# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Asao Nakamura' _publ_contact_author_address ; Kuroda Chiromorphology Project Japan Science and Technology Agency 4-7-6 Komaba Meguro-ku Tokyo 153-0041 JAPAN ; _publ_contact_author_email ASAO@CHIROMOR.JST.GO.JP _publ_section_title ; Formation of racemic crystals of transition metal complexes by grinding 1:1 mixtures of enantiomeric crystals ; loop_ _publ_author_name 'Asao Nakamura' 'Reiko Kuroda' 'Tomohiro Sato' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 242567' # data_251502a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 F24 N12 O P4 Ru2' _chemical_formula_weight 1881.26 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 36.810(3) _cell_length_b 15.7955(12) _cell_length_c 12.1174(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.6810(10) _cell_angle_gamma 90.00 _cell_volume 6899.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20932 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7357 _exptl_absorpt_correction_T_max 0.8279 _exptl_absorpt_process_details 'Bruker 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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20932 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.87 _reflns_number_total 12059 _reflns_number_gt 12030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0359P)^2^+20.9043P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.476(18) _refine_ls_number_reflns 12059 _refine_ls_number_parameters 1030 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.62073(10) 0.78359(18) 0.0975(3) 0.0141(7) Uani 1 1 d . . . C2 C 0.58815(10) 0.8209(2) 0.0962(4) 0.0178(8) Uani 1 1 d . . . H2 H 0.5853 0.8529 0.1582 0.021 Uiso 1 1 calc R . . C3 C 0.55818(11) 0.8136(3) 0.0053(4) 0.0227(9) Uani 1 1 d . . . H3 H 0.5361 0.8417 0.0069 0.027 Uiso 1 1 calc R . . C4 C 0.56120(11) 0.7659(2) -0.0853(4) 0.0195(8) Uani 1 1 d . . . H4 H 0.5412 0.7606 -0.1457 0.023 Uiso 1 1 calc R . . C5 C 0.60137(12) 0.6747(3) -0.1794(4) 0.0238(9) Uani 1 1 d . . . H5 H 0.5822 0.6662 -0.2413 0.029 Uiso 1 1 calc R . . C6 C 0.63522(13) 0.6397(3) -0.1784(4) 0.0252(9) Uani 1 1 d . . . H6 H 0.6389 0.6085 -0.2403 0.030 Uiso 1 1 calc R . . C7 C 0.70062(12) 0.6126(3) -0.0748(4) 0.0234(9) Uani 1 1 d . . . H7 H 0.7059 0.5804 -0.1339 0.028 Uiso 1 1 calc R . . C8 C 0.72705(12) 0.6238(3) 0.0210(4) 0.0228(8) Uani 1 1 d . . . H8 H 0.7503 0.5991 0.0277 0.027 Uiso 1 1 calc R . . C9 C 0.71871(10) 0.6731(2) 0.1094(3) 0.0160(7) Uani 1 1 d . . . H9 H 0.7369 0.6800 0.1743 0.019 Uiso 1 1 calc R . . N10 N 0.68588(9) 0.71030(18) 0.1044(3) 0.0133(6) Uani 1 1 d . . . C11 C 0.65937(10) 0.6978(2) 0.0081(3) 0.0138(7) Uani 1 1 d . . . C12 C 0.66538(11) 0.6499(2) -0.0837(4) 0.0198(8) Uani 1 1 d . . . C13 C 0.59502(12) 0.7241(2) -0.0873(4) 0.0177(8) Uani 1 1 d . . . C14 C 0.62416(11) 0.7360(2) 0.0057(3) 0.0155(8) Uani 1 1 d . . . N15 N 0.64694(9) 0.8795(2) 0.3109(3) 0.0158(7) Uani 1 1 d . . . C16 C 0.62684(11) 0.8687(3) 0.3887(4) 0.0220(9) Uani 1 1 d . . . H16 H 0.6228 0.8140 0.4118 0.026 Uiso 1 1 calc R . . C17 C 0.61143(11) 0.9369(3) 0.4376(4) 0.0244(9) Uani 1 1 d . . . H17 H 0.5968 0.9271 0.4904 0.029 Uiso 1 1 calc R . . C18 C 0.61812(12) 1.0179(3) 0.4073(4) 0.0254(9) Uani 1 1 d . . . H18 H 0.6081 1.0632 0.4401 0.030 Uiso 1 1 calc R . . C19 C 0.64878(12) 1.1140(3) 0.2901(4) 0.0255(10) Uani 1 1 d . . . H19 H 0.6399 1.1621 0.3203 0.031 Uiso 1 1 calc R . . C20 C 0.66988(13) 1.1234(2) 0.2119(4) 0.0259(9) Uani 1 1 d . . . H20 H 0.6758 1.1776 0.1912 0.031 Uiso 1 1 calc R . . C21 C 0.70500(12) 1.0567(3) 0.0781(4) 0.0253(10) Uani 1 1 d . . . H21 H 0.7117 1.1093 0.0540 0.030 Uiso 1 1 calc R . . C22 C 0.71630(11) 0.9846(3) 0.0334(4) 0.0218(9) Uani 1 1 d . . . H22 H 0.7310 0.9875 -0.0206 0.026 Uiso 1 1 calc R . . C23 C 0.70549(10) 0.9059(2) 0.0702(4) 0.0183(8) Uani 1 1 d . . . H23 H 0.7128 0.8570 0.0379 0.022 Uiso 1 1 calc R . . N24 N 0.68531(9) 0.89826(19) 0.1488(3) 0.0145(7) Uani 1 1 d . . . C25 C 0.67456(10) 0.9699(2) 0.1952(3) 0.0163(8) Uani 1 1 d . . . C26 C 0.68343(11) 1.0517(2) 0.1600(4) 0.0179(8) Uani 1 1 d . . . C27 C 0.63970(11) 1.0329(3) 0.3279(4) 0.0209(9) Uani 1 1 d . . . C28 C 0.65355(10) 0.9605(2) 0.2795(3) 0.0158(8) Uani 1 1 d . . . N29 N 0.65612(9) 0.6875(2) 0.3100(3) 0.0163(7) Uani 1 1 d . . . C30 C 0.62697(12) 0.6346(2) 0.2865(4) 0.0218(9) Uani 1 1 d . . . H30 H 0.6100 0.6417 0.2190 0.026 Uiso 1 1 calc R . . C31 C 0.62110(13) 0.5698(3) 0.3584(5) 0.0282(10) Uani 1 1 d . . . H31 H 0.6008 0.5340 0.3384 0.034 Uiso 1 1 calc R . . C32 C 0.64562(13) 0.5590(3) 0.4595(4) 0.0266(9) Uani 1 1 d . . . H32 H 0.6415 0.5172 0.5096 0.032 Uiso 1 1 calc R . . C33 C 0.70443(13) 0.6053(3) 0.5887(4) 0.0253(9) Uani 1 1 d . . . H33 H 0.7020 0.5637 0.6411 0.030 Uiso 1 1 calc R . . C34 C 0.73366(13) 0.6586(3) 0.6100(4) 0.0246(9) Uani 1 1 d . . . H34 H 0.7506 0.6540 0.6780 0.030 Uiso 1 1 calc R . . C35 C 0.76905(12) 0.7772(3) 0.5463(4) 0.0209(9) Uani 1 1 d . . . H35 H 0.7869 0.7758 0.6127 0.025 Uiso 1 1 calc R . . C36 C 0.77200(10) 0.8344(2) 0.4621(4) 0.0202(8) Uani 1 1 d . . . H36 H 0.7922 0.8710 0.4711 0.024 Uiso 1 1 calc R . . C37 C 0.74459(11) 0.8372(2) 0.3635(3) 0.0170(8) Uani 1 1 d . . . H37 H 0.7469 0.8763 0.3080 0.020 Uiso 1 1 calc R . . N38 N 0.71519(10) 0.7854(2) 0.3465(3) 0.0157(7) Uani 1 1 d . . . C39 C 0.71265(11) 0.7280(2) 0.4281(4) 0.0159(8) Uani 1 1 d . . . C40 C 0.73917(12) 0.7221(3) 0.5304(4) 0.0185(8) Uani 1 1 d . . . C41 C 0.67698(12) 0.6116(3) 0.4865(4) 0.0226(9) Uani 1 1 d . . . C42 C 0.68116(11) 0.6736(2) 0.4078(3) 0.0164(7) Uani 1 1 d . . . N51 N 0.88531(9) 0.70320(18) 0.5894(3) 0.0134(6) Uani 1 1 d . . . C52 C 0.85113(10) 0.6711(2) 0.5732(3) 0.0164(8) Uani 1 1 d . . . H52 H 0.8362 0.6734 0.5016 0.020 Uiso 1 1 calc R . . C53 C 0.83707(11) 0.6340(2) 0.6611(4) 0.0194(8) Uani 1 1 d . . . H53 H 0.8135 0.6101 0.6463 0.023 Uiso 1 1 calc R . . C54 C 0.85780(12) 0.6327(2) 0.7683(4) 0.0217(8) Uani 1 1 d . . . H54 H 0.8480 0.6107 0.8273 0.026 Uiso 1 1 calc R . . C55 C 0.91865(12) 0.6635(2) 0.8960(3) 0.0200(8) Uani 1 1 d . . . H55 H 0.9100 0.6443 0.9585 0.024 Uiso 1 1 calc R . . C56 C 0.95425(12) 0.6896(2) 0.9086(4) 0.0226(9) Uani 1 1 d . . . H56 H 0.9699 0.6866 0.9791 0.027 Uiso 1 1 calc R . . C57 C 1.00495(12) 0.7519(3) 0.8216(4) 0.0251(9) Uani 1 1 d . . . H57 H 1.0221 0.7492 0.8893 0.030 Uiso 1 1 calc R . . C58 C 1.01467(12) 0.7849(3) 0.7269(4) 0.0253(10) Uani 1 1 d . . . H58 H 1.0386 0.8049 0.7302 0.030 Uiso 1 1 calc R . . C59 C 0.98850(11) 0.7888(2) 0.6250(4) 0.0206(8) Uani 1 1 d . . . H59 H 0.9955 0.8120 0.5620 0.025 Uiso 1 1 calc R . . N60 N 0.95420(10) 0.76041(19) 0.6157(3) 0.0154(7) Uani 1 1 d . . . C61 C 0.94402(11) 0.7275(2) 0.7080(3) 0.0157(8) Uani 1 1 d . . . C62 C 0.96841(11) 0.7221(2) 0.8142(4) 0.0192(8) Uani 1 1 d . . . C63 C 0.89402(11) 0.6651(2) 0.7880(3) 0.0176(8) Uani 1 1 d . . . C64 C 0.90682(11) 0.6986(2) 0.6953(3) 0.0157(7) Uani 1 1 d . . . N65 N 0.92299(9) 0.6528(2) 0.4042(3) 0.0159(7) Uani 1 1 d . . . C66 C 0.95154(11) 0.6005(2) 0.4385(4) 0.0193(8) Uani 1 1 d . . . H66 H 0.9667 0.6093 0.5089 0.023 Uiso 1 1 calc R . . C67 C 0.95960(11) 0.5326(3) 0.3724(4) 0.0225(9) Uani 1 1 d . . . H67 H 0.9802 0.4984 0.3978 0.027 Uiso 1 1 calc R . . C68 C 0.93697(12) 0.5173(2) 0.2705(4) 0.0237(9) Uani 1 1 d . . . H68 H 0.9423 0.4727 0.2262 0.028 Uiso 1 1 calc R . . C69 C 0.88011(13) 0.5565(3) 0.1280(4) 0.0246(9) Uani 1 1 d . . . H69 H 0.8831 0.5109 0.0821 0.029 Uiso 1 1 calc R . . C70 C 0.85155(13) 0.6106(3) 0.0947(4) 0.0247(9) Uani 1 1 d . . . H70 H 0.8349 0.6009 0.0272 0.030 Uiso 1 1 calc R . . C71 C 0.81913(13) 0.7454(3) 0.1282(4) 0.0231(9) Uani 1 1 d . . . H71 H 0.8028 0.7413 0.0589 0.028 Uiso 1 1 calc R . . C72 C 0.81691(11) 0.8122(3) 0.1986(4) 0.0222(9) Uani 1 1 d . . . H72 H 0.7990 0.8539 0.1770 0.027 Uiso 1 1 calc R . . C73 C 0.84145(11) 0.8180(2) 0.3028(4) 0.0189(8) Uani 1 1 d . . . H73 H 0.8393 0.8635 0.3498 0.023 Uiso 1 1 calc R . . N74 N 0.86790(10) 0.76031(19) 0.3371(3) 0.0149(7) Uani 1 1 d . . . C75 C 0.87052(11) 0.6938(2) 0.2660(3) 0.0164(8) Uani 1 1 d . . . C76 C 0.84642(11) 0.6829(3) 0.1620(3) 0.0202(8) Uani 1 1 d . . . C77 C 0.90580(12) 0.5681(2) 0.2322(4) 0.0206(8) Uani 1 1 d . . . C78 C 0.90013(11) 0.6363(2) 0.3022(3) 0.0166(8) Uani 1 1 d . . . N79 N 0.89824(9) 0.88356(19) 0.5252(3) 0.0141(6) Uani 1 1 d . . . C80 C 0.87774(11) 0.9069(2) 0.5991(4) 0.0196(8) Uani 1 1 d . . . H80 H 0.8677 0.8650 0.6377 0.024 Uiso 1 1 calc R . . C81 C 0.87072(12) 0.9921(3) 0.6211(4) 0.0225(9) Uani 1 1 d . . . H81 H 0.8564 1.0058 0.6735 0.027 Uiso 1 1 calc R . . C82 C 0.88514(12) 1.0548(3) 0.5647(4) 0.0242(9) Uani 1 1 d . . . H82 H 0.8808 1.1113 0.5790 0.029 Uiso 1 1 calc R . . C83 C 0.92276(12) 1.0940(3) 0.4205(4) 0.0273(10) Uani 1 1 d . . . H83 H 0.9191 1.1515 0.4303 0.033 Uiso 1 1 calc R . . C84 C 0.94308(13) 1.0686(3) 0.3462(5) 0.0302(11) Uani 1 1 d . . . H84 H 0.9531 1.1093 0.3057 0.036 Uiso 1 1 calc R . . C85 C 0.97108(11) 0.9517(3) 0.2519(4) 0.0255(10) Uani 1 1 d . . . H85 H 0.9823 0.9899 0.2108 0.031 Uiso 1 1 calc R . . C86 C 0.97521(11) 0.8669(3) 0.2392(4) 0.0248(9) Uani 1 1 d . . . H86 H 0.9889 0.8466 0.1881 0.030 Uiso 1 1 calc R . . C87 C 0.95873(11) 0.8101(3) 0.3035(4) 0.0213(8) Uani 1 1 d . . . H87 H 0.9620 0.7523 0.2944 0.026 Uiso 1 1 calc R . . N88 N 0.93864(9) 0.8358(2) 0.3769(3) 0.0168(7) Uani 1 1 d . . . C89 C 0.93398(11) 0.9209(3) 0.3899(3) 0.0173(8) Uani 1 1 d . . . C90 C 0.94979(11) 0.9810(3) 0.3273(4) 0.0207(9) Uani 1 1 d . . . C91 C 0.90651(11) 1.0335(2) 0.4853(4) 0.0214(9) Uani 1 1 d . . . C92 C 0.91248(11) 0.9465(2) 0.4685(4) 0.0169(7) Uani 1 1 d . . . Ru1 Ru 0.668693(8) 0.789204(16) 0.218488(19) 0.01128(6) Uani 1 1 d . . . Ru2 Ru 0.911079(8) 0.764352(16) 0.47539(2) 0.01185(6) Uani 1 1 d . . . P1 P 1.03237(3) 0.57465(7) 0.15853(9) 0.0203(2) Uani 1 1 d D . . F11 F 1.02798(7) 0.59610(18) 0.0269(2) 0.0306(6) Uani 1 1 d D . . F12 F 1.06321(8) 0.50580(18) 0.1482(3) 0.0354(7) Uani 1 1 d D . . F13 F 1.06424(8) 0.64538(17) 0.1866(2) 0.0330(6) Uani 1 1 d D . . F14 F 1.03693(8) 0.55458(17) 0.2892(2) 0.0299(6) Uani 1 1 d D . . F15 F 1.00184(8) 0.6456(2) 0.1692(3) 0.0396(7) Uani 1 1 d D . . F16 F 1.00045(8) 0.5046(2) 0.1286(3) 0.0458(8) Uani 1 1 d D . . P2 P 0.78382(3) 0.53810(6) 0.34083(9) 0.01418(19) Uani 1 1 d . . . F21 F 0.78743(7) 0.53396(15) 0.2125(2) 0.0237(5) Uani 1 1 d . . . F22 F 0.82811(6) 0.53488(14) 0.3803(2) 0.0216(5) Uani 1 1 d . . . F23 F 0.78544(7) 0.63990(13) 0.3375(2) 0.0199(5) Uani 1 1 d . . . F24 F 0.78015(7) 0.54199(15) 0.4704(2) 0.0243(5) Uani 1 1 d . . . F25 F 0.73938(6) 0.54106(14) 0.3027(2) 0.0225(5) Uani 1 1 d . . . F26 F 0.78238(7) 0.43550(13) 0.3452(2) 0.0211(5) Uani 1 1 d . . . P3 P 0.79614(3) 1.08674(6) 0.32974(10) 0.0224(2) Uani 1 1 d . . . F31 F 0.79650(9) 1.0740(2) 0.1991(3) 0.0470(8) Uani 1 1 d . . . F32 F 0.82275(8) 1.00627(17) 0.3588(3) 0.0374(7) Uani 1 1 d . . . F33 F 0.83132(9) 1.1470(2) 0.3434(4) 0.0649(12) Uani 1 1 d . . . F34 F 0.79548(9) 1.0974(2) 0.4594(3) 0.0435(8) Uani 1 1 d . . . F35 F 0.76912(9) 1.16601(19) 0.2996(3) 0.0461(8) Uani 1 1 d . . . F36 F 0.76109(9) 1.02491(19) 0.3163(3) 0.0391(7) Uani 1 1 d . . . P4 P 1.04665(7) 1.00811(19) 0.5585(2) 0.0312(7) Uiso 0.651(4) 1 d P A 1 F41 F 1.04437(13) 1.0362(3) 0.4268(4) 0.0342(11) Uiso 0.651(4) 1 d P A 1 F42 F 1.00591(12) 0.9698(3) 0.5365(4) 0.0334(10) Uiso 0.651(4) 1 d P A 1 F43 F 1.03052(17) 1.0980(4) 0.5694(5) 0.0573(15) Uiso 0.651(4) 1 d P A 1 F44 F 1.04826(14) 0.9969(3) 0.6941(5) 0.0439(12) Uiso 0.651(4) 1 d P A 1 F45 F 1.08826(18) 1.0450(4) 0.5933(6) 0.0611(16) Uiso 0.651(4) 1 d P A 1 F46 F 1.06222(19) 0.9117(4) 0.5621(6) 0.0733(19) Uiso 0.651(4) 1 d P A 1 P5 P 1.04779(12) 0.9908(3) 0.5542(4) 0.0254(12) Uiso 0.349(4) 1 d PD A 2 F51 F 1.0719(4) 1.0743(7) 0.5963(11) 0.068(3) Uiso 0.349(4) 1 d PD A 2 F52 F 1.0473(3) 1.0054(6) 0.4317(7) 0.039(2) Uiso 0.349(4) 1 d PD A 2 F53 F 1.0830(2) 0.9439(5) 0.5340(7) 0.0337(19) Uiso 0.349(4) 1 d PD A 2 F54 F 1.0230(3) 0.9165(6) 0.4822(9) 0.052(3) Uiso 0.349(4) 1 d PD A 2 F55 F 1.0485(2) 0.9507(6) 0.6698(7) 0.039(2) Uiso 0.349(4) 1 d PD A 2 F56 F 1.0085(3) 1.0362(7) 0.5527(11) 0.066(3) Uiso 0.349(4) 1 d PD A 2 O101 O 1.08825(13) 0.7641(3) 0.0210(4) 0.0526(11) 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 N1 0.0150(16) 0.0128(14) 0.0158(18) 0.0047(11) 0.0060(14) 0.0015(11) C2 0.0119(17) 0.0237(18) 0.019(2) 0.0068(15) 0.0058(15) -0.0016(14) C3 0.0141(18) 0.0252(19) 0.028(2) 0.0078(17) 0.0024(17) -0.0005(15) C4 0.0140(18) 0.0230(19) 0.019(2) 0.0095(15) -0.0023(16) -0.0040(14) C5 0.027(2) 0.025(2) 0.017(2) 0.0013(16) -0.0014(17) -0.0033(16) C6 0.035(2) 0.0239(19) 0.014(2) -0.0062(16) -0.0003(18) 0.0024(17) C7 0.027(2) 0.0246(19) 0.020(2) -0.0051(16) 0.0081(17) 0.0065(16) C8 0.024(2) 0.0239(18) 0.022(2) 0.0000(15) 0.0076(16) 0.0097(15) C9 0.0147(17) 0.0177(17) 0.0137(18) -0.0018(14) -0.0020(14) 0.0043(13) N10 0.0187(16) 0.0096(13) 0.0118(16) 0.0021(11) 0.0031(13) -0.0012(11) C11 0.0168(18) 0.0104(15) 0.0137(18) 0.0029(12) 0.0019(14) -0.0019(12) C12 0.023(2) 0.0192(17) 0.017(2) -0.0007(14) 0.0042(16) -0.0001(14) C13 0.0182(19) 0.0136(16) 0.021(2) 0.0025(14) 0.0026(16) -0.0003(13) C14 0.0192(19) 0.0129(16) 0.0152(19) 0.0038(14) 0.0052(15) -0.0026(14) N15 0.0139(15) 0.0194(15) 0.0148(17) 0.0023(13) 0.0046(13) 0.0022(12) C16 0.0128(18) 0.036(2) 0.018(2) 0.0005(17) 0.0058(15) -0.0013(15) C17 0.0139(19) 0.040(2) 0.020(2) -0.0057(17) 0.0052(16) 0.0011(16) C18 0.018(2) 0.034(2) 0.024(2) -0.0139(18) 0.0026(17) 0.0083(16) C19 0.025(2) 0.022(2) 0.026(2) -0.0038(16) -0.0038(18) 0.0031(16) C20 0.026(2) 0.0187(17) 0.031(2) 0.0002(18) -0.0003(17) -0.0014(17) C21 0.024(2) 0.0232(19) 0.027(2) 0.0071(17) 0.0000(18) -0.0082(16) C22 0.0139(18) 0.029(2) 0.022(2) 0.0056(17) 0.0032(16) -0.0050(15) C23 0.0104(17) 0.0228(19) 0.022(2) 0.0012(16) 0.0029(15) 0.0015(14) N24 0.0105(14) 0.0162(14) 0.0161(17) 0.0015(12) 0.0009(12) 0.0036(11) C25 0.0108(17) 0.0200(18) 0.017(2) 0.0001(14) 0.0010(14) -0.0003(13) C26 0.0180(18) 0.0145(16) 0.018(2) 0.0012(14) -0.0041(15) -0.0023(13) C27 0.0153(19) 0.0217(19) 0.022(2) -0.0066(16) -0.0047(16) 0.0015(14) C28 0.0127(17) 0.0221(18) 0.0114(18) -0.0010(14) -0.0004(14) 0.0024(13) N29 0.0168(16) 0.0156(14) 0.0180(17) 0.0008(12) 0.0071(13) 0.0018(12) C30 0.019(2) 0.0219(19) 0.024(2) 0.0022(16) 0.0034(17) -0.0002(15) C31 0.025(2) 0.024(2) 0.040(3) 0.0107(19) 0.016(2) 0.0032(17) C32 0.031(2) 0.026(2) 0.028(2) 0.0121(17) 0.0160(19) 0.0036(16) C33 0.031(2) 0.029(2) 0.018(2) 0.0092(17) 0.0088(18) 0.0098(17) C34 0.027(2) 0.031(2) 0.015(2) 0.0032(16) 0.0042(17) 0.0107(17) C35 0.020(2) 0.0253(19) 0.017(2) -0.0032(15) 0.0017(16) 0.0110(15) C36 0.0111(17) 0.0229(19) 0.027(2) -0.0076(16) 0.0035(16) 0.0023(14) C37 0.0180(18) 0.0163(16) 0.019(2) -0.0034(14) 0.0088(15) 0.0029(13) N38 0.0185(17) 0.0186(16) 0.0105(17) -0.0013(11) 0.0038(14) 0.0046(12) C39 0.0173(18) 0.0162(17) 0.015(2) -0.0015(14) 0.0055(15) 0.0045(14) C40 0.018(2) 0.0246(19) 0.013(2) -0.0010(15) 0.0027(16) 0.0105(15) C41 0.023(2) 0.0261(19) 0.022(2) 0.0075(16) 0.0131(17) 0.0065(15) C42 0.0180(18) 0.0205(17) 0.0134(18) 0.0004(14) 0.0094(14) 0.0051(14) N51 0.0182(16) 0.0089(13) 