 H74A 127.3 . . ? C75 C74 H74A 127.3 . . ? N71 C75 C74 110.7(4) . . ? N71 C75 C66 116.9(3) . . ? C74 C75 C66 132.4(4) . . ? N72 C81 C82 111.1(3) . . ? N72 C81 H81A 109.4 . . ? C82 C81 H81A 109.4 . . ? N72 C81 H81B 109.4 . . ? C82 C81 H81B 109.4 . . ? H81A C81 H81B 108.0 . . ? C87 C82 C83 117.8(4) . . ? C87 C82 C81 121.9(3) . . ? C83 C82 C81 120.3(4) . . ? C84 C83 C82 120.6(4) . . ? C84 C83 H83A 119.7 . . ? C82 C83 H83A 119.7 . . ? C83 C84 C85 121.9(4) . . ? C83 C84 H84A 119.0 . . ? C85 C84 H84A 119.0 . . ? C86 C85 C84 117.4(4) . . ? C86 C85 C104 121.8(3) . . ? C84 C85 C104 120.8(3) . . ? C87 C86 C85 120.3(4) . . ? C87 C86 H86A 119.8 . . ? C85 C86 H86A 119.8 . . ? C82 C87 C86 121.9(4) . . ? C82 C87 H87A 119.0 . . ? C86 C87 H87A 119.0 . . ? C92 N91 C96 117.6(3) . . ? N91 C92 C93 122.3(3) . . ? N91 C92 C106 116.2(3) . . ? C93 C92 C106 121.4(4) . . ? C92 C93 C94 118.7(4) . . ? C92 C93 H93A 120.7 . . ? C94 C93 H93A 120.7 . . ? C95 C94 C93 119.3(4) . . ? C95 C94 H94A 120.4 . . ? C93 C94 H94A 120.4 . . ? C96 C95 C94 119.0(4) . . ? C96 C95 H95A 120.5 . . ? C94 C95 H95A 120.5 . . ? N91 C96 C95 123.1(4) . . ? N91 C96 H96A 118.4 . . ? C95 C96 H96A 118.4 . . ? C106 N101 C102 117.3(3) . . ? N101 C102 C103 122.7(3) . . ? N101 C102 C112 116.9(4) . . ? C103 C102 C112 120.4(3) . . ? C102 C103 C104 119.8(3) . . ? C102 C103 H10B 120.1 . . ? C104 C103 H10B 120.1 . . ? C105 C104 C103 117.1(4) . . ? C105 C104 C85 121.0(3) . . ? C103 C104 C85 121.9(3) . . ? C106 C105 C104 120.2(4) . . ? C106 C105 H10A 119.9 . . ? C104 C105 H10A 119.9 . . ? N101 C106 C105 122.8(3) . . ? N101 C106 C92 117.0(3) . . ? C105 C106 C92 120.2(3) . . ? C116 N111 C112 117.4(4) . . ? N111 C112 C113 122.1(4) . . ? N111 C112 C102 116.0(4) . . ? C113 C112 C102 121.9(4) . . ? C112 C113 C114 119.3(5) . . ? C112 C113 H11A 120.4 . . ? C114 C113 H11A 120.4 . . ? C115 C114 C113 119.3(6) . . ? C115 C114 H11D 120.4 . . ? C113 C114 H11D 120.4 . . ? C114 C115 C116 118.1(5) . . ? C114 C115 H11C 121.0 . . ? C116 C115 H11C 121.0 . . ? N111 C116 C115 123.6(5) . . ? N111 C116 H11B 118.2 . . ? C115 C116 H11B 118.2 . . ? F2 P1 F5 87.3(6) . . ? F2 P1 F1 91.9(5) . . ? F5 P1 F1 178.8(5) . . ? F2 P1 F4 98.0(5) . . ? F5 P1 F4 88.9(4) . . ? F1 P1 F4 92.1(4) . . ? F2 P1 F3 173.3(6) . . ? F5 P1 F3 90.5(5) . . ? F1 P1 F3 90.2(4) . . ? F4 P1 F3 88.3(4) . . ? F2 P1 F6 77.3(5) . . ? F5 P1 F6 92.3(4) . . ? F1 P1 F6 86.7(4) . . ? F4 P1 F6 175.1(4) . . ? F3 P1 F6 96.5(4) . . ? F7 P2 F7 91.1(4) . 2 ? F7 P2 F8 91.1(2) . 2 ? F7 P2 F8 177.4(2) 2 2 ? F7 P2 F8 177.4(2) . . ? F7 P2 F8 91.1(2) 2 . ? F8 P2 F8 86.8(3) 2 . ? F7 P2 F9 90.47(15) . 2 ? F7 P2 F9 89.77(14) 2 2 ? F8 P2 F9 88.83(14) 2 2 ? F8 P2 F9 90.93(15) . 2 ? F7 P2 F9 89.77(14) . . ? F7 P2 F9 90.47(15) 2 . ? F8 P2 F9 90.93(15) 2 . ? F8 P2 F9 88.83(14) . . ? F9 P2 F9 179.67(19) 2 . ? C202 C201 C202 125.8(12) 4 . ? C202 C201 H201 117.1 4 . ? C202 C201 H201 117.1 . . ? C203 C202 C201 117.0(10) . . ? C203 C202 H202 121.5 . . ? C201 C202 H202 121.5 . . ? C202 C203 C204 117.7(13) . . ? C202 C203 H203 121.2 . . ? C204 C203 H203 121.2 . . ? C203 C204 C203 124.4(16) 4 . ? C203 C204 H204 117.8 4 . ? C203 C204 H204 117.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.061 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.085 #===END data_RuAg2 _database_code_depnum_ccdc_archive 'CCDC 659050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H84 Ag2 Cl4 N24 O19 Ru' _chemical_formula_weight 2288.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 30.736(4) _cell_length_b 14.284(2) _cell_length_c 21.992(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.756(9) _cell_angle_gamma 90.00 _cell_volume 9543(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4648 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_correction_T_max 0.9419 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 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 64337 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8394 _reflns_number_gt 5551 _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^)+(0.1113P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8394 _refine_ls_number_parameters 642 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.0000 0.70246(4) 0.2500 0.0312(2) Uani 1 2 d S . . Ag1 Ag 0.27487(2) 0.85257(5) 0.34272(3) 0.0771(3) Uani 1 1 d . . . Cl1 Cl 0.15187(7) 0.37704(15) 0.49450(9) 0.0731(6) Uani 1 1 d . . . Cl2 Cl 0.10878(6) 0.88595(14) 0.58064(8) 0.0629(5) Uani 1 1 d . . . O1 O 0.1700(3) 0.3003(6) 0.5223(6) 0.199(6) Uani 1 1 d . . . O2 O 0.1147(2) 0.3592(4) 0.4510(3) 0.114(3) Uani 1 1 d . . . O3 O 0.1421(3) 0.4239(10) 0.5440(4) 0.217(6) Uani 1 1 d . . . O4 O 0.1804(2) 0.4323(5) 0.4684(3) 0.118(2) Uani 1 1 d . . . O5 O 0.1033(3) 0.9666(6) 0.5446(5) 0.174(4) Uani 1 1 d . . . O6 O 0.15516(15) 0.8689(4) 0.6004(2) 0.0728(15) Uani 1 1 d . . . O7 O 0.0914(2) 0.8077(5) 0.5466(3) 0.110(2) Uani 1 1 d . . . O8 O 0.08690(19) 0.8975(5) 0.6318(3) 0.0913(18) Uani 1 1 d . . . N1 N 0.3212(2) 0.8162(4) 0.2778(3) 0.0680(17) Uani 1 1 d . . . C2 C 0.3066(2) 0.8219(5) 0.2164(4) 0.0576(19) Uani 1 1 d . . . C3 C 0.3331(3) 0.7995(5) 0.1737(4) 0.068(2) Uani 1 1 d . . . H3A H 0.3225 0.8055 0.1310 0.082 Uiso 1 1 calc R . . C4 C 0.3757(3) 0.7682(5) 0.1934(5) 0.079(3) Uani 1 1 d . . . H4A H 0.3943 0.7508 0.1646 0.095 Uiso 1 1 calc R . . C5 C 0.3899(3) 0.7631(6) 0.2545(5) 0.087(3) Uani 1 1 d . . . H5A H 0.4192 0.7434 0.2690 0.104 Uiso 1 1 calc R . . C6 C 0.3623(3) 0.7862(6) 0.2959(4) 0.083(3) Uani 1 1 d . . . H6A H 0.3728 0.7806 0.3387 0.099 Uiso 1 1 calc R . . N11 N 0.24443(17) 0.9144(4) 0.2387(2) 0.0489(13) Uani 1 1 d . . . N12 N 0.20627(18) 0.9461(4) 0.2080(2) 0.0493(13) Uani 1 1 d . . . C13 C 0.1994(3) 0.9162(5) 0.1486(3) 0.0593(19) Uani 1 1 d . . . H13A H 0.1749 0.9298 0.1181 0.071 Uiso 1 1 calc R . . C14 C 0.2356(3) 0.8618(5) 0.1418(3) 0.065(2) Uani 1 1 d . . . H14A H 0.2409 0.8302 0.1056 0.078 Uiso 1 1 calc R . . C15 C 0.2624(2) 0.8629(5) 0.1980(3) 0.0545(18) Uani 1 1 d . . . C21 C 0.1784(2) 1.0056(5) 0.2382(3) 0.0495(16) Uani 1 1 d . . . H21A H 0.1586 1.0410 0.2066 0.059 Uiso 1 1 calc R . . H21B H 0.1970 1.0515 0.2640 0.059 Uiso 1 1 calc R . . C22 C 0.1506(2) 0.9526(4) 0.2784(3) 0.0450(15) Uani 1 1 d . . . C23 C 0.1236(2) 1.0016(5) 0.3109(3) 0.0557(17) Uani 1 1 d . . . H23A H 0.1237 1.0681 0.3096 0.067 Uiso 1 1 calc R . . C24 C 0.0965(2) 0.9564(5) 0.3456(3) 0.0541(17) Uani 1 1 d . . . H24A H 0.0775 0.9918 0.3671 0.065 Uiso 1 1 calc R . . C25 C 0.09644(18) 0.8604(4) 0.3495(3) 0.0391(14) Uani 1 1 d . . . C26 C 0.12383(18) 0.8104(4) 0.3182(2) 0.0369(13) Uani 1 1 d . . . H26A H 0.1243 0.7440 0.3205 0.044 Uiso 1 1 calc R . . C27 C 0.1511(2) 0.8570(4) 0.2828(3) 0.0409(14) Uani 1 1 d . . . H27A H 0.1703 0.8219 0.2616 0.049 Uiso 1 1 calc R . . C28 C 0.0659(2) 0.8153(4) 0.3882(3) 0.0422(15) Uani 1 1 d . . . H28B H 0.0760 0.8315 0.4318 0.051 Uiso 1 1 calc R . . H28A H 0.0361 0.8424 0.3765 0.051 Uiso 1 1 calc R . . N31 N 0.03996(14) 0.6702(3) 0.3330(2) 0.0349(11) Uani 1 1 d . . . N32 N 0.06262(15) 0.7151(4) 0.3830(2) 0.0405(12) Uani 1 1 d . . . C33 C 0.0809(2) 0.6515(5) 0.4244(3) 0.0464(16) Uani 1 1 d . . . H33A H 0.0985 0.6656 0.4626 0.056 Uiso 1 1 calc R . . C34 C 0.0700(2) 0.5649(5) 0.4031(3) 0.0511(17) Uani 1 1 d . . . H34A H 0.0783 0.5070 0.4228 0.061 Uiso 1 1 calc R . . C35 C 0.04387(18) 0.5784(4) 0.3454(3) 0.0366(13) Uani 1 1 d . . . N41 N 0.0000 0.5621(5) 0.2500 0.0359(15) Uani 1 2 d S . . C42 C 0.02227(18) 0.5165(4) 0.2986(3) 0.0372(14) Uani 1 1 d . . . C43 C 0.0221(2) 0.4184(5) 0.2999(3) 0.0507(17) Uani 1 1 d . . . H43A H 0.0369 0.3857 0.3346 0.061 Uiso 1 1 calc R . . C44 C 0.0000 0.3695(6) 0.2500 0.050(2) Uani 1 2 d S . . H44A H 0.0000 0.3030 0.2500 0.060 Uiso 1 2 calc SR . . N51 N 0.24395(18) 0.9588(4) 0.4036(2) 0.0560(15) Uani 1 1 d . . . C52 C 0.2163(2) 0.9226(5) 0.4380(3) 0.0461(15) Uani 1 1 d . . . C53 C 0.1926(2) 0.9788(5) 0.4728(3) 0.0546(18) Uani 1 1 d . . . H53A H 0.1736 0.9515 0.4982 0.066 Uiso 1 1 calc R . . C54 C 0.1968(3) 1.0745(5) 0.4700(3) 0.065(2) Uani 1 1 d . . . H54A H 0.1803 1.1143 0.4924 0.078 Uiso 1 1 calc R . . C55 C 0.2252(3) 1.1112(6) 0.4344(4) 0.077(2) Uani 1 1 d . . . H55A H 0.2294 1.1770 0.4328 0.092 Uiso 1 1 calc R . . C56 C 0.2474(3) 1.0520(6) 0.4012(4) 0.074(2) Uani 1 1 d . . . H56A H 0.2661 1.0783 0.3751 0.089 Uiso 1 1 calc R . . N61 N 0.23166(15) 0.7684(4) 0.4001(2) 0.0458(13) Uani 1 1 d . . . N62 N 0.22348(16) 0.6792(4) 0.4133(2) 0.0440(12) Uani 1 1 d . . . C63 C 0.1990(2) 0.6737(5) 0.4584(3) 0.0461(16) Uani 1 1 d . . . H63A H 0.1889 0.6176 0.4748 0.055 Uiso 1 1 calc R . . C64 C 0.19097(19) 0.7626(5) 0.4769(3) 0.0472(16) Uani 1 1 d . . . H64A H 0.1744 0.7808 0.5081 0.057 Uiso 1 1 calc R . . C65 C 0.21254(18) 0.8210(5) 0.4398(3) 0.0402(15) Uani 1 1 d . . . C71 C 0.2359(2) 0.6034(5) 0.3742(3) 0.0526(17) Uani 1 1 d . . . H71A H 0.2390 0.5441 0.3977 0.063 Uiso 1 1 calc R . . H71B H 0.2647 0.6179 0.3612 0.063 Uiso 1 1 calc R . . C72 C 0.20156(19) 0.5926(4) 0.3188(3) 0.0428(15) Uani 1 1 d . . . C73 C 0.2049(2) 0.6388(4) 0.2632(3) 0.0465(16) Uani 1 1 d . . . H73A H 0.2311 0.6717 0.2586 0.056 Uiso 1 1 calc R . . C74 C 0.17015(19) 0.6363(4) 0.2154(3) 0.0414(14) Uani 1 1 d . . . H74A H 0.1728 0.6676 0.1780 0.050 Uiso 1 1 calc R . . C75 C 0.13144(19) 0.5888(4) 0.2208(3) 0.0392(14) Uani 1 1 d . . . C76 C 0.1294(2) 0.5385(4) 0.2733(3) 0.0451(15) Uani 1 1 d . . . H76A H 0.1041 0.5019 0.2766 0.054 Uiso 1 1 calc R . . C77 C 0.1642(2) 0.5404(4) 0.3219(3) 0.0456(15) Uani 1 1 d . . . H77A H 0.1622 0.5050 0.3579 0.055 Uiso 1 1 calc R . . C78 C 0.0914(2) 0.5965(5) 0.1708(3) 0.0483(16) Uani 1 1 d . . . H78A H 0.0990 0.5720 0.1316 0.058 Uiso 1 1 calc R . . H78B H 0.0673 0.5575 0.1822 0.058 Uiso 1 1 calc R . . N81 N 0.04989(15) 0.7354(3) 0.19746(19) 0.0360(11) Uani 1 1 d . . . N82 N 0.07646(14) 0.6928(3) 0.1620(2) 0.0364(11) Uani 1 1 d . . . C83 C 0.0942(2) 0.7581(5) 0.1278(3) 0.0457(15) Uani 1 1 d . . . H83A H 0.1142 0.7456 0.0999 0.055 Uiso 1 1 calc R . . C84 C 0.0788(2) 0.8423(5) 0.1398(3) 0.0478(16) Uani 1 1 d . . . H84A H 0.0851 0.9003 0.1219 0.057 Uiso 1 1 calc R . . C85 C 0.05176(19) 0.8272(4) 0.1843(3) 0.0385(14) Uani 1 1 d . . . N91 N 0.0000 0.8449(5) 0.2500 0.0353(15) Uani 1 2 d S . . C92 C 0.0256(2) 0.8901(4) 0.2161(3) 0.0422(15) Uani 1 1 d . . . C93 C 0.0256(2) 0.9872(4) 0.2146(3) 0.0507(17) Uani 1 1 d . . . H93A H 0.0430 1.0201 0.1895 0.061 Uiso 1 1 calc R . . C94 C 0.0000 1.0345(7) 0.2500 0.062(3) Uani 1 2 d S . . H94A H 0.0000 1.1010 0.2500 0.075 Uiso 1 2 calc SR . . C100 C 0.9846(4) 0.8152(11) 0.6105(5) 0.160(6) Uani 1 1 d DU . . N100 N 0.9660(3) 0.8412(11) 0.5564(4) 0.204(6) Uani 1 1 d DU . . O100 O 0.9697(2) 0.7968(4) 0.6509(3) 0.0938(19) Uani 1 1 d DU . . C101 C 0.9834(9) 0.8952(16) 0.5129(11) 0.323(13) Uiso 1 1 d DU . . H10A H 1.0156 0.8900 0.5200 0.484 Uiso 1 1 calc R . . H10B H 0.9750 0.9608 0.5169 0.484 Uiso 1 1 calc R . . H10C H 0.9720 0.8727 0.4715 0.484 Uiso 1 1 calc R . . C102 C 0.9212(4) 0.8559(6) 0.5410(5) 0.111(3) Uani 1 1 d DU . . H10D H 0.9054 0.8171 0.5672 0.167 Uiso 1 1 calc R . . H10E H 0.9119 0.8391 0.4978 0.167 Uiso 1 1 calc R . . H10F H 0.9146 0.9221 0.5470 