0.0126(16) 0.0019(11) 0.0022(13) 0.0005(11) C52 0.0181(18) 0.0098(15) 0.022(2) -0.0012(13) 0.0051(15) -0.0006(12) C53 0.0176(18) 0.0157(16) 0.026(2) 0.0002(15) 0.0066(16) 0.0015(13) C54 0.030(2) 0.0153(17) 0.023(2) 0.0023(15) 0.0125(17) -0.0004(14) C55 0.033(2) 0.0145(16) 0.0126(19) 0.0040(14) 0.0045(16) 0.0016(15) C56 0.030(2) 0.0196(18) 0.016(2) 0.0015(15) -0.0012(17) 0.0068(16) C57 0.020(2) 0.030(2) 0.022(2) -0.0076(17) -0.0024(18) 0.0025(17) C58 0.0119(19) 0.033(2) 0.029(3) -0.0097(18) 0.0005(18) -0.0005(15) C59 0.020(2) 0.0210(19) 0.022(2) -0.0016(15) 0.0059(16) 0.0001(14) N60 0.0144(16) 0.0157(15) 0.0162(18) -0.0009(12) 0.0035(14) 0.0019(11) C61 0.0181(19) 0.0108(15) 0.016(2) -0.0024(13) -0.0011(15) 0.0013(13) C62 0.021(2) 0.0144(16) 0.020(2) -0.0021(14) -0.0012(16) 0.0048(14) C63 0.025(2) 0.0132(15) 0.0153(19) 0.0020(13) 0.0055(15) 0.0036(13) C64 0.0191(18) 0.0087(15) 0.019(2) 0.0011(13) 0.0023(15) 0.0019(12) N65 0.0151(15) 0.0160(14) 0.0161(17) 0.0016(12) 0.0019(13) -0.0009(11) C66 0.0186(19) 0.0199(18) 0.018(2) 0.0041(15) 0.0016(16) -0.0012(14) C67 0.0146(18) 0.0227(19) 0.033(2) 0.0022(17) 0.0119(17) 0.0034(14) C68 0.031(2) 0.0135(17) 0.032(2) -0.0035(16) 0.0171(19) -0.0022(15) C69 0.037(2) 0.0229(19) 0.017(2) -0.0034(16) 0.0129(18) -0.0075(17) C70 0.032(2) 0.030(2) 0.013(2) -0.0038(16) 0.0058(17) -0.0144(17) C71 0.022(2) 0.033(2) 0.013(2) 0.0031(17) 0.0006(17) -0.0099(17) C72 0.0169(19) 0.028(2) 0.021(2) 0.0108(17) 0.0027(16) -0.0011(15) C73 0.0188(19) 0.0224(18) 0.017(2) 0.0041(15) 0.0059(15) -0.0020(14) N74 0.0151(17) 0.0162(15) 0.0137(18) 0.0038(12) 0.0037(14) -0.0023(11) C75 0.0172(18) 0.0213(18) 0.0119(19) 0.0002(14) 0.0057(15) -0.0044(14) C76 0.0175(19) 0.029(2) 0.013(2) 0.0035(16) 0.0027(15) -0.0059(15) C77 0.027(2) 0.0177(17) 0.020(2) -0.0007(15) 0.0130(17) -0.0087(14) C78 0.0169(18) 0.0165(16) 0.018(2) 0.0021(14) 0.0080(15) -0.0053(13) N79 0.0148(15) 0.0139(14) 0.0139(16) 0.0004(12) 0.0040(12) -0.0008(11) C80 0.0152(18) 0.0225(19) 0.019(2) -0.0003(15) -0.0018(16) -0.0009(14) C81 0.023(2) 0.022(2) 0.022(2) -0.0043(16) 0.0028(17) 0.0039(16) C82 0.021(2) 0.0167(18) 0.033(3) -0.0012(16) -0.0011(18) 0.0008(15) C83 0.023(2) 0.0148(17) 0.042(3) 0.0048(17) 0.001(2) -0.0035(15) C84 0.024(2) 0.026(2) 0.038(3) 0.0120(19) 0.002(2) -0.0065(17) C85 0.0146(19) 0.037(2) 0.025(2) 0.0149(18) 0.0030(17) -0.0015(16) C86 0.0147(18) 0.041(2) 0.020(2) 0.0062(18) 0.0063(16) -0.0025(16) C87 0.0171(19) 0.029(2) 0.018(2) 0.0047(16) 0.0047(16) 0.0011(15) N88 0.0153(15) 0.0178(15) 0.0174(17) 0.0021(12) 0.0032(13) -0.0005(12) C89 0.0139(18) 0.0232(19) 0.0133(19) 0.0047(15) -0.0010(15) -0.0031(14) C90 0.0114(18) 0.025(2) 0.025(2) 0.0091(17) 0.0002(16) -0.0070(15) C91 0.0157(19) 0.0182(17) 0.025(2) 0.0039(16) -0.0073(16) -0.0034(14) C92 0.0075(15) 0.0207(16) 0.020(2) 0.0028(17) -0.0024(13) -0.0022(14) Ru1 0.01097(13) 0.01327(12) 0.01000(13) 0.00040(10) 0.00303(10) 0.00141(10) Ru2 0.01051(12) 0.01320(12) 0.01203(13) 0.00121(11) 0.00273(10) -0.00067(10) P1 0.0155(5) 0.0272(5) 0.0177(5) -0.0019(4) 0.0025(4) -0.0005(4) F11 0.0217(13) 0.0507(16) 0.0199(14) 0.0022(12) 0.0054(11) 0.0038(11) F12 0.0381(16) 0.0382(15) 0.0318(16) -0.0027(12) 0.0115(13) 0.0138(12) F13 0.0309(14) 0.0358(14) 0.0323(16) -0.0031(11) 0.0063(12) -0.0117(11) F14 0.0308(14) 0.0384(14) 0.0202(14) 0.0021(11) 0.0047(11) 0.0004(11) F15 0.0289(14) 0.0628(19) 0.0280(16) 0.0009(13) 0.0079(12) 0.0247(13) F16 0.0369(16) 0.070(2) 0.0340(18) -0.0157(15) 0.0144(14) -0.0339(15) P2 0.0175(5) 0.0131(4) 0.0121(5) -0.0008(3) 0.0033(4) 0.0001(3) F21 0.0277(13) 0.0278(12) 0.0168(12) -0.0030(9) 0.0074(10) -0.0037(9) F22 0.0130(11) 0.0219(11) 0.0273(14) -0.0018(9) -0.0020(10) -0.0007(8) F23 0.0216(12) 0.0130(10) 0.0238(12) 0.0016(8) 0.0017(10) 0.0011(8) F24 0.0354(14) 0.0249(12) 0.0152(12) -0.0018(9) 0.0112(10) 0.0002(10) F25 0.0154(11) 0.0260(12) 0.0265(14) 0.0007(9) 0.0049(10) -0.0009(9) F26 0.0257(13) 0.0116(10) 0.0258(13) -0.0021(9) 0.0047(11) -0.0023(9) P3 0.0224(5) 0.0185(5) 0.0256(6) 0.0043(4) 0.0027(4) 0.0010(4) F31 0.0519(19) 0.065(2) 0.0290(17) 0.0163(15) 0.0184(14) 0.0272(16) F32 0.0350(15) 0.0279(13) 0.0439(19) 0.0045(12) -0.0044(13) 0.0158(11) F33 0.0385(18) 0.0361(17) 0.120(4) 0.0078(19) 0.016(2) -0.0145(14) F34 0.0535(19) 0.0474(17) 0.0247(16) -0.0121(13) -0.0040(14) 0.0069(14) F35 0.0476(18) 0.0391(16) 0.056(2) 0.0171(14) 0.0197(16) 0.0239(13) F36 0.0369(16) 0.0457(16) 0.0317(17) -0.0043(13) -0.0001(13) -0.0173(13) O101 0.065(3) 0.048(2) 0.050(3) -0.0090(19) 0.023(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.333(5) . ? N1 C14 1.370(5) . ? N1 Ru1 2.055(4) . ? C2 C3 1.397(6) . ? C3 C4 1.355(7) . ? C4 C13 1.413(6) . ? C5 C6 1.361(6) . ? C5 C13 1.420(6) . ? C6 C12 1.434(6) . ? C7 C8 1.367(6) . ? C7 C12 1.409(6) . ? C8 C9 1.408(6) . ? C9 N10 1.334(5) . ? N10 C11 1.375(5) . ? N10 Ru1 2.054(3) . ? C11 C12 1.399(6) . ? C11 C14 1.425(5) . ? C13 C14 1.402(6) . ? N15 C16 1.323(5) . ? N15 C28 1.370(5) . ? N15 Ru1 2.072(3) . ? C16 C17 1.404(6) . ? C17 C18 1.366(7) . ? C18 C27 1.386(7) . ? C19 C20 1.349(7) . ? C19 C27 1.424(6) . ? C20 C26 1.434(6) . ? C21 C22 1.362(6) . ? C21 C26 1.393(6) . ? C22 C23 1.405(6) . ? C23 N24 1.327(5) . ? N24 C25 1.358(5) . ? N24 Ru1 2.065(3) . ? C25 C28 1.409(6) . ? C25 C26 1.419(5) . ? C27 C28 1.426(6) . ? N29 C30 1.344(5) . ? N29 C42 1.365(5) . ? N29 Ru1 2.057(3) . ? C30 C31 1.389(6) . ? C31 C32 1.378(7) . ? C32 C41 1.406(6) . ? C33 C34 1.349(6) . ? C33 C41 1.435(6) . ? C34 C40 1.435(6) . ? C35 C36 1.383(6) . ? C35 C40 1.385(6) . ? C36 C37 1.400(6) . ? C37 N38 1.339(5) . ? N38 C39 1.359(5) . ? N38 Ru1 2.065(4) . ? C39 C40 1.417(6) . ? C39 C42 1.424(6) . ? C41 C42 1.396(6) . ? N51 C52 1.334(5) . ? N51 C64 1.366(5) . ? N51 Ru2 2.067(3) . ? C52 C53 1.403(6) . ? C53 C54 1.367(6) . ? C54 C63 1.403(6) . ? C55 C56 1.353(6) . ? C55 C63 1.434(5) . ? C56 C62 1.444(6) . ? C57 C58 1.372(7) . ? C57 C62 1.411(6) . ? C58 C59 1.405(6) . ? C59 N60 1.323(5) . ? N60 C61 1.353(6) . ? N60 Ru2 2.079(4) . ? C61 C62 1.415(5) . ? C61 C64 1.422(5) . ? C63 C64 1.406(6) . ? N65 C66 1.335(5) . ? N65 C78 1.372(5) . ? N65 Ru2 2.048(3) . ? C66 C67 1.406(6) . ? C67 C68 1.363(6) . ? C68 C77 1.400(6) . ? C69 C70 1.351(7) . ? C69 C77 1.428(6) . ? C70 C76 1.438(6) . ? C71 C72 1.370(7) . ? C71 C76 1.408(6) . ? C72 C73 1.399(6) . ? C73 N74 1.337(5) . ? N74 C75 1.375(5) . ? N74 Ru2 2.064(4) . ? C75 C76 1.397(6) . ? C75 C78 1.418(5) . ? C77 C78 1.413(6) . ? N79 C80 1.335(6) . ? N79 C92 1.371(5) . ? N79 Ru2 2.061(3) . ? C80 C81 1.405(5) . ? C81 C82 1.370(6) . ? C82 C91 1.401(7) . ? C83 C84 1.343(7) . ? C83 C91 1.441(6) . ? C84 C90 1.433(7) . ? C85 C86 1.361(7) . ? C85 C90 1.398(7) . ? C86 C87 1.405(6) . ? C87 N88 1.330(6) . ? N88 C89 1.369(5) . ? N88 Ru2 2.054(3) . ? C89 C90 1.411(6) . ? C89 C92 1.415(6) . ? C91 C92 1.414(5) . ? P1 F14 1.590(3) . ? P1 F12 1.595(3) . ? P1 F16 1.602(3) . ? P1 F13 1.606(3) . ? P1 F11 1.606(3) . ? P1 F15 1.611(3) . ? P2 F21 1.589(3) . ? P2 F22 1.604(2) . ? P2 F24 1.605(3) . ? P2 F25 1.608(2) . ? P2 F23 1.610(2) . ? P2 F26 1.623(2) . ? P3 F34 1.585(3) . ? P3 F33 1.589(3) . ? P3 F35 1.595(3) . ? P3 F31 1.599(3) . ? P3 F32 1.600(3) . ? P3 F36 1.600(3) . ? P4 F43 1.555(6) . ? P4 F42 1.589(5) . ? P4 F45 1.613(7) . ? P4 F46 1.625(7) . ? P4 F44 1.642(6) . ? P4 F41 1.642(6) . ? P5 F52 1.499(9) . ? P5 F55 1.533(9) . ? P5 F53 1.554(8) . ? P5 F56 1.610(10) . ? P5 F51 1.613(11) . ? P5 F54 1.627(9) . ? 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 C2 N1 C14 117.6(4) . . ? C2 N1 Ru1 129.1(3) . . ? C14 N1 Ru1 113.3(3) . . ? N1 C2 C3 122.6(4) . . ? C4 C3 C2 120.2(4) . . ? C3 C4 C13 119.4(4) . . ? C6 C5 C13 120.8(4) . . ? C5 C6 C12 121.4(4) . . ? C8 C7 C12 119.8(4) . . ? C7 C8 C9 119.4(4) . . ? N10 C9 C8 122.9(4) . . ? C9 N10 C11 117.2(3) . . ? C9 N10 Ru1 129.5(3) . . ? C11 N10 Ru1 113.3(2) . . ? N10 C11 C12 123.6(4) . . ? N10 C11 C14 116.3(3) . . ? C12 C11 C14 120.1(4) . . ? C11 C12 C7 117.1(4) . . ? C11 C12 C6 118.4(4) . . ? C7 C12 C6 124.5(4) . . ? C14 C13 C4 117.2(4) . . ? C14 C13 C5 119.0(4) . . ? C4 C13 C5 123.8(4) . . ? N1 C14 C13 123.0(4) . . ? N1 C14 C11 116.7(3) . . ? C13 C14 C11 120.3(4) . . ? C16 N15 C28 118.3(4) . . ? C16 N15 Ru1 129.0(3) . . ? C28 N15 Ru1 112.5(3) . . ? N15 C16 C17 122.3(4) . . ? C18 C17 C16 119.6(4) . . ? C17 C18 C27 120.4(4) . . ? C20 C19 C27 122.0(4) . . ? C19 C20 C26 121.5(4) . . ? C22 C21 C26 120.0(4) . . ? C21 C22 C23 119.0(4) . . ? N24 C23 C22 122.9(4) . . ? C23 N24 C25 118.3(3) . . ? C23 N24 Ru1 128.7(3) . . ? C25 N24 Ru1 113.0(3) . . ? N24 C25 C28 117.5(3) . . ? N24 C25 C26 122.0(4) . . ? C28 C25 C26 120.5(4) . . ? C21 C26 C25 117.7(4) . . ? C21 C26 C20 124.5(4) . . ? C25 C26 C20 117.8(4) . . ? C18 C27 C19 125.6(4) . . ? C18 C27 C28 116.8(4) . . ? C19 C27 C28 117.6(4) . . ? N15 C28 C25 117.0(3) . . ? N15 C28 C27 122.4(4) . . ? C25 C28 C27 120.5(4) . . ? C30 N29 C42 117.0(3) . . ? C30 N29 Ru1 128.9(3) . . ? C42 N29 Ru1 114.1(3) . . ? N29 C30 C31 123.0(4) . . ? C32 C31 C30 119.5(4) . . ? C31 C32 C41 119.5(4) . . ? C34 C33 C41 121.1(4) . . ? C33 C34 C40 121.6(4) . . ? C36 C35 C40 119.1(4) . . ? C35 C36 C37 120.0(4) . . ? N38 C37 C36 122.2(4) . . ? C37 N38 C39 117.9(4) . . ? C37 N38 Ru1 128.3(3) . . ? C39 N38 Ru1 113.4(3) . . ? N38 C39 C40 123.0(4) . . ? N38 C39 C42 116.8(4) . . ? C40 C39 C42 120.2(4) . . ? C35 C40 C39 117.8(4) . . ? C35 C40 C34 124.2(4) . . ? C39 C40 C34 117.9(4) . . ? C42 C41 C32 117.0(4) . . ? C42 C41 C33 118.8(4) . . ? C32 C41 C33 124.1(4) . . ? N29 C42 C41 123.9(4) . . ? N29 C42 C39 115.8(4) . . ? C41 C42 C39 120.3(4) . . ? C52 N51 C64 117.9(3) . . ? C52 N51 Ru2 128.8(3) . . ? C64 N51 Ru2 113.3(3) . . ? N51 C52 C53 121.9(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 C63 118.9(4) . . ? C56 C55 C63 121.1(4) . . ? C55 C56 C62 121.1(4) . . ? C58 C57 C62 118.7(4) . . ? C57 C58 C59 120.2(4) . . ? N60 C59 C58 122.2(4) . . ? C59 N60 C61 118.6(4) . . ? C59 N60 Ru2 128.1(3) . . ? C61 N60 Ru2 113.2(3) . . ? N60 C61 C62 122.9(4) . . ? N60 C61 C64 117.1(4) . . ? C62 C61 C64 119.9(4) . . ? C57 C62 C61 117.3(4) . . ? C57 C62 C56 124.1(4) . . ? C61 C62 C56 118.5(4) . . ? C54 C63 C64 117.6(4) . . ? C54 C63 C55 123.5(4) . . ? C64 C63 C55 118.9(4) . . ? N51 C64 C63 123.1(4) . . ? N51 C64 C61 116.5(4) . . ? C63 C64 C61 120.4(4) . . ? C66 N65 C78 117.6(3) . . ? C66 N65 Ru2 128.6(3) . . ? C78 N65 Ru2 113.5(2) . . ? N65 C66 C67 122.6(4) . . ? C68 C67 C66 119.3(4) . . ? C67 C68 C77 120.5(4) . . ? C70 C69 C77 121.2(4) . . ? C69 C70 C76 121.1(4) . . ? C72 C71 C76 119.2(4) . . ? C71 C72 C73 120.2(4) . . ? N74 C73 C72 122.2(4) . . ? C73 N74 C75 117.7(4) . . ? C73 N74 Ru2 128.6(3) . . ? C75 N74 Ru2 113.1(3) . . ? N74 C75 C76 123.2(4) . . ? N74 C75 C78 116.3(4) . . ? C76 C75 C78 120.5(4) . . ? C75 C76 C71 117.5(4) . . ? C75 C76 C70 118.5(4) . . ? C71 C76 C70 124.0(4) . . ? C68 C77 C78 116.7(4) . . ? C68 C77 C69 124.9(4) . . ? C78 C77 C69 118.5(4) . . ? N65 C78 C77 123.2(4) . . ? N65 C78 C75 116.7(3) . . ? C77 C78 C75 120.1(4) . . ? C80 N79 C92 117.4(3) . . ? C80 N79 Ru2 130.0(3) . . ? C92 N79 Ru2 112.5(3) . . ? N79 C80 C81 122.9(4) . . ? C82 C81 C80 119.5(4) . . ? C81 C82 C91 119.9(4) . . ? C84 C83 C91 121.1(4) . . ? C83 C84 C90 122.2(4) . . ? C86 C85 C90 119.3(4) . . ? C85 C86 C87 119.7(4) . . ? N88 C87 C86 122.5(4) . . ? C87 N88 C89 118.5(4) . . ? C87 N88 Ru2 128.9(3) . . ? C89 N88 Ru2 112.6(3) . . ? N88 C89 C90 121.6(4) . . ? N88 C89 C92 117.3(3) . . ? C90 C89 C92 121.2(4) . . ? C85 C90 C89 118.4(4) . . ? C85 C90 C84 124.2(4) . . ? C89 C90 C84 117.4(4) . . ? C82 C91 C92 117.2(4) . . ? C82 C91 C83 124.6(4) . . ? C92 C91 C83 118.2(4) . . ? N79 C92 C91 123.1(4) . . ? N79 C92 C89 116.9(3) . . ? C91 C92 C89 119.9(4) . . ? N10 Ru1 N1 80.27(13) . . ? N10 Ru1 N29 91.29(13) . . ? N1 Ru1 N29 95.51(13) . . ? N10 Ru1 N38 99.58(13) . . ? N1 Ru1 N38 174.87(14) . . ? N29 Ru1 N38 79.37(14) . . ? N10 Ru1 N24 94.22(12) . . ? N1 Ru1 N24 91.55(12) . . ? N29 Ru1 N24 171.69(14) . . ? N38 Ru1 N24 93.57(13) . . ? N10 Ru1 N15 170.70(13) . . ? N1 Ru1 N15 92.57(13) . . ? N29 Ru1 N15 95.33(13) . . ? N38 Ru1 N15 88.08(13) . . ? N24 Ru1 N15 79.95(14) . . ? N65 Ru2 N88 93.13(13) . . ? N65 Ru2 N79 172.13(14) . . ? N88 Ru2 N79 80.66(13) . . ? N65 Ru2 N74 80.03(13) . . ? N88 Ru2 N74 86.26(13) . . ? N79 Ru2 N74 94.66(13) . . ? N65 Ru2 N51 92.63(13) . . ? N88 Ru2 N51 173.14(13) . . ? N79 Ru2 N51 93.89(13) . . ? N74 Ru2 N51 98.41(13) . . ? N65 Ru2 N60 97.22(13) . . ? N88 Ru2 N60 96.13(14) . . ? N79 Ru2 N60 88.30(12) . . ? N74 Ru2 N60 176.47(11) . . ? N51 Ru2 N60 79.44(14) . . ? F14 P1 F12 90.53(16) . . ? F14 P1 F16 90.73(16) . . ? F12 P1 F16 90.68(18) . . ? F14 P1 F13 90.13(15) . . ? F12 P1 F13 89.42(16) . . ? F16 P1 F13 179.13(18) . . ? F14 P1 F11 179.27(18) . . ? F12 P1 F11 89.75(16) . . ? F16 P1 F11 89.94(16) . . ? F13 P1 F11 89.19(16) . . ? F14 P1 F15 89.64(16) . . ? F12 P1 F15 178.88(18) . . ? F16 P1 F15 90.42(18) . . ? F13 P1 F15 89.47(17) . . ? F11 P1 F15 90.07(15) . . ? F21 P2 F22 90.51(14) . . ? F21 P2 F24 179.83(17) . . ? F22 P2 F24 89.51(14) . . ? F21 P2 F25 90.12(14) . . ? F22 P2 F25 179.34(16) . . ? F24 P2 F25 89.86(14) . . ? F21 P2 F23 90.33(14) . . ? F22 P2 F23 89.92(12) . . ? F24 P2 F23 89.84(14) . . ? F25 P2 F23 90.26(12) . . ? F21 P2 F26 90.02(14) . . ? F22 P2 F26 89.79(13) . . ? F24 P2 F26 89.81(14) . . ? F25 P2 F26 90.02(12) . . ? F23 P2 F26 179.55(17) . . ? F34 P3 F33 90.5(2) . . ? F34 P3 F35 90.54(18) . . ? F33 P3 F35 90.63(19) . . ? F34 P3 F31 178.8(2) . . ? F33 P3 F31 90.5(2) . . ? F35 P3 F31 90.09(18) . . ? F34 P3 F32 89.90(17) . . ? F33 P3 F32 90.17(18) . . ? F35 P3 F32 179.1(2) . . ? F31 P3 F32 89.45(17) . . ? F34 P3 F36 89.53(18) . . ? F33 P3 F36 179.18(19) . . ? F35 P3 F36 90.19(18) . . ? F31 P3 F36 89.50(19) . . ? F32 P3 F36 89.01(16) . . ? F43 P4 F42 89.9(3) . . ? F43 P4 F45 90.4(4) . . ? F42 P4 F45 174.5(4) . . ? F43 P4 F46 172.9(4) . . ? F42 P4 F46 87.9(3) . . ? F45 P4 F46 91.2(4) . . ? F43 P4 F44 87.2(3) . . ? F42 P4 F44 88.2(3) . . ? F45 P4 F44 86.4(3) . . ? F46 P4 F44 86.0(3) . . ? F43 P4 F41 83.7(3) . . ? F42 P4 F41 94.6(3) . . ? F45 P4 F41 90.9(3) . . ? F46 P4 F41 103.2(4) . . ? F44 P4 F41 170.5(3) . . ? F52 P5 F55 164.5(6) . . ? F52 P5 F53 76.2(5) . . ? F55 P5 F53 94.9(5) . . ? F52 P5 F56 95.2(6) . . ? F55 P5 F56 92.5(6) . . ? F53 P5 F56 170.2(6) . . ? F52 P5 F51 94.8(6) . . ? F55 P5 F51 98.1(6) . . ? F53 P5 F51 91.0(6) . . ? F56 P5 F51 94.2(7) . . ? F52 P5 F54 71.8(6) . . ? F55 P5 F54 95.5(6) . . ? F53 P5 F54 88.1(5) . . ? F56 P5 F54 84.9(6) . . ? F51 P5 F54 166.4(7) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.202 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.090 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 242568' # data_252001a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H54 F24 N12 O3 P4 Ru2' _chemical_formula_weight 1917.30 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.9342(13) _cell_length_b 17.6216(18) _cell_length_c 31.042(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7075.