0.167 Uiso 1 1 calc R . . O200 O 0.1383(8) 0.5972(12) 0.5705(8) 0.186(9) Uani 0.50 1 d P . . H202 H 0.1265 0.6514 0.5638 0.224 Uiso 0.50 1 d PR . . H201 H 0.1397 0.5400 0.5610 0.224 Uiso 0.50 1 d 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 Ru1 0.0325(4) 0.0379(4) 0.0251(4) 0.000 0.0104(3) 0.000 Ag1 0.0612(4) 0.1223(6) 0.0536(4) 0.0133(3) 0.0270(3) -0.0069(3) Cl1 0.0827(15) 0.0761(13) 0.0588(12) 0.0226(10) 0.0056(11) 0.0089(11) Cl2 0.0695(12) 0.0673(12) 0.0552(11) -0.0001(9) 0.0207(9) 0.0095(9) O1 0.111(6) 0.100(6) 0.356(15) 0.107(8) -0.066(8) -0.006(5) O2 0.094(5) 0.091(5) 0.139(6) 0.000(4) -0.039(5) 0.002(3) O3 0.162(9) 0.387(19) 0.119(7) -0.087(10) 0.077(7) -0.065(10) O4 0.150(6) 0.147(6) 0.057(4) 0.043(4) 0.016(4) -0.044(5) O5 0.161(8) 0.163(8) 0.223(10) 0.112(7) 0.106(7) 0.087(6) O6 0.038(3) 0.107(4) 0.073(4) -0.005(3) 0.010(2) -0.001(3) O7 0.082(4) 0.156(6) 0.091(4) -0.072(4) 0.011(3) -0.010(4) O8 0.084(4) 0.123(5) 0.075(4) -0.027(3) 0.038(3) 0.018(3) N1 0.057(4) 0.077(4) 0.078(5) 0.028(4) 0.037(3) -0.001(3) C2 0.068(5) 0.044(4) 0.070(5) 0.004(3) 0.039(4) -0.010(3) C3 0.079(6) 0.048(4) 0.088(6) -0.006(4) 0.046(5) -0.010(4) C4 0.082(6) 0.050(5) 0.119(8) -0.003(5) 0.061(6) -0.009(4) C5 0.065(6) 0.072(6) 0.135(9) 0.028(6) 0.055(6) 0.011(4) C6 0.059(5) 0.088(6) 0.107(7) 0.043(5) 0.032(5) 0.007(4) N11 0.049(3) 0.053(3) 0.048(3) 0.007(3) 0.020(3) -0.009(3) N12 0.054(3) 0.056(3) 0.041(3) 0.005(3) 0.016(3) -0.005(3) C13 0.073(5) 0.063(5) 0.045(4) 0.001(3) 0.017(4) -0.014(4) C14 0.084(6) 0.068(5) 0.049(5) -0.004(4) 0.030(4) -0.019(4) C15 0.061(5) 0.058(4) 0.050(4) 0.005(3) 0.027(4) -0.015(3) C21 0.052(4) 0.050(4) 0.048(4) 0.006(3) 0.012(3) -0.003(3) C22 0.049(4) 0.049(4) 0.037(3) 0.005(3) 0.005(3) -0.006(3) C23 0.058(4) 0.051(4) 0.062(4) -0.007(3) 0.020(4) -0.003(3) C24 0.062(4) 0.045(4) 0.058(4) -0.006(3) 0.018(3) 0.000(3) C25 0.030(3) 0.060(4) 0.026(3) -0.001(3) 0.004(2) -0.002(3) C26 0.036(3) 0.042(3) 0.033(3) 0.004(3) 0.007(3) 0.001(3) C27 0.044(4) 0.047(4) 0.033(3) 0.000(3) 0.011(3) 0.001(3) C28 0.043(4) 0.053(4) 0.031(3) -0.003(3) 0.008(3) -0.002(3) N31 0.030(3) 0.046(3) 0.032(3) 0.004(2) 0.014(2) 0.002(2) N32 0.035(3) 0.060(3) 0.029(3) 0.006(2) 0.011(2) 0.002(2) C33 0.043(4) 0.066(5) 0.031(3) 0.005(3) 0.008(3) -0.006(3) C34 0.047(4) 0.063(4) 0.046(4) 0.016(3) 0.015(3) 0.016(3) C35 0.031(3) 0.049(4) 0.033(3) 0.005(3) 0.015(3) 0.005(3) N41 0.031(4) 0.044(4) 0.035(4) 0.000 0.010(3) 0.000 C42 0.037(3) 0.036(3) 0.044(4) 0.006(3) 0.024(3) 0.004(3) C43 0.038(4) 0.054(4) 0.063(4) 0.014(3) 0.018(3) 0.005(3) C44 0.044(5) 0.035(5) 0.077(7) 0.000 0.028(5) 0.000 N51 0.061(4) 0.067(4) 0.040(3) 0.010(3) 0.008(3) -0.017(3) C52 0.038(4) 0.060(4) 0.037(4) 0.006(3) -0.003(3) 0.001(3) C53 0.054(4) 0.063(5) 0.044(4) 0.010(3) -0.001(3) 0.001(3) C54 0.070(5) 0.059(5) 0.060(5) 0.002(4) -0.008(4) 0.010(4) C55 0.089(6) 0.071(6) 0.064(5) 0.024(5) -0.007(5) -0.011(5) C56 0.070(5) 0.082(6) 0.068(5) 0.017(5) 0.004(4) -0.018(5) N61 0.036(3) 0.059(3) 0.042(3) 0.011(3) 0.003(2) -0.001(2) N62 0.036(3) 0.058(3) 0.039(3) 0.006(2) 0.010(2) 0.001(2) C63 0.039(4) 0.065(4) 0.033(3) 0.012(3) 0.002(3) -0.002(3) C64 0.031(3) 0.075(5) 0.036(3) 0.006(3) 0.006(3) 0.002(3) C65 0.025(3) 0.069(4) 0.027(3) 0.008(3) 0.004(2) 0.005(3) C71 0.044(4) 0.059(4) 0.057(4) -0.002(3) 0.016(3) 0.017(3) C72 0.038(3) 0.044(3) 0.049(4) -0.004(3) 0.015(3) 0.008(3) C73 0.042(4) 0.048(4) 0.052(4) -0.001(3) 0.018(3) 0.005(3) C74 0.039(4) 0.048(4) 0.040(4) 0.003(3) 0.016(3) 0.004(3) C75 0.041(3) 0.042(3) 0.037(3) -0.001(3) 0.015(3) 0.004(3) C76 0.044(4) 0.049(4) 0.046(4) -0.004(3) 0.017(3) 0.003(3) C77 0.051(4) 0.039(3) 0.051(4) -0.001(3) 0.018(3) 0.004(3) C78 0.048(4) 0.060(4) 0.039(4) -0.012(3) 0.016(3) 0.000(3) N81 0.035(3) 0.047(3) 0.026(2) 0.000(2) 0.008(2) -0.001(2) N82 0.032(3) 0.051(3) 0.029(3) -0.001(2) 0.014(2) 0.002(2) C83 0.042(4) 0.064(4) 0.034(3) 0.005(3) 0.016(3) -0.007(3) C84 0.043(4) 0.068(5) 0.034(3) 0.013(3) 0.013(3) -0.006(3) C85 0.038(3) 0.049(4) 0.031(3) 0.002(3) 0.011(3) -0.007(3) N91 0.034(4) 0.048(4) 0.026(3) 0.000 0.011(3) 0.000 C92 0.046(4) 0.046(4) 0.034(3) 0.001(3) 0.001(3) 0.000(3) C93 0.076(5) 0.040(4) 0.038(4) 0.000(3) 0.016(3) -0.006(3) C94 0.092(8) 0.054(6) 0.039(5) 0.000 0.005(5) 0.000 C100 0.118(9) 0.306(17) 0.055(6) 0.025(8) 0.014(5) -0.083(9) N100 0.109(6) 0.428(18) 0.072(5) 0.067(8) 0.003(5) -0.152(9) O100 0.122(5) 0.090(4) 0.072(4) 0.011(3) 0.023(4) -0.027(4) C102 0.169(9) 0.076(7) 0.088(7) 0.013(5) 0.018(7) 0.005(7) O200 0.31(3) 0.107(12) 0.137(14) 0.011(11) 0.029(16) 0.079(15) _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 N41 2.005(7) . ? Ru1 N91 2.035(7) . ? Ru1 N31 2.090(5) . ? Ru1 N31 2.090(4) 2 ? Ru1 N81 2.109(4) . ? Ru1 N81 2.109(4) 2 ? Ag1 N1 2.226(6) . ? Ag1 N61 2.305(5) . ? Ag1 N51 2.321(6) . ? Ag1 N11 2.498(5) . ? Cl1 O1 1.334(7) . ? Cl1 O3 1.350(9) . ? Cl1 O4 1.368(6) . ? Cl1 O2 1.398(6) . ? Cl2 O5 1.393(7) . ? Cl2 O7 1.405(6) . ? Cl2 O8 1.405(5) . ? Cl2 O6 1.446(5) . ? N1 C6 1.338(9) . ? N1 C2 1.358(9) . ? C2 C3 1.372(9) . ? C2 C15 1.478(10) . ? C3 C4 1.387(11) . ? C3 H3A 0.9500 . ? C4 C5 1.351(12) . ? C4 H4A 0.9500 . ? C5 C6 1.375(11) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N11 N12 1.339(7) . ? N11 C15 1.340(8) . ? N12 C13 1.360(8) . ? N12 C21 1.439(8) . ? C13 C14 1.383(10) . ? C13 H13A 0.9500 . ? C14 C15 1.377(10) . ? C14 H14A 0.9500 . ? C21 C22 1.521(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.368(9) . ? C22 C27 1.369(8) . ? C23 C24 1.375(9) . ? C23 H23A 0.9500 . ? C24 C25 1.374(8) . ? C24 H24A 0.9500 . ? C25 C26 1.367(8) . ? C25 C28 1.504(8) . ? C26 C27 1.397(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 N32 1.438(7) . ? C28 H28B 0.9900 . ? C28 H28A 0.9900 . ? N31 C35 1.341(7) . ? N31 N32 1.368(6) . ? N32 C33 1.347(7) . ? C33 C34 1.347(9) . ? C33 H33A 0.9500 . ? C34 C35 1.409(8) . ? C34 H34A 0.9500 . ? C35 C42 1.439(8) . ? N41 C42 1.346(6) . ? N41 C42 1.346(6) 2 ? C42 C43 1.402(8) . ? C43 C44 1.388(8) . ? C43 H43A 0.9500 . ? C44 C43 1.388(8) 2 ? C44 H44A 0.9500 . ? N51 C52 1.326(8) . ? N51 C56 1.337(9) . ? C52 C53 1.390(9) . ? C52 C65 1.457(9) . ? C53 C54 1.376(10) . ? C53 H53A 0.9500 . ? C54 C55 1.360(11) . ? C54 H54A 0.9500 . ? C55 C56 1.367(12) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? N61 N62 1.338(7) . ? N61 C65 1.351(8) . ? N62 C63 1.336(7) . ? N62 C71 1.469(8) . ? C63 C64 1.368(9) . ? C63 H63A 0.9500 . ? C64 C65 1.402(8) . ? C64 H64A 0.9500 . ? C71 C72 1.493(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C77 1.379(8) . ? C72 C73 1.407(8) . ? C73 C74 1.381(9) . ? C73 H73A 0.9500 . ? C74 C75 1.390(8) . ? C74 H74A 0.9500 . ? C75 C76 1.371(8) . ? C75 C78 1.524(8) . ? C76 C77 1.392(9) . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? C78 N82 1.453(8) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? N81 C85 1.346(7) . ? N81 N82 1.356(6) . ? N82 C83 1.365(7) . ? C83 C84 1.333(9) . ? C83 H83A 0.9500 . ? C84 C85 1.395(8) . ? C84 H84A 0.9500 . ? C85 C92 1.455(8) . ? N91 C92 1.330(7) 2 ? N91 C92 1.330(7) . ? C92 C93 1.387(8) . ? C93 C94 1.366(8) . ? C93 H93A 0.9500 . ? C94 C93 1.366(8) 2 ? C94 H94A 0.9500 . ? C100 O100 1.092(11) . ? C100 N100 1.293(14) . ? N100 C102 1.382(13) . ? N100 C101 1.399(18) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? O200 H202 0.8586 . ? O200 H201 0.8461 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Ru1 N91 180.000(2) . . ? N41 Ru1 N31 77.27(13) . . ? N91 Ru1 N31 102.73(13) . . ? N41 Ru1 N31 77.27(13) . 2 ? N91 Ru1 N31 102.73(13) . 2 ? N31 Ru1 N31 154.5(3) . 2 ? N41 Ru1 N81 102.89(13) . . ? N91 Ru1 N81 77.11(13) . . ? N31 Ru1 N81 98.50(16) . . ? N31 Ru1 N81 87.17(16) 2 . ? N41 Ru1 N81 102.89(13) . 2 ? N91 Ru1 N81 77.11(13) . 2 ? N31 Ru1 N81 87.17(16) . 2 ? N31 Ru1 N81 98.50(16) 2 2 ? N81 Ru1 N81 154.2(3) . 2 ? N1 Ag1 N61 135.0(2) . . ? N1 Ag1 N51 151.7(2) . . ? N61 Ag1 N51 72.82(19) . . ? N1 Ag1 N11 71.4(2) . . ? N61 Ag1 N11 121.29(16) . . ? N51 Ag1 N11 99.66(18) . . ? O1 Cl1 O3 99.6(8) . . ? O1 Cl1 O4 114.6(6) . . ? O3 Cl1 O4 106.7(6) . . ? O1 Cl1 O2 113.9(5) . . ? O3 Cl1 O2 112.5(6) . . ? O4 Cl1 O2 109.1(4) . . ? O5 Cl2 O7 110.6(6) . . ? O5 Cl2 O8 109.1(5) . . ? O7 Cl2 O8 109.3(4) . . ? O5 Cl2 O6 109.8(5) . . ? O7 Cl2 O6 107.6(4) . . ? O8 Cl2 O6 110.4(3) . . ? C6 N1 C2 118.1(7) . . ? C6 N1 Ag1 123.4(6) . . ? C2 N1 Ag1 118.5(5) . . ? N1 C2 C3 121.6(7) . . ? N1 C2 C15 116.5(6) . . ? C3 C2 C15 121.5(7) . . ? C2 C3 C4 119.5(8) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 118.4(8) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 C6 120.4(9) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? N1 C6 C5 122.0(9) . . ? N1 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? N12 N11 C15 105.5(5) . . ? N12 N11 Ag1 139.3(4) . . ? C15 N11 Ag1 106.4(4) . . ? N11 N12 C13 111.9(6) . . ? N11 N12 C21 120.3(5) . . ? C13 N12 C21 127.8(6) . . ? N12 C13 C14 105.7(7) . . ? N12 C13 H13A 127.1 . . ? C14 C13 H13A 127.1 . . ? C15 C14 C13 106.1(7) . . ? C15 C14 H14A 127.0 . . ? C13 C14 H14A 127.0 . . ? N11 C15 C14 110.8(7) . . ? N11 C15 C2 119.3(6) . . ? C14 C15 C2 129.8(7) . . ? N12 C21 C22 113.6(5) . . ? N12 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N12 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 118.3(6) . . ? C23 C22 C21 119.2(6) . . ? C27 C22 C21 122.5(6) . . ? C22 C23 C24 121.2(6) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C26 C25 C24 118.9(6) . . ? C26 C25 C28 123.1(6) . . ? C24 C25 C28 117.9(5) . . ? C25 C26 C27 120.0(6) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C22 C27 C26 120.9(6) . . ? C22 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? N32 C28 C25 115.0(5) . . ? N32 C28 H28B 108.5 . . ? C25 C28 H28B 108.5 . . ? N32 C28 H28A 108.5 . . ? C25 C28 H28A 108.5 . . ? H28B C28 H28A 107.5 . . ? C35 N31 N32 106.0(4) . . ? C35 N31 Ru1 114.6(4) . . ? N32 N31 Ru1 139.3(4) . . ? C33 N32 N31 109.7(5) . . ? C33 N32 C28 126.9(5) . . ? N31 N32 C28 123.5(4) . . ? C34 C33 N32 109.1(6) . . ? C34 C33 H33A 125.4 . . ? N32 C33 H33A 125.4 . . ? C33 C34 C35 105.4(6) . . ? C33 C34 H34A 127.3 . . ? C35 C34 H34A 127.3 . . ? N31 C35 C34 109.8(5) . . ? N31 C35 C42 116.0(5) . . ? C34 C35 C42 134.2(6) . . ? C42 N41 C42 122.2(7) . 2 ? C42 N41 Ru1 118.9(4) . . ? C42 N41 Ru1 118.9(4) 2 . ? N41 C42 C43 119.7(6) . . ? N41 C42 C35 113.2(5) . . ? C43 C42 C35 127.1(6) . . ? C44 C43 C42 119.4(6) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C43 C44 C43 119.5(8) . 2 ? C43 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 2 . ? C52 N51 C56 118.2(7) . . ? C52 N51 Ag1 115.3(5) . . ? C56 N51 Ag1 126.0(5) . . ? N51 C52 C53 121.6(6) . . ? N51 C52 C65 117.7(6) . . ? C53 C52 C65 120.7(6) . . ? C54 C53 C52 119.2(7) . . ? C54 C53 H53A 120.4 . . ? C52 C53 H53A 120.4 . . ? C55 C54 C53 118.8(8) . . ? C55 C54 H54A 120.6 . . ? C53 C54 H54A 120.6 . . ? C54 C55 C56 119.0(8) . . ? C54 C55 H55A 120.5 . . ? C56 C55 H55A 120.5 . . ? N51 C56 C55 123.2(8) . . ? N51 C56 H56A 118.4 . . ? C55 C56 H56A 118.4 . . ? N62 N61 C65 106.0(5) . . ? N62 N61 Ag1 139.2(4) . . ? C65 N61 Ag1 114.0(4) . . ? C63 N62 N61 111.2(5) . . ? C63 N62 C71 128.1(6) . . ? N61 N62 C71 120.1(5) . . ? N62 C63 C64 108.3(6) . . ? N62 C63 H63A 125.9 . . ? C64 C63 H63A 125.9 . . ? C63 C64 C65 104.8(6) . . ? C63 C64 H64A 127.6 . . ? C65 C64 H64A 127.6 . . ? N61 C65 C64 109.6(6) . . ? N61 C65 C52 119.5(5) . . ? C64 C65 C52 130.9(6) . . ? N62 C71 C72 109.7(5) . . ? N62 C71 H71A 109.7 . . ? C72 C71 H71A 109.7 . . ? N62 C71 H71B 109.7 . . ? C72 C71 H71B 109.7 . . ? H71A C71 H71B 108.2 . . ? C77 C72 C73 117.9(6) . . ? C77 C72 C71 120.5(6) . . ? C73 C72 C71 121.6(6) . . ? C74 C73 C72 120.0(6) . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 121.4(6) . . ? C73 C74 H74A 119.3 . . ? C75 C74 H74A 119.3 . . ? C76 C75 C74 118.5(6) . . ? C76 C75 C78 120.7(5) . . ? C74 C75 C78 120.7(5) . . ? C75 C76 C77 120.5(6) . . ? C75 C76 H76A 119.7 . . ? C77 C76 H76A 119.7 . . ? C72 C77 C76 121.5(6) . . ? C72 C77 H77A 119.3 . . ? C76 C77 H77A 119.3 . . ? N82 C78 C75 111.6(5) . . ? N82 C78 H78A 109.3 . . ? C75 C78 H78A 109.3 . . ? N82 C78 H78B 109.3 . . ? C75 C78 H78B 109.3 . . ? H78A C78 H78B 108.0 . . ? C85 N81 N82 105.4(4) . . ? C85 N81 Ru1 113.2(4) . . ? N82 N81 Ru1 140.0(4) . . ? N81 N82 C83 109.6(5) . . ? N81 N82 C78 123.7(4) . . ? C83 N82 C78 125.1(5) . . ? C84 C83 N82 108.9(5) . . ? C84 C83 H83A 125.5 . . ? N82 C83 H83A 125.5 . . ? C83 C84 C85 105.5(6) . . ? C83 C84 H84A 127.2 . . ? C85 C84 H84A 127.2 . . ? N81 C85 C84 110.5(5) . . ? N81 C85 C92 117.0(5) . . ? C84 C85 C92 132.5(6) . . ? C92 N91 C92 121.9(7) 2 . ? C92 N91 Ru1 119.1(4) 2 . ? C92 N91 Ru1 119.1(4) . . ? N91 C92 C93 120.1(6) . . ? N91 C92 C85 112.7(5) . . ? C93 C92 C85 127.2(6) . . ? C94 C93 C92 118.6(7) . . ? C94 C93 H93A 120.7 . . ? C92 C93 H93A 120.7 . . ? C93 C94 C93 120.7(9) 2 . ? C93 C94 H94A 119.6 2 . ? C93 C94 H94A 119.6 . . ? O100 C100 N100 129.4(13) . . ? C100 N100 C102 123.8(9) . . ? C100 N100 C101 128.6(14) . . ? C102 N100 C101 102.6(15) . . ? N100 C101 H10A 109.5 . . ? N100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? N100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N100 C102 H10D 109.5 . . ? N100 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N100 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? H202 O200 H201 149.8 . . ? 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 O200 H202 O7 0.86 2.48 3.341(17) 178.7 . O200 H201 O3 0.85 1.70 2.55(2) 178.3 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.104 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.110 #===END data_RuCu4 _database_code_depnum_ccdc_archive 'CCDC 659051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H107 B4 Cu4 F52 N26 O6.50 Ru Sb6' _chemical_formula_weight 4134.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1145(8) _cell_length_b 43.921(2) _cell_length_c 24.9915(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.158(3) _cell_angle_gamma 90.00 _cell_volume 17586.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8060 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7342 _exptl_absorpt_correction_T_max 0.7655 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-2 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 127534 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 23020 _reflns_number_gt 10637 _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23020 _refine_ls_number_parameters 1904 _refine_ls_number_restraints 311 _refine_ls_R_factor_all 0.2086 _refine_ls_R_factor_gt 0.1281 _refine_ls_wR_factor_ref 0.3847 _refine_ls_wR_factor_gt 0.3540 _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_restrained_S_all 1.605 _refine_ls_shift/su_max 0.015 _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 Ru1 Ru 0.04778(10) 0.32921(3) 0.91869(6) 0.0379(5) Uani 1 1 d . . . Cu1 Cu -0.2816(2) 0.38398(8) 0.50443(14) 0.0963(12) Uani 1 1 d . . . Cu2 Cu -0.4756(2) 0.37469(9) 1.17129(14) 0.0988(13) Uani 1 1 d . . . Cu3 Cu 0.2080(2) 0.09522(6) 1.11636(12) 0.0769(10) Uani 1 1 d . . . Cu4 Cu 0.64916(15) 0.45369(6) 0.90641(10) 0.0480(7) Uani 1 1 d . . . C12 C 0.069(2) 0.0925(5) 1.0314(11) 0.077(8) Uani 1 1 d . . . C13 C 0.0149(15) 0.0813(6) 0.9913(11) 0.069(7) Uani 1 1 d . . . H13 H -0.0202 0.0947 0.9693 0.083 Uiso 1 1 calc R . . C14 C 0.011(2) 0.0514(6) 0.9821(13) 0.094(11) Uani 1 1 d . . . H14 H -0.0289 0.0437 0.9546 0.113 Uiso 1 1 calc R . . C15 C 0.060(2) 0.0328(9) 1.0101(16) 0.130(15) Uani 1 1 d . . . H15 H 0.0546 0.0115 1.0034 0.156 Uiso 1 1 calc R . . C16 C 0.120(2) 0.0430(6) 1.0494(14) 0.101(11) Uani 1 1 d . . . H16 H 0.1581 0.0289 1.0670 0.121 Uiso 1 1 calc R . . C22 C 0.1736(15) 0.1578(5) 1.1003(9) 0.050(6) Uani 1 1 d . . . C23 C 0.1280(15) 0.1825(5) 1.0780(8) 0.050(6) Uani 1 1 d . . . H23 H 0.1465 0.2026 1.0867 0.060 Uiso 1 1 calc R . . C24 C 0.0555(17) 0.1782(4) 1.0429(9) 0.054(6) Uani 1 1 d . . . C25 C 0.0390(15) 0.1489(4) 1.0223(9) 0.063(7) Uani 1 1 d . . . H25 H -0.0034 0.1457 0.9934 0.076 Uiso 1 1 calc R . . C26 C 0.085(2) 0.1250(5) 1.0445(11) 0.072(8) Uani 1 1 d . . . C32 C 0.330(2) 0.1256(5) 1.1920(12) 0.073(8) Uani 1 1 d . . . H32 H 0.3462 0.1056 1.2032 0.088 Uiso 1 1 calc R . . C33 C 0.3739(17) 0.1501(9) 1.2159(11) 0.091(9) Uani 1 1 d . . . H33 H 0.4223 0.1467 1.2404 0.110 Uiso 1 1 calc R . . C34 C 0.346(2) 0.1803(7) 1.2040(11) 0.085(8) Uani 1 1 d . . . H34 H 0.3729 0.1975 1.2215 0.101 Uiso 1 1 calc R . . C35 C 0.2816(16) 0.1829(6) 1.1670(11) 0.062(7) Uani 1 1 d . . . H35 H 0.2601 0.2026 1.1573 0.074 Uiso 1 1 calc R . . C36 C 0.2452(15) 0.1576(5) 1.1427(9) 0.049(6) Uani 1 1 d . . . C41 C 0.0077(13) 0.2050(4) 1.0184(9) 0.043(5) Uani 1 1 d . . . C42 C -0.0393(13) 0.2028(4) 0.9710(10) 0.054(6) Uani 1 1 d . . . H42 H -0.0433 0.1840 0.9519 0.064 Uiso 1 1 calc R . . C43 C -0.0819(14) 0.2283(5) 0.9503(9) 0.058(6) Uani 1 1 d . . . H43 H -0.1136 0.2273 0.9161 0.070 Uiso 1 1 calc R . . C44 C -0.0787(13) 0.2565(4) 0.9804(10) 0.049(6) Uani 1 1 d . . . C45 C -0.0360(14) 0.2578(5) 1.0276(9) 0.047(6) Uani 1 1 d . . . H45 H -0.0356 0.2761 1.0480 0.056 Uiso 1 1 calc R . . C46 C 0.0104(13) 0.2319(5) 1.0492(9) 0.051(6) Uani 1 1 d . . . H46 H 0.0422 0.2328 1.0834 0.061 Uiso 1 1 calc R . . C47 C -0.1291(11) 0.2821(4) 0.9533(8) 0.039(5) Uani 1 1 d . . . H47A H -0.1148 0.2844 0.9160 0.047 Uiso 1 1 calc R . . H47B H -0.1892 0.2771 0.9516 0.047 Uiso 1 1 calc R . . C53 C -0.0371(13) 0.3499(5) 1.0112(8) 0.042(5) Uani 1 1 d . . . C54 C -0.0987(15) 0.3475(6) 1.0446(9) 0.058(6) Uani 1 1 d . . . H54 H -0.1089 0.3606 1.0735 0.069 Uiso 1 1 calc R . . C55 C -0.1425(16) 0.3221(6) 1.0268(9) 0.068(8) Uani 1 1 d . . . H55 H -0.1873 0.3135 1.0436 0.082 Uiso 1 1 calc R . . C62 C 0.1360(14) 0.3839(4) 0.9541(9) 0.044(5) Uani 1 1 d . . . C63 C 0.1574(15) 0.4098(6) 0.9868(11) 0.070(7) Uani 1 1 d . . . H63 H 0.2001 0.4236 0.9794 0.084 Uiso 1 1 calc R . . C64 C 0.113(2) 0.4136(6) 1.0290(13) 0.098(10) Uani 1 1 d . . . H64 H 0.1295 0.4298 1.0531 0.118 Uiso 1 1 calc R . . C65 C 0.0434(16) 0.3951(6) 1.0408(9) 0.063(7) Uani 1 1 d . . . H65 H 0.0102 0.3997 1.0690 0.076 Uiso 1 1 calc R . . C66 C 0.0293(16) 0.3702(5) 1.0074(9) 0.050(6) Uani 1 1 d . . . C73 C 0.2557(15) 0.3648(7) 0.8474(10) 0.069(7) Uani 1 1 d . . . H73 H 0.2976 0.3655 0.8234 0.083 Uiso 1 1 calc R . . C74 C 0.2443(14) 0.3861(6) 0.8853(10) 0.063(7) Uani 1 1 d . . . H74 H 0.2743 0.4045 0.8922 0.076 Uiso 1 1 calc R . . C75 C 0.1770(12) 0.3747(4) 0.9126(9) 0.043(5) Uani 1 1 d . . . C81 C 0.1862(14) 0.3180(5) 0.8100(9) 0.065(7) Uani 1 1 d . . . H81A H 0.1672 0.2996 0.8281 0.078 Uiso 1 1 calc R . . H81B H 0.2384 0.3130 0.7944 0.078 Uiso 1 1 calc R . . C82 C 0.1163(14) 0.3288(6) 0.7638(9) 0.057(6) Uani 1 1 d . . . C83 C 0.0920(16) 0.3595(5) 0.7573(11) 0.066(7) Uani 1 1 d . . . H83 H 0.1164 0.3749 0.7806 0.079 Uiso 1 1 calc R . . C84 C 0.0297(14) 0.3665(5) 0.7146(10) 0.056(7) Uani 1 1 d . . . H84 H 0.0123 0.3871 0.7102 0.068 Uiso 1 1 calc R . . C85 C -0.0066(15) 0.3454(5) 0.6793(10) 0.052(6) Uani 1 1 d . . . C86 C 0.0204(16) 0.3149(6) 0.6850(10) 0.066(7) Uani 1 1 d . . . H86 H -0.0017 0.2999 0.6602 0.079 Uiso 1 1 calc R . . C87 C 0.0795(15) 0.3072(5) 0.7271(12) 0.065(7) Uani 1 1 d . . . H87 H 0.0959 0.2865 0.7314 0.078 Uiso 1 1 calc R . . C92 C -0.176(3) 0.4243(6) 0.5642(15) 0.101(11) Uani 1 1 d . . . C93 C -0.137(2) 0.4503(6) 0.5926(11) 0.088(9) Uani 1 1 d . . . H93 H -0.0965 0.4486 0.6229 0.106 Uiso 1 1 calc R . . C94 C -0.166(2) 0.4778(7) 0.5708(13) 0.105(10) Uani 1 1 d . . . H94 H -0.1404 0.4962 0.5844 0.126 Uiso 1 1 calc R . . C95 C -0.231(3) 0.4791(10) 0.5289(14) 0.116(12) Uani 1 1 d . . . H95 H -0.2494 0.4980 0.5133 0.140 Uiso 1 1 calc R . . C96 C -0.271(3) 0.4507(10) 0.5102(13) 0.115(12) Uani 1 1 d . . . H96 H -0.3212 0.4510 0.4863 0.138 Uiso 1 1 calc R . . C102 C -0.150(2) 0.3919(6) 0.5838(14) 0.087(10) Uani 1 1 d . . . C103 C -0.0817(19) 0.3853(6) 0.6241(10) 0.072(7) Uani 1 1 d . . . H103 H -0.0478 0.4011 0.6407 0.086 Uiso 1 1 calc R . . C104 C -0.0671(16) 0.3540(6) 0.6383(10) 0.056(6) Uani 1 1 d . . . C105 C -0.1204(17) 0.3343(6) 0.6119(10) 0.066(7) Uani 1 1 d . . . H105 H -0.1144 0.3133 0.6211 0.079 Uiso 1 1 calc R . . C106 C -0.1847(17) 0.3424(6) 0.5716(10) 0.063(7) Uani 1 1 d . . . C112 C -0.248(2) 0.3231(9) 0.5366(15) 0.114(13) Uani 1 1 d . . . C113 C -0.2442(18) 0.2892(6) 0.5428(12) 0.092(10) Uani 1 1 d . . . H113 H -0.2049 0.2782 0.5665 0.110 Uiso 1 1 calc R . . C114 C -0.309(3) 0.2762(7) 0.5075(16) 0.123(13) Uani 1 1 d . . . H114 H -0.3164 0.2548 0.5094 0.148 Uiso 1 1 calc R . . C115 C -0.365(2) 0.2923(11) 0.4693(13) 0.125(14) Uani 1 1 d . . . H115 H -0.4051 0.2822 0.4447 0.150 Uiso 1 1 calc R . . C116 C -0.357(2) 0.3240(8) 0.4706(12) 0.088(9) Uani 1 1 d . . . H116 H -0.3947 0.3353 0.4463 0.105 Uiso 1 1 calc R . . C122 C -0.4450(17) 0.3327(9) 1.0879(13) 0.088(9) Uani 1 1 d . . . C123 C -0.4500(17) 0.3065(9) 1.0568(14) 0.095(10) Uani 1 1 d . . . H123 H -0.4168 0.3048 1.0278 0.114 Uiso 1 1 calc R . . C124 C -0.501(2) 0.2839(8) 1.0670(13) 0.097(10) Uani 1 1 d . . . H124 H -0.5000 0.2655 1.0470 0.117 Uiso 1 1 calc R . . C125 C -0.551(2) 0.2867(9) 1.1044(17) 0.106(12) Uani 1 1 d . . . H125 H -0.5891 0.2706 1.1096 0.127 Uiso 1 1 calc R . . C126 C -0.552(2) 0.3102(10) 1.1338(16) 0.116(12) Uani 1 1 d . . . H126 H -0.5893 0.3109 1.1606 0.139 Uiso 1 1 calc R . . C132 C -0.3619(15) 0.4069(6) 1.1151(9) 0.053(6) Uani 1 1 d . . . C133 C -0.3071(12) 0.4118(5) 1.0774(8) 0.051(6) Uani 1 1 d . . . H133 H -0.2757 0.4301 1.0781 0.062 Uiso 1 1 calc R . . C134 C -0.2977(12) 0.3899(5) 1.0383(8) 0.039(5) Uani 1 1 d . . . C135 C -0.3408(12) 0.3626(5) 1.0420(8) 0.046(5) Uani 1 1 d . . . H135 H -0.3353 0.3464 1.0175 0.056 Uiso 1 1 calc R . . C136 C -0.3931(13) 0.3600(7) 1.0839(10) 0.056(6) Uani 1 1 d . . . C142 C -0.3770(17) 0.4294(9) 1.1597(10) 0.092(11) Uani 1 1 d . . . C143 C -0.339(2) 0.4591(7) 1.1700(12) 0.088(9) Uani 1 1 d . . . H143 H -0.2942 0.4657 1.1509 0.105 Uiso 1 1 calc R . . C144 C -0.3677(19) 0.4766(8) 1.2064(12) 0.093(10) Uani 1 1 d . . . H144 H -0.3444 0.4963 1.2125 0.111 Uiso 1 1 calc R . . C145 C -0.427(3) 0.4679(8) 1.2343(13) 0.100(13) Uani 1 1 d . . . H145 H -0.4453 0.4813 1.2606 0.120 Uiso 1 1 calc R . . C146 C -0.463(2) 0.4416(11) 1.2272(12) 0.126(14) Uani 1 1 d . . . H146 H -0.5054 0.4371 1.2493 0.151 Uiso 1 1 calc