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13893 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 28.40 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3832 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7611 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_process_details 'Bruker 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 'CCD area detector' _diffrn_measurement_method '\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51702 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.40 _reflns_number_total 17596 _reflns_number_gt 13893 _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, 1997)' _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^)+(0.0172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(13) _refine_ls_number_reflns 17596 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _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 N1 N 0.4657(2) 0.62418(14) 0.98907(8) 0.0142(6) Uani 1 1 d . . . C2 C 0.3871(2) 0.65276(17) 0.96771(10) 0.0173(7) Uani 1 1 d . . . H2 H 0.3209 0.6352 0.9738 0.021 Uiso 1 1 calc R . . C3 C 0.3991(3) 0.70819(18) 0.93634(10) 0.0188(8) Uani 1 1 d . . . H3 H 0.3418 0.7269 0.9217 0.023 Uiso 1 1 calc R . . C4 C 0.4955(3) 0.73513(18) 0.92717(10) 0.0209(8) Uani 1 1 d . . . H4 H 0.5049 0.7716 0.9058 0.025 Uiso 1 1 calc R . . C5 C 0.6819(3) 0.73238(19) 0.94361(10) 0.0203(8) Uani 1 1 d . . . H5 H 0.6949 0.7691 0.9228 0.024 Uiso 1 1 calc R . . C6 C 0.7610(3) 0.70497(17) 0.96650(10) 0.0196(7) Uani 1 1 d . . . H6 H 0.8275 0.7234 0.9619 0.024 Uiso 1 1 calc R . . C7 C 0.8221(2) 0.61611(17) 1.02329(10) 0.0194(8) Uani 1 1 d . . . H7 H 0.8899 0.6332 1.0211 0.023 Uiso 1 1 calc R . . C8 C 0.7969(3) 0.56007(18) 1.05121(10) 0.0205(8) Uani 1 1 d . . . H8 H 0.8480 0.5377 1.0680 0.025 Uiso 1 1 calc R . . C9 C 0.6960(2) 0.53599(19) 1.05495(10) 0.0184(7) Uani 1 1 d . . . H9 H 0.6806 0.4976 1.0745 0.022 Uiso 1 1 calc R . . N10 N 0.62060(19) 0.56517(13) 1.03196(8) 0.0131(6) Uani 1 1 d . . . C11 C 0.6442(2) 0.62103(17) 1.00406(9) 0.0141(7) Uani 1 1 d . . . C12 C 0.5614(2) 0.65247(17) 0.98061(9) 0.0129(7) Uani 1 1 d . . . C13 C 0.5789(3) 0.70745(18) 0.95001(10) 0.0151(7) Uani 1 1 d . . . C14 C 0.7439(2) 0.64780(18) 0.99785(9) 0.0154(7) Uani 1 1 d . . . N15 N 0.50288(18) 0.46111(15) 0.98167(7) 0.0126(6) Uani 1 1 d . . . C16 C 0.5098(2) 0.47415(19) 0.93967(9) 0.0179(7) Uani 1 1 d . . . H16 H 0.4975 0.5229 0.9294 0.022 Uiso 1 1 calc R . . C17 C 0.5346(3) 0.41737(19) 0.91066(10) 0.0203(7) Uani 1 1 d . . . H17 H 0.5398 0.4285 0.8815 0.024 Uiso 1 1 calc R . . C18 C 0.5512(2) 0.34690(19) 0.92438(10) 0.0193(8) Uani 1 1 d . . . H18 H 0.5661 0.3087 0.9047 0.023 Uiso 1 1 calc R . . C19 C 0.5633(2) 0.25739(18) 0.98610(10) 0.0182(8) Uani 1 1 d . . . H19 H 0.5769 0.2167 0.9679 0.022 Uiso 1 1 calc R . . C20 C 0.5603(2) 0.24616(18) 1.02893(11) 0.0202(7) Uani 1 1 d . . . H20 H 0.5736 0.1981 1.0400 0.024 Uiso 1 1 calc R . . C21 C 0.5340(3) 0.29833(18) 1.10181(10) 0.0191(7) Uani 1 1 d . . . H21 H 0.5483 0.2516 1.1145 0.023 Uiso 1 1 calc R . . C22 C 0.5099(2) 0.35913(18) 1.12667(10) 0.0183(8) Uani 1 1 d . . . H22 H 0.5077 0.3545 1.1565 0.022 Uiso 1 1 calc R . . C23 C 0.4887(2) 0.42798(18) 1.10725(9) 0.0162(7) Uani 1 1 d . . . H23 H 0.4717 0.4690 1.1247 0.019 Uiso 1 1 calc R . . N24 N 0.49122(19) 0.43854(13) 1.06539(8) 0.0123(6) Uani 1 1 d . . . C25 C 0.5159(2) 0.37755(17) 1.04081(9) 0.0126(7) Uani 1 1 d . . . C26 C 0.5219(2) 0.38932(17) 0.99556(9) 0.0135(7) Uani 1 1 d . . . C27 C 0.5461(2) 0.33017(18) 0.96848(10) 0.0174(7) Uani 1 1 d . . . C28 C 0.5372(2) 0.30640(17) 1.05729(10) 0.0154(7) Uani 1 1 d . . . N29 N 0.31252(18) 0.51447(13) 1.03057(8) 0.0127(6) Uani 1 1 d . . . C30 C 0.2559(2) 0.47453(18) 1.00333(10) 0.0164(7) Uani 1 1 d . . . H30 H 0.2874 0.4551 0.9788 0.020 Uiso 1 1 calc R . . C31 C 0.1530(3) 0.46057(19) 1.00974(10) 0.0184(7) Uani 1 1 d . . . H31 H 0.1164 0.4316 0.9899 0.022 Uiso 1 1 calc R . . C32 C 0.1044(3) 0.48854(17) 1.04456(10) 0.0194(8) Uani 1 1 d . . . H32 H 0.0349 0.4780 1.0494 0.023 Uiso 1 1 calc R . . C33 C 0.1172(3) 0.56920(18) 1.11010(10) 0.0181(7) Uani 1 1 d . . . H33 H 0.0482 0.5605 1.1169 0.022 Uiso 1 1 calc R . . C34 C 0.1725(3) 0.61465(18) 1.13507(10) 0.0189(8) Uani 1 1 d . . . H34 H 0.1412 0.6376 1.1587 0.023 Uiso 1 1 calc R . . C35 C 0.3395(3) 0.67806(18) 1.14982(10) 0.0189(8) Uani 1 1 d . . . H35 H 0.3124 0.7040 1.1733 0.023 Uiso 1 1 calc R . . C36 C 0.4403(3) 0.68808(17) 1.13803(10) 0.0198(8) Uani 1 1 d . . . H36 H 0.4823 0.7215 1.1532 0.024 Uiso 1 1 calc R . . C37 C 0.4792(3) 0.64807(17) 1.10333(9) 0.0180(7) Uani 1 1 d . . . H37 H 0.5479 0.6557 1.0956 0.022 Uiso 1 1 calc R . . N38 N 0.42468(19) 0.60027(14) 1.08087(8) 0.0122(6) Uani 1 1 d . . . C39 C 0.3231(2) 0.59156(17) 1.09164(9) 0.0127(7) Uani 1 1 d . . . C40 C 0.2643(2) 0.54523(17) 1.06470(9) 0.0124(7) Uani 1 1 d . . . C41 C 0.1599(2) 0.53351(19) 1.07331(10) 0.0160(7) Uani 1 1 d . . . C42 C 0.2789(3) 0.62907(17) 1.12650(9) 0.0149(7) Uani 1 1 d . . . Ru43 Ru 0.46859(2) 0.534934(14) 1.030134(8) 0.01253(6) Uani 1 1 d . . . N51 N 0.2770(2) 0.23699(14) 0.15301(7) 0.0121(6) Uani 1 1 d . . . C52 C 0.2605(2) 0.31055(18) 0.15229(10) 0.0175(8) Uani 1 1 d . . . H52 H 0.2509 0.3360 0.1782 0.021 Uiso 1 1 calc R . . C53 C 0.2570(2) 0.35129(19) 0.11435(10) 0.0221(8) Uani 1 1 d . . . H53 H 0.2432 0.4031 0.1151 0.027 Uiso 1 1 calc R . . C54 C 0.2734(2) 0.31619(18) 0.07586(10) 0.0233(8) Uani 1 1 d . . . H54 H 0.2728 0.3440 0.0504 0.028 Uiso 1 1 calc R . . C55 C 0.3068(2) 0.1955(2) 0.03748(11) 0.0251(9) Uani 1 1 d . . . H55 H 0.3109 0.2204 0.0111 0.030 Uiso 1 1 calc R . . C56 C 0.3160(3) 0.1201(2) 0.03861(11) 0.0254(9) Uani 1 1 d . . . H56 H 0.3266 0.0934 0.0131 0.030 Uiso 1 1 calc R . . C57 C 0.3123(2) 0.0016(2) 0.08186(10) 0.0230(8) Uani 1 1 d . . . H57 H 0.3207 -0.0283 0.0574 0.028 Uiso 1 1 calc R . . C58 C 0.3027(2) -0.0312(2) 0.12060(11) 0.0236(8) Uani 1 1 d . . . H58 H 0.3022 -0.0838 0.1231 0.028 Uiso 1 1 calc R . . C59 C 0.2935(3) 0.01399(18) 0.15699(10) 0.0202(8) Uani 1 1 d . . . H59 H 0.2878 -0.0093 0.1838 0.024 Uiso 1 1 calc R . . N60 N 0.2923(2) 0.08883(14) 0.15510(8) 0.0131(6) Uani 1 1 d . . . C61 C 0.2992(2) 0.12138(17) 0.11584(9) 0.0136(7) Uani 1 1 d . . . C62 C 0.2907(2) 0.20103(17) 0.11457(9) 0.0147(7) Uani 1 1 d . . . C63 C 0.2913(2) 0.23816(18) 0.07505(10) 0.0175(7) Uani 1 1 d . . . C64 C 0.3098(2) 0.07993(19) 0.07832(10) 0.0175(8) Uani 1 1 d . . . N65 N 0.12692(18) 0.15272(14) 0.20989(7) 0.0120(6) Uani 1 1 d . . . C66 C 0.0539(2) 0.19299(17) 0.19089(9) 0.0157(7) Uani 1 1 d . . . H66 H 0.0728 0.2303 0.1712 0.019 Uiso 1 1 calc R . . C67 C -0.0502(2) 0.18126(18) 0.19945(10) 0.0202(8) Uani 1 1 d . . . H67 H -0.1000 0.2110 0.1860 0.024 Uiso 1 1 calc R . . C68 C -0.0788(3) 0.12651(19) 0.22748(10) 0.0219(8) Uani 1 1 d . . . H68 H -0.1485 0.1180 0.2331 0.026 Uiso 1 1 calc R . . C69 C -0.0242(3) 0.02329(18) 0.27748(9) 0.0217(8) Uani 1 1 d . . . H69 H -0.0925 0.0114 0.2841 0.026 Uiso 1 1 calc R . . C70 C 0.0515(2) -0.01604(18) 0.29595(11) 0.0206(8) Uani 1 1 d . . . H70 H 0.0351 -0.0552 0.3148 0.025 Uiso 1 1 calc R . . C71 C 0.2402(3) -0.0370(2) 0.30450(9) 0.0231(8) Uani 1 1 d . . . H71 H 0.2291 -0.0779 0.3228 0.028 Uiso 1 1 calc R . . C72 C 0.3381(3) -0.01566(18) 0.29519(11) 0.0220(8) Uani 1 1 d . . . H72 H 0.3941 -0.0412 0.3072 0.026 Uiso 1 1 calc R . . C73 C 0.3534(3) 0.04528(19) 0.26730(10) 0.0215(8) Uani 1 1 d . . . H73 H 0.4206 0.0605 0.2611 0.026 Uiso 1 1 calc R . . N74 N 0.2765(2) 0.08164(14) 0.24958(8) 0.0144(6) Uani 1 1 d . . . C75 C 0.1787(2) 0.05918(18) 0.25910(9) 0.0142(7) Uani 1 1 d . . . C76 C 0.0982(2) 0.09903(17) 0.23818(9) 0.0125(7) Uani 1 1 d . . . C77 C -0.0038(2) 0.08288(19) 0.24801(10) 0.0164(7) Uani 1 1 d . . . C78 C 0.1568(3) 0.00068(18) 0.28739(9) 0.0158(7) Uani 1 1 d . . . N79 N 0.2888(2) 0.24324(14) 0.25293(7) 0.0142(6) Uani 1 1 d . . . C80 C 0.2131(3) 0.26744(17) 0.27795(9) 0.0164(7) Uani 1 1 d . . . H80 H 0.1461 0.2512 0.2723 0.020 Uiso 1 1 calc R . . C81 C 0.2295(3) 0.31620(17) 0.31240(9) 0.0189(8) Uani 1 1 d . . . H81 H 0.1747 0.3297 0.3303 0.023 Uiso 1 1 calc R . . C82 C 0.3250(3) 0.34398(18) 0.31990(9) 0.0186(7) Uani 1 1 d . . . H82 H 0.3361 0.3779 0.3424 0.022 Uiso 1 1 calc R . . C83 C 0.5092(2) 0.34787(17) 0.29849(10) 0.0175(7) Uani 1 1 d . . . H83 H 0.5244 0.3843 0.3192 0.021 Uiso 1 1 calc R . . C84 C 0.5850(3) 0.32075(18) 0.27328(10) 0.0196(8) Uani 1 1 d . . . H84 H 0.6517 0.3395 0.2767 0.024 Uiso 1 1 calc R . . C85 C 0.6424(3) 0.23180(19) 0.21642(10) 0.0209(8) Uani 1 1 d . . . H85 H 0.7108 0.2476 0.2188 0.025 Uiso 1 1 calc R . . C86 C 0.6169(3) 0.17678(19) 0.18814(10) 0.0198(8) Uani 1 1 d . . . H86 H 0.6676 0.1544 0.1711 0.024 Uiso 1 1 calc R . . C87 C 0.5142(2) 0.15357(18) 0.18451(9) 0.0151(7) Uani 1 1 d . . . H87 H 0.4978 0.1152 0.1651 0.018 Uiso 1 1 calc R . . N88 N 0.43939(19) 0.18415(13) 0.20768(8) 0.0125(6) Uani 1 1 d . . . C89 C 0.4655(3) 0.23886(17) 0.23613(9) 0.0132(7) Uani 1 1 d . . . C90 C 0.3856(2) 0.26878(17) 0.26177(10) 0.0139(7) Uani 1 1 d . . . C91 C 0.4062(2) 0.32156(17) 0.29378(10) 0.0151(7) Uani 1 1 d . . . C92 C 0.5668(2) 0.26483(18) 0.24185(10) 0.0154(7) Uani 1 1 d . . . Ru93 Ru 0.283314(19) 0.164990(14) 0.204523(8) 0.01210(6) Uani 1 1 d . . . P1 P 0.34579(7) 0.49573(5) 0.22154(3) 0.0181(2) Uani 1 1 d . . . F2 F 0.39891(15) 0.41588(10) 0.21406(6) 0.0269(5) Uani 1 1 d . . . F3 F 0.25941(15) 0.45722(12) 0.25074(7) 0.0410(6) Uani 1 1 d . . . F4 F 0.41432(14) 0.50844(10) 0.26289(5) 0.0258(5) Uani 1 1 d . . . F5 F 0.29238(16) 0.57551(10) 0.22844(6) 0.0288(5) Uani 1 1 d . . . F6 F 0.43113(13) 0.53452(10) 0.19230(5) 0.0211(4) Uani 1 1 d . . . F7 F 0.27642(16) 0.48233(10) 0.18012(6) 0.0298(5) Uani 1 1 d . . . P11 P 0.08963(7) 0.82825(6) 0.19178(3) 0.0252(2) Uani 1 1 d . . . F12 F 0.01936(16) 0.75940(11) 0.17761(6) 0.0361(5) Uani 1 1 d . . . F13 F 0.15716(17) 0.77175(13) 0.21970(7) 0.0494(7) Uani 1 1 d . . . F14 F 0.01532(17) 0.84301(13) 0.23070(7) 0.0498(7) Uani 1 1 d . . . F15 F 0.16025(17) 0.89675(12) 0.20588(7) 0.0456(6) Uani 1 1 d . . . F16 F 0.02238(18) 0.88342(12) 0.16261(8) 0.0527(7) Uani 1 1 d . . . F17 F 0.16292(16) 0.81322(11) 0.15218(6) 0.0368(6) Uani 1 1 d . . . P21 P 0.57936(7) 0.85313(5) 0.05684(3) 0.0201(2) Uani 1 1 d . . . F22 F 0.50459(13) 0.79373(10) 0.03465(6) 0.0277(5) Uani 1 1 d . . . F23 F 0.65076(16) 0.78612(11) 0.07263(7) 0.0360(6) Uani 1 1 d . . . F24 F 0.51473(15) 0.84692(11) 0.09986(6) 0.0345(5) Uani 1 1 d . . . F25 F 0.65532(16) 0.91234(11) 0.07903(6) 0.0348(5) Uani 1 1 d . . . F26 F 0.50776(14) 0.92079(10) 0.04141(6) 0.0290(5) Uani 1 1 d . . . F27 F 0.64403(14) 0.86008(11) 0.01370(6) 0.0283(5) Uani 1 1 d . . . P31 P 0.86451(7) 0.33615(6) 0.09391(3) 0.0221(2) Uani 1 1 d . . . F32 F 0.85028(16) 0.25276(11) 0.07515(6) 0.0331(5) Uani 1 1 d . . . F33 F 0.80657(19) 0.31047(11) 0.13606(6) 0.0460(7) Uani 1 1 d . . . F34 F 0.97175(18) 0.31157(11) 0.11426(7) 0.0432(6) Uani 1 1 d . . . F35 F 0.88001(17) 0.41900(11) 0.11241(6) 0.0323(5) Uani 1 1 d . . . F36 F 0.92173(15) 0.36077(11) 0.05131(5) 0.0289(5) Uani 1 1 d . . . F37 F 0.75839(14) 0.36061(11) 0.07318(7) 0.0388(6) Uani 1 1 d . . . O1W O 0.7766(2) 0.09841(16) 0.10242(8) 0.0480(8) Uani 1 1 d . . . O2W O 0.56299(19) 0.07595(14) 0.09214(7) 0.0336(7) Uani 1 1 d . . . O3W O 0.1438(2) 0.49199(15) 0.33467(10) 0.0550(8) 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 N1 0.0137(14) 0.0110(14) 0.0179(14) 0.0008(11) 0.0025(13) 0.0012(12) C2 0.0134(16) 0.0203(19) 0.0181(16) -0.0021(16) -0.0001(15) 0.0015(14) C3 0.0155(18) 0.0216(19) 0.0195(18) 0.0004(15) -0.0018(15) 0.0030(15) C4 0.026(2) 0.0198(19) 0.0168(17) 0.0073(15) 0.0034(15) 0.0014(15) C5 0.0189(19) 0.0197(19) 0.0222(18) 0.0059(15) 0.0016(15) -0.0029(15) C6 0.0183(18) 0.0201(18) 0.0203(17) 0.0003(16) 0.0055(16) -0.0029(14) C7 0.0120(17) 0.0163(18) 0.030(2) -0.0058(15) 0.0051(15) -0.0019(13) C8 0.0146(18) 0.0238(19) 0.0230(18) 0.0020(15) -0.0061(16) 0.0009(15) C9 0.0200(19) 0.0180(17) 0.0173(16) 0.0047(15) 0.0029(14) 0.0022(16) N10 0.0100(13) 0.0137(14) 0.0155(13) -0.0002(12) 0.0023(12) 0.0005(11) C11 0.0163(18) 0.0125(17) 0.0133(16) -0.0021(13) 0.0025(14) 0.0004(14) C12 0.0141(17) 0.0125(17) 0.0122(16) -0.0025(13) 0.0022(12) 0.0013(13) C13 0.0151(17) 0.0182(18) 0.0120(16) -0.0014(14) -0.0005(14) 0.0010(14) C14 0.0140(17) 0.0169(19) 0.0154(16) -0.0040(14) 0.0023(13) 0.0006(13) N15 0.0093(13) 0.0150(13) 0.0134(13) -0.0017(12) 0.0019(10) -0.0028(11) C16 0.0117(17) 0.0225(18) 0.0196(16) -0.0009(15) -0.0001(13) -0.0030(14) C17 0.0124(17) 0.034(2) 0.0146(16) -0.0042(15) 0.0001(15) -0.0013(17) C18 0.0119(17) 0.026(2) 0.0201(17) -0.0140(16) 0.0036(14) -0.0002(15) C19 0.0123(18) 0.0146(18) 0.0276(19) -0.0078(15) 0.0066(14) -0.0011(14) C20 0.0140(18) 0.0184(18) 0.0283(19) 0.0020(17) 0.0007(16) 0.0002(14) C21 0.0135(17) 0.0209(18) 0.0229(18) 0.0077(15) -0.0029(16) -0.0010(16) C22 0.020(2) 0.0221(19) 0.0124(16) 0.0032(14) -0.0022(14) -0.0044(15) C23 0.0139(18) 0.0212(18) 0.0136(16) -0.0045(14) 0.0003(14) -0.0027(14) N24 0.0103(14) 0.0128(14) 0.0138(13) -0.0030(11) 0.0013(11) -0.0016(11) C25 0.0048(15) 0.0165(17) 0.0164(17) -0.0001(13) 0.0017(13) -0.0032(13) C26 0.0050(15) 0.0185(18) 0.0171(16) -0.0018(13) 0.0023(14) -0.0038(14) C27 0.0068(15) 0.0210(17) 0.0244(16) -0.0103(16) -0.0014(14) -0.0038(14) C28 0.0093(16) 0.0148(16) 0.0219(17) -0.0007(14) -0.0009(15) -0.0020(14) N29 0.0122(14) 0.0116(14) 0.0142(13) 0.0024(12) 0.0003(12) -0.0011(10) C30 0.0196(18) 0.0114(17) 0.0180(17) 0.0008(14) 0.0001(14) 0.0013(14) C31 0.0206(19) 0.0156(18) 0.0191(17) 0.0001(15) -0.0067(15) -0.0054(16) C32 0.0136(17) 0.0168(19) 0.0279(19) 0.0045(15) -0.0021(15) 0.0007(14) C33 0.0108(17) 0.0203(18) 0.0232(18) 0.0100(15) 0.0040(15) 0.0038(14) C34 0.0195(19) 0.020(2) 0.0176(18) 0.0069(15) 0.0069(15) 0.0071(15) C35 0.0239(19) 0.0193(19) 0.0135(16) 0.0031(14) 0.0014(14) 0.0035(15) C36 0.025(2) 0.0153(18) 0.0189(18) -0.0042(14) -0.0031(15) -0.0027(15) C37 0.0168(18) 0.0155(18) 0.0217(17) 0.0020(14) 0.0016(15) -0.0021(15) N38 0.0116(14) 0.0107(14) 0.0142(14) 0.0023(11) -0.0001(12) 0.0004(11) C39 0.0151(17) 0.0110(17) 0.0121(16) 0.0040(13) 0.0000(14) 0.0018(13) C40 0.0155(17) 0.0087(16) 0.0130(15) 0.0080(13) 0.0002(13) 0.0019(13) C41 0.0107(16) 0.0159(17) 0.0214(17) 0.0097(15) -0.0004(14) 0.0017(15) C42 0.0179(17) 0.0130(16) 0.0138(16) 0.0048(13) -0.0020(15) 0.0039(15) Ru43 0.01124(13) 0.01279(13) 0.01357(12) 0.00022(11) 0.00150(12) -0.00096(11) N51 0.0086(13) 0.0142(14) 0.0136(13) 0.0027(11) -0.0018(12) -0.0018(12) C52 0.0096(17) 0.0214(19) 0.0216(17) -0.0007(15) -0.0050(14) -0.0033(14) C53 0.0167(18) 0.0182(19) 0.0314(19) 0.0098(16) -0.0076(15) -0.0038(14) C54 0.0140(18) 0.030(2) 0.0263(18) 0.0157(15) -0.0076(16) -0.0084(16) C55 0.0152(19) 0.043(2) 0.0169(19) 0.0084(17) -0.0014(15) -0.0005(16) C56 0.021(2) 0.041(2) 0.0150(19) -0.0100(17) -0.0006(15) -0.0031(17) C57 0.020(2) 0.028(2) 0.0203(18) -0.0150(16) 0.0006(15) 0.0019(16) C58 0.0165(19) 0.0189(19) 0.035(2) -0.0061(17) 0.0043(16) 0.0006(16) C59 0.0163(18) 0.023(2) 0.0218(17) 0.0001(14) 0.0008(16) -0.0017(15) N60 0.0074(14) 0.0155(14) 0.0166(14) 0.0017(11) 0.0010(12) -0.0008(12) C61 0.0077(16) 0.0173(18) 0.0157(16) -0.0031(14) 0.0014(13) -0.0001(13) C62 0.0077(16) 0.0234(18) 0.0130(15) 