R . . C151 C -0.2432(13) 0.3946(5) 0.9947(9) 0.053(6) Uani 1 1 d . . . C152 C -0.1821(13) 0.4178(4) 0.9981(9) 0.051(6) Uani 1 1 d . . . H152 H -0.1825 0.4327 1.0255 0.061 Uiso 1 1 calc R . . C153 C -0.1226(14) 0.4195(5) 0.9635(9) 0.057(6) Uani 1 1 d . . . H153 H -0.0785 0.4339 0.9687 0.068 Uiso 1 1 calc R . . C154 C -0.1290(12) 0.3987(4) 0.9186(8) 0.038(5) Uani 1 1 d . . . C155 C -0.1921(13) 0.3785(4) 0.9140(8) 0.044(5) Uani 1 1 d . . . H155 H -0.1982 0.3653 0.8836 0.053 Uiso 1 1 calc R . . C156 C -0.2473(12) 0.3762(4) 0.9511(8) 0.037(5) Uani 1 1 d . . . H156 H -0.2901 0.3612 0.9463 0.045 Uiso 1 1 calc R . . C157 C -0.0625(12) 0.4013(5) 0.8776(8) 0.047(5) Uani 1 1 d . . . H15A H -0.0723 0.4201 0.8560 0.056 Uiso 1 1 calc R . . H15B H -0.0059 0.4025 0.8974 0.056 Uiso 1 1 calc R . . C163 C -0.1161(15) 0.3733(5) 0.7983(11) 0.057(6) Uani 1 1 d . . . H163 H -0.1437 0.3898 0.7795 0.068 Uiso 1 1 calc R . . C164 C -0.1219(14) 0.3444(6) 0.7818(8) 0.054(6) Uani 1 1 d . . . H164 H -0.1547 0.3368 0.7508 0.065 Uiso 1 1 calc R . . C165 C -0.0693(12) 0.3273(5) 0.8198(8) 0.042(5) Uani 1 1 d . . . C172 C -0.0390(15) 0.2976(5) 0.8255(9) 0.053(6) Uani 1 1 d . . . C173 C -0.0605(15) 0.2733(5) 0.7933(9) 0.059(6) Uani 1 1 d . . . H173 H -0.1015 0.2756 0.7633 0.070 Uiso 1 1 calc R . . C174 C -0.0225(18) 0.2446(6) 0.8040(11) 0.080(8) Uani 1 1 d . . . H174 H -0.0377 0.2278 0.7810 0.096 Uiso 1 1 calc R . . C175 C 0.0341(14) 0.2411(5) 0.8459(10) 0.049(6) Uani 1 1 d . . . H175 H 0.0619 0.2223 0.8533 0.059 Uiso 1 1 calc R . . C176 C 0.0516(13) 0.2673(5) 0.8796(9) 0.046(6) Uani 1 1 d . . . C183 C 0.1969(15) 0.2593(6) 1.0051(10) 0.058(6) Uani 1 1 d . . . H183 H 0.2360 0.2513 1.0326 0.069 Uiso 1 1 calc R . . C184 C 0.1595(14) 0.2443(5) 0.9629(11) 0.065(7) Uani 1 1 d . . . H184 H 0.1639 0.2232 0.9559 0.078 Uiso 1 1 calc R . . C185 C 0.1081(15) 0.2676(5) 0.9277(11) 0.060(7) Uani 1 1 d . . . C191 C 0.1961(13) 0.3118(5) 1.0418(9) 0.059(6) Uani 1 1 d . . . H19A H 0.1481 0.3253 1.0463 0.071 Uiso 1 1 calc R . . H19B H 0.2148 0.3025 1.0771 0.071 Uiso 1 1 calc R . . C192 C 0.2670(12) 0.3305(5) 1.0227(9) 0.041(5) Uani 1 1 d . . . C193 C 0.2847(15) 0.3580(5) 1.0472(8) 0.056(6) Uani 1 1 d . . . H193 H 0.2524 0.3647 1.0745 0.067 Uiso 1 1 calc R . . C194 C 0.3481(15) 0.3757(5) 1.0327(9) 0.057(6) Uani 1 1 d . . . H194 H 0.3619 0.3941 1.0516 0.068 Uiso 1 1 calc R . . C195 C 0.3912(12) 0.3673(5) 0.9919(9) 0.044(5) Uani 1 1 d . . . C196 C 0.3775(12) 0.3389(5) 0.9671(9) 0.051(6) Uani 1 1 d . . . H196 H 0.4110 0.3321 0.9405 0.061 Uiso 1 1 calc R . . C197 C 0.3120(16) 0.3206(5) 0.9831(9) 0.061(7) Uani 1 1 d . . . H197 H 0.2997 0.3015 0.9662 0.073 Uiso 1 1 calc R . . C202 C 0.6811(13) 0.4210(5) 0.8044(11) 0.062(7) Uani 1 1 d . . . H202 H 0.7162 0.4376 0.7975 0.075 Uiso 1 1 calc R . . C203 C 0.6723(14) 0.3975(7) 0.7665(9) 0.066(7) Uani 1 1 d . . . H203 H 0.7000 0.3988 0.7348 0.079 Uiso 1 1 calc R . . C204 C 0.6247(15) 0.3731(6) 0.7745(9) 0.065(7) Uani 1 1 d . . . H204 H 0.6207 0.3566 0.7498 0.078 Uiso 1 1 calc R . . C205 C 0.5785(14) 0.3725(5) 0.8231(10) 0.064(7) Uani 1 1 d . . . H205 H 0.5428 0.3562 0.8305 0.077 Uiso 1 1 calc R . . C206 C 0.5918(13) 0.3983(6) 0.8575(8) 0.049(6) Uani 1 1 d . . . C212 C 0.5366(12) 0.4331(5) 0.9787(9) 0.042(5) Uani 1 1 d . . . C213 C 0.4839(13) 0.4140(5) 0.9982(8) 0.041(5) Uani 1 1 d . . . H213 H 0.4644 0.4184 1.0318 0.049 Uiso 1 1 calc R . . C214 C 0.4566(12) 0.3880(5) 0.9713(8) 0.046(6) Uani 1 1 d . . . C215 C 0.4924(12) 0.3820(5) 0.9232(8) 0.048(6) Uani 1 1 d . . . H215 H 0.4762 0.3642 0.9031 0.058 Uiso 1 1 calc R . . C216 C 0.5493(12) 0.4009(5) 0.9051(9) 0.044(5) Uani 1 1 d . . . C222 C 0.5710(12) 0.4617(4) 1.0041(8) 0.039(5) Uani 1 1 d . . . C223 C 0.5495(12) 0.4749(5) 1.0497(8) 0.042(5) Uani 1 1 d . . . H223 H 0.5109 0.4648 1.0698 0.051 Uiso 1 1 calc R . . C224 C 0.5806(14) 0.5015(5) 1.0671(8) 0.055(6) Uani 1 1 d . . . H224 H 0.5618 0.5113 1.0975 0.066 Uiso 1 1 calc R . . C225 C 0.6443(14) 0.5152(5) 1.0380(10) 0.061(6) Uani 1 1 d . . . H225 H 0.6713 0.5334 1.0506 0.074 Uiso 1 1 calc R . . C226 C 0.6639(12) 0.5021(4) 0.9945(8) 0.039(5) Uani 1 1 d . . . H226 H 0.7041 0.5117 0.9750 0.047 Uiso 1 1 calc R . . C301 C -0.729(2) 0.3709(9) 1.2321(19) 0.21(3) Uani 1 1 d D . . H30A H -0.7509 0.3504 1.2378 0.318 Uiso 1 1 calc R . . H30B H -0.7645 0.3809 1.2029 0.318 Uiso 1 1 calc R . . H30C H -0.7296 0.3828 1.2652 0.318 Uiso 1 1 calc R . . C302 C -0.638(2) 0.3685(8) 1.2168(19) 0.20(2) Uani 1 1 d D . . C304 C 0.1406(16) 0.0447(6) 1.2730(9) 0.098(10) Uani 1 1 d D . . H30D H 0.1445 0.0227 1.2668 0.148 Uiso 1 1 calc R . . H30E H 0.0871 0.0493 1.2865 0.148 Uiso 1 1 calc R . . H30F H 0.1864 0.0511 1.2996 0.148 Uiso 1 1 calc R . . C305 C 0.1466(16) 0.0621(5) 1.2190(10) 0.081(9) Uani 1 1 d D . . C307 C 0.4139(16) 0.0224(6) 1.1475(14) 0.123(11) Uani 1 1 d D . . H30G H 0.4691 0.0319 1.1545 0.184 Uiso 1 1 calc R . . H30H H 0.4141 0.0080 1.1176 0.184 Uiso 1 1 calc R . . H30I H 0.4006 0.0116 1.1798 0.184 Uiso 1 1 calc R . . C308 C 0.3468(16) 0.0476(6) 1.1326(12) 0.084(9) Uani 1 1 d D . . C310 C -0.472(3) 0.4196(12) 0.384(2) 0.25(3) Uiso 1 1 d D . . H30J H -0.5212 0.4251 0.4012 0.381 Uiso 1 1 calc R . . H30K H -0.4878 0.4052 0.3543 0.381 Uiso 1 1 calc R . . H30L H -0.4483 0.4380 0.3688 0.381 Uiso 1 1 calc R . . C311 C -0.405(2) 0.4046(9) 0.4255(15) 0.147(14) Uiso 1 1 d D . . C313 C 0.8654(15) 0.5116(5) 0.8624(12) 0.096(10) Uani 1 1 d D . . H30M H 0.8554 0.5318 0.8771 0.144 Uiso 1 1 calc R . . H30N H 0.8625 0.5128 0.8231 0.144 Uiso 1 1 calc R . . H30O H 0.9209 0.5044 0.8769 0.144 Uiso 1 1 calc R . . C314 C 0.7977(14) 0.4890(5) 0.8785(10) 0.072(8) Uani 1 1 d D . . N11 N 0.1248(14) 0.0740(4) 1.0644(9) 0.094(7) Uani 1 1 d . . . N21 N 0.1471(12) 0.1298(4) 1.0843(8) 0.055(5) Uani 1 1 d . . . N31 N 0.2694(15) 0.1292(4) 1.1549(8) 0.077(7) Uani 1 1 d . . . N51 N -0.1132(11) 0.3110(4) 0.9822(7) 0.048(5) Uani 1 1 d . . . N52 N -0.0403(9) 0.3280(4) 0.9728(7) 0.040(4) Uani 1 1 d . . . N61 N 0.0740(10) 0.3654(4) 0.9677(7) 0.044(4) Uani 1 1 d . . . N71 N 0.1508(10) 0.3489(4) 0.8872(7) 0.047(4) Uani 1 1 d . . . N72 N 0.2006(11) 0.3431(4) 0.8488(7) 0.046(4) Uani 1 1 d . . . N91 N -0.2379(18) 0.4248(6) 0.5260(10) 0.094(8) Uani 1 1 d . . . N101 N -0.1969(12) 0.3712(5) 0.5590(7) 0.062(5) Uani 1 1 d . . . N111 N -0.3041(18) 0.3393(6) 0.5009(11) 0.100(9) Uani 1 1 d . . . N121 N -0.4963(14) 0.3365(5) 1.1285(9) 0.089(7) Uani 1 1 d . . . N131 N -0.4024(12) 0.3809(6) 1.1164(8) 0.066(6) Uani 1 1 d . . . N141 N -0.4433(14) 0.4173(6) 1.1879(8) 0.093(8) Uani 1 1 d . . . N161 N -0.0359(9) 0.3486(4) 0.8588(6) 0.037(4) Uani 1 1 d . . . N162 N -0.0674(11) 0.3761(4) 0.8438(7) 0.044(4) Uani 1 1 d . . . N171 N 0.0167(11) 0.2934(3) 0.8688(7) 0.039(4) Uani 1 1 d . . . N181 N 0.1191(10) 0.2936(4) 0.9560(8) 0.048(4) Uani 1 1 d . . . N182 N 0.1696(10) 0.2871(4) 1.0013(7) 0.047(4) Uani 1 1 d . . . N201 N 0.6443(10) 0.4218(4) 0.8490(7) 0.046(4) Uani 1 1 d . . . N211 N 0.5709(9) 0.4259(4) 0.9332(7) 0.043(4) Uani 1 1 d . . . N221 N 0.6305(10) 0.4756(5) 0.9753(6) 0.052(5) Uani 1 1 d . . . N303 N -0.576(2) 0.3747(10) 1.2087(17) 0.071(13) Uiso 0.50 1 d PD . . N306 N 0.1593(17) 0.0767(5) 1.1862(10) 0.095(8) Uani 1 1 d D . . N309 N 0.3003(14) 0.0648(5) 1.1218(9) 0.090(7) Uani 1 1 d D . . N312 N -0.359(2) 0.3931(7) 0.4525(13) 0.052(9) Uiso 0.50 1 d PD . . N315 N 0.7487(11) 0.4748(5) 0.8911(8) 0.077(7) Uani 1 1 d D . . O1 O 0.5695(8) 0.4869(3) 0.8562(6) 0.059(4) Uani 1 1 d . . . O2 O -0.380(3) 0.3562(8) 1.2362(11) 0.128(18) Uani 0.50 1 d P . . O3 O 0.8350(19) 0.3724(7) 0.4454(10) 0.189(12) Uani 1 1 d . . . O4 O 0.5531(9) 0.3944(4) 0.6097(6) 0.078(5) Uiso 1 1 d . . . O03 O 0.903(2) 0.4083(9) 0.1503(16) 0.114(13) Uiso 0.50 1 d P . . O04 O 0.601(3) 0.9783(10) 0.1925(17) 0.123(14) Uiso 0.50 1 d P A 1 O05 O 0.6858(19) 0.1747(6) 0.1716(12) 0.192(11) Uiso 1 1 d . . . O06 O 0.058(3) 0.3068(11) 0.126(2) 0.157(18) Uiso 0.50 1 d P B 2 O07 O 0.015(4) 0.3281(15) 0.197(3) 0.23(3) Uiso 0.50 1 d P C 1 B1 B 0.6701(6) 0.9398(2) 0.3709(4) 0.077(10) Uani 1 1 d D . . B2 B 0.3969(6) 0.4352(2) 0.8023(4) 0.047(7) Uani 1 1 d D . . B8 B 0.6447(7) 0.1910(2) 0.4184(4) 0.100 Uiso 1 1 d D . . B9 B 0.8895(6) 0.4537(2) 0.7335(4) 0.043(6) Uiso 1 1 d GD . . F1 F 0.5926(7) 0.9319(3) 0.3844(5) 0.113(6) Uani 1 1 d D . . F2 F 0.7182(8) 0.9503(3) 0.4157(5) 0.110(5) Uani 1 1 d D . . F3 F 0.6618(8) 0.9621(3) 0.3322(5) 0.097(5) Uani 1 1 d D . . F4 F 0.7080(9) 0.9148(3) 0.3515(6) 0.135(7) Uani 1 1 d D . . F5 F 0.3342(7) 0.4450(3) 0.7655(5) 0.111(5) Uani 1 1 d D . . F6 F 0.4030(7) 0.4043(2) 0.7998(5) 0.084(4) Uani 1 1 d D . . F7 F 0.4704(7) 0.4481(3) 0.7915(5) 0.092(4) Uani 1 1 d D . . F8 F 0.3805(8) 0.4433(3) 0.8527(5) 0.112(5) Uani 1 1 d D . . F11 F 0.9610(5) 1.02906(17) 0.5615(3) 0.075(4) Uani 1 1 d D . . F12 F 0.8275(5) 0.96410(16) 0.5978(3) 0.071(4) Uani 1 1 d D . . F13 F 0.9834(5) 0.96939(19) 0.5747(3) 0.084(4) Uani 1 1 d D . . F14 F 0.8051(5) 1.02331(18) 0.5847(3) 0.082(4) Uani 1 1 d D . . F15 F 0.8585(5) 0.9901(2) 0.5066(3) 0.076(4) Uani 1 1 d D . . F16 F 0.9301(5) 1.0027(2) 0.6525(3) 0.067(4) Uani 1 1 d D . . F21 F 0.3283(14) 0.2916(6) 0.2595(10) 0.145(10) Uiso 0.672(9) 1 d PD D 1 F22 F 0.1729(16) 0.2897(8) 0.2446(14) 0.169(12) Uiso 0.672(9) 1 d PD D 1 F23 F 0.3265(13) 0.2562(6) 0.1809(10) 0.230 Uiso 1 1 d D . . F24 F 0.2573(14) 0.3029(4) 0.1740(8) 0.102(7) Uiso 0.672(9) 1 d PDU D 1 F25 F 0.2564(11) 0.2390(3) 0.2566(7) 0.130(6) Uani 1 1 d D . . F26 F 0.244(4) 0.2564(12) 0.1352(13) 0.137(11) Uiso 0.328(9) 1 d PDU D 2 F31 F 0.8895(10) 0.2833(6) 0.1423(10) 0.202(10) Uani 1 1 d D E . F32 F 0.8165(13) 0.2902(6) 0.2327(5) 0.176(9) Uani 1 1 d D E . F33 F 0.824(4) 0.2423(6) 0.165(2) 0.144(11) Uiso 0.41(3) 1 d PDU E 1 F34 F 0.685(2) 0.2993(14) 0.182(2) 0.148(11) Uiso 0.41(3) 1 d PDU E 1 F35 F 0.800(4) 0.3223(5) 0.148(2) 0.132(11) Uiso 0.41(3) 1 d PDU E 1 F36 F 0.778(3) 0.2685(10) 0.0905(8) 0.106(9) Uiso 0.41(3) 1 d PDU E 1 F41 F 0.240(2) 0.9879(7) 0.1040(14) 0.144(10) Uiso 0.50 1 d PDU F 1 F42 F 0.150(3) 0.9246(9) 0.116(2) 0.212(16) Uiso 0.50 1 d PDU F 1 F43 F 0.0968(19) 0.9774(11) 0.138(2) 0.21(2) Uiso 0.50 1 d PD F 1 F44 F 0.251(5) 0.9263(11) 0.183(3) 0.26(2) Uiso 0.50 1 d PDU F 1 F45 F 0.296(2) 0.9366(11) 0.150(2) 0.164(12) Uiso 0.50 1 d PDU F 1 F46 F 0.226(3) 0.9873(8) 0.2000(14) 0.145(11) Uiso 0.50 1 d PDU F 1 F51 F -0.0275(14) 0.3690(6) 0.3918(9) 0.24(3) Uani 0.50 1 d PD . . F52 F -0.0062(18) 0.3301(4) 0.3172(12) 0.19(2) Uani 0.50 1 d PD . . F53 F 0.1036(14) 0.3348(5) 0.4028(8) 0.120(13) Uani 0.50 1 d PD . . F54 F 0.1165(19) 0.3936(4) 0.3852(11) 0.200 Uiso 0.50 1 d PD . . F55 F 0.1448(14) 0.3540(6) 0.3071(10) 0.28(4) Uani 0.50 1 d PD . . F56 F 0.007(2) 0.3889(5) 0.2995(11) 0.200 Uiso 0.50 1 d PD . . F61 F 0.392(3) 0.3389(9) 0.5641(13) 0.155(12) Uiso 0.50 1 d PDU G 1 F62 F 0.410(3) 0.2826(6) 0.489(2) 0.181(14) Uiso 0.50 1 d PDU G 1 F63 F 0.2730(10) 0.3163(10) 0.5052(18) 0.150(11) Uiso 0.50 1 d PDU G 1 F64 F 0.4355(13) 0.3379(5) 0.4763(8) 0.185(9) Uani 1 1 d D . . F65 F 0.326(2) 0.2918(7) 0.5473(13) 0.130(10) Uiso 0.50 1 d PDU G 1 F66 F 0.467(2) 0.3122(14) 0.550(2) 0.227(19) Uiso 0.50 1 d PDU G 1 F71 F 0.604(2) 0.5217(18) 0.482(3) 0.27(2) Uiso 0.50 1 d PDU . 1 F72 F 0.459(3) 0.5286(12) 0.4514(16) 0.195(15) Uiso 0.50 1 d PDU . 1 F73 F 0.4626(17) 0.5249(6) 0.5483(10) 0.200 Uiso 1 1 d D . . F81 F 0.6929(13) 0.1714(4) 0.4030(7) 0.26(3) Uiso 0.40 1 d PD . . F81' F 0.5973(14) 0.2083(4) 0.3722(8) 0.054(6) Uiso 0.60 1 d P . . F82 F 0.5744(10) 0.1794(4) 0.4208(6) 0.152(7) Uiso 1 1 d D . . F83 F 0.6735(9) 0.2007(3) 0.4636(5) 0.108(5) Uiso 1 1 d D . . F84 F 0.6377(6) 0.21226(18) 0.3856(3) 0.015(2) Uiso 1 1 d D . . F21' F 0.147(7) 0.302(3) 0.269(4) 0.30(5) Uiso 0.328(9) 1 d PD D 2 F22' F 0.0786(13) 0.275(2) 0.204(5) 0.28(5) Uiso 0.328(9) 1 d PD D 2 F24' F 0.209(3) 0.3234(6) 0.1695(18) 0.114(9) Uiso 0.328(9) 1 d PDU D 2 F26' F 0.1955(16) 0.2514(6) 0.1679(9) 0.138(9) Uiso 0.672(9) 1 d PDU D 1 F33' F 0.780(3) 0.2409(4) 0.1810(15) 0.145(10) Uiso 0.59(3) 1 d PDU E 2 F34' F 0.6723(11) 0.2805(10) 0.1793(15) 0.146(11) Uiso 0.59(3) 1 d PDU E 2 F35' F 0.756(2) 0.3218(4) 0.1442(15) 0.133(10) Uiso 0.59(3) 1 d PDU E 2 F36' F 0.734(2) 0.2784(7) 0.0906(7) 0.106(8) Uiso 0.59(3) 1 d PDU E 2 F41' F 0.166(2) 0.9798(8) 0.0832(10) 0.129(10) Uiso 0.50 1 d PDU F 2 F42' F 0.188(4) 0.9296(11) 0.0921(18) 0.212(16) Uiso 0.50 1 d PDU F 2 F43' F 0.130(2) 0.9297(9) 0.1747(19) 0.178(17) Uiso 0.50 1 d PD F 2 F44' F 0.230(4) 0.9418(16) 0.2154(16) 0.26(2) Uiso 0.50 1 d PDU F 2 F45' F 0.3090(15) 0.9558(11) 0.1285(18) 0.157(12) Uiso 0.50 1 d PDU F 2 F46' F 0.239(3) 0.9972(6) 0.1718(17) 0.146(11) Uiso 0.50 1 d PDU F 2 F61' F 0.331(3) 0.3461(6) 0.5410(18) 0.157(12) Uiso 0.50 1 d PDU H 2 F62' F 0.361(3) 0.2767(9) 0.4615(14) 0.184(14) Uiso 0.50 1 d PDU H 2 F63' F 0.299(2) 0.3106(9) 0.4631(13) 0.152(11) Uiso 0.50 1 d PDU H 2 F65' F 0.342(2) 0.2732(7) 0.5766(13) 0.135(10) Uiso 0.50 1 d PDU H 2 F66' F 0.436(4) 0.3350(12) 0.5893(19) 0.228(19) Uiso 0.50 1 d PDU H 2 F71' F 0.592(4) 0.4960(18) 0.475(3) 0.27(2) Uiso 0.50 1 d PDU . 2 F72' F 0.452(3) 0.5056(14) 0.4465(15) 0.196(15) Uiso 0.50 1 d PDU . 2 F91 F 0.8718(9) 0.4829(2) 0.7110(6) 0.135(6) Uiso 1 1 d GD . . F92 F 0.8817(9) 0.4518(3) 0.7902(3) 0.128(6) Uiso 1 1 d GD . . F93 F 0.9596(6) 0.4349(3) 0.7245(6) 0.135(6) Uiso 1 1 d GD . . F94 F 0.8248(6) 0.4329(2) 0.7120(5) 0.099(5) Uiso 1 1 d GD . . Sb1 Sb 0.89459(9) 0.99638(3) 0.57932(6) 0.0549(5) Uani 1 1 d D . . Sb2 Sb 0.2547(3) 0.27210(8) 0.21729(12) 0.0774(12) Uiso 0.672(9) 1 d PDU D 1 Sb3 Sb 0.78114(15) 0.28155(6) 0.16110(9) 0.1245(10) Uani 1 1 d D . . Sb4 Sb 0.19948(18) 0.95886(6) 0.14724(10) 0.1308(10) Uani 1 1 d D . . Sb5 Sb 0.0588(3) 0.36161(9) 0.34941(16) 0.1000(14) Uani 0.50 1 d PD . . Sb6 Sb 0.3770(3) 0.31593(13) 0.5108(2) 0.1068(17) Uiso 0.50 1 d PDU G 1 Sb7 Sb 0.5147(6) 0.51180(14) 0.5011(4) 0.153(3) Uani 0.50 1 d PD . . Sb2' Sb 0.2154(6) 0.27889(15) 0.2096(2) 0.071(2) Uiso 0.328(9) 1 d PDU D 2 Sb6' Sb 0.3920(4) 0.30519(14) 0.5276(2) 0.1175(19) Uiso 0.50 1 d PDU H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0420(11) 0.0263(9) 0.0462(11) 0.0021(7) 0.0080(8) 0.0012(8) Cu1 0.122(3) 0.089(3) 0.076(2) 0.0107(19) 0.001(2) 0.012(2) Cu2 0.088(2) 0.136(3) 0.080(2) 0.040(2) 0.044(2) 0.031(2) Cu3 0.113(3) 0.0405(17) 0.077(2) 0.0201(15) 0.0112(19) 0.0252(18) Cu4 0.0411(16) 0.0524(17) 0.0503(18) -0.0050(13) 0.0036(12) 0.0011(14) C12 0.12(2) 0.031(15) 0.08(2) 0.039(14) 0.022(18) 0.044(17) C13 0.069(18) 0.055(19) 0.08(2) 0.019(15) -0.013(15) 0.013(15) C14 0.09(2) 0.05(2) 0.13(3) 0.050(18) -0.015(19) 0.034(18) C15 0.11(3) 0.13(4) 0.15(3) -0.08(3) 0.02(2) -0.06(3) C16 0.13(3) 0.031(16) 0.15(3) 0.041(17) 0.04(2) 0.016(18) C22 0.078(18) 0.034(14) 0.046(15) 0.024(12) 0.040(14) 0.017(14) C23 0.075(17) 0.046(14) 0.032(14) 0.007(11) 0.026(13) 0.001(14) C24 0.092(19) 0.032(14) 0.044(15) 0.025(11) 0.034(14) 0.006(14) C25 0.099(19) 0.015(12) 0.075(17) 0.026(11) 0.004(14) -0.008(13) C26 0.11(2) 0.044(17) 0.071(19) 0.014(14) 0.049(18) 0.026(17) C32 0.14(3) 0.023(13) 0.062(19) 0.015(13) 0.033(19) 0.003(17) C33 0.07(2) 0.13(3) 0.07(2) 0.01(2) -0.002(15) 0.02(2) C34 0.10(2) 0.08(2) 0.08(2) 0.025(16) 0.011(19) 0.006(19) C35 0.062(17) 0.058(18) 0.068(18) 0.042(15) 0.021(14) 0.032(15) C36 0.077(18) 0.032(14) 0.039(15) 0.012(12) 0.020(13) 0.001(14) C41 0.054(14) 0.030(13) 0.045(15) 0.008(11) 0.012(12) 0.007(11) C42 0.056(15) 0.027(12) 0.078(19) 0.024(12) 0.010(14) 0.011(12) C43 0.062(16) 0.040(14) 0.073(17) 0.017(12) 0.010(13) -0.003(13) C44 0.041(13) 0.025(12) 0.082(19) 0.010(12) 0.012(13) -0.003(11) C45 0.067(15) 0.047(14) 0.027(14) 0.006(10) 0.003(12) -0.001(12) C46 0.058(14) 0.043(14) 0.052(15) 0.027(12) 0.011(11) 0.000(12) C47 0.030(12) 0.017(10) 0.071(15) 0.004(10) 0.006(10) -0.011(10) C53 0.044(14) 0.038(14) 0.046(15) 0.010(11) 0.010(12) -0.004(13) C54 0.059(16) 0.051(16) 0.063(17) 0.023(13) 0.003(14) 0.018(14) C55 0.084(19) 0.078(19) 0.050(17) 0.049(14) 0.046(15) 0.015(17) C62 0.055(15) 0.015(11) 0.060(16) 0.002(11) 0.002(13) 0.013(12) C63 0.063(17) 0.09(2) 0.057(18) 0.011(15) 0.010(14) -0.011(15) C64 0.13(3) 0.061(19) 0.09(2) -0.028(17) -0.03(2) -0.01(2) C65 0.083(19) 0.054(16) 0.052(16) 0.007(13) 0.001(13) 0.002(15) C66 0.086(19) 0.025(13) 0.038(15) 0.008(11) 0.002(14) 0.020(14) C73 0.054(16) 0.10(2) 0.059(18) 0.008(16) 0.018(13) 0.003(17) C74 0.051(16) 0.061(16) 0.075(19) 0.030(15) -0.010(14) 0.016(14) C75 0.031(13) 0.024(12) 0.073(17) 0.003(12) -0.001(12) -0.012(11) C81 0.063(16) 0.066(17) 0.073(18) 0.003(14) 0.042(15) -0.001(14) C82 0.051(15) 0.075(19) 0.051(16) -0.003(14) 0.027(13) 0.000(15) C83 0.081(19) 0.038(15) 0.09(2) -0.007(13) 0.046(17) 0.004(14) C84 0.037(14) 0.059(17) 0.077(19) 0.028(15) 0.025(13) 0.018(13) C85 0.051(16) 0.038(15) 0.069(19) -0.012(13) 0.017(14) -0.006(14) C86 0.067(18) 0.08(2) 0.057(18) -0.042(14) 0.029(15) 0.001(16) C87 0.053(16) 0.050(16) 0.10(2) -0.014(16) 0.034(16) -0.002(14) C92 0.16(3) 0.05(2) 0.10(3) -0.001(19) 0.07(3) -0.01(2) C93 0.15(3) 0.040(16) 0.073(19) 0.021(15) 0.014(18) 0.020(18) C94 0.16(3) 0.08(2) 0.08(2) -0.001(18) 0.03(2) -0.01(2) C95 0.15(3) 0.13(3) 0.07(2) 0.04(2) 0.03(2) 0.06(3) C96 0.16(4) 0.10(3) 0.09(3) -0.01(2) 0.04(2) 0.00(3) C102 0.12(3) 0.042(18) 0.11(3) 0.001(17) 0.08(2) 0.026(19) C103 0.11(2) 0.047(17) 0.052(17) 0.008(13) -0.002(16) -0.015(16) C104 0.059(16) 0.062(18) 0.045(16) -0.014(13) -0.001(14) -0.006(15) C105 0.076(19) 0.056(17) 0.066(18) 0.018(14) 0.011(16) 0.032(16) C106 0.09(2) 0.039(15) 0.068(18) -0.021(13) 0.030(16) 0.004(16) C112 0.11(3) 0.14(3) 0.11(3) -0.07(3) 0.08(2) -0.07(3) C113 0.10(2) 0.07(2) 0.11(2) -0.053(17) 0.021(18) -0.050(18) C114 0.17(4) 0.057(19) 0.16(4) -0.01(2) 0.09(3) -0.01(2) C115 0.10(3) 0.19(4) 0.08(2) 0.00(3) -0.014(19) 0.07(3) C116 0.10(2) 0.07(2) 0.09(2) -0.001(17) -0.016(19) 0.04(2) C122 0.067(19) 0.12(3) 0.08(2) 0.06(2) 0.034(18) 0.01(2) C123 0.07(2) 0.11(3) 0.12(3) 0.03(2) 0.041(18) -0.03(2) C124 0.09(2) 0.11(3) 0.10(2) 0.025(19) 0.04(2) 0.01(2) C125 0.07(2) 0.11(3) 0.13(4) 0.01(2) -0.03(2) -0.03(2) C126 0.09(2) 0.14(3) 0.13(3) 0.06(3) 0.05(2) 0.00(3) C132 0.060(16) 0.059(16) 0.038(15) 0.007(12) 0.004(13) 0.021(14) C133 0.046(14) 0.062(16) 0.048(15) 0.020(13) 0.013(12) 0.008(12) C134 0.035(12) 0.038(13) 0.041(14) 0.004(11) -0.013(11) 0.017(12) C135 0.043(13) 0.058(15) 0.040(14) 0.015(11) 0.009(11) 0.000(12) C136 0.037(14) 0.078(19) 0.051(17) 0.021(15) -0.003(13) 0.026(15) C142 0.07(2) 0.17(3) 0.033(17) 0.04(2) 0.004(15) 0.07(2) C143 0.11(2) 0.063(18) 0.09(2) 0.000(17) -0.015(18) 0.022(19) C144 0.08(2) 0.14(3) 0.048(19) -0.04(2) -0.003(16) 0.04(2) C145 0.15(4) 0.10(3) 0.05(2) -0.031(19) -0.01(2) 0.04(3) C146 0.12(3) 0.21(4) 0.05(2) 0.00(3) 0.020(19) 0.09(3) C151 0.049(14) 0.053(15) 0.060(17) 0.002(12) 0.020(12) 0.018(13) C152 0.058(15) 0.030(12) 0.068(16) -0.014(11) 0.024(13) -0.009(13) C153 0.056(15) 0.052(15) 0.064(17) -0.009(12) 0.015(13) -0.011(13) C154 0.040(13) 0.019(11) 0.057(15) 0.001(10) 0.015(11) 0.006(11) C155 0.063(15) 0.018(11) 0.051(15) 0.004(9) 0.007(12) 0.002(12) C156 0.036(12) 0.042(13) 0.032(13) -0.005(10) -0.005(10) -0.001(10) C157 0.046(13) 0.042(13) 0.051(15) 0.002(11) -0.003(11) 0.001(11) C163 0.057(16) 0.054(17) 0.066(19) 0.015(14) 0.042(15) 0.001(14) C164 0.057(15) 0.078(18) 0.028(14) -0.005(13) 0.004(11) -0.008(15) C165 0.033(12) 0.060(16) 0.032(14) -0.014(12) -0.005(10) -0.017(12) C172 0.070(17) 0.050(16) 0.039(15) -0.011(12) 0.007(13) 0.013(14) C173 0.077(17) 0.047(15) 0.051(16) -0.013(12) 0.003(13) 0.001(14) C174 0.10(2) 0.07(2) 0.07(2) -0.034(16) 0.029(18) -0.037(18) C175 0.058(15) 0.038(14) 0.053(16) -0.002(12) 0.013(13) 0.000(12) C176 0.037(13) 0.059(17) 0.043(15) 0.003(12) 0.004(12) -0.013(13) C183 0.059(16) 0.049(16) 0.065(18) -0.013(13) 0.003(13) 0.008(14) C184 0.048(15) 0.043(14) 0.11(2) 0.027(15) 0.033(15) 0.030(13) C185 0.064(17) 0.023(13) 0.10(2) 0.011(13) 0.051(17) 0.011(13) C191 0.051(15) 0.055(15) 0.072(17) 0.009(13) 0.012(12) -0.001(13) C192 0.032(12) 0.032(13) 0.057(15) 0.017(11) -0.004(11) 0.001(11) C193 0.065(17) 0.062(16) 0.040(14) -0.008(12) 0.008(12) 0.005(15) C194 0.058(16) 0.049(15) 0.062(17) -0.002(12) -0.003(14) -0.009(14) C195 0.033(12) 0.049(14) 0.051(15) 0.009(12) 0.004(11) -0.005(12) C196 0.025(12) 0.058(16) 0.071(16) -0.017(13) 0.011(11) 0.004(12) C197 0.072(18) 0.052(15) 0.050(16) 0.000(12) -0.025(14) 0.006(15) C202 0.036(13) 0.064(17) 0.09(2) 0.014(15) 0.012(14) -0.005(13) C203 0.041(15) 0.10(2) 0.058(17) -0.032(16) 0.014(12) 0.022(16) C204 0.059(16) 0.09(2) 0.049(16) -0.033(14) 0.026(13) 0.011(16) C205 0.057(16) 0.058(16) 0.071(18) -0.006(13) -0.019(14) 0.006(13) C206 0.039(13) 0.074(18) 0.033(14) 0.000(12) -0.009(11) 0.024(14) C212 0.028(12) 0.045(14) 0.051(16) -0.004(12) -0.007(11) 0.019(12) C213 0.052(14) 0.035(13) 0.034(13) -0.001(10) -0.003(11) 0.009(12) C214 0.046(14) 0.038(13) 0.053(15) 0.003(11) -0.008(12) 0.024(12) C215 0.035(12) 0.063(15) 0.045(15) -0.013(12) -0.002(11) 0.001(13) C216 0.031(13) 0.034(13) 0.063(16) 0.000(12) -0.009(12) -0.005(12) C222 0.037(12) 0.033(12) 0.046(15) 0.017(11) 0.001(11) -0.004(11) C223 0.049(14) 0.037(13) 0.041(14) 0.007(11) 0.005(11) -0.013(12) C224 0.067(16) 0.056(16) 0.037(14) -0.008(12) -0.007(12) -0.002(14) C225 0.054(15) 0.053(15) 0.076(19) -0.008(14) -0.001(14) -0.011(13) C226 0.045(13) 0.030(12) 0.043(14) -0.011(10) 0.009(11) 0.012(11) C301 0.18(4) 0.17(4) 0.32(6) 0.15(4) 0.20(4) 0.11(3) C302 0.29(7) 0.09(3) 0.22(5) 0.10(3) 0.02(5) -0.02(4) C304 0.09(2) 0.13(2) 0.08(2) 0.062(18) 0.021(16) 0.010(18) C305 0.067(18) 0.044(17) 0.13(3) -0.016(16) -0.009(19) 0.004(15) C307 0.10(2) 0.10(2) 0.16(3) -0.02(2) 0.01(2) -0.03(2) C308 0.07(2) 0.061(19) 0.12(2) 0.015(16) 0.003(17) 0.032(16) C313 0.09(2) 0.057(16) 0.15(3) -0.024(16) 0.09(2) -0.032(16) C314 0.064(19) 0.09(2) 0.067(19) -0.026(15) 0.019(15) 0.031(17) N11 0.117(18) 0.037(12) 0.12(2) 0.008(12) -0.003(15) 0.022(13) N21 0.054(13) 0.055(14) 0.059(14) 0.012(10) 0.019(11) 0.021(11) N31 0.114(18) 0.066(16) 0.051(14) 0.043(11) 0.004(13) 0.043(13) N51 0.054(12) 0.046(12) 0.044(12) 0.021(9) 0.010(9) 0.022(10) N52 0.033(10) 0.036(10) 0.052(12) 0.011(9) 0.003(9) 0.009(9) N61 0.037(10) 0.030(10) 0.063(13) 0.009(9) -0.005(10) -0.013(9) N71 0.035(10) 0.047(12) 