0.0004(14) -0.0022(14) -0.0028(14) C63 0.0080(16) 0.0271(19) 0.0174(16) 0.0067(14) -0.0015(15) -0.0045(15) C64 0.0085(17) 0.028(2) 0.0165(17) -0.0042(15) -0.0002(14) -0.0037(14) N65 0.0112(13) 0.0147(15) 0.0101(13) -0.0016(12) 0.0017(11) 0.0014(11) C66 0.0161(18) 0.0158(17) 0.0154(16) -0.0019(13) 0.0004(14) 0.0019(14) C67 0.0141(18) 0.024(2) 0.0227(18) 0.0023(15) -0.0025(15) 0.0046(14) C68 0.0109(17) 0.029(2) 0.0255(19) -0.0004(16) -0.0010(15) -0.0027(15) C69 0.0169(18) 0.027(2) 0.0208(17) 0.0033(15) 0.0053(16) -0.0086(17) C70 0.0185(19) 0.024(2) 0.0189(17) 0.0058(15) 0.0047(16) -0.0026(14) C71 0.029(2) 0.0262(19) 0.0138(17) 0.0081(16) 0.0021(15) -0.0028(17) C72 0.0139(18) 0.028(2) 0.0243(18) 0.0149(17) 0.0000(17) 0.0038(15) C73 0.0127(18) 0.028(2) 0.0239(18) 0.0069(16) 0.0038(15) 0.0004(16) N74 0.0112(14) 0.0176(14) 0.0145(13) 0.0037(11) -0.0027(13) -0.0003(12) C75 0.0120(17) 0.0211(19) 0.0093(15) -0.0033(13) 0.0011(13) -0.0011(14) C76 0.0137(17) 0.0150(17) 0.0087(15) -0.0012(13) 0.0002(13) 0.0009(14) C77 0.0107(16) 0.0221(18) 0.0163(16) -0.0039(14) 0.0004(13) -0.0013(13) C78 0.0185(18) 0.0167(17) 0.0122(17) 0.0008(14) 0.0020(14) -0.0013(15) N79 0.0141(15) 0.0162(14) 0.0122(13) 0.0034(11) 0.0002(13) 0.0013(13) C80 0.0127(17) 0.0218(18) 0.0147(15) 0.0016(14) -0.0017(15) 0.0007(15) C81 0.0189(19) 0.024(2) 0.0141(16) -0.0002(14) 0.0009(15) 0.0032(15) C82 0.0250(19) 0.0163(19) 0.0144(16) -0.0023(15) -0.0028(14) 0.0010(15) C83 0.0223(18) 0.0161(18) 0.0140(15) 0.0024(15) -0.0064(15) -0.0047(14) C84 0.0159(18) 0.021(2) 0.0214(18) 0.0076(15) -0.0063(15) -0.0012(15) C85 0.0114(18) 0.028(2) 0.0236(19) 0.0104(16) -0.0023(15) -0.0028(15) C86 0.0168(18) 0.024(2) 0.0185(17) 0.0012(15) 0.0023(14) 0.0031(15) C87 0.0173(18) 0.0171(18) 0.0109(15) 0.0020(14) 0.0011(13) 0.0029(15) N88 0.0123(14) 0.0156(15) 0.0096(13) 0.0082(11) 0.0009(11) 0.0004(11) C89 0.0138(17) 0.0157(17) 0.0100(15) 0.0042(13) -0.0026(14) -0.0017(15) C90 0.0111(17) 0.0170(18) 0.0137(16) 0.0060(14) -0.0039(14) -0.0014(14) C91 0.0177(17) 0.0159(18) 0.0116(15) 0.0027(14) -0.0065(15) 0.0028(13) C92 0.0151(18) 0.0202(18) 0.0111(16) 0.0074(14) -0.0030(14) -0.0005(14) Ru93 0.00999(12) 0.01467(13) 0.01162(12) 0.00155(11) 0.00100(11) 0.00007(11) P1 0.0151(5) 0.0192(5) 0.0201(4) 0.0036(4) -0.0016(4) -0.0003(4) F2 0.0357(12) 0.0164(10) 0.0285(11) 0.0012(9) -0.0101(10) 0.0061(9) F3 0.0178(12) 0.0478(14) 0.0574(14) 0.0282(12) 0.0034(10) -0.0060(10) F4 0.0244(11) 0.0356(12) 0.0175(9) -0.0043(9) -0.0040(9) 0.0025(9) F5 0.0273(12) 0.0275(11) 0.0314(11) 0.0022(9) 0.0088(10) 0.0121(10) F6 0.0183(10) 0.0235(10) 0.0215(10) 0.0048(9) 0.0027(8) -0.0013(9) F7 0.0307(12) 0.0261(12) 0.0328(11) 0.0028(9) -0.0192(10) -0.0040(10) P11 0.0168(5) 0.0313(6) 0.0273(5) -0.0030(5) 0.0026(4) -0.0025(5) F12 0.0236(12) 0.0371(13) 0.0477(13) -0.0160(11) 0.0004(11) -0.0075(10) F13 0.0292(13) 0.0695(17) 0.0497(14) 0.0237(13) -0.0069(12) -0.0063(12) F14 0.0416(15) 0.0573(15) 0.0505(14) -0.0291(13) 0.0278(12) -0.0229(13) F15 0.0412(14) 0.0522(15) 0.0433(13) -0.0155(12) 0.0105(12) -0.0243(12) F16 0.0396(15) 0.0442(15) 0.0742(17) 0.0135(13) -0.0043(14) 0.0113(13) F17 0.0335(13) 0.0429(14) 0.0341(12) -0.0007(10) 0.0133(11) 0.0011(11) P21 0.0169(5) 0.0234(5) 0.0200(5) 0.0010(4) -0.0014(4) -0.0003(4) F22 0.0173(11) 0.0294(11) 0.0365(11) -0.0079(10) -0.0031(9) -0.0031(8) F23 0.0219(12) 0.0348(13) 0.0514(14) 0.0158(11) -0.0076(11) -0.0003(10) F24 0.0362(13) 0.0438(13) 0.0234(10) 0.0040(10) 0.0088(9) -0.0042(11) F25 0.0379(13) 0.0361(13) 0.0302(11) -0.0021(10) -0.0082(11) -0.0148(11) F26 0.0248(12) 0.0305(11) 0.0316(11) 0.0057(9) 0.0035(9) 0.0102(9) F27 0.0190(11) 0.0368(13) 0.0290(11) 0.0004(9) 0.0055(9) 0.0009(9) P31 0.0255(5) 0.0237(5) 0.0172(4) -0.0008(4) 0.0019(4) 0.0063(4) F32 0.0351(13) 0.0267(12) 0.0374(12) -0.0092(10) 0.0015(11) -0.0003(10) F33 0.0751(19) 0.0270(13) 0.0361(12) 0.0065(10) 0.0270(13) 0.0130(12) F34 0.0445(14) 0.0389(13) 0.0462(13) -0.0042(11) -0.0259(12) 0.0157(12) F35 0.0497(15) 0.0238(11) 0.0233(10) 0.0004(9) 0.0011(10) 0.0050(10) F36 0.0277(11) 0.0399(13) 0.0192(10) -0.0038(9) 0.0046(9) -0.0039(10) F37 0.0158(11) 0.0388(13) 0.0617(15) 0.0060(11) -0.0021(10) 0.0029(9) O1W 0.0363(17) 0.0581(19) 0.0496(17) -0.0050(15) 0.0064(15) -0.0114(15) O2W 0.0360(17) 0.0389(16) 0.0259(13) -0.0043(12) 0.0026(12) 0.0036(13) O3W 0.0468(19) 0.0319(17) 0.086(2) 0.0102(16) 0.0101(18) 0.0087(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 N1 C2 1.314(4) . ? N1 C12 1.360(4) . ? N1 Ru43 2.025(2) . ? C2 C3 1.388(4) . ? C3 C4 1.364(4) . ? C4 C13 1.380(4) . ? C5 C6 1.336(4) . ? C5 C13 1.417(4) . ? C6 C14 1.418(4) . ? C7 C8 1.354(4) . ? C7 C14 1.399(4) . ? C8 C9 1.377(4) . ? C9 N10 1.313(4) . ? N10 C11 1.346(4) . ? N10 Ru43 2.038(2) . ? C11 C14 1.387(4) . ? C11 C12 1.408(4) . ? C12 C13 1.375(4) . ? N15 C16 1.327(4) . ? N15 C26 1.359(4) . ? N15 Ru43 2.038(2) . ? C16 C17 1.384(4) . ? C17 C18 1.330(4) . ? C18 C27 1.402(4) . ? C19 C20 1.345(4) . ? C19 C27 1.412(4) . ? C20 C28 1.411(4) . ? C21 C22 1.357(4) . ? C21 C28 1.390(4) . ? C22 C23 1.382(4) . ? C23 N24 1.313(4) . ? N24 C25 1.356(3) . ? N24 Ru43 2.042(2) . ? C25 C28 1.382(4) . ? C25 C26 1.422(4) . ? C26 C27 1.375(4) . ? N29 C30 1.322(4) . ? N29 C40 1.344(4) . ? N29 Ru43 2.051(2) . ? C30 C31 1.369(4) . ? C31 C32 1.344(4) . ? C32 C41 1.393(4) . ? C33 C34 1.324(4) . ? C33 C41 1.416(4) . ? C34 C42 1.425(5) . ? C35 C36 1.365(4) . ? C35 C42 1.372(4) . ? C36 C37 1.382(4) . ? C37 N38 1.301(4) . ? N38 C39 1.364(4) . ? N38 Ru43 2.032(2) . ? C39 C42 1.391(4) . ? C39 C40 1.395(4) . ? C40 C41 1.392(4) . ? N51 C52 1.314(4) . ? N51 C62 1.363(4) . ? N51 Ru93 2.043(2) . ? C52 C53 1.380(4) . ? C53 C54 1.362(4) . ? C54 C63 1.394(4) . ? C55 C56 1.335(4) . ? C55 C63 1.402(4) . ? C56 C64 1.423(4) . ? C57 C58 1.340(4) . ? C57 C64 1.386(4) . ? C58 C59 1.387(4) . ? C59 N60 1.320(4) . ? N60 C61 1.350(4) . ? N60 Ru93 2.042(2) . ? C61 C64 1.381(4) . ? C61 C62 1.408(4) . ? C62 C63 1.390(4) . ? N65 C66 1.320(4) . ? N65 C76 1.343(4) . ? N65 Ru93 2.041(2) . ? C66 C67 1.388(4) . ? C67 C68 1.351(4) . ? C68 C77 1.392(4) . ? C69 C70 1.330(4) . ? C69 C77 1.418(4) . ? C70 C78 1.419(4) . ? C71 C72 1.352(4) . ? C71 C78 1.373(4) . ? C72 C73 1.394(4) . ? C73 N74 1.305(4) . ? N74 C75 1.358(4) . ? N74 Ru93 2.030(2) . ? C75 C78 1.383(4) . ? C75 C76 1.413(4) . ? C76 C77 1.384(4) . ? N79 C80 1.321(4) . ? N79 C90 1.359(4) . ? N79 Ru93 2.041(2) . ? C80 C81 1.388(4) . ? C81 C82 1.349(4) . ? C82 C91 1.385(4) . ? C83 C84 1.342(4) . ? C83 C91 1.418(4) . ? C84 C92 1.407(4) . ? C85 C86 1.349(4) . ? C85 C92 1.385(4) . ? C86 C87 1.394(4) . ? C87 N88 1.321(4) . ? N88 C89 1.350(4) . ? N88 Ru93 2.049(2) . ? C89 C92 1.399(4) . ? C89 C90 1.407(4) . ? C90 C91 1.387(4) . ? P1 F4 1.5757(19) . ? P1 F5 1.5809(19) . ? P1 F2 1.5831(19) . ? P1 F6 1.5842(18) . ? P1 F7 1.5858(19) . ? P1 F3 1.591(2) . ? P11 F14 1.565(2) . ? P11 F17 1.575(2) . ? P11 F15 1.576(2) . ? P11 F12 1.579(2) . ? P11 F13 1.583(2) . ? P11 F16 1.588(2) . ? P21 F23 1.577(2) . ? P21 F24 1.5795(19) . ? P21 F22 1.5828(19) . ? P21 F27 1.5837(19) . ? P21 F26 1.584(2) . ? P21 F25 1.590(2) . ? P31 F33 1.574(2) . ? P31 F36 1.5762(19) . ? P31 F37 1.576(2) . ? P31 F35 1.582(2) . ? P31 F34 1.584(2) . ? P31 F32 1.591(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C12 117.8(3) . . ? C2 N1 Ru43 129.0(2) . . ? C12 N1 Ru43 112.9(2) . . ? N1 C2 C3 122.5(3) . . ? C4 C3 C2 119.6(3) . . ? C3 C4 C13 118.9(3) . . ? C6 C5 C13 122.2(3) . . ? C5 C6 C14 120.2(3) . . ? C8 C7 C14 118.6(3) . . ? C7 C8 C9 120.5(3) . . ? N10 C9 C8 122.5(3) . . ? C9 N10 C11 117.9(3) . . ? C9 N10 Ru43 129.0(2) . . ? C11 N10 Ru43 113.1(2) . . ? N10 C11 C14 123.3(3) . . ? N10 C11 C12 116.6(3) . . ? C14 C11 C12 120.1(3) . . ? N1 C12 C13 122.7(3) . . ? N1 C12 C11 116.6(3) . . ? C13 C12 C11 120.6(3) . . ? C12 C13 C4 118.4(3) . . ? C12 C13 C5 118.0(3) . . ? C4 C13 C5 123.6(3) . . ? C11 C14 C7 117.3(3) . . ? C11 C14 C6 118.8(3) . . ? C7 C14 C6 123.9(3) . . ? C16 N15 C26 117.4(3) . . ? C16 N15 Ru43 129.0(2) . . ? C26 N15 Ru43 113.55(18) . . ? N15 C16 C17 122.0(3) . . ? C18 C17 C16 120.3(3) . . ? C17 C18 C27 120.1(3) . . ? C20 C19 C27 120.8(3) . . ? C19 C20 C28 120.8(3) . . ? C22 C21 C28 119.5(3) . . ? C21 C22 C23 119.4(3) . . ? N24 C23 C22 123.4(3) . . ? C23 N24 C25 116.8(3) . . ? C23 N24 Ru43 130.1(2) . . ? C25 N24 Ru43 113.04(19) . . ? N24 C25 C28 123.9(3) . . ? N24 C25 C26 116.9(3) . . ? C28 C25 C26 119.2(3) . . ? N15 C26 C27 123.6(3) . . ? N15 C26 C25 116.1(3) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C18 116.6(3) . . ? C26 C27 C19 119.2(3) . . ? C18 C27 C19 124.2(3) . . ? C25 C28 C21 117.1(3) . . ? C25 C28 C20 119.6(3) . . ? C21 C28 C20 123.4(3) . . ? C30 N29 C40 117.5(3) . . ? C30 N29 Ru43 129.4(2) . . ? C40 N29 Ru43 113.1(2) . . ? N29 C30 C31 122.8(3) . . ? C32 C31 C30 120.4(3) . . ? C31 C32 C41 118.9(3) . . ? C34 C33 C41 122.0(3) . . ? C33 C34 C42 121.4(3) . . ? C36 C35 C42 119.0(3) . . ? C35 C36 C37 119.4(3) . . ? N38 C37 C36 123.4(3) . . ? C37 N38 C39 117.6(3) . . ? C37 N38 Ru43 129.1(2) . . ? C39 N38 Ru43 113.3(2) . . ? N38 C39 C42 122.2(3) . . ? N38 C39 C40 116.4(3) . . ? C42 C39 C40 121.4(3) . . ? N29 C40 C41 122.8(3) . . ? N29 C40 C39 117.1(3) . . ? C41 C40 C39 120.1(3) . . ? C40 C41 C32 117.5(3) . . ? C40 C41 C33 117.9(3) . . ? C32 C41 C33 124.7(3) . . ? C35 C42 C39 118.3(3) . . ? C35 C42 C34 124.4(3) . . ? C39 C42 C34 117.2(3) . . ? N1 Ru43 N38 92.45(10) . . ? N1 Ru43 N15 92.01(10) . . ? N38 Ru43 N15 174.18(10) . . ? N1 Ru43 N10 80.34(11) . . ? N38 Ru43 N10 95.73(10) . . ? N15 Ru43 N10 88.71(10) . . ? N1 Ru43 N24 170.50(10) . . ? N38 Ru43 N24 95.51(9) . . ? N15 Ru43 N24 80.41(10) . . ? N10 Ru43 N24 93.68(10) . . ? N1 Ru43 N29 97.04(10) . . ? N38 Ru43 N29 79.59(10) . . ? N15 Ru43 N29 96.14(10) . . ? N10 Ru43 N29 174.59(10) . . ? N24 Ru43 N29 89.50(10) . . ? C52 N51 C62 117.7(3) . . ? C52 N51 Ru93 129.2(2) . . ? C62 N51 Ru93 113.03(19) . . ? N51 C52 C53 122.2(3) . . ? C54 C53 C52 120.5(3) . . ? C53 C54 C63 119.3(3) . . ? C56 C55 C63 121.7(3) . . ? C55 C56 C64 120.8(3) . . ? C58 C57 C64 119.9(3) . . ? C57 C58 C59 119.5(3) . . ? N60 C59 C58 122.6(3) . . ? C59 N60 C61 117.6(3) . . ? C59 N60 Ru93 128.6(2) . . ? C61 N60 Ru93 113.8(2) . . ? N60 C61 C64 122.9(3) . . ? N60 C61 C62 116.3(3) . . ? C64 C61 C62 120.7(3) . . ? N51 C62 C63 123.7(3) . . ? N51 C62 C61 116.7(3) . . ? C63 C62 C61 119.6(3) . . ? C62 C63 C54 116.6(3) . . ? C62 C63 C55 118.8(3) . . ? C54 C63 C55 124.6(3) . . ? C61 C64 C57 117.5(3) . . ? C61 C64 C56 118.2(3) . . ? C57 C64 C56 124.2(3) . . ? C66 N65 C76 118.2(3) . . ? C66 N65 Ru93 128.0(2) . . ? C76 N65 Ru93 113.7(2) . . ? N65 C66 C67 121.9(3) . . ? C68 C67 C66 119.7(3) . . ? C67 C68 C77 119.9(3) . . ? C70 C69 C77 121.8(3) . . ? C69 C70 C78 121.2(3) . . ? C72 C71 C78 121.2(3) . . ? C71 C72 C73 118.7(3) . . ? N74 C73 C72 122.1(3) . . ? C73 N74 C75 118.4(3) . . ? C73 N74 Ru93 127.8(2) . . ? C75 N74 Ru93 113.7(2) . . ? N74 C75 C78 123.1(3) . . ? N74 C75 C76 116.2(3) . . ? C78 C75 C76 120.8(3) . . ? N65 C76 C77 123.5(3) . . ? N65 C76 C75 116.5(3) . . ? C77 C76 C75 119.9(3) . . ? C76 C77 C68 116.7(3) . . ? C76 C77 C69 118.2(3) . . ? C68 C77 C69 125.1(3) . . ? C71 C78 C75 116.5(3) . . ? C71 C78 C70 125.5(3) . . ? C75 C78 C70 118.0(3) . . ? C80 N79 C90 117.2(3) . . ? C80 N79 Ru93 128.7(2) . . ? C90 N79 Ru93 113.9(2) . . ? N79 C80 C81 122.7(3) . . ? C82 C81 C80 119.8(3) . . ? C81 C82 C91 119.4(3) . . ? C84 C83 C91 120.7(3) . . ? C83 C84 C92 122.1(3) . . ? C86 C85 C92 120.0(3) . . ? C85 C86 C87 119.8(3) . . ? N88 C87 C86 122.3(3) . . ? C87 N88 C89 117.6(3) . . ? C87 N88 Ru93 128.9(2) . . ? C89 N88 Ru93 113.3(2) . . ? N88 C89 C92 123.4(3) . . ? N88 C89 C90 117.0(3) . . ? C92 C89 C90 119.6(3) . . ? N79 C90 C91 122.9(3) . . ? N79 C90 C89 116.0(3) . . ? C91 C90 C89 121.1(3) . . ? C82 C91 C90 117.7(3) . . ? C82 C91 C83 124.0(3) . . ? C90 C91 C83 118.2(3) . . ? C85 C92 C89 116.8(3) . . ? C85 C92 C84 124.8(3) . . ? C89 C92 C84 118.3(3) . . ? N74 Ru93 N79 89.03(9) . . ? N74 Ru93 N65 79.87(10) . . ? N79 Ru93 N65 92.65(10) . . ? N74 Ru93 N60 92.56(9) . . ? N79 Ru93 N60 174.54(11) . . ? N65 Ru93 N60 92.77(10) . . ? N74 Ru93 N51 170.70(10) . . ? N79 Ru93 N51 99.10(9) . . ? N65 Ru93 N51 95.15(10) . . ? N60 Ru93 N51 79.77(9) . . ? N74 Ru93 N88 97.42(10) . . ? N79 Ru93 N88 79.57(10) . . ? N65 Ru93 N88 171.85(10) . . ? N60 Ru93 N88 95.04(10) . . ? N51 Ru93 N88 88.55(10) . . ? F4 P1 F5 90.52(11) . . ? F4 P1 F2 90.10(11) . . ? F5 P1 F2 179.33(12) . . ? F4 P1 F6 90.77(10) . . ? F5 P1 F6 89.91(10) . . ? F2 P1 F6 89.83(11) . . ? F4 P1 F7 179.52(12) . . ? F5 P1 F7 89.71(11) . . ? F2 P1 F7 89.67(10) . . ? F6 P1 F7 89.65(10) . . ? F4 P1 F3 89.52(11) . . ? F5 P1 F3 89.73(11) . . ? F2 P1 F3 90.53(11) . . ? F6 P1 F3 179.54(13) . . ? F7 P1 F3 90.07(11) . . ? F14 P11 F17 179.13(14) . . ? F14 P11 F15 90.82(12) . . ? F17 P11 F15 89.81(12) . . ? F14 P11 F12 89.39(12) . . ? F17 P11 F12 89.98(11) . . ? F15 P11 F12 179.72(15) . . ? F14 P11 F13 91.20(13) . . ? F17 P11 F13 89.39(12) . . ? F15 P11 F13 90.57(13) . . ? F12 P11 F13 89.24(13) . . ? F14 P11 F16 90.12(14) . . ? F17 P11 F16 89.28(12) . . ? F15 P11 F16 90.40(13) . . ? F12 P11 F16 89.78(12) . . ? F13 P11 F16 178.35(14) . . ? F23 P21 F24 89.73(12) . . ? F23 P21 F22 89.88(11) . . ? F24 P21 F22 89.93(11) . . ? F23 P21 F27 90.66(11) . . ? F24 P21 F27 179.54(12) . . ? F22 P21 F27 90.33(11) . . ? F23 P21 F26 179.46(13) . . ? F24 P21 F26 89.91(11) . . ? F22 P21 F26 90.52(11) . . ? F27 P21 F26 89.71(10) . . ? F23 P21 F25 89.70(12) . . ? F24 P21 F25 90.35(11) . . ? F22 P21 F25 179.49(13) . . ? F27 P21 F25 89.39(11) . . ? F26 P21 F25 89.91(11) . . ? F33 P31 F36 179.10(13) . . ? F33 P31 F37 90.19(13) . . ? F36 P31 F37 89.49(11) . . ? F33 P31 F35 91.36(11) . . ? F36 P31 F35 89.49(11) . . ? F37 P31 F35 90.35(12) . . ? F33 P31 F34 90.39(13) . . ? F36 P31 F34 89.93(12) . . ? F37 P31 F34 179.40(13) . . ? F35 P31 F34 89.81(12) . . ? F33 P31 F32 89.07(12) . . ? F36 P31 F32 90.09(11) . . ? F37 P31 F32 90.13(11) . . ? F35 P31 F32 179.35(13) . . ? F34 P31 F32 89.71(11) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.879 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.076 data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 242569' # data_370801a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 F24 N12 O Os2 P4' _chemical_formula_weight 2059.52 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' 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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 36.6813(19) _cell_length_b 15.8390(8) _cell_length_c 12.1451(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.6650(10) _cell_angle_gamma 90.00 _cell_volume 6910.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10791 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 3.890 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5101 _exptl_absorpt_correction_T_max 0.5930 _exptl_absorpt_process_details 'Bruker 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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21341 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.90 _reflns_number_total 10791 _reflns_number_gt 10539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0344P)^2^+35.4633P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.204(6) _refine_ls_number_reflns 10791 _refine_ls_number_parameters 601 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.198 _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 N1 N 0.19930(18) 0.2857(4) -0.3066(6) 0.0134(14) Uiso 1 1 d . . . C2 C 0.2285(2) 0.3370(5) -0.2881(6) 0.0195(15) Uiso 1 1 d . . . H2 H 0.2310 0.3759 -0.3434 0.023 Uiso 1 1 calc R . . C3 C 0.2555(2) 0.3353(5) -0.1901(7) 0.0227(16) Uiso 1 1 d . . . H3 H 0.2754 0.3727 -0.1810 0.027 Uiso 1 1 calc R . . C4 C 0.2529(2) 0.2778(5) -0.1056(7) 0.0221(16) Uiso 1 1 d . . . H4 H 0.2709 0.2763 -0.0395 0.027 Uiso 1 1 calc R . . C5 C 0.2173(2) 0.1591(5) -0.0414(7) 0.0237(16) Uiso 1 1 d . . . H5 H 0.2340 0.1554 0.0272 0.028 Uiso 1 1 calc R . . C6 C 0.1882(2) 0.1058(5) -0.0649(7) 0.0237(16) Uiso 1 1 d . . . H6 H 0.1857 0.0640 -0.0131 0.028 Uiso 1 1 calc R . . C7 C 0.1295(2) 0.0581(5) -0.1965(7) 0.0245(16) Uiso 1 1 d . . . H7 H 0.1253 0.0159 -0.1473 0.029 Uiso 1 1 calc R . . C8 C 0.1054(2) 0.0688(5) -0.2962(7) 0.0242(17) Uiso 1 1 d . . . H8 H 0.0853 0.0323 -0.3166 0.029 Uiso 1 1 calc R . . C9 C 0.1108(2) 0.1348(5) -0.3690(7) 0.0248(16) Uiso 1 1 d . . . H9 H 0.0936 0.1423 -0.4360 0.030 Uiso 1 1 calc R . . N10 N 0.14005(17) 0.1869(4) -0.3437(5) 0.0181(13) Uiso 1 1 d . . . C11 C 0.1651(2) 0.1742(5) -0.2455(6) 0.0181(14) Uiso 1 1 d . . . C12 C 0.1610(2) 0.1114(5) -0.1675(6) 0.0204(15) Uiso 1 1 d . . . C13 C 0.2227(2) 0.2223(5) -0.1226(7) 0.0203(16) Uiso 1 1 d . . . C14 C 0.1966(2) 0.2275(5) -0.2230(6) 0.0166(15) Uiso 1 1 d . . . N21 N 0.10493(19) 0.2838(4) -0.5555(6) 0.0177(15) Uiso 1 1 d . . . C22 C 0.0718(2) 0.3222(5) -0.5570(6) 0.0185(14) Uiso 1 1 d . . . H22 H 0.0690 0.3548 -0.4956 0.022 Uiso 1 1 calc R . . C23 C 0.0419(2) 0.3143(5) -0.6466(7) 0.0237(16) Uiso 1 1 d . . . H23 H 0.0196 0.3416 -0.6445 0.028 Uiso 1 1 calc R . . C24 C 0.0450(2) 0.2668(5) -0.7383(7) 0.0219(16) Uiso 1 1 d . . . H24 H 0.0250 0.2622 -0.7986 0.026 Uiso 1 1 calc R . . C25 C 0.0851(2) 0.1762(5) -0.8336(7) 0.0238(16) Uiso 1 1 d . . . H25 H 0.0659 0.1685 -0.8957 0.029 Uiso 1 1 calc R . . C26 C 0.1191(2) 0.1405(5) -0.8326(7) 0.0219(15) Uiso 1 1 d . . . H26 H 0.1228 0.1099 -0.8948 0.026 Uiso 1 1 calc R . . C27 C 0.1843(2) 0.1131(5) -0.7284(7) 0.0234(16) Uiso 1 1 d . . . H27 H 0.1898 0.0813 -0.7874 0.028 Uiso 1 1 calc R . . C28 C 0.2108(2) 0.1247(5) -0.6320(7) 0.0223(15) Uiso 1 1 d . . . H28 H 0.2342 0.1000 -0.6253 0.027 Uiso 1 1 calc R . . C29 C 0.2027(2) 0.1740(5) -0.5432(6) 0.0195(15) Uiso 1 1 d . . . H29 H 0.2209 0.1808 -0.4784 0.023 Uiso 1 1 calc R . . N30 N 0.16957(17) 0.2114(4) -0.5491(5) 0.0153(12) Uiso 1 1 d . . . C31 C 0.14264(19) 0.1981(4) -0.6459(6) 0.0164(14) Uiso 1 1 d . . . C32 C 0.1490(2) 0.1495(5) -0.7375(6) 0.0210(15) Uiso 1 1 d . . . C33 C 0.0785(2) 0.2249(5) -0.7407(6) 0.0183(15) Uiso 1 1 d . . . C34 C 0.1077(2) 0.2363(5) -0.6481(6) 0.0175(14) Uiso 1 1 d . . . N41 N 0.13061(17) 0.3797(4) -0.3423(5) 0.0166(12) Uiso 1 1 d . . . C42 C 0.1107(2) 0.3679(5) -0.2636(7) 0.0233(16) Uiso 1 1 d . . . H42 H 0.1070 0.3131 -0.2404 0.028 Uiso 1 1 calc R . . C43 C 0.0949(2) 0.4357(5) -0.2142(7) 0.0256(17) Uiso 1 1 d . . . H43 H 0.0802 0.4256 -0.1615 0.031 Uiso 1 1 calc R . . C44 C 0.1014(2) 0.5164(5) -0.2448(7) 0.0267(17) Uiso 1 1 d . . . H44 H 0.0911 0.5613 -0.2120 0.032 Uiso 1 1 calc R . . C45 C 0.1317(2) 0.6128(5) -0.3609(7) 0.0280(18) Uiso 1 1 d . . . H45 H 0.1223 0.6601 -0.3308 0.034 Uiso 1 1 calc R . . C46 C 0.1533(3) 0.6239(5) -0.4385(8) 0.0282(16) Uiso 1 1 d . . . H46 H 0.1591 0.6782 -0.4582 0.034 Uiso 1 1 calc R . . C47 C 0.1885(2) 0.5576(5) -0.5741(7) 0.0265(17) Uiso 1 1 d . . . H47 H 0.1950 0.6101 -0.5987 0.032 Uiso 1 1 calc R . . C48 C 0.1998(2) 0.4850(5) -0.6192(7) 0.0228(16) Uiso 1 1 d . . . H48 H 0.2143 0.4876 -0.6738 0.027 Uiso 1 1 calc R . . C49 C 0.1892(2) 0.4070(5) -0.5817(6) 0.0181(14) Uiso 1 1 d . . . H49 H 0.1968 0.3583 -0.6134 0.022 Uiso 1 1 calc R . . N50 N 0.16886(17) 0.3987(4) -0.5034(5) 0.0175(12) Uiso 1 1 d . . . C51 C 0.1580(2) 0.4700(5) -0.4564(6) 0.0181(15) Uiso 1 1 d . . . C52 C 0.1673(2) 0.5517(5) -0.4908(6) 0.0208(15) Uiso 1 1 d . . . C53 C 0.1231(2) 0.5328(5) -0.3247(7) 0.0212(15) Uiso 1 1 d . . . C54 C 0.1368(2) 0.4602(5) -0.3730(6) 0.0185(15) Uiso 1 1 d . . . N61 N 0.35209(19) 0.2601(4) -0.3169(6) 0.0153(14) Uiso 1 1 d . . . C62 C 0.3252(2) 0.3187(5) -0.3513(7) 0.0221(16) Uiso 1 1 d . . . H62 H 0.3230 0.3638 -0.3039 0.027 Uiso 1 1 calc R . . C63 C 0.3008(2) 0.3139(5) -0.4546(7) 0.0247(16) Uiso 1 1 d . . . H63 H 0.2832 0.3561 -0.4762 0.030 Uiso 1 1 calc R . . C64 C 0.3026(2) 0.2458(5) -0.5260(7) 0.0233(17) Uiso 1 1 d . . . H64 H 0.2861 0.2416 -0.5948 0.028 Uiso 1 1 calc R . . C65 C 0.3349(2) 0.1117(5) -0.5589(7) 0.0242(16) Uiso 1 1 d . . . H65 H 0.3184 0.1019 -0.6264 0.029 Uiso 1 1 calc R . . C66 C 0.3639(2) 0.0576(5) -0.5243(7) 0.0221(16) Uiso 1 1 d . . . H66 H 0.3669 0.0121 -0.5699 0.027 Uiso 1 1 calc R . . C67 C 0.4208(2) 0.0164(5) -0.3830(7) 0.0236(16) Uiso 1 1 d . . . H67 H 0.4261 -0.0279 -0.4274 0.028 Uiso 1 1 calc R . . C68 C 0.4433(2) 0.0324(5) -0.2791(6) 0.0212(15) Uiso 1 1 d . . . H68 H 0.4637 -0.0019 -0.2524 0.025 Uiso 1 1 calc R . . C69 C 0.4352(2) 0.1007(5) -0.2141(6) 0.0200(15) Uiso 1 1 d . . . H69 H 0.4501 0.1096 -0.1435 0.024 Uiso 1 1 calc R . . N70 N 0.40657(16) 0.1536(4) -0.2508(5) 0.0144(12) Uiso 1 1 d . . . C71 C 0.3839(2) 0.1361(5) -0.3518(6) 0.0181(14) Uiso 1 1 d . . . C72 C 0.3898(2) 0.0686(5) -0.4197(6) 0.0207(15) Uiso 1 1 d . . . C73 C 0.3298(2) 0.1835(5) -0.4924(6) 0.0181(14) Uiso 1 1 d . . . C74 C 0.3539(2) 0.1939(5) -0.3884(7) 0.0185(15) Uiso 1 1 d . . . N81 N 0.36925(17) 0.2037(4) -0.0634(5) 0.0164(12) Uiso 1 1 d . . . C82 C 0.3351(2) 0.1708(5) -0.0795(6) 0.0201(15) Uiso 1 1 d . . . H82 H 0.3204 0.1729 -0.1513 0.024 Uiso 1 1 calc R . . C83 C 0.3204(2) 0.1336(5) 0.0058(6) 0.0191(14) Uiso 1 1 d . . . H83 H 0.2967 0.1103 -0.0095 0.023 Uiso 1 1 calc R . . C84 C 0.3416(2) 0.1318(5) 0.1134(7) 0.0229(15) Uiso 1 1 d . . . H84 H 0.3319 0.1087 0.1718 0.027 Uiso 1 1 calc R . . C85 C 0.4026(2) 0.1636(5) 0.2413(7) 0.0233(16) Uiso 1 1 d . . . H85 H 0.3940 0.1442 0.3037 0.028 Uiso 1 1 calc R . . C86 C 0.4386(2) 0.1898(5) 0.2548(7) 0.0255(16) Uiso 1 1 d . . . H86 H 0.4543 0.1864 0.3251 0.031 Uiso 1 1 calc R . . C87 C 0.4892(2) 0.2522(5) 0.1691(8) 0.0265(18) Uiso 1 1 d . . . H87 H 0.5064 0.2498 0.2367 0.032 Uiso 1 1 calc R . . C88 C 0.4986(2) 0.2851(5) 0.0719(8) 0.0262(17) Uiso 1 1 d . . . H88 H 0.5226 0.3046 0.0744 0.031 Uiso 1 1 calc R . . C89 C 0.4727(2) 0.2890(5) -0.0283(7) 0.0230(16) Uiso 1 1 d . . . H89 H 0.4800 0.3122 -0.0909 0.028 Uiso 1 1 calc R . . N90 N 0.43767(19) 0.2610(4) -0.0392(6) 0.0162(15) Uiso 1 1 d . . . C91 C 0.4280(2) 0.2276(5) 0.0564(6) 0.0184(15) Uiso 1 1 d . . . C92 C 0.4524(2) 0.2230(5) 0.1601(7) 0.0212(15) Uiso 1 1 d . . . C93 C 0.3776(2) 0.1647(5) 0.1347(6) 0.0215(15) Uiso 1 1 d . . . C94 C 0.39061(19) 0.1988(4) 0.0413(6) 0.0164(14) Uiso 1 1 d . . . N101 N 0.38198(16) 0.3844(4) -0.1295(5) 0.0151(12) Uiso 1 1 d . . . C102 C 0.3616(2) 0.4072(5) -0.0542(7) 0.0218(15) Uiso 1 1 d . . . H102 H 0.3517 0.3653 -0.0154 0.026 Uiso 1 1 calc R . . C103 C 0.3548(2) 0.4915(5) -0.0320(7) 0.0217(16) Uiso 1 1 d . . . H103 H 0.3406 0.5044 0.0211 0.026 Uiso 1 1 calc R . . C104 C 0.3688(2) 0.5558(5) -0.0873(7) 0.0259(17) Uiso 1 1 d . . . H104 H 0.3641 0.6121 -0.0732 0.031 Uiso 1 1 calc R . . C105 C 0.4068(2) 0.5940(5) -0.2306(7) 0.0277(17) Uiso 1 1 d . . . H105 H 0.4032 0.6513 -0.2204 0.033 Uiso 1 1 calc R . . C106 C 0.4272(2) 0.5682(6) -0.3057(8) 0.0289(19) Uiso 1 1 d . . . H106 H 0.4374 0.6088 -0.3458 0.035 Uiso 1 1 calc R . . C107 C 0.4545(2) 0.4530(5) -0.4015(7) 0.0244(16) Uiso 1 1 d . . . H107 H 0.4653 0.4911 -0.4435 0.029 Uiso 1 1 calc R . . C108 C 0.4591(2) 0.3669(5) -0.4138(7) 0.0251(16) Uiso 1 1 d . . . H108 H 0.4731 0.3468 -0.4641 0.030 Uiso 1 1 calc R . . C109 C 0.4426(2) 0.3108(5) -0.3505(7) 0.0233(16) Uiso 1 1 d . . . H109 H 0.4457 0.2532 -0.3600 0.028 Uiso 1 1 calc R . . N110 N 0.42240(17) 0.3368(4) -0.2759(5) 0.0173(12) Uiso 1 1 d . . . C111 C 0.4174(2) 0.4220(5) -0.2645(6) 0.0185(15) Uiso 1 1 d . . . C112 C 0.4336(2) 0.4817(5) -0.3254(7) 0.0226(17) Uiso 1 1 d . . . C113 C 0.3906(2) 0.5330(4) -0.1665(6) 0.0184(14) Uiso 1 1 d . . . C114 C 0.3963(2) 0.4476(4) -0.1852(7) 0.0187(13) Uiso 1 1 d . . . Os1 Os 0.152889(7) 0.289367(16) -0.432825(14) 0.01258(6) Uani 1 1 d . . . Os2 Os 0.395054(8) 0.264740(16) -0.176239(17) 0.01312(6) Uani 1 1 d . . . P1 P 0.26717(5) 0.03834(12) -0.31223(16) 0.0162(4) Uani 1 1 d D . . F11 F 0.27115(13) 0.0340(3) -0.4399(4) 0.0240(10) Uani 1 1 d D . . F12 F 0.31185(12) 0.0348(3) -0.2714(4) 0.0224(10) Uani 1 1 d D . . F13 F 0.26580(12) -0.0628(3) -0.3098(4) 0.0235(10) Uani 1 1 d D . . F14 F 0.26312(13) 0.0418(3) -0.1835(4) 0.0244(10) Uani 1 1 d D . . F15 F 0.22271(12) 0.0421(3) -0.3513(4) 0.0247(10) Uani 1 1 d D . . F16 F 0.26871(12) 0.1395(3) -0.3151(4) 0.0224(10) Uani 1 1 d D . . P2 P 0.51602(6) 0.07410(14) -0.49445(18) 0.0229(4) Uani 1 1 d . . . F21 F 0.51169(13) 0.0948(4) -0.6255(4) 0.0329(12) Uani 1 1 d . . . F22 F 0.54771(15) 0.0061(4) -0.5044(5) 0.0410(14) Uani 1 1 d . . . F23 F 0.48450(16) 0.0034(4) -0.5233(5) 0.0499(16) Uani 1 1 d . . . F24 F 0.52045(13) 0.0543(3) -0.3651(4) 0.0315(11) Uani 1 1 d . . . F25 F 0.48512(15) 0.1442(4) -0.4847(4) 0.0413(13) Uani 1 1 d . . . F26 F 0.54783(14) 0.1456(3) -0.4670(4) 0.0369(12) Uani 1 1 d . . . P3 P 0.53114(13) 0.5091(3) -0.0929(4) 0.0341(13) Uiso 0.652(6) 1 d PD A 1 F31 F 0.5713(3) 0.5498(7) -0.0605(9) 0.060(3) Uiso 0.652(6) 1 d PD A 1 F32 F 0.5478(3) 0.4147(7) -0.0965(11) 0.083(4) Uiso 0.652(6) 1 d PD A 1 F33 F 0.5331(2) 0.4968(6) 0.0392(7) 0.047(2) Uiso 0.652(6) 1 d PD A 1 F34 F 0.4904(3) 0.4705(7) -0.1191(9) 0.060 Uiso 0.652(6) 1 d PD A 1 F35 F 0.5135(3) 0.5990(6) -0.0835(9) 0.062(3) Uiso 0.652(6) 1 d PD A 1 F36 F 0.5301(4) 0.5223(8) -0.2232(8) 0.060 Uiso 0.652(6) 1 d PD A 1 P5 P 0.53134(19) 0.4925(5) -0.1058(6) 0.0187(18) Uiso 0.348(6) 1 d PD A 2 F51 F 0.5339(4) 0.4475(9) 0.0085(10) 0.034(4) Uiso 0.348(6) 1 d PD A 2 F52 F 0.5553(5) 0.5748(11) -0.0527(17) 0.067(6) Uiso 0.348(6) 1 d PD A 2 F53 F 0.5667(3) 0.4438(8) -0.1180(11) 0.025(3) Uiso 0.348(6) 1 d PD A 2 F54 F 0.4934(4) 0.5419(11) -0.1081(16) 0.060 Uiso 0.348(6) 1 d PD A 2 F55 F 0.5073(4) 0.4164(8) -0.1712(12) 0.040(4) Uiso 0.348(6) 1 d PD A 2 F56 F 0.5268(6) 0.5414(12) -0.2253(13) 0.060 Uiso 0.348(6) 1 d PD A 2 P4 P 0.27995(6) 0.58641(13) -0.3223(2) 0.0245(4) Uani 1 1 d . . . F41 F 0.31512(17) 0.6463(4) -0.3080(7) 0.064(2) Uani 1 1 d . . . F42 F 0.30670(16) 0.5059(3) -0.2940(5) 0.0396(13) Uani 1 1 d . . . F43 F 0.27965(18) 0.5973(4) -0.1924(5) 0.0482(15) Uani 1 1 d . . . F44 F 0.24450(16) 0.5252(4) -0.3357(5) 0.0410(14) Uani 1 1 d . . . F45 F 0.25267(16) 0.6653(4) -0.3525(5) 0.0463(15) Uani 1 1 d . . . F46 F 0.28052(17) 0.5742(4) -0.4520(5) 0.0500(16) Uani 1 1 d . . . O1W O 0.5720(2) 0.2643(5) -0.6314(7) 0.055(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01258(12) 0.01414(12) 0.01146(12) 0.00066(10) 0.00344(9) 0.00139(10) Os2 0.01291(12) 0.01369(12) 0.01282(12) 0.00114(11) 0.00273(9) -0.00096(10) P1 0.0172(10) 0.0183(10) 0.0129(8) -0.0008(7) 0.0028(8) -0.0002(7) F11 0.029(2) 0.026(2) 0.018(2) -0.0043(18) 0.0074(19) -0.0033(19) F12 0.017(2) 0.022(2) 0.026(2) -0.0015(18) -0.0004(18) -0.0002(17) F13 0.031(3) 0.014(2) 0.025(2) 0.0007(17) 0.006(2) -0.0037(18) F14 0.038(3) 0.026(2) 0.012(2) -0.0021(17) 0.0108(19) 0.001(2) F15 0.018(2) 0.026(2) 0.030(3) 0.0011(19) 0.0058(19) 0.0011(18) F16 0.024(2) 0.018(2) 0.025(2) 0.0003(17) 0.0037(19) 0.0006(17) P2 0.0181(9) 0.0326(11) 0.0170(10) -0.0007(8) 0.0011(8) 0.0004(8) F21 0.027(2) 0.055(3) 0.017(2) -0.003(2) 0.007(2) 0.004(2) F22 0.039(3) 0.046(3) 0.038(3) -0.006(3) 0.006(3) 0.010(3) F23 0.045(3) 0.070(4) 0.037(3) -0.015(3) 0.014(3) -0.032(3) F24 0.028(2) 0.043(3) 0.023(3) 0.005(2) 0.005(2) 0.003(2) F25 0.036(3) 0.058(4) 0.032(3) 0.004(2) 0.012(2) 0.023(3) F26 0.037(3) 0.038(3) 0.035(3) -0.002(2) 0.006(2) -0.008(2) P4 0.0238(11) 0.0219(10) 0.0269(12) 0.0020(8) 0.0026(8) 0.0015(9) F41 0.043(4) 0.044(4) 0.105(6) 0.006(4) 0.015(4) -0.016(3) F42 0.046(3) 0.027(3) 0.040(3) 0.008(2) -0.004(3) 0.015(2) F43 0.059(4) 0.050(4) 0.030(3) -0.013(3) -0.005(3) 0.001(3) F44 0.032(3) 0.051(4) 0.036(3) -0.002(3) -0.003(2) -0.016(3) F45 0.051(3) 0.043(3) 0.047(4) 0.011(3) 0.015(3) 0.022(3) F46 0.057(4) 0.066(4) 0.032(3) 0.016(3) 0.023(3) 0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.327(9) . ? N1 C14 1.390(10) . ? N1 Os1 2.048(7) . ? C2 C3 1.386(11) . ? C3 C4 1.389(11) . ? C4 C13 1.397(11) . ? C5 C6 1.346(11) . ? C5 C13 1.446(11) . ? C6 C12 1.434(11) . ? C7 C8 1.358(11) . ? C7 C12 1.416(11) . ? C8 C9 1.408(11) . ? C9 N10 1.341(10) . ? N10 C11 1.365(10) . ? N10 Os1 2.057(6) . ? C11 C12 1.403(10) . ? C11 C14 1.411(10) . ? C13 C14 1.394(11) . ? N21 C22 1.357(10) . ? N21 C34 1.374(10) . ? N21 Os1 2.065(7) . ? C22 C23 1.384(11) . ? C23 C24 1.367(11) . ? C24 C33 1.404(11) . ? C25 C26 1.367(10) . ? C25 C33 1.426(11) . ? C26 C32 1.430(11) . ? C27 C28 1.374(11) . ? C27 C32 1.403(10) . ? C28 C29 1.412(10) . ? C29 N30 1.340(9) . ? N30 C31 1.391(9) . ? N30 Os1 2.059(6) . ? C31 C32 1.410(10) . ? C31 C34 1.414(10) . ? C33 C34 1.397(11) . ? N41 C42 1.329(10) . ? N41 C54 1.360(9) . ? N41 Os1 2.071(6) . ? C42 C43 1.410(11) . ? C43 C44 1.365(12) . ? C44 C53 1.399(11) . ? C45 C46 1.359(12) . ? C45 C53 1.398(11) . ? C46 C52 1.451(11) . ? C47 C48 1.373(11) . ? C47 C52 1.400(11) . ? C48 C49 1.398(10) . ? C49 N50 1.330(9) . ? N50 C51 1.360(9) . ? N50 Os1 2.069(6) . ? C51 C54 1.406(10) . ? C51 C52 1.423(10) . ? C53 C54 1.426(10) . ? N61 C62 1.358(10) . ? N61 C74 1.371(10) . ? N61 Os2 2.078(7) . ? C62 C63 1.389(11) . ? C63 C64 1.394(11) . ? C64 C73 1.404(11) . ? C65 C66 1.363(11) . ? C65 C73 1.429(11) . ? C66 C72 1.435(11) . ? C67 C68 1.384(11) . ? C67 C72 1.404(11) . ? C68 C69 1.405(10) . ? C69 N70 1.346(9) . ? N70 C71 1.364(9) . ? N70 Os2 2.062(6) . ? C71 C72 1.393(10) . ? C71 C74 1.431(10) . ? C73 C74 1.397(11) . ? N81 C82 1.332(9) . ? N81 C94 1.354(9) . ? N81 Os2 2.058(6) . ? C82 C83 1.392(10) . ? C83 C84 1.379(11) . ? C84 C93 1.395(10) . ? C85 C86 1.360(11) . ? C85 C93 1.427(11) . ? C86 C92 1.446(11) . ? C87 C88 1.395(12) . ? C87 C92 1.409(11) . ? C88 C89 1.384(12) . ? C89 N90 1.341(10) . ? N90 C91 1.386(10) . ? N90 Os2 2.041(7) . ? C91 C92 1.393(11) . ? C91 C94 1.421(10) . ? C93 C94 1.423(10) . ? N101 C102 1.342(9) . ? N101 C114 1.371(9) . ? N101 Os2 2.063(6) . ? C102 C103 1.394(11) . ? C103 C104 1.376(11) . ? C104 C113 1.417(11) . ? C105 C106 1.354(12) . ? C105 C113 1.441(11) . ? C106 C112 1.418(12) . ? C107 C108 1.385(11) . ? C107 C112 1.392(11) . ? C108 C109 1.390(11) . ? C109 N110 1.346(10) . ? N110 C111 1.372(10) . ? N110 Os2 2.065(6) . ? C111 C112 1.403(11) . ? C111 C114 1.411(10) . ? C113 C114 1.395(9) . ? P1 F11 1.588(5) . ? P1 F14 1.601(4) . ? P1 F16 1.603(5) . ? P1 F15 1.605(5) . ? P1 F13 1.604(5) . ? P1 F12 1.615(5) . ? P2 F24 1.577(5) . ? P2 F23 