0.058(12) 0.014(9) 0.004(9) -0.004(10) N72 0.034(10) 0.032(10) 0.075(14) 0.003(9) 0.024(10) -0.010(10) N91 0.13(2) 0.10(2) 0.056(17) 0.019(15) -0.003(15) 0.029(17) N101 0.072(14) 0.060(15) 0.051(13) -0.008(11) 0.000(10) 0.018(13) N111 0.085(19) 0.12(2) 0.09(2) -0.002(17) -0.034(15) 0.018(18) N121 0.082(15) 0.096(18) 0.093(18) 0.045(14) 0.023(14) -0.005(15) N131 0.070(14) 0.086(17) 0.049(14) 0.021(12) 0.041(11) 0.037(14) N141 0.097(17) 0.15(2) 0.030(13) 0.006(13) -0.004(12) 0.064(17) N161 0.043(10) 0.037(10) 0.031(10) 0.009(8) 0.014(8) 0.008(9) N162 0.049(11) 0.044(12) 0.038(12) 0.005(9) -0.006(10) 0.006(10) N171 0.046(11) 0.014(9) 0.061(13) -0.004(8) 0.017(10) 0.008(9) N181 0.050(11) 0.030(11) 0.064(13) 0.001(9) 0.006(10) 0.013(9) N182 0.039(11) 0.043(12) 0.057(13) 0.008(10) -0.002(10) 0.000(10) N201 0.039(10) 0.051(12) 0.049(12) -0.001(9) 0.009(9) -0.005(10) N211 0.029(10) 0.051(12) 0.045(12) 0.001(9) -0.007(9) 0.001(9) N221 0.044(11) 0.081(15) 0.028(10) 0.003(10) -0.006(9) 0.012(11) N306 0.14(2) 0.043(14) 0.11(2) 0.028(12) 0.035(16) 0.032(15) N309 0.098(18) 0.078(16) 0.097(18) 0.031(13) 0.028(14) 0.041(15) N315 0.037(13) 0.13(2) 0.067(15) 0.015(13) 0.011(11) 0.007(13) O1 0.050(9) 0.046(9) 0.082(11) -0.001(8) 0.008(8) 0.014(8) O2 0.26(5) 0.10(3) 0.023(19) 0.012(17) 0.02(2) 0.11(3) O3 0.23(3) 0.23(3) 0.111(19) -0.016(19) 0.065(19) -0.09(2) B1 0.15(4) 0.041(18) 0.04(2) 0.002(15) 0.01(2) -0.01(2) B2 0.047(18) 0.058(19) 0.031(17) -0.018(13) -0.012(13) 0.009(16) F1 0.077(10) 0.177(17) 0.083(11) 0.049(11) 0.009(9) 0.014(11) F2 0.110(12) 0.095(12) 0.117(14) 0.022(10) -0.023(10) 0.006(10) F3 0.108(11) 0.103(12) 0.084(11) 0.005(9) 0.025(9) 0.029(10) F4 0.186(18) 0.094(12) 0.132(15) -0.021(11) 0.047(13) 0.044(12) F5 0.078(11) 0.099(12) 0.153(16) -0.030(11) -0.001(10) 0.006(9) F6 0.099(10) 0.056(8) 0.093(11) -0.026(7) -0.006(8) -0.005(8) F7 0.068(9) 0.098(11) 0.110(12) 0.000(9) 0.002(8) -0.031(9) F8 0.131(13) 0.091(11) 0.117(14) -0.041(10) 0.030(11) -0.033(10) F11 0.073(9) 0.071(9) 0.084(10) 0.022(7) 0.016(7) -0.012(7) F12 0.070(8) 0.047(7) 0.097(10) 0.013(7) 0.015(7) -0.013(7) F13 0.083(9) 0.073(9) 0.099(11) 0.007(8) 0.027(8) 0.042(8) F14 0.065(8) 0.058(8) 0.122(12) 0.038(8) 0.010(8) 0.015(7) F15 0.056(8) 0.099(10) 0.069(9) 0.013(7) -0.008(7) -0.001(7) F16 0.066(8) 0.076(9) 0.058(8) 0.000(6) 0.001(7) -0.001(7) F25 0.178(17) 0.085(11) 0.131(14) 0.033(10) 0.030(12) -0.035(12) F31 0.18(2) 0.27(3) 0.16(2) 0.016(19) 0.049(17) -0.04(2) F32 0.163(18) 0.26(3) 0.097(14) 0.008(15) -0.027(13) 0.048(18) F51 0.34(7) 0.21(5) 0.21(5) 0.04(4) 0.19(5) 0.04(5) F52 0.24(5) 0.023(16) 0.30(6) 0.01(2) -0.08(4) -0.02(2) F53 0.10(2) 0.21(4) 0.044(17) 0.03(2) -0.018(15) 0.07(2) F55 0.20(5) 0.34(7) 0.35(8) -0.14(6) 0.25(5) -0.08(5) F64 0.151(18) 0.24(3) 0.17(2) -0.011(18) 0.062(16) -0.054(18) Sb1 0.0543(10) 0.0490(10) 0.0626(11) 0.0164(8) 0.0123(8) 0.0076(8) Sb3 0.118(2) 0.161(2) 0.0921(18) 0.0451(15) -0.0025(14) -0.0116(17) Sb4 0.155(2) 0.130(2) 0.1049(19) 0.0087(15) 0.0046(16) -0.0192(18) Sb5 0.132(4) 0.093(3) 0.079(3) -0.001(2) 0.030(3) 0.004(3) Sb7 0.153(7) 0.180(9) 0.136(4) 0.047(7) 0.055(5) 0.052(7) _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 N61 2.026(17) . ? Ru1 N171 2.035(15) . ? Ru1 N52 2.064(16) . ? Ru1 N161 2.085(15) . ? Ru1 N71 2.097(16) . ? Ru1 N181 2.100(17) . ? Cu1 N312 1.74(3) . ? Cu1 N101 1.908(18) . ? Cu1 N91 1.98(3) . ? Cu1 N111 1.99(3) . ? Cu2 N131 1.923(17) . ? Cu2 N303 1.95(3) . ? Cu2 N141 1.98(3) . ? Cu2 N121 2.00(2) . ? Cu2 O2 2.27(4) . ? Cu3 N21 1.934(18) . ? Cu3 N31 1.98(2) . ? Cu3 N309 1.99(2) . ? Cu3 N11 2.00(2) . ? Cu3 N306 2.15(2) . ? Cu4 N211 1.927(16) . ? Cu4 N315 1.926(19) . ? Cu4 N201 2.000(17) . ? Cu4 N221 2.022(17) . ? Cu4 O1 2.239(13) . ? C12 C13 1.35(3) . ? C12 N11 1.41(3) . ? C12 C26 1.48(3) . ? C13 C14 1.33(3) . ? C13 H13 0.9500 . ? C14 C15 1.29(4) . ? C14 H14 0.9500 . ? C15 C16 1.38(4) . ? C15 H15 0.9500 . ? C16 N11 1.41(3) . ? C16 H16 0.9500 . ? C22 N21 1.35(3) . ? C22 C23 1.39(3) . ? C22 C36 1.48(3) . ? C23 C24 1.40(3) . ? C23 H23 0.9500 . ? C24 C25 1.40(3) . ? C24 C41 1.50(3) . ? C25 C26 1.37(3) . ? C25 H25 0.9500 . ? C26 N21 1.35(3) . ? C32 N31 1.29(3) . ? C32 C33 1.38(3) . ? C32 H32 0.9500 . ? C33 C34 1.42(4) . ? C33 H33 0.9500 . ? C34 C35 1.32(3) . ? C34 H34 0.9500 . ? C35 C36 1.37(3) . ? C35 H35 0.9500 . ? C36 N31 1.33(2) . ? C41 C42 1.34(3) . ? C41 C46 1.40(3) . ? C42 C43 1.38(3) . ? C42 H42 0.9500 . ? C43 C44 1.45(3) . ? C43 H43 0.9500 . ? C44 C45 1.30(3) . ? C44 C47 1.51(3) . ? C45 C46 1.44(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 N51 1.47(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C53 N52 1.35(2) . ? C53 C54 1.37(3) . ? C53 C66 1.41(3) . ? C54 C55 1.37(3) . ? C54 H54 0.9500 . ? C55 N51 1.35(3) . ? C55 H55 0.9500 . ? C62 C75 1.35(3) . ? C62 N61 1.36(2) . ? C62 C63 1.42(3) . ? C63 C64 1.34(4) . ? C63 H63 0.9500 . ? C64 C65 1.44(4) . ? C64 H64 0.9500 . ? C65 C66 1.38(3) . ? C65 H65 0.9500 . ? C66 N61 1.30(3) . ? C73 N72 1.30(3) . ? C73 C74 1.36(3) . ? C73 H73 0.9500 . ? C74 C75 1.43(3) . ? C74 H74 0.9500 . ? C75 N71 1.35(2) . ? C81 N72 1.47(3) . ? C81 C82 1.60(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C87 1.41(3) . ? C82 C83 1.41(3) . ? C83 C84 1.42(3) . ? C83 H83 0.9500 . ? C84 C85 1.37(3) . ? C84 H84 0.9500 . ? C85 C104 1.39(3) . ? C85 C86 1.41(3) . ? C86 C87 1.38(3) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C92 N91 1.31(4) . ? C92 C93 1.45(4) . ? C92 C102 1.55(4) . ? C93 C94 1.38(4) . ? C93 H93 0.9500 . ? C94 C95 1.41(4) . ? C94 H94 0.9500 . ? C95 C96 1.46(5) . ? C95 H95 0.9500 . ? C96 N91 1.30(4) . ? C96 H96 0.9500 . ? C102 N101 1.30(3) . ? C102 C103 1.44(4) . ? C103 C104 1.43(3) . ? C103 H103 0.9500 . ? C104 C105 1.34(3) . ? C105 C106 1.41(3) . ? C105 H105 0.9500 . ? C106 N101 1.31(3) . ? C106 C112 1.52(4) . ? C112 N111 1.40(4) . ? C112 C113 1.50(4) . ? C113 C114 1.42(4) . ? C113 H113 0.9500 . ? C114 C115 1.43(4) . ? C114 H114 0.9500 . ? C115 C116 1.40(4) . ? C115 H115 0.9500 . ? C116 N111 1.27(3) . ? C116 H116 0.9500 . ? C122 N121 1.39(3) . ? C122 C123 1.38(4) . ? C122 C136 1.47(4) . ? C123 C124 1.33(4) . ? C123 H123 0.9500 . ? C124 C125 1.31(4) . ? C124 H124 0.9500 . ? C125 C126 1.27(4) . ? C125 H125 0.9500 . ? C126 N121 1.47(4) . ? C126 H126 0.9500 . ? C132 N131 1.31(3) . ? C132 C133 1.38(3) . ? C132 C142 1.53(4) . ? C133 C134 1.39(3) . ? C133 H133 0.9500 . ? C134 C135 1.39(3) . ? C134 C151 1.49(3) . ? C135 C136 1.42(3) . ? C135 H135 0.9500 . ? C136 N131 1.25(3) . ? C142 C143 1.45(4) . ? C142 N141 1.44(3) . ? C143 C144 1.31(3) . ? C143 H143 0.9500 . ? C144 C145 1.30(4) . ? C144 H144 0.9500 . ? C145 C146 1.29(5) . ? C145 H145 0.9500 . ? C146 N141 1.51(4) . ? C146 H146 0.9500 . ? C151 C156 1.35(3) . ? C151 C152 1.41(3) . ? C152 C153 1.36(3) . ? C152 H152 0.9500 . ? C153 C154 1.44(3) . ? C153 H153 0.9500 . ? C154 C155 1.35(2) . ? C154 C157 1.56(3) . ? C155 C156 1.36(3) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C157 N162 1.39(2) . ? C157 H15A 0.9900 . ? C157 H15B 0.9900 . ? C163 N162 1.32(3) . ? C163 C164 1.34(3) . ? C163 H163 0.9500 . ? C164 C165 1.42(3) . ? C164 H164 0.9500 . ? C165 C172 1.40(3) . ? C165 N161 1.42(2) . ? C172 N171 1.34(2) . ? C172 C173 1.36(3) . ? C173 C174 1.41(3) . ? C173 H173 0.9500 . ? C174 C175 1.32(3) . ? C174 H174 0.9500 . ? C175 C176 1.43(3) . ? C175 H175 0.9500 . ? C176 N171 1.29(2) . ? C176 C185 1.43(3) . ? C183 N182 1.30(2) . ? C183 C184 1.33(3) . ? C183 H183 0.9500 . ? C184 C185 1.53(3) . ? C184 H184 0.9500 . ? C185 N181 1.34(3) . ? C191 C192 1.52(3) . ? C191 N182 1.51(3) . ? C191 H19A 0.9900 . ? C191 H19B 0.9900 . ? C192 C197 1.36(3) . ? C192 C193 1.37(3) . ? C193 C194 1.36(3) . ? C193 H193 0.9500 . ? C194 C195 1.35(3) . ? C194 H194 0.9500 . ? C195 C196 1.40(3) . ? C195 C214 1.52(3) . ? C196 C197 1.42(3) . ? C196 H196 0.9500 . ? C197 H197 0.9500 . ? C202 N201 1.32(3) . ? C202 C203 1.40(3) . ? C202 H202 0.9500 . ? C203 C204 1.35(3) . ? C203 H203 0.9500 . ? C204 C205 1.49(3) . ? C204 H204 0.9500 . ? C205 C206 1.42(3) . ? C205 H205 0.9500 . ? C206 N201 1.37(3) . ? C206 C216 1.44(3) . ? C212 C213 1.32(3) . ? C212 N211 1.36(2) . ? C212 C222 1.49(3) . ? C213 C214 1.37(3) . ? C213 H213 0.9500 . ? C214 C215 1.41(3) . ? C215 C216 1.35(3) . ? C215 H215 0.9500 . ? C216 N211 1.33(2) . ? C222 C223 1.36(3) . ? C222 N221 1.40(2) . ? C223 C224 1.33(3) . ? C223 H223 0.9500 . ? C224 C225 1.45(3) . ? C224 H224 0.9500 . ? C225 C226 1.30(3) . ? C225 H225 0.9500 . ? C226 N221 1.35(2) . ? C226 H226 0.9500 . ? C301 C302 1.57(2) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 N303 1.078(16) . ? C304 C305 1.56(2) . ? C304 H30D 0.9800 . ? C304 H30E 0.9800 . ? C304 H30F 0.9800 . ? C305 N306 1.079(16) . ? C307 C308 1.56(2) . ? C307 H30G 0.9800 . ? C307 H30H 0.9800 . ? C307 H30I 0.9800 . ? C308 N309 1.078(16) . ? C310 C311 1.57(2) . ? C310 H30J 0.9800 . ? C310 H30K 0.9800 . ? C310 H30L 0.9800 . ? C311 N312 1.076(16) . ? C313 C314 1.56(2) . ? C313 H30M 0.9800 . ? C313 H30N 0.9800 . ? C313 H30O 0.9800 . ? C314 N315 1.079(16) . ? N51 N52 1.43(2) . ? N71 N72 1.34(2) . ? N161 N162 1.349(19) . ? N181 N182 1.35(2) . ? B1 F2 1.372(9) . ? B1 F1 1.373(9) . ? B1 F4 1.373(9) . ? B1 F3 1.373(9) . ? B2 F5 1.362(8) . ? B2 F8 1.363(8) . ? B2 F6 1.364(8) . ? B2 F7 1.364(8) . ? B8 F84 1.239(10) . ? B8 F83 1.248(10) . ? B8 F81 1.248(10) . ? B8 F82 1.249(10) . ? B8 F81' 1.52(2) . ? B9 F91 1.416(4) . ? B9 F93 1.435(5) . ? B9 F92 1.439(5) . ? B9 F94 1.445(5) . ? F11 Sb1 1.873(7) . ? F12 Sb1 1.871(7) . ? F13 Sb1 1.871(6) . ? F14 Sb1 1.881(6) . ? F15 Sb1 1.867(6) . ? F16 Sb1 1.877(6) . ? F21 Sb2 1.728(11) . ? F22 Sb2 1.731(12) . ? F23 F26 1.65(6) . ? F23 Sb2 1.697(11) . ? F23 Sb2' 2.234(13) . ? F24 Sb2 1.736(11) . ? F25 Sb2 1.754(10) . ? F25 Sb2' 2.173(13) . ? F26 Sb2' 2.197(14) . ? F31 Sb3 1.858(12) . ? F32 Sb3 1.857(12) . ? F33 Sb3 1.858(13) . ? F34 Sb3 1.859(13) . ? F35 Sb3 1.851(15) . ? F36 Sb3 1.849(15) . ? F41 Sb4 1.84(2) . ? F42 Sb4 1.83(2) . ? F43 Sb4 1.84(2) . ? F44 F45 1.25(7) . ? F44 Sb4 1.84(2) . ? F45 Sb4 1.83(2) . ? F46 Sb4 1.83(2) . ? F51 Sb5 1.864(15) . ? F52 Sb5 1.866(15) . ? F53 Sb5 1.866(15) . ? F54 Sb5 1.862(15) . ? F55 Sb5 1.862(15) . ? F56 Sb5 1.863(15) . ? F61 Sb6 1.669(14) . ? F61 F66 1.74(6) . ? F62 Sb6 1.671(14) . ? F63 Sb6 1.666(14) . ? F63 F65 1.67(5) . ? F64 Sb6 1.656(13) . ? F64 Sb6' 2.097(13) . ? F65 Sb6 1.674(14) . ? F66 Sb6 1.671(14) . ? F71 Sb7 1.627(19) . ? F71 Sb7 2.49(4) 3_666 ? F72 Sb7 1.626(19) . ? F72 Sb7 2.15(4) 3_666 ? F73 F71' 1.36(8) 3_666 ? F73 Sb7 1.626(19) . ? F73 Sb7 2.09(3) 3_666 ? F81' F84 0.72(2) . ? F21' Sb2' 2.198(14) . ? F22' Sb2' 2.199(14) . ? F24' Sb2' 2.194(14) . ? F26' Sb2 1.735(11) . ? F33' Sb3 1.854(12) . ? F34' Sb3 1.858(12) . ? F35' Sb3 1.851(15) . ? F36' Sb3 1.848(15) . ? F41' Sb4 1.87(2) . ? F42' Sb4 1.88(2) . ? F43' Sb4 1.88(2) . ? F44' Sb4 1.88(2) . ? F45' Sb4 1.88(2) . ? F46' Sb4 1.88(2) . ? F61' Sb6' 2.093(14) . ? F62' F63' 1.79(5) . ? F62' Sb6' 2.091(14) . ? F63' Sb6' 2.092(14) . ? F65' Sb6' 2.084(14) . ? F66' Sb6' 2.090(14) . ? F71' F73 1.36(8) 3_666 ? F71' Sb7 1.627(19) . ? F71' Sb7 1.92(6) 3_666 ? F72' Sb7 1.56(4) 3_666 ? F72' Sb7 1.629(19) . ? Sb7 Sb7 1.139(13) 3_666 ? Sb7 F72' 1.56(4) 3_666 ? Sb7 F71' 1.92(6) 3_666 ? Sb7 F73 2.09(3) 3_666 ? Sb7 F72 2.15(4) 3_666 ? Sb7 F71 2.49(4) 3_666 ? 