1.597(6) . ? P2 F21 1.601(5) . ? P2 F22 1.607(6) . ? P2 F25 1.608(5) . ? P2 F26 1.612(5) . ? P3 F35 1.577(10) . ? P3 F34 1.587(10) . ? P3 F31 1.583(10) . ? P3 F33 1.603(9) . ? P3 F36 1.590(10) . ? P3 F32 1.619(12) . ? P5 F53 1.542(11) . ? P5 F51 1.547(12) . ? P5 F54 1.591(13) . ? P5 F55 1.606(13) . ? P5 F56 1.624(13) . ? P5 F52 1.630(14) . ? P4 F41 1.582(6) . ? P4 F43 1.589(6) . ? P4 F46 1.591(6) . ? P4 F45 1.597(6) . ? P4 F44 1.604(6) . ? P4 F42 1.603(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C14 117.2(7) . . ? C2 N1 Os1 129.0(5) . . ? C14 N1 Os1 113.2(5) . . ? N1 C2 C3 123.1(7) . . ? C2 C3 C4 120.2(7) . . ? C3 C4 C13 118.3(8) . . ? C6 C5 C13 120.1(8) . . ? C5 C6 C12 121.9(7) . . ? C8 C7 C12 119.9(7) . . ? C7 C8 C9 120.3(8) . . ? N10 C9 C8 121.4(8) . . ? C9 N10 C11 118.4(6) . . ? C9 N10 Os1 128.6(5) . . ? C11 N10 Os1 113.0(5) . . ? N10 C11 C12 123.4(7) . . ? N10 C11 C14 117.4(7) . . ? C12 C11 C14 119.2(7) . . ? C11 C12 C7 116.6(7) . . ? C11 C12 C6 118.7(7) . . ? C7 C12 C6 124.7(7) . . ? C4 C13 C14 118.5(7) . . ? C4 C13 C5 123.3(8) . . ? C14 C13 C5 118.2(7) . . ? N1 C14 C13 122.7(7) . . ? N1 C14 C11 115.6(7) . . ? C13 C14 C11 121.7(7) . . ? C22 N21 C34 116.7(7) . . ? C22 N21 Os1 128.4(5) . . ? C34 N21 Os1 114.9(5) . . ? N21 C22 C23 122.3(7) . . ? C24 C23 C22 120.6(7) . . ? C23 C24 C33 119.6(8) . . ? C26 C25 C33 121.1(7) . . ? C25 C26 C32 121.0(7) . . ? C28 C27 C32 119.7(7) . . ? C27 C28 C29 120.2(7) . . ? N30 C29 C28 122.2(7) . . ? C29 N30 C31 117.3(6) . . ? C29 N30 Os1 128.3(5) . . ? C31 N30 Os1 114.3(4) . . ? N30 C31 C32 123.2(6) . . ? N30 C31 C34 115.9(6) . . ? C32 C31 C34 120.8(7) . . ? C27 C32 C31 117.3(7) . . ? C27 C32 C26 124.6(7) . . ? C31 C32 C26 118.0(7) . . ? C34 C33 C24 116.9(7) . . ? C34 C33 C25 118.9(7) . . ? C24 C33 C25 124.1(7) . . ? N21 C34 C33 124.0(7) . . ? N21 C34 C31 115.8(7) . . ? C33 C34 C31 120.2(7) . . ? C42 N41 C54 118.4(6) . . ? C42 N41 Os1 128.2(5) . . ? C54 N41 Os1 113.4(5) . . ? N41 C42 C43 122.1(7) . . ? C44 C43 C42 119.2(8) . . ? C43 C44 C53 121.1(8) . . ? C46 C45 C53 122.4(8) . . ? C45 C46 C52 120.6(7) . . ? C48 C47 C52 119.3(8) . . ? C47 C48 C49 119.0(7) . . ? N50 C49 C48 123.6(7) . . ? C49 N50 C51 118.2(6) . . ? C49 N50 Os1 128.8(5) . . ? C51 N50 Os1 112.9(5) . . ? N50 C51 C54 117.6(6) . . ? N50 C51 C52 121.6(6) . . ? C54 C51 C52 120.8(7) . . ? C47 C52 C51 118.3(7) . . ? C47 C52 C46 124.2(7) . . ? C51 C52 C46 117.5(7) . . ? C44 C53 C45 125.7(7) . . ? C44 C53 C54 115.6(7) . . ? C45 C53 C54 118.7(7) . . ? N41 C54 C51 116.6(6) . . ? N41 C54 C53 123.4(7) . . ? C51 C54 C53 120.0(7) . . ? C62 N61 C74 117.0(7) . . ? C62 N61 Os2 127.7(5) . . ? C74 N61 Os2 114.9(5) . . ? N61 C62 C63 122.4(7) . . ? C62 C63 C64 120.1(8) . . ? C63 C64 C73 118.9(8) . . ? C66 C65 C73 120.6(8) . . ? C65 C66 C72 122.1(7) . . ? C68 C67 C72 118.5(7) . . ? C67 C68 C69 119.9(7) . . ? N70 C69 C68 122.2(7) . . ? C69 N70 C71 117.6(6) . . ? C69 N70 Os2 127.0(5) . . ? C71 N70 Os2 115.3(5) . . ? N70 C71 C72 123.3(7) . . ? N70 C71 C74 116.1(6) . . ? C72 C71 C74 120.5(7) . . ? C71 C72 C67 118.4(7) . . ? C71 C72 C66 117.6(7) . . ? C67 C72 C66 124.0(7) . . ? C74 C73 C64 117.6(7) . . ? C74 C73 C65 118.3(7) . . ? C64 C73 C65 124.1(7) . . ? N61 C74 C73 124.0(7) . . ? N61 C74 C71 115.2(7) . . ? C73 C74 C71 120.7(7) . . ? C82 N81 C94 117.6(6) . . ? C82 N81 Os2 129.1(5) . . ? C94 N81 Os2 113.3(5) . . ? N81 C82 C83 123.4(7) . . ? C84 C83 C82 119.0(7) . . ? C83 C84 C93 119.9(7) . . ? C86 C85 C93 122.4(7) . . ? C85 C86 C92 120.1(8) . . ? C88 C87 C92 117.0(8) . . ? C89 C88 C87 121.2(8) . . ? N90 C89 C88 123.0(8) . . ? C89 N90 C91 116.6(7) . . ? C89 N90 Os2 129.2(6) . . ? C91 N90 Os2 114.2(5) . . ? N90 C91 C92 123.4(7) . . ? N90 C91 C94 114.8(7) . . ? C92 C91 C94 121.8(7) . . ? C91 C92 C87 118.9(7) . . ? C91 C92 C86 118.3(7) . . ? C87 C92 C86 122.8(8) . . ? C84 C93 C94 116.9(7) . . ? C84 C93 C85 125.1(7) . . ? C94 C93 C85 118.0(7) . . ? N81 C94 C91 117.6(6) . . ? N81 C94 C93 123.2(7) . . ? C91 C94 C93 119.3(7) . . ? C102 N101 C114 117.5(6) . . ? C102 N101 Os2 128.8(5) . . ? C114 N101 Os2 113.7(4) . . ? N101 C102 C103 122.3(7) . . ? C104 C103 C102 121.1(7) . . ? C103 C104 C113 117.4(7) . . ? C106 C105 C113 120.4(8) . . ? C105 C106 C112 122.5(8) . . ? C108 C107 C112 119.3(7) . . ? C107 C108 C109 119.5(7) . . ? N110 C109 C108 122.5(7) . . ? C109 N110 C111 118.1(6) . . ? C109 N110 Os2 128.6(5) . . ? C111 N110 Os2 113.2(5) . . ? N110 C111 C112 122.0(7) . . ? N110 C111 C114 117.0(6) . . ? C112 C111 C114 120.9(7) . . ? C107 C112 C111 118.5(7) . . ? C107 C112 C106 124.1(8) . . ? C111 C112 C106 117.4(7) . . ? C114 C113 C104 118.8(7) . . ? C114 C113 C105 118.0(7) . . ? C104 C113 C105 123.2(7) . . ? N101 C114 C113 122.9(7) . . ? N101 C114 C111 116.4(6) . . ? C113 C114 C111 120.7(7) . . ? N1 Os1 N10 80.1(2) . . ? N1 Os1 N30 100.3(2) . . ? N10 Os1 N30 91.1(3) . . ? N1 Os1 N21 175.4(2) . . ? N10 Os1 N21 95.4(3) . . ? N30 Os1 N21 78.9(2) . . ? N1 Os1 N50 94.1(2) . . ? N10 Os1 N50 172.9(3) . . ? N30 Os1 N50 94.0(2) . . ? N21 Os1 N50 90.5(3) . . ? N1 Os1 N41 88.8(2) . . ? N10 Os1 N41 96.2(2) . . ? N30 Os1 N41 169.2(2) . . ? N21 Os1 N41 92.4(2) . . ? N50 Os1 N41 79.4(2) . . ? N90 Os2 N81 79.8(3) . . ? N90 Os2 N70 98.2(2) . . ? N81 Os2 N70 93.1(2) . . ? N90 Os2 N101 89.1(2) . . ? N81 Os2 N101 94.9(2) . . ? N70 Os2 N101 170.0(2) . . ? N90 Os2 N110 96.4(3) . . ? N81 Os2 N110 173.4(2) . . ? N70 Os2 N110 92.7(2) . . ? N101 Os2 N110 79.7(2) . . ? N90 Os2 N61 176.3(2) . . ? N81 Os2 N61 99.0(2) . . ? N70 Os2 N61 78.3(2) . . ? N101 Os2 N61 94.5(2) . . ? N110 Os2 N61 85.1(3) . . ? F11 P1 F14 179.5(3) . . ? F11 P1 F16 90.6(3) . . ? F14 P1 F16 89.9(3) . . ? F11 P1 F15 90.1(3) . . ? F14 P1 F15 89.9(3) . . ? F16 P1 F15 89.7(2) . . ? F11 P1 F13 89.1(3) . . ? F14 P1 F13 90.4(3) . . ? F16 P1 F13 179.7(3) . . ? F15 P1 F13 90.5(2) . . ? F11 P1 F12 90.6(2) . . ? F14 P1 F12 89.4(3) . . ? F16 P1 F12 90.2(2) . . ? F15 P1 F12 179.3(3) . . ? F13 P1 F12 89.6(2) . . ? F24 P2 F23 90.2(3) . . ? F24 P2 F21 179.6(4) . . ? F23 P2 F21 90.2(3) . . ? F24 P2 F22 90.6(3) . . ? F23 P2 F22 90.9(3) . . ? F21 P2 F22 89.5(3) . . ? F24 P2 F25 89.8(3) . . ? F23 P2 F25 90.6(3) . . ? F21 P2 F25 90.1(3) . . ? F22 P2 F25 178.4(3) . . ? F24 P2 F26 90.5(3) . . ? F23 P2 F26 179.3(3) . . ? F21 P2 F26 89.1(3) . . ? F22 P2 F26 89.0(3) . . ? F25 P2 F26 89.5(3) . . ? F35 P3 F34 88.8(6) . . ? F35 P3 F31 89.3(6) . . ? F34 P3 F31 176.8(7) . . ? F35 P3 F33 88.5(6) . . ? F34 P3 F33 90.2(6) . . ? F31 P3 F33 87.1(6) . . ? F35 P3 F36 91.5(6) . . ? F34 P3 F36 91.1(6) . . ? F31 P3 F36 91.6(6) . . ? F33 P3 F36 178.7(7) . . ? F35 P3 F32 176.4(7) . . ? F34 P3 F32 89.1(7) . . ? F31 P3 F32 92.6(7) . . ? F33 P3 F32 88.5(6) . . ? F36 P3 F32 91.6(7) . . ? F53 P5 F51 87.5(8) . . ? F53 P5 F54 173.5(10) . . ? F51 P5 F54 97.9(9) . . ? F53 P5 F55 87.9(8) . . ? F51 P5 F55 91.4(8) . . ? F54 P5 F55 88.3(9) . . ? F53 P5 F56 95.0(9) . . ? F51 P5 F56 177.4(11) . . ? F54 P5 F56 79.6(10) . . ? F55 P5 F56 88.2(10) . . ? F53 P5 F52 92.4(9) . . ? F51 P5 F52 94.8(9) . . ? F54 P5 F52 90.8(10) . . ? F55 P5 F52 173.7(10) . . ? F56 P5 F52 85.5(11) . . ? F41 P4 F43 89.7(4) . . ? F41 P4 F46 90.5(4) . . ? F43 P4 F46 179.1(4) . . ? F41 P4 F45 90.9(4) . . ? F43 P4 F45 90.8(3) . . ? F46 P4 F45 90.1(3) . . ? F41 P4 F44 179.4(4) . . ? F43 P4 F44 89.9(3) . . ? F46 P4 F44 89.9(3) . . ? F45 P4 F44 89.6(3) . . ? F41 P4 F42 90.2(3) . . ? F43 P4 F42 90.0(3) . . ? F46 P4 F42 89.1(3) . . ? F45 P4 F42 178.7(4) . . ? F44 P4 F42 89.4(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.730 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.128 data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 242570' # data_371601a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H54 F24 N12 O3 Os2 P4' _chemical_formula_weight 2095.56 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' 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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.0513(10) _cell_length_b 17.7690(14) _cell_length_c 31.426(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7288.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13679 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 27.95 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 3.692 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6074 _exptl_absorpt_correction_T_max 0.7091 _exptl_absorpt_process_details 'Bruker 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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46061 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.95 _reflns_number_total 16877 _reflns_number_gt 13679 _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, 1997)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(6) _refine_ls_number_reflns 16877 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 N1 N -0.1231(5) 0.4338(3) 0.5315(2) 0.0141(14) Uiso 1 1 d . . . C2 C -0.1975(6) 0.4641(5) 0.5547(2) 0.0158(17) Uiso 1 1 d . . . H2 H -0.1817 0.5025 0.5737 0.019 Uiso 1 1 calc R . . C3 C -0.2986(6) 0.4398(4) 0.5513(2) 0.0176(18) Uiso 1 1 d . . . H3 H -0.3490 0.4612 0.5684 0.021 Uiso 1 1 calc R . . C4 C -0.3241(6) 0.3831(4) 0.5223(2) 0.0161(18) Uiso 1 1 d . . . H4 H -0.3916 0.3670 0.5195 0.019 Uiso 1 1 calc R . . C5 C -0.2644(6) 0.2946(4) 0.4662(2) 0.0175(17) Uiso 1 1 d . . . H5 H -0.3304 0.2765 0.4617 0.021 Uiso 1 1 calc R . . C6 C -0.1845(6) 0.2673(4) 0.4431(2) 0.0180(18) Uiso 1 1 d . . . H6 H -0.1982 0.2312 0.4225 0.022 Uiso 1 1 calc R . . C7 C 0.0036(6) 0.2639(4) 0.4267(2) 0.0180(18) Uiso 1 1 d . . . H7 H -0.0048 0.2271 0.4060 0.022 Uiso 1 1 calc R . . C8 C 0.0998(7) 0.2923(4) 0.4359(2) 0.0170(18) Uiso 1 1 d . . . H8 H 0.1565 0.2751 0.4208 0.020 Uiso 1 1 calc R . . C9 C 0.1118(6) 0.3462(4) 0.4673(2) 0.0167(17) Uiso 1 1 d . . . H9 H 0.1775 0.3631 0.4737 0.020 Uiso 1 1 calc R . . N10 N 0.0318(5) 0.3750(3) 0.48877(17) 0.0104(13) Uiso 1 1 d . . . C11 C -0.0630(6) 0.3464(4) 0.4803(2) 0.0122(17) Uiso 1 1 d . . . C12 C -0.0796(6) 0.2913(4) 0.4489(2) 0.0142(17) Uiso 1 1 d . . . C13 C -0.2460(6) 0.3511(4) 0.4975(2) 0.0116(16) Uiso 1 1 d . . . C14 C -0.1466(6) 0.3781(4) 0.5039(2) 0.0165(18) Uiso 1 1 d . . . N21 N 0.0066(5) 0.5613(3) 0.56498(19) 0.0137(14) Uiso 1 1 d . . . C22 C 0.0102(6) 0.5729(4) 0.6071(2) 0.0176(18) Uiso 1 1 d . . . H22 H 0.0284 0.5327 0.6245 0.021 Uiso 1 1 calc R . . C23 C -0.0114(6) 0.6404(4) 0.6260(3) 0.0192(19) Uiso 1 1 d . . . H23 H -0.0083 0.6449 0.6555 0.023 Uiso 1 1 calc R . . C24 C -0.0377(7) 0.7018(4) 0.6014(2) 0.0176(17) Uiso 1 1 d . . . H24 H -0.0547 0.7474 0.6140 0.021 Uiso 1 1 calc R . . C25 C -0.0633(6) 0.7541(4) 0.5287(3) 0.0174(17) Uiso 1 1 d . . . H25 H -0.0773 0.8017 0.5396 0.021 Uiso 1 1 calc R . . C26 C -0.0669(6) 0.7433(5) 0.4863(3) 0.022(2) Uiso 1 1 d . . . H26 H -0.0822 0.7836 0.4685 0.026 Uiso 1 1 calc R . . C27 C -0.0535(6) 0.6544(5) 0.4244(2) 0.0203(19) Uiso 1 1 d . . . H27 H -0.0703 0.6923 0.4053 0.024 Uiso 1 1 calc R . . C28 C -0.0346(7) 0.5834(4) 0.4107(2) 0.0203(18) Uiso 1 1 d . . . H28 H -0.0373 0.5723 0.3818 0.024 Uiso 1 1 calc R . . C29 C -0.0108(6) 0.5266(4) 0.4402(2) 0.0187(18) Uiso 1 1 d . . . H29 H 0.0012 0.4782 0.4301 0.022 Uiso 1 1 calc R . . N30 N -0.0045(5) 0.5387(4) 0.48203(18) 0.0141(14) Uiso 1 1 d . . . C31 C -0.0239(6) 0.6111(4) 0.4954(2) 0.0117(15) Uiso 1 1 d . . . C32 C -0.0473(5) 0.6694(4) 0.4679(2) 0.0132(15) Uiso 1 1 d . . . C33 C -0.0383(6) 0.6939(4) 0.5575(2) 0.0160(16) Uiso 1 1 d . . . C34 C -0.0192(6) 0.6227(4) 0.5403(2) 0.0118(16) Uiso 1 1 d . . . N41 N 0.0759(5) 0.3994(3) 0.58074(18) 0.0119(14) Uiso 1 1 d . . . C42 C 0.0185(6) 0.3507(4) 0.6038(2) 0.0156(17) Uiso 1 1 d . . . H42 H -0.0499 0.3435 0.5965 0.019 Uiso 1 1 calc R . . C43 C 0.0598(6) 0.3107(4) 0.6385(2) 0.0193(19) Uiso 1 1 d . . . H43 H 0.0190 0.2768 0.6534 0.023 Uiso 1 1 calc R . . C44 C 0.1594(6) 0.3216(4) 0.6505(2) 0.0180(18) Uiso 1 1 d . . . H44 H 0.1860 0.2965 0.6740 0.022 Uiso 1 1 calc R . . C45 C 0.3259(6) 0.3853(4) 0.6361(2) 0.0185(19) Uiso 1 1 d . . . H45 H 0.3562 0.3633 0.6598 0.022 Uiso 1 1 calc R . . C46 C 0.3829(6) 0.4306(4) 0.6107(2) 0.0174(18) Uiso 1 1 d . . . H46 H 0.4512 0.4390 0.6175 0.021 Uiso 1 1 calc R . . C47 C 0.3965(7) 0.5113(4) 0.5448(2) 0.0178(18) Uiso 1 1 d . . . H47 H 0.4654 0.5220 0.5494 0.021 Uiso 1 1 calc R . . C48 C 0.3457(6) 0.5391(5) 0.5099(2) 0.0146(16) Uiso 1 1 d . . . H48 H 0.3814 0.5682 0.4903 0.018 Uiso 1 1 calc R . . C49 C 0.2440(6) 0.5252(4) 0.5033(2) 0.0166(18) Uiso 1 1 d . . . H49 H 0.2133 0.5441 0.4788 0.020 Uiso 1 1 calc R . . N50 N 0.1859(5) 0.4852(3) 0.5309(2) 0.0144(14) Uiso 1 1 d . . . C51 C 0.2354(6) 0.4539(4) 0.5656(2) 0.0135(17) Uiso 1 1 d . . . C52 C 0.3404(6) 0.4660(5) 0.5734(2) 0.0161(17) Uiso 1 1 d . . . C53 C 0.2204(7) 0.3704(4) 0.6273(2) 0.0165(17) Uiso 1 1 d . . . C54 C 0.1761(6) 0.4081(4) 0.5923(2) 0.0125(16) Uiso 1 1 d . . . N61 N 0.2093(5) 0.9116(3) 0.65515(18) 0.0134(14) Uiso 1 1 d . . . C62 C 0.2086(7) 0.9873(4) 0.6572(2) 0.0202(18) Uiso 1 1 d . . . H62 H 0.2149 1.0101 0.6837 0.024 Uiso 1 1 calc R . . C63 C 0.1988(6) 1.0330(5) 0.6213(2) 0.0220(19) Uiso 1 1 d . . . H63 H 0.2005 1.0852 0.6240 0.026 Uiso 1 1 calc R . . C64 C 0.1868(6) 1.0009(5) 0.5825(3) 0.022(2) Uiso 1 1 d . . . H64 H 0.1767 1.0310 0.5586 0.027 Uiso 1 1 calc R . . C65 C 0.1818(6) 0.8813(5) 0.5386(3) 0.023(2) Uiso 1 1 d . . . H65 H 0.1702 0.9078 0.5136 0.027 Uiso 1 1 calc R . . C66 C 0.1911(6) 0.8056(4) 0.5374(3) 0.0202(19) Uiso 1 1 d . . . H66 H 0.1872 0.7810 0.5113 0.024 Uiso 1 1 calc R . . C67 C 0.2220(7) 0.6843(4) 0.5759(3) 0.0233(19) Uiso 1 1 d . . . H67 H 0.2195 0.6567 0.5508 0.028 Uiso 1 1 calc R . . C68 C 0.2403(6) 0.6494(5) 0.6136(2) 0.024(2) Uiso 1 1 d . . . H68 H 0.2537 0.5980 0.6140 0.029 Uiso 1 1 calc R . . C69 C 0.2393(6) 0.6902(4) 0.6519(2) 0.0174(18) Uiso 1 1 d . . . H69 H 0.2498 0.6646 0.6773 0.021 Uiso 1 1 calc R . . N70 N 0.2241(5) 0.7642(3) 0.65304(18) 0.0124(13) Uiso 1 1 d . . . C71 C 0.2084(6) 0.8002(4) 0.6141(2) 0.0134(16) Uiso 1 1 d . . . C72 C 0.2068(6) 0.7624(4) 0.5753(2) 0.0146(17) Uiso 1 1 d . . . C73 C 0.1896(6) 0.9213(5) 0.5783(2) 0.0188(19) Uiso 1 1 d . . . C74 C 0.1999(6) 0.8789(4) 0.6159(2) 0.0147(17) Uiso 1 1 d . . . N81 N 0.3766(5) 0.8485(3) 0.70994(19) 0.0141(15) Uiso 1 1 d . . . C82 C 0.4471(6) 0.8080(4) 0.6906(2) 0.0153(18) Uiso 1 1 d . . . H82 H 0.4278 0.7711 0.6713 0.018 Uiso 1 1 calc R . . C83 C 0.5512(6) 0.8204(4) 0.6991(3) 0.021(2) Uiso 1 1 d . . . H83 H 0.6005 0.7909 0.6857 0.026 Uiso 1 1 calc R . . C84 C 0.5807(7) 0.8754(5) 0.7269(2) 0.024(2) Uiso 1 1 d . . . H84 H 0.6498 0.8835 0.7324 0.028 Uiso 1 1 calc R . . C85 C 0.5269(7) 0.9790(4) 0.7767(2) 0.0210(18) Uiso 1 1 d . . . H85 H 0.5947 0.9908 0.7829 0.025 Uiso 1 1 calc R . . C86 C 0.4503(6) 1.0180(4) 0.7957(3) 0.0226(19) Uiso 1 1 d . . . H86 H 0.4664 1.0565 0.8146 0.027 Uiso 1 1 calc R . . C87 C 0.2624(6) 1.0385(5) 0.8050(2) 0.0239(19) Uiso 1 1 d . . . H87 H 0.2731 1.0787 0.8235 0.029 Uiso 1 1 calc R . . C88 C 0.1644(7) 1.0159(5) 0.7952(3) 0.0232(19) Uiso 1 1 d . . . H88 H 0.1087 1.0413 0.8067 0.028 Uiso 1 1 calc R . . C89 C 0.1485(7) 0.9553(5) 0.7684(2) 0.0224(19) Uiso 1 1 d . . . H89 H 0.0816 0.9395 0.7634 0.027 Uiso 1 1 calc R . . N90 N 0.2242(6) 0.9190(3) 0.74945(18) 0.0154(14) Uiso 1 1 d . . . C91 C 0.3238(6) 0.9419(4) 0.7593(2) 0.0137(17) Uiso 1 1 d . . . C92 C 0.3448(6) 1.0011(4) 0.7873(2) 0.0177(18) Uiso 1 1 d . . . C93 C 0.5052(6) 0.9200(5) 0.7472(3) 0.0184(18) Uiso 1 1 d . . . C94 C 0.4025(6) 0.9024(4) 0.7380(2) 0.0115(16) Uiso 1 1 d . . . N101 N 0.0623(5) 0.8153(3) 0.70782(19) 0.0115(14) Uiso 1 1 d . . . C102 C -0.0143(6) 0.8461(4) 0.6846(2) 0.0153(17) Uiso 1 1 d . . . H102 H 0.0013 0.8842 0.6654 0.018 Uiso 1 1 calc R . . C103 C -0.1146(6) 0.8230(5) 0.6885(2) 0.0189(19) Uiso 1 1 d . . . H103 H -0.1641 0.8453 0.6713 0.023 Uiso 1 1 calc R . . C104 C -0.1437(7) 0.7693(5) 0.7164(2) 0.022(2) Uiso 1 1 d . . . H104 H -0.2119 0.7548 0.7189 0.026 Uiso 1 1 calc R . . C105 C -0.0844(7) 0.6792(5) 0.7733(3) 0.024(2) Uiso 1 1 d . . . H105 H -0.1506 0.6607 0.7767 0.029 Uiso 1 1 calc R . . C106 C -0.0089(6) 0.6519(4) 0.7985(2) 0.0189(18) Uiso 1 1 d . . . H106 H -0.0239 0.6159 0.8190 0.023 Uiso 1 1 calc R . . C107 C 0.1755(6) 0.6553(5) 0.8199(2) 0.0201(18) Uiso 1 1 d . . . H107 H 0.1642 0.6219 0.8422 0.024 Uiso 1 1 calc R . . C108 C 0.2711(7) 0.6828(4) 0.8122(2) 0.0219(19) Uiso 1 1 d . . . H108 H 0.3254 0.6688 0.8296 0.026 Uiso 1 1 calc R . . C109 C 0.2881(7) 0.7325(4) 0.7778(2) 0.0229(19) Uiso 1 1 d . . . H109 H 0.3546 0.7488 0.7724 0.027 Uiso 1 1 calc R . . N110 N 0.2115(5) 0.7574(3) 0.75253(18) 0.0142(14) Uiso 1 1 d . . . C111 C 0.1151(6) 0.7303(4) 0.7618(2) 0.0136(17) Uiso 1 1 d . . . C112 C 0.0940(6) 0.6783(4) 0.7935(2) 0.0154(17) Uiso 1 1 d . . . C113 C -0.0657(6) 0.7353(4) 0.7420(2) 0.0138(17) Uiso 1 1 d . . . C114 C 0.0348(6) 0.7611(4) 0.7363(2) 0.0118(15) Uiso 1 1 d . . . Os1 Os 0.03020(2) 0.464668(16) 0.530068(9) 0.01113(7) Uani 1 1 d . . . Os2 Os 0.21790(2) 0.835483(17) 0.704561(9) 0.01137(7) Uani 1 1 d . . . P1 P 0.84766(17) 0.00485(12) 0.77889(7) 0.0178(5) Uani 1 1 d . . . F11 F 0.7612(4) 0.0438(3) 0.75022(17) 0.0428(15) Uani 1 1 d . . . F12 F 0.7782(4) 0.0181(3) 0.82044(15) 0.0349(13) Uani 1 1 d . . . F13 F 0.9015(4) 0.0852(3) 0.78614(15) 0.0308(13) Uani 1 1 d . . . F14 F 0.9334(3) -0.0341(3) 0.80792(13) 0.0212(10) Uani 1 1 d . . . F15 F 0.9166(4) -0.0085(3) 0.73773(14) 0.0230(11) Uani 1 1 d . . . F16 F 0.7938(4) -0.0755(3) 0.77238(14) 0.0271(12) Uani 1 1 d . . . P2 P 0.91808(17) 0.14640(12) 0.55693(7) 0.0182(5) Uani 1 1 d . . . F21 F 0.8417(4) 0.0870(3) 0.57894(15) 0.0321(13) Uani 1 1 d . . . F22 F 0.8475(4) 0.2147(3) 0.57243(17) 0.0335(13) Uani 1 1 d . . . F23 F 0.9828(4) 0.1522(3) 0.59987(14) 0.0322(13) Uani 1 1 d . . . F24 F 0.9939(3) 0.2059(3) 0.53508(15) 0.0275(12) Uani 1 1 d . . . F25 F 0.9896(4) 0.0782(3) 0.54150(14) 0.0262(12) Uani 1 1 d . . . F26 F 0.8538(4) 0.1401(3) 0.51351(14) 0.0250(12) Uani 1 1 d . . . P3 P 0.63474(17) 0.66385(14) 0.59326(6) 0.0199(5) Uani 1 1 d . . . F31 F 0.5773(4) 0.6388(3) 0.55100(13) 0.0272(12) Uani 1 1 d . . . F32 F 0.5265(5) 0.6890(3) 0.61380(16) 0.0386(14) Uani 1 1 d . . . F33 F 0.6495(4) 0.7474(3) 0.57421(15) 0.0322(13) Uani 1 1 d . . . F34 F 0.6923(5) 0.6896(3) 0.63512(16) 0.0420(16) Uani 1 1 d . . . F35 F 0.7410(4) 0.6383(3) 0.57244(17) 0.0371(14) Uani 1 1 d . . . F36 F 0.6193(4) 0.5813(3) 0.61203(14) 0.0298(13) Uani 1 1 d . . . P4 P 0.59035(18) 0.67412(14) 0.80743(7) 0.0235(5) Uani 1 1 d . . . F41 F 0.5189(4) 0.6607(3) 0.76768(17) 0.0525(17) Uani 1 1 d . . . F42 F 0.5186(4) 0.7428(3) 0.82182(15) 0.0318(13) Uani 1 1 d . . . F43 F 0.6588(4) 0.7321(3) 0.78075(16) 0.0424(15) Uani 1 1 d . . . F44 F 0.6621(4) 0.6883(3) 0.84757(15) 0.0315(13) Uani 1 1 d . . . F45 F 0.6620(4) 0.6060(3) 0.79305(18) 0.0445(15) Uani 1 1 d . . . F46 F 0.5214(5) 0.6175(3) 0.83515(19) 0.0531(17) Uani 1 1 d . . . O1W O 0.6443(7) 0.0078(4) 0.6642(2) 0.064(2) Uiso 1 1 d . . . O2W O 0.9356(5) 0.9248(4) 0.5921(2) 0.0459(19) Uiso 1 1 d . . . O3W O 0.7227(6) 0.9034(4) 0.6025(2) 0.056(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.00878(15) 0.01211(14) 0.01250(14) -0.00036(13) -0.00154(13) -0.00068(13) Os2 0.00899(15) 0.01411(15) 0.01100(14) -0.00182(13) -0.00068(13) 0.00051(13) P1 0.0129(11) 0.0188(11) 0.0217(11) 0.0034(9) 0.0034(9) 0.0023(9) F11 0.020(3) 0.047(3) 0.061(4) 0.032(3) -0.002(3) 0.009(3) F12 0.040(3) 0.024(3) 0.041(3) -0.002(2) 0.027(3) 0.004(3) F13 0.038(3) 0.025(3) 0.029(3) -0.003(2) 0.009(2) -0.008(2) F14 0.017(3) 0.025(2) 0.022(2) 0.007(2) -0.0046(19) -0.008(2) F15 0.024(3) 0.027(3) 0.018(2) -0.002(2) 0.005(2) -0.003(2) F16 0.017(3) 0.030(3) 0.034(3) 0.006(2) -0.014(2) -0.013(2) P2 0.0117(11) 0.0248(13) 0.0182(11) -0.0033(9) 0.0007(9) -0.0009(9) F21 0.034(3) 0.037(3) 0.025(3) 0.001(2) 0.002(2) -0.012(3) F22 0.018(3) 0.030(3) 0.053(4) -0.018(3) 0.005(3) 0.004(2) F23 0.031(3) 0.041(3) 0.025(3) -0.003(2) -0.010(2) -0.004(3) F24 0.014(3) 0.037(3) 0.031(3) 0.007(2) 0.002(2) -0.006(2) F25 0.018(3) 0.030(3) 0.031(3) -0.006(2) -0.004(2) 0.008(2) F26 0.012(3) 0.035(3) 0.028(3) 0.003(2) -0.006(2) 0.000(2) P3 0.0205(12) 0.0224(11) 0.0169(11) -0.0020(10) -0.0018(9) 0.0053(10) F31 0.027(3) 0.039(3) 0.015(2) 0.006(2) -0.004(2) -0.003(2) F32 0.039(3) 0.038(3) 0.039(3) 0.005(3) 0.021(3) 0.011(3) F33 0.035(3) 0.026(3) 0.036(3) 0.006(2) -0.002(3) 0.000(2) F34 0.067(5) 0.029(3) 0.029(3) -0.003(2) -0.028(3) 0.012(3) F35 0.017(3) 0.036(3) 0.059(4) -0.009(3) 0.002(2) 0.004(2) F36 0.048(4) 0.026(3) 0.015(2) 0.000(2) -0.003(2) 0.004(2) P4 0.0131(12) 0.0308(13) 0.0265(12) -0.0054(11) -0.0020(9) 0.0036(10) F41 0.044(4) 0.058(4) 0.055(4) -0.035(3) -0.033(3) 0.027(3) F42 0.019(3) 0.037(3) 0.040(3) -0.018(2) -0.006(2) 0.012(2) F43 0.027(3) 0.063(4) 0.038(3) 0.017(3) 0.004(3) 0.009(3) F44 0.025(3) 0.036(3) 0.033(3) 0.006(2) -0.010(2) -0.001(2) F45 0.038(3) 0.051(4) 0.044(3) -0.018(3) -0.009(3) 0.027(3) F46 0.037(4) 0.049(4) 0.073(4) 0.008(3) 0.007(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.329(9) . ? N1 C14 1.352(9) . ? N1 Os1 2.075(6) . ? C2 C3 1.392(11) . ? C3 C4 1.400(10) . ? C4 C13 1.404(10) . ? C5 C6 1.360(11) . ? C5 C13 1.425(10) . ? C6 C12 1.445(11) . ? C7 C12 1.377(10) . ? C7 C8 1.383(11) . ? C8 C9 1.385(10) . ? C9 N10 1.345(9) . ? N10 C11 1.364(9) . ? N10 Os1 2.055(6) . ? C11 C12 1.408(10) . ? C11 C14 1.434(10) . ? C13 C14 1.398(11) . ? N21 C22 1.340(9) . ? N21 C34 1.379(9) . ? N21 Os1 2.061(6) . ? C22 C23 1.368(10) . ? C23 C24 1.381(10) . ? C24 C33 1.388(10) . ? C25 C26 1.346(10) . ? C25 C33 1.439(10) . ? C26 C32 1.457(11) . ? C27 C28 1.356(11) . ? C27 C32 1.395(10) . ? C28 C29 1.404(10) . ? C29 N30 1.335(9) . ? N30 C31 1.376(9) . ? N30 Os1 2.053(6) . ? C31 C32 1.384(10) . ? C31 C34 1.428(9) . ? C33 C34 1.397(10) . ? N41 C42 1.355(9) . ? N41 C54 1.367(9) . ? N41 Os1 2.058(6) . ? C42 C43 1.410(10) . ? C43 C44 1.368(11) . ? C44 C53 1.384(11) . ? C45 C46 1.355(11) . ? C45 C53 1.429(11) . ? C46 C52 1.443(10) . ? C47 C48 1.374(10) . ? C47 C52 1.411(11) . ? C48 C49 1.366(10) . ? C49 N50 1.353(9) . ? N50 C51 1.385(9) . ? N50 Os1 2.065(6) . ? C51 C54 1.401(10) . ? C51 C52 1.409(10) . ? C53 C54 1.411(10) . ? N61 C62 1.346(9) . ? N61 C74 1.370(9) . ? N61 Os2 2.062(6) . ? C62 C63 1.397(10) . ? C63 C64 1.355(11) . ? C64 C73 1.421(10) . ? C65 C66 1.351(10) . ? C65 C73 1.440(11) . ? C66 C72 1.433(10) . ? C67 C68 1.357(10) . ? C67 C72 1.401(10) . ? C68 C69 1.406(10) . ? C69 N70 1.330(9) . ? N70 C71 1.397(9) . ? N70 Os2 2.057(6) . ? C71 C72 1.393(10) . ? C71 C74 1.404(9) . ? C73 C74 1.406(10) . ? N81 C82 1.316(9) . ? N81 C94 1.346(9) . ? N81 Os2 2.091(6) . ? C82 C83 1.401(11) . ? C83 C84 1.366(11) . ? C84 C93 1.418(11) . ? C85 C86 1.357(11) . ? C85 C93 1.426(11) . ? C86 C92 1.434(11) . ? C87 C88 1.375(11) . ? C87 C92 1.383(11) . ? C88 C89 1.383(11) . ? C89 N90 1.321(10) . ? N90 C91 1.396(10) . ? N90 Os2 2.050(6) . ? C91 C92 1.398(10) . ? C91 C94 1.411(10) . ? C93 C94 1.407(11) . ? N101 C102 1.353(9) . ? N101 C114 1.363(9) . ? N101 Os2 2.065(6) . ? C102 C103 1.378(11) . ? C103 C104 1.350(11) . ? C104 C113 1.430(11) . ? C105 C106 1.353(11) . ? C105 C113 1.423(11) . ? C106 C112 1.432(10) . ? C107 C108 1.361(11) . ? C107 C112 1.410(11) . ? C108 C109 1.414(10) . ? C109 N110 1.352(10) . ? N110 C111 1.378(10) . ? N110 Os2 2.050(6) . ? C111 C112 1.385(10) . ? C111 C114 1.429(10) . ? C113 C114 1.401(11) . ? P1 F15 1.594(5) . ? P1 F14 1.601(5) . ? P1 F11 1.601(5) . ? P1 F16 1.604(5) . ? P1 F13 1.607(5) . ? P1 F12 1.607(5) . ? P2 F23 1.595(5) . ? P2 F22 1.600(5) . ? P2 F24 1.603(5) . ? P2 F25 1.604(5) . ? P2 F26 1.606(5) . ? P2 F21 1.608(5) . ? P3 F34 1.582(5) . ? P3 F31 1.589(5) . ? P3 F36 1.594(5) . ? P3 F35 1.599(5) . ? P3 F33 1.613(5) . ? P3 F32 1.617(6) . ? P4 F41 1.577(5) . ? P4 F44 1.591(5) . ? P4 F45 1.596(5) . ? P4 F43 1.601(6) . ? P4 F42 1.603(5) . ? P4 F46 1.607(6) . ? 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 C2 N1 C14 118.9(7) . . ? C2 N1 Os1 127.6(5) . . ? C14 N1 Os1 113.5(5) . . ? N1 C2 C3 121.7(7) . . ? C2 C3 C4 119.9(8) . . ? C3 C4 C13 118.7(7) . . ? C6 C5 C13 119.3(7) . . ? C5 C6 C12 123.7(8) . . ? C12 C7 C8 118.8(8) . . ? C7 C8 C9 120.2(8) . . ? N10 C9 C8 122.2(7) . . ? C9 N10 C11 117.7(6) . . ? C9 N10 Os1 128.3(5) . . ? C11 N10 Os1 113.8(5) . . ? N10 C11 C12 122.4(7) . . ? N10 C11 C14 116.3(7) . . ? C12 C11 C14 121.2(7) . . ? C7 C12 C11 118.6(7) . . ? C7 C12 C6 125.5(7) . . ? C11 C12 C6 116.0(7) . . ? C14 C13 C4 117.1(7) . . ? C14 C13 C5 119.8(7) . . ? C4 C13 C5 123.1(7) . . ? N1 C14 C13 123.6(7) . . ? N1 C14 C11 116.5(7) . . ? C13 C14 C11 119.8(7) . . ? C22 N21 C34 116.3(6) . . ? C22 N21 Os1 130.4(5) . . ? C34 N21 Os1 113.3(5) . . ? N21 C22 C23 123.8(7) . . ? C22 C23 C24 120.0(7) . . ? C23 C24 C33 118.7(7) . . ? C26 C25 C33 121.7(7) . . ? C25 C26 C32 120.9(8) . . ? C28 C27 C32 118.6(8) . . ? C27 C28 C29 119.9(7) . . ? N30 C29 C28 123.2(7) . . ? C29 N30 C31 116.1(6) . . ? C29 N30 Os1 129.4(5) . . ? C31 N30 Os1 114.5(4) . . ? N30 C31 C32 123.3(6) . . ? N30 C31 C34 115.5(6) . . ? C32 C31 C34 121.2(7) . . ? C31 C32 C27 118.8(7) . . ? C31 C32 C26 117.8(7) . . ? C27 C32 C26 123.3(7) . . ? C24 C33 C34 118.3(7) . . ? C24 C33 C25 123.5(7) . . ? C34 C33 C25 118.1(7) . . ? N21 C34 C33 122.9(6) . . ? N21 C34 C31 116.8(6) . . ? C33 C34 C31 120.3(6) . . ? C42 N41 C54 117.3(6) . . ? C42 N41 Os1 127.8(5) . . ? C54 N41 Os1 114.8(5) . . ? N41 C42 C43 121.6(8) . . ? C44 C43 C42 120.4(8) . . ? C43 C44 C53 119.3(8) . . ? C46 C45 C53 121.7(8) . . ? C45 C46 C52 121.8(8) . . ? C48 C47 C52 117.6(8) . . ? C49 C48 C47 121.7(8) . . ? N50 C49 C48 122.8(7) . . ? C49 N50 C51 117.1(7) . . ? C49 N50 Os1 129.5(5) . . ? C51 N50 Os1 113.4(5) . . ? N50 C51 C54 116.6(7) . . ? N50 C51 C52 121.9(7) . . ? C54 C51 C52 121.5(7) . . ? C51 C52 C47 118.8(7) . . ? C51 C52 C46 116.6(7) . . ? C47 C52 C46 124.6(8) . . ? C44 C53 C54 118.2(8) . . ? C44 C53 C45 124.6(7) . . ? C54 C53 C45 117.2(7) . . ? N41 C54 C51 115.7(7) . . ? N41 C54 C53 123.1(7) . . ? C51 C54 C53 121.1(7) . . ? C62 N61 C74 117.7(6) . . ? C62 N61 Os2 128.3(5) . . ? C74 N61 Os2 114.0(5) . . ? N61 C62 C63 123.0(7) . . ? C64 C63 C62 119.5(8) . . ? C63 C64 C73 119.9(8) . . ? C66 C65 C73 120.8(8) . . ? C65 C66 C72 121.5(8) . . ? C68 C67 C72 119.4(7) . . ? C67 C68 C69 120.6(8) . . ? N70 C69 C68 122.3(7) . . ? C69 N70 C71 116.8(6) . . ? C69 N70 Os2 129.5(5) . . ? C71 N70 Os2 113.7(4) . . ? C72 C71 N70 123.3(6) . . ? C72 C71 C74 121.0(7) . . ? N70 C71 C74 115.6(6) . . ? C71 C72 C67 117.6(7) . . ? C71 C72 C66 118.1(7) . . ? C67 C72 C66 124.3(7) . . ? C74 C73 C64 117.3(7) . . ? C74 C73 C65 117.9(7) . . ? C64 C73 C65 124.8(8) . . ? N61 C74 C71 116.8(7) . . ? N61 C74 C73 122.5(7) . . ? C71 C74 C73 120.5(7) . . ? C82 N81 C94 121.1(7) . . ? C82 N81 Os2 126.5(5) . . ? C94 N81 Os2 112.3(5) . . ? N81 C82 C83 120.3(7) . . ? C84 C83 C82 120.4(8) . . ? C83 C84 C93 119.5(8) . . ? C86 C85 C93 121.0(8) . . ? C85 C86 C92 121.2(8) . . ? C88 C87 C92 119.4(8) . . ? C87 C88 C89 120.3(8) . . ? N90 C89 C88 122.8(8) . . ? C89 N90 C91 117.1(7) . . ? C89 N90 Os2 129.3(6) . . ? C91 N90 Os2 113.6(5) . . ? N90 C91 C92 122.7(7) . . ? N90 C91 C94 115.3(7) . . ? C92 C91 C94 122.0(7) . . ? C87 C92 C91 117.7(8) . . ? C87 C92 C86 124.8(8) . . ? C91 C92 C86 117.5(8) . . ? C94 C93 C84 116.4(7) . . ? C94 C93 C85 119.1(7) . . ? C84 C93 C85 124.5(8) . . ? N81 C94 C93 122.2(7) . . ? N81 C94 C91 118.8(7) . . ? C93 C94 C91 119.0(7) . . ? C102 N101 C114 116.4(7) . . ? C102 N101 Os2 129.1(5) . . ? C114 N101 Os2 114.5(5) . . ? N101 C102 C103 122.3(7) . . ? C104 C103 C102 122.3(8) . . ? C103 C104 C113 117.6(8) . . ? C106 C105 C113 122.0(8) . . ? C105 C106 C112 120.2(8) . . ? C108 C107 C112 118.8(8) . . ? C107 C108 C109 120.3(8) . . ? N110 C109 C108 122.5(9) . . ? C109 N110 C111 115.9(7) . . ? C109 N110 Os2 128.5(6) . . ? C111 N110 Os2 115.5(5) . . ? N110 C111 C112 124.5(7) . . ? N110 C111 C114 114.6(7) . . ? C112 C111 C114 120.9(7) . . ? C111 C112 C107 117.8(7) . . ? C111 C112 C106 118.9(7) . . ? C107 C112 C106 123.3(7) . . ? C114 C113 C105 118.6(7) . . ? C114 C113 C104 117.1(7) . . ? C105 C113 C104 124.3(8) . . ? N101 C114 C113 124.2(7) . . ? N101 C114 C111 116.5(7) . . ? C113 C114 C111 119.3(7) . . ? N30 Os1 N10 92.0(2) . . ? N30 Os1 N41 173.7(2) . . ? N10 Os1 N41 92.8(2) . . ? N30 Os1 N21 79.9(2) . . ? N10 Os1 N21 169.6(2) . . ? N41 Os1 N21 95.8(2) . . ? N30 Os1 N50 96.5(2) . . ? N10 Os1 N50 97.7(3) . . ? N41 Os1 N50 78.7(2) . . ? N21 Os1 N50 89.6(2) . . ? N30 Os1 N1 88.4(2) . . ? N10 Os1 N1 79.6(3) . . ? N41 Os1 N1 96.6(2) . . ? N21 Os1 N1 93.7(2) . . ? N50 Os1 N1 174.5(2) . . ? N90 Os2 N110 89.2(2) . . ? N90 Os2 N70 170.4(2) . . ? N110 Os2 N70 99.4(2) . . ? N90 Os2 N61 92.6(2) . . ? N110 Os2 N61 174.3(3) . . ? N70 Os2 N61 79.2(2) . . ? N90 Os2 N101 97.5(3) . . ? N110 Os2 N101 78.8(3) . . ? N70 Os2 N101 88.3(3) . . ? N61 Os2 N101 95.6(3) . . ? N90 Os2 N81 79.9(3) . . ? N110 Os2 N81 93.2(3) . . ? N70 Os2 N81 95.3(3) . . ? N61 Os2 N81 92.4(3) . . ? N101 Os2 N81 171.7(2) . . ? F15 P1 F14 90.2(3) . . ? F15 P1 F11 90.3(3) . . ? F14 P1 F11 179.5(3) . . ? F15 P1 F16 90.6(3) . . ? F14 P1 F16 89.7(3) . . ? F11 P1 F16 90.2(3) . . ? F15 P1 F13 90.0(3) . . ? F14 P1 F13 89.9(3) . . ? F11 P1 F13 90.2(3) . . ? F16 P1 F13 179.2(3) . . ? F15 P1 F12 179.8(3) . . ? F14 P1 F12 89.7(3) . . ? F11 P1 F12 89.8(3) . . ? F16 P1 F12 89.2(3) . . ? F13 P1 F12 90.1(3) . . ? F23 P2 F22 89.9(3) . . ? F23 P2 F24 89.6(3) . . ? F22 P2 F24 89.1(3) . . ? F23 P2 F25 89.8(3) . . ? F22 P2 F25 179.6(3) . . ? F24 P2 F25 90.6(3) . . ? F23 P2 F26 179.4(3) . . ? F22 P2 F26 90.6(3) . . ? F24 P2 F26 90.3(3) . . ? F25 P2 F26 89.7(3) . . ? F23 P2 F21 90.4(3) . . ? F22 P2 F21 90.6(3) . . ? F24 P2 F21 179.7(3) . . ? F25 P2 F21 89.7(3) . . ? F26 P2 F21 89.8(3) . . ? F34 P3 F31 179.4(3) . . ? F34 P3 F36 91.1(3) . . ? F31 P3 F36 89.5(3) . . ? F34 P3 F35 90.6(3) . . ? F31 P3 F35 89.3(3) . . ? F36 P3 F35 90.0(3) . . ? F34 P3 F33 89.2(3) . . ? F31 P3 F33 90.2(3) . . ? F36 P3 F33 179.6(3) . . ? F35 P3 F33 90.4(3) . . ? F34 P3 F32 90.1(3) . . ? F31 P3 F32 90.0(3) . . ? F36 P3 F32 89.8(3) . . ? F35 P3 F32 179.2(3) . . ? F33 P3 F32 89.9(3) . . ? F41 P4 F44 179.5(3) . . ? F41 P4 F45 90.5(3) . . ? F44 P4 F45 90.0(3) . . ? F41 P4 F43 90.7(3) . . ? F44 P4 F43 89.2(3) . . ? F45 P4 F43 90.8(3) . . ? F41 P4 F42 89.6(3) . . ? F44 P4 F42 