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 N61 Ru1 N171 177.7(7) . . ? N61 Ru1 N52 74.8(7) . . ? N171 Ru1 N52 103.9(6) . . ? N61 Ru1 N161 101.0(6) . . ? N171 Ru1 N161 77.2(7) . . ? N52 Ru1 N161 92.5(5) . . ? N61 Ru1 N71 77.4(8) . . ? N171 Ru1 N71 104.0(7) . . ? N52 Ru1 N71 152.1(7) . . ? N161 Ru1 N71 92.3(6) . . ? N61 Ru1 N181 104.4(7) . . ? N171 Ru1 N181 77.5(7) . . ? N52 Ru1 N181 94.1(6) . . ? N161 Ru1 N181 154.7(7) . . ? N71 Ru1 N181 93.2(6) . . ? N312 Cu1 N101 175.9(13) . . ? N312 Cu1 N91 101.5(14) . . ? N101 Cu1 N91 82.3(11) . . ? N312 Cu1 N111 94.7(14) . . ? N101 Cu1 N111 81.6(11) . . ? N91 Cu1 N111 163.7(12) . . ? N131 Cu2 N303 160.9(14) . . ? N131 Cu2 N141 81.2(11) . . ? N303 Cu2 N141 96.4(14) . . ? N131 Cu2 N121 79.5(11) . . ? N303 Cu2 N121 99.1(14) . . ? N141 Cu2 N121 158.9(9) . . ? N131 Cu2 O2 97.9(12) . . ? N303 Cu2 O2 101.1(17) . . ? N141 Cu2 O2 92.5(12) . . ? N121 Cu2 O2 98.3(11) . . ? N21 Cu3 N31 79.3(9) . . ? N21 Cu3 N309 153.7(8) . . ? N31 Cu3 N309 98.2(9) . . ? N21 Cu3 N11 79.6(9) . . ? N31 Cu3 N11 158.9(8) . . ? N309 Cu3 N11 100.2(9) . . ? N21 Cu3 N306 114.8(8) . . ? N31 Cu3 N306 95.5(9) . . ? N309 Cu3 N306 91.5(8) . . ? N11 Cu3 N306 94.2(10) . . ? N211 Cu4 N315 164.6(8) . . ? N211 Cu4 N201 80.2(8) . . ? N315 Cu4 N201 99.3(9) . . ? N211 Cu4 N221 81.0(8) . . ? N315 Cu4 N221 98.3(9) . . ? N201 Cu4 N221 161.0(8) . . ? N211 Cu4 O1 104.6(6) . . ? N315 Cu4 O1 90.8(7) . . ? N201 Cu4 O1 94.5(6) . . ? N221 Cu4 O1 92.2(6) . . ? C13 C12 N11 123(2) . . ? C13 C12 C26 127(2) . . ? N11 C12 C26 110(3) . . ? C14 C13 C12 120(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 121(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 121(4) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 N11 121(3) . . ? C15 C16 H16 119.3 . . ? N11 C16 H16 119.3 . . ? N21 C22 C23 117(2) . . ? N21 C22 C36 113.7(19) . . ? C23 C22 C36 129(2) . . ? C22 C23 C24 121(2) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C25 118(2) . . ? C23 C24 C41 120(2) . . ? C25 C24 C41 120(2) . . ? C26 C25 C24 119(2) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N21 C26 C25 120(2) . . ? N21 C26 C12 114(2) . . ? C25 C26 C12 125(3) . . ? N31 C32 C33 122(2) . . ? N31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C32 C33 C34 120(3) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 116(3) . . ? C35 C34 H34 122.2 . . ? C33 C34 H34 122.2 . . ? C34 C35 C36 121(2) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? N31 C36 C35 124(2) . . ? N31 C36 C22 111(2) . . ? C35 C36 C22 125(2) . . ? C42 C41 C46 121.9(19) . . ? C42 C41 C24 121.2(19) . . ? C46 C41 C24 117(2) . . ? C41 C42 C43 119(2) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C42 C43 C44 121(2) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 119.7(19) . . ? C45 C44 C47 125(2) . . ? C43 C44 C47 115(2) . . ? C44 C45 C46 121(2) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C41 C46 C45 118(2) . . ? C41 C46 H46 120.8 . . ? C45 C46 H46 120.8 . . ? N51 C47 C44 111.6(16) . . ? N51 C47 H47A 109.3 . . ? C44 C47 H47A 109.3 . . ? N51 C47 H47B 109.3 . . ? C44 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? N52 C53 C54 114(2) . . ? N52 C53 C66 112.0(19) . . ? C54 C53 C66 134(2) . . ? C55 C54 C53 104(2) . . ? C55 C54 H54 127.9 . . ? C53 C54 H54 127.9 . . ? N51 C55 C54 110(2) . . ? N51 C55 H55 124.8 . . ? C54 C55 H55 124.8 . . ? C75 C62 N61 116.6(19) . . ? C75 C62 C63 125(2) . . ? N61 C62 C63 118(2) . . ? C64 C63 C62 116(2) . . ? C64 C63 H63 122.1 . . ? C62 C63 H63 122.1 . . ? C63 C64 C65 126(2) . . ? C63 C64 H64 117.2 . . ? C65 C64 H64 117.2 . . ? C66 C65 C64 114(2) . . ? C66 C65 H65 123.1 . . ? C64 C65 H65 123.1 . . ? N61 C66 C65 121(2) . . ? N61 C66 C53 116(2) . . ? C65 C66 C53 123(2) . . ? N72 C73 C74 110(2) . . ? N72 C73 H73 125.1 . . ? C74 C73 H73 125.1 . . ? C73 C74 C75 105(2) . . ? C73 C74 H74 127.5 . . ? C75 C74 H74 127.5 . . ? C62 C75 N71 117.4(19) . . ? C62 C75 C74 136(2) . . ? N71 C75 C74 107(2) . . ? N72 C81 C82 107.6(18) . . ? N72 C81 H81A 110.2 . . ? C82 C81 H81A 110.2 . . ? N72 C81 H81B 110.2 . . ? C82 C81 H81B 110.2 . . ? H81A C81 H81B 108.5 . . ? C87 C82 C83 119(2) . . ? C87 C82 C81 119(2) . . ? C83 C82 C81 122(2) . . ? C82 C83 C84 117(2) . . ? C82 C83 H83 121.3 . . ? C84 C83 H83 121.3 . . ? C85 C84 C83 124(2) . . ? C85 C84 H84 118.1 . . ? C83 C84 H84 118.1 . . ? C84 C85 C104 121(2) . . ? C84 C85 C86 118(2) . . ? C104 C85 C86 121(2) . . ? C87 C86 C85 119(2) . . ? C87 C86 H86 120.3 . . ? C85 C86 H86 120.3 . . ? C86 C87 C82 122(2) . . ? C86 C87 H87 118.8 . . ? C82 C87 H87 118.8 . . ? N91 C92 C93 127(3) . . ? N91 C92 C102 114(3) . . ? C93 C92 C102 119(4) . . ? C94 C93 C92 113(3) . . ? C94 C93 H93 123.6 . . ? C92 C93 H93 123.6 . . ? C93 C94 C95 121(3) . . ? C93 C94 H94 119.4 . . ? C95 C94 H94 119.4 . . ? C94 C95 C96 118(3) . . ? C94 C95 H95 120.8 . . ? C96 C95 H95 120.8 . . ? N91 C96 C95 120(4) . . ? N91 C96 H96 120.1 . . ? C95 C96 H96 120.1 . . ? N101 C102 C103 124(2) . . ? N101 C102 C92 112(3) . . ? C103 C102 C92 125(3) . . ? C104 C103 C102 117(2) . . ? C104 C103 H103 121.3 . . ? C102 C103 H103 121.3 . . ? C105 C104 C85 123(2) . . ? C105 C104 C103 115(2) . . ? C85 C104 C103 122(2) . . ? C104 C105 C106 125(2) . . ? C104 C105 H105 117.6 . . ? C106 C105 H105 117.6 . . ? N101 C106 C105 120(2) . . ? N101 C106 C112 109(3) . . ? C105 C106 C112 132(3) . . ? N111 C112 C113 126(3) . . ? N111 C112 C106 116(3) . . ? C113 C112 C106 118(4) . . ? C114 C113 C112 109(3) . . ? C114 C113 H113 125.7 . . ? C112 C113 H113 125.7 . . ? C113 C114 C115 126(3) . . ? C113 C114 H114 117.0 . . ? C115 C114 H114 117.0 . . ? C116 C115 C114 115(3) . . ? C116 C115 H115 122.4 . . ? C114 C115 H115 122.4 . . ? N111 C116 C115 127(3) . . ? N111 C116 H116 116.7 . . ? C115 C116 H116 116.7 . . ? N121 C122 C123 120(3) . . ? N121 C122 C136 110(3) . . ? C123 C122 C136 130(3) . . ? C124 C123 C122 121(3) . . ? C124 C123 H123 119.5 . . ? C122 C123 H123 119.5 . . ? C125 C124 C123 120(3) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C126 C125 C124 122(4) . . ? C126 C125 H125 118.9 . . ? C124 C125 H125 118.9 . . ? C125 C126 N121 123(3) . . ? C125 C126 H126 118.5 . . ? N121 C126 H126 118.5 . . ? N131 C132 C133 121(2) . . ? N131 C132 C142 115(2) . . ? C133 C132 C142 124(3) . . ? C132 C133 C134 120(2) . . ? C132 C133 H133 120.0 . . ? C134 C133 H133 120.0 . . ? C133 C134 C135 117(2) . . ? C133 C134 C151 122(2) . . ? C135 C134 C151 120.4(19) . . ? C134 C135 C136 117(2) . . ? C134 C135 H135 121.4 . . ? C136 C135 H135 121.4 . . ? N131 C136 C135 123(2) . . ? N131 C136 C122 117(3) . . ? C135 C136 C122 120(3) . . ? C143 C142 N141 124(3) . . ? C143 C142 C132 128(3) . . ? N141 C142 C132 108(3) . . ? C144 C143 C142 118(3) . . ? C144 C143 H143 120.9 . . ? C142 C143 H143 120.9 . . ? C145 C144 C143 122(4) . . ? C145 C144 H144 118.8 . . ? C143 C144 H144 118.8 . . ? C146 C145 C144 122(4) . . ? C146 C145 H145 119.1 . . ? C144 C145 H145 119.1 . . ? C145 C146 N141 127(4) . . ? C145 C146 H146 116.3 . . ? N141 C146 H146 116.4 . . ? C156 C151 C152 116.8(19) . . ? C156 C151 C134 122(2) . . ? C152 C151 C134 121(2) . . ? C153 C152 C151 122.5(19) . . ? C153 C152 H152 118.8 . . ? C151 C152 H152 118.8 . . ? C152 C153 C154 117.6(19) . . ? C152 C153 H153 121.2 . . ? C154 C153 H153 121.2 . . ? C155 C154 C153 118.4(18) . . ? C155 C154 C157 123.7(18) . . ? C153 C154 C157 117.9(18) . . ? C154 C155 C156 122.4(19) . . ? C154 C155 H155 118.8 . . ? C156 C155 H155 118.8 . . ? C151 C156 C155 122(2) . . ? C151 C156 H156 119.1 . . ? C155 C156 H156 119.1 . . ? N162 C157 C154 110.1(16) . . ? N162 C157 H15A 109.6 . . ? C154 C157 H15A 109.7 . . ? N162 C157 H15B 109.6 . . ? C154 C157 H15B 109.6 . . ? H15A C157 H15B 108.2 . . ? N162 C163 C164 112(2) . . ? N162 C163 H163 124.0 . . ? C164 C163 H163 124.0 . . ? C163 C164 C165 106(2) . . ? C163 C164 H164 126.9 . . ? C165 C164 H164 126.9 . . ? C172 C165 N161 116.4(19) . . ? C172 C165 C164 138(2) . . ? N161 C165 C164 105.5(19) . . ? N171 C172 C173 118(2) . . ? N171 C172 C165 114.0(19) . . ? C173 C172 C165 128(2) . . ? C172 C173 C174 121(2) . . ? C172 C173 H173 119.7 . . ? C174 C173 H173 119.7 . . ? C175 C174 C173 120(2) . . ? C175 C174 H174 120.0 . . ? C173 C174 H174 120.0 . . ? C174 C175 C176 117(2) . . ? C174 C175 H175 121.7 . . ? C176 C175 H175 121.7 . . ? N171 C176 C185 113(2) . . ? N171 C176 C175 122(2) . . ? C185 C176 C175 125(2) . . ? N182 C183 C184 107(2) . . ? N182 C183 H183 126.7 . . ? C184 C183 H183 126.7 . . ? C183 C184 C185 107(2) . . ? C183 C184 H184 126.4 . . ? C185 C184 H184 126.4 . . ? N181 C185 C176 119.1(19) . . ? N181 C185 C184 103(2) . . ? C176 C185 C184 137(2) . . ? C192 C191 N182 110.1(18) . . ? C192 C191 H19A 109.6 . . ? N182 C191 H19A 109.6 . . ? C192 C191 H19B 109.6 . . ? N182 C191 H19B 109.6 . . ? H19A C191 H19B 108.1 . . ? C197 C192 C193 120(2) . . ? C197 C192 C191 122(2) . . ? C193 C192 C191 117(2) . . ? C194 C193 C192 121(2) . . ? C194 C193 H193 119.7 . . ? C192 C193 H193 119.7 . . ? C195 C194 C193 120(2) . . ? C195 C194 H194 119.8 . . ? C193 C194 H194 119.8 . . ? C194 C195 C196 121(2) . . ? C194 C195 C214 122(2) . . ? C196 C195 C214 118(2) . . ? C195 C196 C197 118(2) . . ? C195 C196 H196 121.0 . . ? C197 C196 H196 121.0 . . ? C192 C197 C196 120(2) . . ? C192 C197 H197 120.2 . . ? C196 C197 H197 120.2 . . ? N201 C202 C203 125(2) . . ? N201 C202 H202 117.6 . . ? C203 C202 H202 117.6 . . ? C204 C203 C202 120(2) . . ? C204 C203 H203 119.8 . . ? C202 C203 H203 119.8 . . ? C203 C204 C205 118(2) . . ? C203 C204 H204 120.8 . . ? C205 C204 H204 120.8 . . ? C206 C205 C204 115(2) . . ? C206 C205 H205 122.5 . . ? C204 C205 H205 122.5 . . ? N201 C206 C205 124(2) . . ? N201 C206 C216 115(2) . . ? C205 C206 C216 121(2) . . ? C213 C212 N211 119.6(19) . . ? C213 C212 C222 127(2) . . ? N211 C212 C222 113(2) . . ? C212 C213 C214 122(2) . . ? C212 C213 H213 118.8 . . ? C214 C213 H213 118.8 . . ? C213 C214 C215 116(2) . . ? C213 C214 C195 122(2) . . ? C215 C214 C195 122(2) . . ? C216 C215 C214 122(2) . . ? C216 C215 H215 119.2 . . ? C214 C215 H215 119.2 . . ? N211 C216 C215 119(2) . . ? N211 C216 C206 113(2) . . ? C215 C216 C206 129(2) . . ? C223 C222 N221 119.8(18) . . ? C223 C222 C212 127.0(19) . . ? N221 C222 C212 113.2(19) . . ? C224 C223 C222 122.0(19) . . ? C224 C223 H223 119.0 . . ? C222 C223 H223 119.0 . . ? C223 C224 C225 118(2) . . ? C223 C224 H224 121.2 . . ? C225 C224 H224 121.2 . . ? C226 C225 C224 119(2) . . ? C226 C225 H225 120.5 . . ? C224 C225 H225 120.5 . . ? C225 C226 N221 124(2) . . ? C225 C226 H226 118.1 . . ? N221 C226 H226 118.1 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? N303 C302 C301 161(5) . . ? C305 C304 H30D 109.5 . . ? C305 C304 H30E 109.5 . . ? H30D C304 H30E 109.5 . . ? C305 C304 H30F 109.5 . . ? H30D C304 H30F 109.5 . . ? H30E C304 H30F 109.5 . . ? N306 C305 C304 169(3) . . ? C308 C307 H30G 109.5 . . ? C308 C307 H30H 109.5 . . ? H30G C307 H30H 109.5 . . ? C308 C307 H30I 109.5 . . ? H30G C307 H30I 109.5 . . ? H30H C307 H30I 109.5 . . ? N309 C308 C307 179(4) . . ? C311 C310 H30J 109.5 . . ? C311 C310 H30K 109.5 . . ? H30J C310 H30K 109.5 . . ? C311 C310 H30L 109.5 . . ? H30J C310 H30L 109.5 . . ? H30K C310 H30L 109.5 . . ? N312 C311 C310 176(5) . . ? C314 C313 H30M 109.5 . . ? C314 C313 H30N 109.5 . . ? H30M C313 H30N 109.5 . . ? C314 C313 H30O 109.5 . . ? H30M C313 H30O 109.5 . . ? H30N C313 H30O 109.5 . . ? N315 C314 C313 176(3) . . ? C16 N11 C12 113(2) . . ? C16 N11 Cu3 130(2) . . ? C12 N11 Cu3 117.2(18) . . ? C26 N21 C22 123(2) . . ? C26 N21 Cu3 119.2(17) . . ? C22 N21 Cu3 117.7(17) . . ? C32 N31 C36 117(2) . . ? C32 N31 Cu3 124.1(16) . . ? C36 N31 Cu3 118.4(18) . . ? C55 N51 N52 108.2(18) . . ? C55 N51 C47 131(2) . . ? N52 N51 C47 118.2(16) . . ? C53 N52 N51 102.9(16) . . ? C53 N52 Ru1 118.0(14) . . ? N51 N52 Ru1 139.0(13) . . ? C66 N61 C62 125.1(19) . . ? C66 N61 Ru1 119.4(15) . . ? C62 N61 Ru1 115.4(15) . . ? N72 N71 C75 108.4(17) . . ? N72 N71 Ru1 138.6(14) . . ? C75 N71 Ru1 113.0(15) . . ? C73 N72 N71 110.1(18) . . ? C73 N72 C81 126(2) . . ? N71 N72 C81 123.3(17) . . ? C96 N91 C92 120(3) . . ? C96 N91 Cu1 126(3) . . ? C92 N91 Cu1 114(2) . . ? C102 N101 C106 120(2) . . ? C102 N101 Cu1 118(2) . . ? C106 N101 Cu1 122(2) . . ? C116 N111 C112 117(3) . . ? C116 N111 Cu1 131(2) . . ? C112 N111 Cu1 112(2) . . ? C122 N121 C126 113(3) . . ? C122 N121 Cu2 115(2) . . ? C126 N121 Cu2 133(2) . . ? C136 N131 C132 122(2) . . ? C136 N131 Cu2 119(2) . . ? C132 N131 Cu2 119.1(19) . . ? C142 N141 C146 106(3) . . ? C142 N141 Cu2 116(2) . . ? C146 N141 Cu2 138(3) . . ? N162 N161 C165 107.3(16) . . ? N162 N161 Ru1 139.5(13) . . ? C165 N161 Ru1 113.1(13) . . ? C163 N162 N161 109.1(17) . . ? C163 N162 C157 126.2(19) . . ? N161 N162 C157 123.3(17) . . ? C176 N171 C172 121.8(18) . . ? C176 N171 Ru1 119.0(16) . . ? C172 N171 Ru1 119.2(14) . . ? N182 N181 C185 107.2(18) . . ? N182 N181 Ru1 141.3(14) . . ? C185 N181 Ru1 111.3(16) . . ? C183 N182 N181 115.4(19) . . ? C183 N182 C191 124(2) . . ? N181 N182 C191 120.6(17) . . ? C202 N201 C206 117.0(18) . . ? C202 N201 Cu4 129.7(17) . . ? C206 N201 Cu4 113.2(14) . . ? C216 N211 C212 122.0(18) . . ? C216 N211 Cu4 119.0(15) . . ? C212 N211 Cu4 118.9(15) . . ? C226 N221 C222 117.6(17) . . ? C226 N221 Cu4 128.5(14) . . ? C222 N221 Cu4 113.8(15) . . ? C302 N303 Cu2 157(5) . . ? C305 N306 Cu3 163(2) . . ? C308 N309 Cu3 169(2) . . ? C311 N312 Cu1 165(4) . . ? C314 N315 Cu4 171(2) . . ? F2 B1 F1 109.5(5) . . ? F2 B1 F4 108.9(5) . . ? F1 B1 F4 109.6(5) . . ? F2 B1 F3 109.9(5) . . ? F1 B1 F3 109.4(5) . . ? F4 B1 F3 109.5(5) . . ? F5 B2 F8 109.7(5) . . ? F5 B2 F6 109.6(5) . . ? F8 B2 F6 109.0(5) . . ? F5 B2 F7 109.4(5) . . ? F8 B2 F7 109.4(5) . . ? F6 B2 F7 109.6(5) . . ? F84 B8 F83 109.9(5) . . ? F84 B8 F81 109.2(6) . . ? F83 B8 F81 109.3(6) . . ? F84 B8 F82 108.7(5) . . ? F83 B8 F82 110.3(5) . . ? F81 B8 F82 109.3(6) . . ? F84 B8 F81' 28.1(8) . . ? F83 B8 F81' 128.8(10) . . ? F81 B8 F81' 112.8(10) . . ? F82 B8 F81' 81.7(9) . . ? F91 B9 F93 125.9(4) . . ? F91 B9 F92 114.1(3) . . ? F93 B9 F92 105.8(3) . . ? F91 B9 F94 108.6(3) . . ? F93 B9 F94 97.3(3) . . ? F92 B9 F94 101.1(3) . . ? F26 F23 Sb2 79.9(9) . . ? F26 F23 Sb2' 66.9(8) . . ? Sb2 F23 Sb2' 13.6(3) . . ? Sb2 F25 Sb2' 16.8(2) . . ? F23 F26 Sb2' 69.3(9) . . ? F45 F44 Sb4 70.0(12) . . ? F44 F45 Sb4 70.3(12) . . ? Sb6 F61 F66 58.7(13) . . ? Sb6 F63 F65 60.2(9) . . ? Sb6 F64 Sb6' 15.2(3) . . ? Sb6 F65 F63 59.7(9) . . ? Sb6 F66 F61 58.5(13) . . ? Sb7 F71 Sb7 21.3(13) . 3_666 ? Sb7 F72 Sb7 31.4(10) . 3_666 ? F71' F73 Sb7 79.2(16) 3_666 . ? F71' F73 Sb7 51.2(8) 3_666 3_666 ? Sb7 F73 Sb7 32.9(6) . 3_666 ? F84 F81' B8 53.9(16) . . ? F81' F84 B8 98.0(19) . . ? F63' F62' Sb6' 64.7(9) . . ? F62' F63' Sb6' 64.7(9) . . ? F73 F71' Sb7 88(3) 3_666 . ? F73 F71' Sb7 56(2) 3_666 3_666 ? Sb7 F71' Sb7 36.4(12) . 3_666 ? Sb7 F72' Sb7 41.8(9) 3_666 . ? F15 Sb1 F12 90.1(3) . . ? F15 Sb1 F13 90.4(2) . . ? F12 Sb1 F13 90.1(3) . . ? F15 Sb1 F11 90.4(3) . . ? F12 Sb1 F11 179.2(3) . . ? F13 Sb1 F11 90.6(3) . . ? F15 Sb1 F16 179.6(3) . . ? F12 Sb1 F16 89.7(3) . . ? F13 Sb1 F16 89.9(2) . . ? F11 Sb1 F16 89.8(3) . . ? F15 Sb1 F14 90.0(2) . . ? F12 Sb1 F14 89.5(3) . . ? F13 Sb1 F14 179.4(4) . . ? F11 Sb1 F14 89.8(3) . . ? F16 Sb1 F14 89.7(2) . . ? F23 Sb2 F21 94.0(14) . . ? F23 Sb2 F22 170.8(16) . . ? F21 Sb2 F22 92.3(16) . . ? F23 Sb2 F26' 75.9(14) . . ? F21 Sb2 F26' 169.6(14) . . ? F22 Sb2 F26' 97.5(16) . . ? F23 Sb2 F24 85.7(12) . . ? F21 Sb2 F24 86.1(12) . . ? F22 Sb2 F24 88.1(14) . . ? F26' Sb2 F24 90.8(12) . . ? F23 Sb2 F25 89.3(12) . . ? F21 Sb2 F25 95.8(12) . . ? F22 Sb2 F25 96.7(14) . . ? F26' Sb2 F25 86.4(11) . . ? F24 Sb2 F25 174.8(10) . . ? F36' Sb3 F33' 99.7(15) . . ? F36' Sb3 F36 25.8(14) . . ? F33' Sb3 F36 87.6(19) . . ? F36' Sb3 F32 170.4(13) . . ? F33' Sb3 F32 87.1(14) . . ? F36 Sb3 F32 163.1(18) . . ? F36' Sb3 F35' 78.3(16) . . ? F33' Sb3 F35' 167(2) . . ? F36 Sb3 F35' 95.4(19) . . ? F32 Sb3 F35' 93.6(14) . . ? F36' Sb3 F35 88(2) . . ? F33' Sb3 F35 170(2) . . ? F36 Sb3 F35 97(2) . . ? F32 Sb3 F35 86.3(18) . . ? F35' Sb3 F35 22.0(19) . . ? F36' Sb3 F31 93.7(14) . . ? F33' Sb3 F31 98.1(16) . . ? F36 Sb3 F31 72.9(18) . . ? F32 Sb3 F31 92.0(10) . . ? F35' Sb3 F31 95.3(15) . . ? F35 Sb3 F31 75(2) . . ? F36' Sb3 F33 95(2) . . ? F33' Sb3 F33 26.6(18) . . ? F36 Sb3 F33 75(2) . . ? F32 Sb3 F33 93.7(18) . . ? F35' Sb3 F33 166(3) . . ? F35 Sb3 F33 147(3) . . ? F31 Sb3 F33 72(2) . . ? F36' Sb3 F34' 85.9(17) . . ? F33' Sb3 F34' 83(2) . . ? F36 Sb3 F34' 107(2) . . ? F32 Sb3 F34' 88.2(14) . . ? F35' Sb3 F34' 83.7(15) . . ? F35 Sb3 F34' 104(2) . . ? F31 Sb3 F34' 179.0(16) . . ? F33 Sb3 F34' 109(3) . . ? F36' Sb3 F34 91(2) . . ? F33' Sb3 F34 107(3) . . ? F36 Sb3 F34 117(3) . . ? F32 Sb3 F34 80.2(18) . . ? F35' Sb3 F34 60(2) . . ? F35 Sb3 F34 79(2) . . ? F31 Sb3 F34 153(2) . . ? F33 Sb3 F34 134(3) . . ? F34' Sb3 F34 26.4(18) . . ? F45 Sb4 F46 102(2) . . ? F45 Sb4 F42 85(3) . . ? F46 Sb4 F42 157(3) . . ? F45 Sb4 F41 92(2) . . ? F46 Sb4 F41 83.0(18) . . ? F42 Sb4 F41 119(2) . . ? F45 Sb4 F44 40(2) . . ? F46 Sb4 F44 97(3) . . ? F42 Sb4 F44 74(3) . . ? F41 Sb4 F44 131(3) . . ? F45 Sb4 F43 172(2) . . ? F46 Sb4 F43 86(2) . . ? F42 Sb4 F43 88(3) . . ? F41 Sb4 F43 89(2) . . ? F44 Sb4 F43 139(3) . . ? F45 Sb4 F41' 117(2) . . ? F46 Sb4 F41' 107.6(18) . . ? F42 Sb4 F41' 89(2) . . ? F41 Sb4 F41' 40.7(14) . . ? F44 Sb4 F41' 150(3) . . ? F43 Sb4 F41' 60(2) . . ? F45 Sb4 F44' 67(3) . . ? F46 Sb4 F44' 66(3) . . ? F42 Sb4 F44' 97(3) . . ? F41 Sb4 F44' 137(3) . . ? F44 Sb4 F44' 36(3) . . ? F43 Sb4 F44' 116(3) . . ? F41' Sb4 F44' 174(3) . . ? F45 Sb4 F43' 99(2) . . ? F46 Sb4 F43' 108(2) . . ? F42 Sb4 F43' 49(2) . . ? F41 Sb4 F43' 162(2) . . ? F44 Sb4 F43' 63(3) . . ? F43 Sb4 F43' 78(2) . . ? F41' Sb4 F43' 121.5(19) . . ? F44' Sb4 F43' 60(2) . . ? F45 Sb4 F45' 32.2(18) . . ? F46 Sb4 F45' 94.1(19) . . ? F42 Sb4 F45' 103(2) . . ? F41 Sb4 F45' 60.0(19) . . ? F44 Sb4 F45' 71(3) . . ? F43 Sb4 F45' 149(2) . . ? F41' Sb4 F45' 90.6(19) . . ? F44' Sb4 F45' 92(3) . . ? F43' Sb4 F45' 131(2) . . ? F45 Sb4 F42' 71(2) . . ? F46 Sb4 F42' 172(2) . . ? F42 Sb4 F42' 29(2) . . ? F41 Sb4 F42' 93(2) . . ? F44 Sb4 F42' 80(3) . . ? F43 Sb4 F42' 101(2) . . ? F41' Sb4 F42' 73(2) . . ? F44' Sb4 F42' 113(3) . . ? F43' Sb4 F42' 78(2) . . ? F45' Sb4 F42' 78(2) . . ? F45 Sb4 F46' 102(2) . . ? F46 Sb4 F46' 27.1(16) . . ? F42 Sb4 F46' 171(2) . . ? F41 Sb4 F46' 56.0(18) . . ? F44 Sb4 F46' 115(3) . . ? F43 Sb4 F46' 85(2) . . ? F41' Sb4 F46' 83.9(18) . . ? F44' Sb4 F46' 91(3) . . ? F43' Sb4 F46' 133(2) . . ? F45' Sb4 F46' 81(2) . . ? F42' Sb4 F46' 149(2) . . ? F54 Sb5 F55 92.5(8) . . ? F54 Sb5 F56 90.0(3) . . ? F55 Sb5 F56 92.4(8) . . ? F54 Sb5 F51 87.7(8) . . ? F55 Sb5 F51 179.8(4) . . ? F56 Sb5 F51 87.7(8) . . ? F54 Sb5 F53 89.9(3) . . ? F55 Sb5 F53 92.3(8) . . ? F56 Sb5 F53 175.3(15) . . ? F51 Sb5 F53 87.6(8) . . ? F54 Sb5 F52 175.2(15) . . ? F55 Sb5 F52 92.3(8) . . ? F56 Sb5 F52 89.9(3) . . ? F51 Sb5 F52 87.5(8) . . ? F53 Sb5 F52 89.8(3) . . ? F64 Sb6 F63 125.0(17) . . ? F64 Sb6 F61 91.0(18) . . ? F63 Sb6 F61 97(2) . . ? F64 Sb6 F62 96.9(19) . . ? F63 Sb6 F62 109(2) . . ? F61 Sb6 F62 140(3) . . ? F64 Sb6 F66 82(2) . . ? F63 Sb6 F66 148(3) . . ? F61 Sb6 F66 63(3) . . ? F62 Sb6 F66 80(3) . . ? F64 Sb6 F65 174.8(15) . . ? F63 Sb6 F65 60.1(18) . . ? F61 Sb6 F65 89(2) . . ? F62 Sb6 F65 80(2) . . ? F66 Sb6 F65 94(3) . . ? Sb7 Sb7 F72' 72.3(18) 3_666 3_666 ? Sb7 Sb7 F73 96.4(14) 3_666 . ? F72' Sb7 F73 74(2) 3_666 . ? Sb7 Sb7 F72 101(2) 3_666 . ? F72' Sb7 F72 167(3) 3_666 . ? F73 Sb7 F72 96(2) . . ? Sb7 Sb7 F71 127(3) 3_666 . ? F72' Sb7 F71 98(3) 3_666 . ? F73 Sb7 F71 132(3) . . ? F72 Sb7 F71 95(3) . . ? Sb7 Sb7 F71' 86(3) 3_666 . ? F72' Sb7 F71' 85(3) 3_666 . ? F73 Sb7 F71' 157(3) . . ? F72 Sb7 F71' 106(3) . . ? F71 Sb7 F71' 42(3) . . ? Sb7 Sb7 F72' 66(2) 3_666 . ? F72' Sb7 F72' 138.2(9) 3_666 . ? F73 Sb7 F72' 110(2) . . ? F72 Sb7 F72' 37(2) . . ? F71 Sb7 F72' 107(3) . . ? F71' Sb7 F72' 91(4) . . ? Sb7 Sb7 F71' 58(2) 3_666 3_666 ? F72' Sb7 F71' 84(3) 3_666 3_666 ? F73 Sb7 F71' 44(2) . 3_666 ? F72 Sb7 F71' 83(3) . 3_666 ? F71 Sb7 F71' 175(3) . 3_666 ? F71' Sb7 F71' 143.6(12) . 3_666 ? F72' Sb7 F71' 75(3) . 3_666 ? Sb7 Sb7 F73 50.8(10) 3_666 3_666 ? F72' Sb7 F73 93(2) 3_666 3_666 ? F73 Sb7 F73 147.1(6) . 3_666 ? F72 Sb7 F73 91(2) . 3_666 ? F71 Sb7 F73 79(3) . 3_666 ? F71' Sb7 F73 41(3) . 3_666 ? F72' Sb7 F73 60(2) . 3_666 ? F71' Sb7 F73 105(2) 3_666 3_666 ? Sb7 Sb7 F72 48.0(15) 3_666 3_666 ? F72' Sb7 F72 26.3(18) 3_666 3_666 ? F73 Sb7 F72 88.6(18) . 3_666 ? F72 Sb7 F72 148.6(10) . 3_666 ? F71 Sb7 F72 105(3) . 3_666 ? F71' Sb7 F72 76(3) . 3_666 ? F72' Sb7 F72 113(2) . 3_666 ? F71' Sb7 F72 79(3) 3_666 3_666 ? F73 Sb7 F72 69.8(16) 3_666 3_666 ? Sb7 Sb7 F71 31(2) 3_666 3_666 ? F72' Sb7 F71 76(3) 3_666 3_666 ? F73 Sb7 F71 67(2) . 3_666 ? F72 Sb7 F71 92(3) . 3_666 ? F71 Sb7 F71 158.7(13) . 3_666 ? F71' Sb7 F71 117(3) . 3_666 ? F72' Sb7 F71 68(3) . 3_666 ? F71' Sb7 F71 27(2) 3_666 3_666 ? F73 Sb7 F71 80.3(19) 3_666 3_666 ? F72 Sb7 F71 62(2) 3_666 3_666 ? F25 Sb2' F24' 164.1(15) . . ? F25 Sb2' F21' 99(4) . . ? F24' Sb2' F21' 84(4) . . ? F25 Sb2' F26 90.9(16) . . ? F24' Sb2' F26 91(2) . . ? F21' Sb2' F26 162(4) . . ? F25 Sb2' F22' 103(3) . . ? F24' Sb2' F22' 92(3) . . ? F21' Sb2' F22' 60(4) . . ? F26 Sb2' F22' 102(3) . . ? F25 Sb2' F23 66.8(10) . . ? F24' Sb2' F23 104.4(16) . . ? F21' Sb2' F23 155(3) . . ? F26 Sb2' F23 43.8(16) . . ? F22' Sb2' F23 141(3) . . ? F65' Sb6' F66' 97(2) . . ? F65' Sb6' F62' 89.1(18) . . ? F66' Sb6' F62' 173(2) . . ? F65' Sb6' F63' 103.7(16) . . ? F66' Sb6' F63' 131(2) . . ? F62' Sb6' F63' 50.6(17) . . ? F65' Sb6' F61' 105.4(16) . . ? F66' Sb6' F61' 58(2) . . ? F62' Sb6' F61' 124.2(19) . . ? F63' Sb6' F61' 73.5(18) . . ? F65' Sb6' F64 176.6(13) . . ? F66' Sb6' F64 85(2) . . ? F62' Sb6' F64 89.7(16) . . ? F63' Sb6' F64 73.1(13) . . ? F61' Sb6' F64 72.6(14) . . ? _diffrn_measured_fraction_theta_max 0.745 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.745 _refine_diff_density_max 3.978 _refine_diff_density_min -2.048 _refine_diff_density_rms 0.227 #===END