90.0(3) . . ? F45 P4 F42 179.8(4) . . ? F43 P4 F42 89.0(3) . . ? F41 P4 F46 90.2(4) . . ? F44 P4 F46 89.9(3) . . ? F45 P4 F46 90.4(3) . . ? F43 P4 F46 178.6(3) . . ? F42 P4 F46 89.8(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.770 _refine_diff_density_min -1.351 _refine_diff_density_rms 0.180 data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 249783' # data_461602a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H48 F24 N12 P4 Ru2' _chemical_formula_weight 1863.24 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' 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.1694(16) _cell_length_b 17.940(2) _cell_length_c 32.024(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7566.1(15) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 27.91 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9429 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47632 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1853 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.91 _reflns_number_total 17473 _reflns_number_gt 7879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.040(16) _refine_ls_number_reflns 17473 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 0.648 _refine_ls_restrained_S_all 0.648 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4641(3) 0.62472(16) 0.98844(10) 0.0460(9) Uani 1 1 d . . . C2 C 0.3871(3) 0.6525(2) 0.96814(14) 0.0580(13) Uani 1 1 d . . . H2 H 0.3223 0.6357 0.9749 0.070 Uiso 1 1 calc R . . C3 C 0.3969(4) 0.7065(3) 0.93663(16) 0.0729(16) Uani 1 1 d . . . H3 H 0.3399 0.7235 0.9224 0.087 Uiso 1 1 calc R . . C4 C 0.4900(4) 0.7334(2) 0.92713(15) 0.0754(16) Uani 1 1 d . . . H4 H 0.4977 0.7685 0.9060 0.091 Uiso 1 1 calc R . . C5 C 0.6768(4) 0.7309(3) 0.94173(16) 0.0800(18) Uani 1 1 d . . . H5 H 0.6890 0.7651 0.9204 0.096 Uiso 1 1 calc R . . C6 C 0.7540(4) 0.7062(2) 0.96337(16) 0.0765(16) Uani 1 1 d . . . H6 H 0.8186 0.7248 0.9580 0.092 Uiso 1 1 calc R . . C7 C 0.8186(3) 0.6186(2) 1.01911(15) 0.0660(15) Uani 1 1 d . . . H7 H 0.8854 0.6339 1.0152 0.079 Uiso 1 1 calc R . . C8 C 0.7969(3) 0.5651(3) 1.04790(15) 0.0662(16) Uani 1 1 d . . . H8 H 0.8478 0.5451 1.0646 0.079 Uiso 1 1 calc R . . C9 C 0.6973(3) 0.5412(2) 1.05173(14) 0.0566(13) Uani 1 1 d . . . H9 H 0.6838 0.5032 1.0707 0.068 Uiso 1 1 calc R . . N10 N 0.6209(2) 0.56864(16) 1.03044(11) 0.0448(9) Uani 1 1 d . . . C11 C 0.6418(3) 0.6240(2) 1.00215(13) 0.0439(12) Uani 1 1 d . . . C12 C 0.5586(3) 0.6529(2) 0.97948(13) 0.0443(12) Uani 1 1 d . . . C13 C 0.5747(4) 0.7079(2) 0.94936(15) 0.0578(14) Uani 1 1 d . . . C14 C 0.7405(3) 0.6507(2) 0.99530(13) 0.0487(12) Uani 1 1 d . . . N15 N 0.5030(2) 0.46214(18) 0.98234(9) 0.0457(9) Uani 1 1 d . . . C16 C 0.5071(3) 0.4737(2) 0.94160(12) 0.0588(13) Uani 1 1 d . . . H16 H 0.4957 0.5216 0.9315 0.071 Uiso 1 1 calc R . . C17 C 0.5277(4) 0.4171(3) 0.91334(14) 0.0724(15) Uani 1 1 d . . . H17 H 0.5292 0.4271 0.8848 0.087 Uiso 1 1 calc R . . C18 C 0.5457(3) 0.3473(3) 0.92745(15) 0.0680(14) Uani 1 1 d . . . H18 H 0.5571 0.3090 0.9085 0.082 Uiso 1 1 calc R . . C19 C 0.5665(3) 0.2615(2) 0.98862(17) 0.0705(16) Uani 1 1 d . . . H19 H 0.5787 0.2207 0.9714 0.085 Uiso 1 1 calc R . . C20 C 0.5676(3) 0.2520(2) 1.02995(17) 0.0706(15) Uani 1 1 d . . . H20 H 0.5832 0.2053 1.0409 0.085 Uiso 1 1 calc R . . C21 C 0.5429(3) 0.3054(2) 1.10101(15) 0.0647(14) Uani 1 1 d . . . H21 H 0.5582 0.2602 1.1137 0.078 Uiso 1 1 calc R . . C22 C 0.5178(4) 0.3661(2) 1.12504(14) 0.0619(14) Uani 1 1 d . . . H22 H 0.5165 0.3624 1.1540 0.074 Uiso 1 1 calc R . . C23 C 0.4945(3) 0.4332(2) 1.10544(13) 0.0524(13) Uani 1 1 d . . . H23 H 0.4767 0.4737 1.1220 0.063 Uiso 1 1 calc R . . N24 N 0.4962(2) 0.44238(15) 1.06460(10) 0.0415(9) Uani 1 1 d . . . C25 C 0.5212(3) 0.3810(2) 1.04084(12) 0.0420(11) Uani 1 1 d . . . C26 C 0.5242(3) 0.3919(2) 0.99637(13) 0.0448(11) Uani 1 1 d . . . C27 C 0.5471(3) 0.3324(3) 0.96993(15) 0.0547(12) Uani 1 1 d . . . C28 C 0.5454(3) 0.3117(2) 1.05751(14) 0.0482(12) Uani 1 1 d . . . N29 N 0.3163(2) 0.51477(17) 1.03055(12) 0.0493(10) Uani 1 1 d . . . C30 C 0.2618(4) 0.4741(2) 1.00420(14) 0.0606(13) Uani 1 1 d . . . H30 H 0.2932 0.4542 0.9807 0.073 Uiso 1 1 calc R . . C31 C 0.1575(4) 0.4603(3) 1.01078(17) 0.0747(16) Uani 1 1 d . . . H31 H 0.1210 0.4321 0.9916 0.090 Uiso 1 1 calc R . . C32 C 0.1107(4) 0.4880(3) 1.04506(18) 0.0758(18) Uani 1 1 d . . . H32 H 0.0428 0.4771 1.0502 0.091 Uiso 1 1 calc R . . C33 C 0.1237(4) 0.5666(3) 1.10893(17) 0.0737(17) Uani 1 1 d . . . H33 H 0.0568 0.5563 1.1162 0.088 Uiso 1 1 calc R . . C34 C 0.1776(4) 0.6119(3) 1.13266(16) 0.0754(17) Uani 1 1 d . . . H34 H 0.1461 0.6342 1.1555 0.091 Uiso 1 1 calc R . . C35 C 0.3432(4) 0.6764(2) 1.14695(14) 0.0665(14) Uani 1 1 d . . . H35 H 0.3165 0.7013 1.1700 0.080 Uiso 1 1 calc R . . C36 C 0.4404(4) 0.6882(2) 1.13588(14) 0.0633(15) Uani 1 1 d . . . H36 H 0.4806 0.7213 1.1509 0.076 Uiso 1 1 calc R . . C37 C 0.4810(4) 0.6492(2) 1.10092(13) 0.0581(13) Uani 1 1 d . . . H37 H 0.5484 0.6573 1.0935 0.070 Uiso 1 1 calc R . . N38 N 0.4265(3) 0.60220(17) 1.07883(11) 0.0463(10) Uani 1 1 d . . . C39 C 0.3260(3) 0.5921(2) 1.08980(14) 0.0466(12) Uani 1 1 d . . . C40 C 0.2686(3) 0.5459(2) 1.06375(14) 0.0448(11) Uani 1 1 d . . . C41 C 0.1652(4) 0.5333(3) 1.07271(16) 0.0581(13) Uani 1 1 d . . . C42 C 0.2831(4) 0.6285(2) 1.12488(14) 0.0514(12) Uani 1 1 d . . . Ru43 Ru 0.47064(3) 0.537164(18) 1.029325(11) 0.04271(10) Uani 1 1 d . . . N51 N 0.2671(2) 0.23716(18) 0.15434(10) 0.0454(9) Uani 1 1 d . . . C52 C 0.2529(3) 0.3091(2) 0.15374(14) 0.0606(14) Uani 1 1 d . . . H52 H 0.2399 0.3336 0.1788 0.073 Uiso 1 1 calc R . . C53 C 0.2565(3) 0.3511(2) 0.11666(16) 0.0683(15) Uani 1 1 d . . . H53 H 0.2456 0.4023 0.1173 0.082 Uiso 1 1 calc R . . C54 C 0.2761(4) 0.3158(3) 0.07966(16) 0.0750(16) Uani 1 1 d . . . H54 H 0.2795 0.3433 0.0551 0.090 Uiso 1 1 calc R . . C55 C 0.3112(4) 0.1968(3) 0.04201(15) 0.0796(18) Uani 1 1 d . . . H55 H 0.3196 0.2211 0.0166 0.096 Uiso 1 1 calc R . . C56 C 0.3181(4) 0.1225(4) 0.04358(17) 0.0885(19) Uani 1 1 d . . . H56 H 0.3300 0.0966 0.0189 0.106 Uiso 1 1 calc R . . C57 C 0.3107(4) 0.0045(3) 0.0845(2) 0.101(2) Uani 1 1 d . . . H57 H 0.3230 -0.0244 0.0609 0.121 Uiso 1 1 calc R . . C58 C 0.2955(4) -0.0286(3) 0.12199(19) 0.0932(19) Uani 1 1 d . . . H58 H 0.2948 -0.0803 0.1242 0.112 Uiso 1 1 calc R . . C59 C 0.2807(4) 0.0158(3) 0.15735(17) 0.0766(16) Uani 1 1 d . . . H59 H 0.2705 -0.0075 0.1829 0.092 Uiso 1 1 calc R . . N60 N 0.2806(3) 0.08921(18) 0.15609(11) 0.0512(10) Uani 1 1 d . . . C61 C 0.2919(3) 0.1218(2) 0.11777(14) 0.0482(12) Uani 1 1 d . . . C62 C 0.2851(3) 0.2010(2) 0.11689(13) 0.0473(12) Uani 1 1 d . . . C63 C 0.2912(3) 0.2393(3) 0.07855(15) 0.0581(13) Uani 1 1 d . . . C64 C 0.3080(4) 0.0815(3) 0.08124(17) 0.0703(15) Uani 1 1 d . . . N65 N 0.1146(2) 0.15004(17) 0.20860(10) 0.0396(9) Uani 1 1 d . . . C66 C 0.0417(3) 0.1869(2) 0.18863(12) 0.0491(12) Uani 1 1 d . . . H66 H 0.0601 0.2244 0.1700 0.059 Uiso 1 1 calc R . . C67 C -0.0603(3) 0.1719(3) 0.19432(14) 0.0609(14) Uani 1 1 d . . . H67 H -0.1091 0.1993 0.1800 0.073 Uiso 1 1 calc R . . C68 C -0.0892(4) 0.1162(3) 0.22123(15) 0.0691(15) Uani 1 1 d . . . H68 H -0.1575 0.1045 0.2247 0.083 Uiso 1 1 calc R . . C69 C -0.0356(4) 0.0198(2) 0.27292(15) 0.0701(15) Uani 1 1 d . . . H69 H -0.1027 0.0066 0.2781 0.084 Uiso 1 1 calc R . . C70 C 0.0393(4) -0.0155(2) 0.29319(15) 0.0698(14) Uani 1 1 d . . . H70 H 0.0233 -0.0531 0.3121 0.084 Uiso 1 1 calc R . . C71 C 0.2259(4) -0.0315(3) 0.30517(15) 0.0832(16) Uani 1 1 d . . . H71 H 0.2146 -0.0705 0.3237 0.100 Uiso 1 1 calc R . . C72 C 0.3217(4) -0.0100(3) 0.29692(18) 0.100(2) Uani 1 1 d . . . H72 H 0.3768 -0.0333 0.3095 0.120 Uiso 1 1 calc R . . C73 C 0.3359(3) 0.0499(3) 0.26804(15) 0.0818(17) Uani 1 1 d . . . H73 H 0.4018 0.0658 0.2625 0.098 Uiso 1 1 calc R . . N74 N 0.2613(3) 0.08321(18) 0.24910(10) 0.0509(10) Uani 1 1 d . . . C75 C 0.1646(3) 0.0611(2) 0.25795(13) 0.0508(13) Uani 1 1 d . . . C76 C 0.0854(3) 0.0964(2) 0.23603(13) 0.0414(11) Uani 1 1 d . . . C77 C -0.0139(3) 0.0773(2) 0.24350(13) 0.0481(12) Uani 1 1 d . . . C78 C 0.1434(4) 0.0036(2) 0.28636(14) 0.0559(13) Uani 1 1 d . . . N79 N 0.2774(3) 0.24381(19) 0.25107(10) 0.0517(10) Uani 1 1 d . . . C80 C 0.2024(4) 0.2714(2) 0.27365(14) 0.0611(14) Uani 1 1 d . . . H80 H 0.1364 0.2569 0.2674 0.073 Uiso 1 1 calc R . . C81 C 0.2178(4) 0.3219(3) 0.30679(14) 0.0721(15) Uani 1 1 d . . . H81 H 0.1631 0.3384 0.3226 0.087 Uiso 1 1 calc R . . C82 C 0.3123(4) 0.3461(3) 0.31540(15) 0.0733(16) Uani 1 1 d . . . H82 H 0.3232 0.3797 0.3370 0.088 Uiso 1 1 calc R . . C83 C 0.4978(4) 0.3435(3) 0.29719(16) 0.0758(16) Uani 1 1 d . . . H83 H 0.5145 0.3786 0.3174 0.091 Uiso 1 1 calc R . . C84 C 0.5705(4) 0.3140(3) 0.27279(18) 0.0762(18) Uani 1 1 d . . . H84 H 0.6367 0.3308 0.2765 0.091 Uiso 1 1 calc R . . C85 C 0.6271(4) 0.2262(3) 0.21791(17) 0.0832(19) Uani 1 1 d . . . H85 H 0.6948 0.2401 0.2208 0.100 Uiso 1 1 calc R . . C86 C 0.6000(4) 0.1728(3) 0.18986(16) 0.0827(18) Uani 1 1 d . . . H86 H 0.6497 0.1508 0.1733 0.099 Uiso 1 1 calc R . . C87 C 0.4986(3) 0.1505(3) 0.18537(14) 0.0697(16) Uani 1 1 d . . . H87 H 0.4825 0.1130 0.1665 0.084 Uiso 1 1 calc R . . N88 N 0.4252(3) 0.1821(2) 0.20763(12) 0.0547(11) Uani 1 1 d . . . C89 C 0.4519(4) 0.2373(2) 0.23590(14) 0.0518(13) Uani 1 1 d . . . C90 C 0.3735(4) 0.2680(2) 0.26031(14) 0.0528(13) Uani 1 1 d . . . C91 C 0.3932(4) 0.3203(3) 0.29171(16) 0.0606(13) Uani 1 1 d . . . C92 C 0.5531(4) 0.2594(3) 0.24207(17) 0.0651(15) Uani 1 1 d . . . Ru93 Ru 0.26987(3) 0.16480(2) 0.204296(11) 0.04679(10) Uani 1 1 d . . . P1 P 0.36012(10) 0.49694(7) 0.21971(4) 0.0595(4) Uani 1 1 d . . . F2 F 0.4203(2) 0.42169(14) 0.21158(9) 0.1012(10) Uani 1 1 d . . . F3 F 0.2758(2) 0.45198(18) 0.24105(12) 0.1421(14) Uani 1 1 d . . . F4 F 0.4189(3) 0.50617(15) 0.26076(9) 0.1228(12) Uani 1 1 d . . . F5 F 0.2996(2) 0.57099(14) 0.22503(9) 0.1032(11) Uani 1 1 d . . . F6 F 0.44307(19) 0.54028(16) 0.19454(10) 0.1051(10) Uani 1 1 d . . . F7 F 0.3024(2) 0.48707(15) 0.17618(10) 0.1189(12) Uani 1 1 d . . . P11 P 0.10309(12) 0.82326(10) 0.19562(6) 0.0885(5) Uani 1 1 d . . . F12 F 0.0318(3) 0.75977(19) 0.17944(12) 0.1553(15) Uani 1 1 d . . . F13 F 0.1676(3) 0.7600(2) 0.21715(12) 0.1472(14) Uani 1 1 d . . . F14 F 0.0336(3) 0.8314(2) 0.23409(11) 0.1472(14) Uani 1 1 d . . . F15 F 0.1766(3) 0.8836(2) 0.21171(13) 0.1517(15) Uani 1 1 d . . . F16 F 0.0415(3) 0.8811(2) 0.17272(15) 0.197(2) Uani 1 1 d . . . F17 F 0.1729(3) 0.8128(2) 0.15682(12) 0.1547(15) Uani 1 1 d . . . P21 P 0.57839(13) 0.85872(10) 0.06000(6) 0.0911(5) Uani 1 1 d . . . F22 F 0.5055(2) 0.79772(18) 0.03949(12) 0.1434(14) Uani 1 1 d . . . F23 F 0.6443(3) 0.7944(2) 0.07812(14) 0.1736(18) Uani 1 1 d . . . F24 F 0.5138(3) 0.8570(2) 0.09943(11) 0.1876(18) Uani 1 1 d . . . F25 F 0.6545(3) 0.9163(2) 0.07773(12) 0.1665(16) Uani 1 1 d . . . F26 F 0.5114(2) 0.92238(18) 0.04146(10) 0.1297(12) Uani 1 1 d . . . F27 F 0.6414(3) 0.8594(2) 0.01880(12) 0.1478(15) Uani 1 1 d . . . P31 P 0.86863(12) 0.34216(9) 0.09160(5) 0.0766(4) Uani 1 1 d . . . F32 F 0.8467(3) 0.26402(16) 0.07263(11) 0.1373(14) Uani 1 1 d . . . F33 F 0.8105(4) 0.3196(2) 0.13118(11) 0.184(2) Uani 1 1 d . . . F34 F 0.9697(3) 0.31474(19) 0.10930(13) 0.1736(17) Uani 1 1 d . . . F35 F 0.8918(3) 0.42219(15) 0.10952(9) 0.1202(12) Uani 1 1 d . . . F36 F 0.9231(2) 0.36533(17) 0.05054(9) 0.1196(12) Uani 1 1 d . . . F37 F 0.7688(3) 0.37156(18) 0.07270(14) 0.1592(15) 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 N1 0.039(2) 0.047(2) 0.051(2) 0.0044(17) 0.001(2) 0.011(2) C2 0.050(3) 0.061(3) 0.063(3) 0.009(3) 0.009(3) 0.002(3) C3 0.056(3) 0.082(4) 0.081(4) 0.025(3) 0.002(3) 0.012(3) C4 0.081(4) 0.067(3) 0.078(4) 0.033(3) 0.013(3) 0.007(3) C5 0.093(5) 0.072(4) 0.076(4) 0.032(3) 0.017(4) 0.000(3) C6 0.079(4) 0.065(3) 0.085(4) 0.010(3) 0.033(4) -0.011(3) C7 0.034(3) 0.077(3) 0.087(4) -0.004(3) 0.008(3) -0.007(3) C8 0.040(3) 0.084(4) 0.074(4) 0.016(3) -0.010(3) -0.004(3) C9 0.050(3) 0.053(3) 0.067(3) 0.017(3) 0.010(3) 0.008(3) N10 0.044(2) 0.040(2) 0.051(2) 0.0004(19) 0.006(2) -0.0016(18) C11 0.046(3) 0.041(3) 0.045(3) 0.000(2) 0.008(2) -0.004(2) C12 0.046(3) 0.036(3) 0.051(3) -0.002(2) 0.003(2) 0.000(2) C13 0.054(3) 0.054(3) 0.065(4) 0.016(3) 0.014(3) -0.008(3) C14 0.042(3) 0.048(3) 0.056(3) -0.003(2) 0.013(3) -0.005(3) N15 0.046(2) 0.0446(19) 0.046(2) -0.0030(19) 0.0073(17) -0.0050(19) C16 0.073(4) 0.063(3) 0.041(3) -0.005(2) 0.004(3) -0.004(3) C17 0.086(4) 0.092(4) 0.039(3) -0.007(3) 0.005(3) -0.024(4) C18 0.061(3) 0.078(4) 0.064(4) -0.031(3) 0.015(3) -0.018(3) C19 0.074(4) 0.048(3) 0.089(4) -0.028(3) 0.020(3) -0.002(3) C20 0.078(4) 0.047(3) 0.086(4) -0.001(3) 0.000(4) 0.002(3) C21 0.060(3) 0.057(3) 0.077(4) 0.019(3) -0.006(3) -0.006(3) C22 0.080(4) 0.054(3) 0.052(3) -0.001(3) 0.008(3) -0.010(3) C23 0.065(3) 0.052(3) 0.041(3) -0.005(2) 0.006(3) -0.003(2) N24 0.043(2) 0.038(2) 0.044(2) -0.0069(17) 0.0010(18) -0.0054(16) C25 0.031(2) 0.042(3) 0.053(3) -0.006(2) 0.005(2) -0.003(2) C26 0.032(2) 0.054(3) 0.048(3) -0.005(2) 0.009(2) -0.008(2) C27 0.041(3) 0.065(3) 0.058(3) -0.013(3) 0.005(3) -0.010(3) C28 0.043(3) 0.037(3) 0.065(3) 0.005(2) 0.007(3) -0.003(2) N29 0.043(2) 0.042(2) 0.063(3) 0.004(2) -0.002(2) -0.0054(18) C30 0.066(3) 0.052(3) 0.064(3) 0.000(2) -0.015(3) -0.013(3) C31 0.052(3) 0.063(3) 0.109(5) 0.012(3) -0.019(3) -0.019(3) C32 0.037(3) 0.069(4) 0.121(5) 0.032(3) 0.003(3) 0.001(3) C33 0.043(3) 0.082(4) 0.097(5) 0.041(3) 0.022(3) 0.010(3) C34 0.069(4) 0.078(4) 0.079(4) 0.026(3) 0.032(3) 0.026(3) C35 0.081(4) 0.060(3) 0.058(3) -0.002(3) 0.009(3) 0.021(3) C36 0.072(4) 0.054(3) 0.065(3) -0.007(3) 0.004(3) -0.008(3) C37 0.052(3) 0.054(3) 0.068(3) -0.008(3) 0.011(3) -0.006(3) N38 0.044(2) 0.039(2) 0.055(2) 0.0049(18) 0.003(2) -0.0057(18) C39 0.042(3) 0.039(3) 0.058(3) 0.022(2) 0.004(3) 0.014(2) C40 0.032(3) 0.047(3) 0.055(3) 0.019(2) 0.010(2) -0.004(3) C41 0.049(3) 0.051(3) 0.074(4) 0.033(3) 0.006(3) 0.006(3) C42 0.043(3) 0.051(3) 0.060(3) 0.016(2) 0.015(3) 0.023(3) Ru43 0.0411(2) 0.04102(19) 0.0460(2) 0.00078(19) 0.0035(2) -0.00332(19) N51 0.037(2) 0.048(2) 0.051(2) 0.0124(19) -0.005(2) 0.001(2) C52 0.064(4) 0.047(3) 0.070(3) 0.016(3) -0.014(3) -0.004(3) C53 0.072(4) 0.040(3) 0.094(4) 0.029(3) -0.028(3) -0.016(3) C54 0.071(3) 0.081(4) 0.073(4) 0.038(3) -0.023(3) -0.033(3) C55 0.078(4) 0.127(5) 0.034(3) 0.015(3) 0.005(3) -0.014(4) C56 0.073(4) 0.135(5) 0.058(4) -0.033(4) 0.017(3) -0.023(4) C57 0.111(5) 0.090(5) 0.101(5) -0.024(4) 0.031(4) 0.001(4) C58 0.099(5) 0.062(4) 0.118(5) -0.013(4) 0.027(4) 0.025(4) C59 0.084(4) 0.055(3) 0.092(4) 0.012(3) 0.020(4) 0.007(3) N60 0.044(2) 0.047(2) 0.063(3) 0.014(2) 0.015(2) 0.003(2) C61 0.044(3) 0.053(3) 0.048(3) -0.004(3) 0.007(2) -0.002(2) C62 0.034(3) 0.065(3) 0.044(3) 0.006(3) 0.003(2) -0.015(2) C63 0.047(3) 0.076(4) 0.050(3) 0.019(3) -0.004(3) -0.017(3) C64 0.064(4) 0.081(4) 0.065(4) -0.010(4) 0.021(3) -0.009(3) N65 0.0318(19) 0.047(2) 0.039(2) 0.0041(19) 0.0002(18) 0.0055(18) C66 0.052(3) 0.050(3) 0.045(3) -0.001(2) 0.001(3) 0.000(3) C67 0.037(3) 0.081(4) 0.065(3) 0.009(3) -0.013(2) 0.009(3) C68 0.042(3) 0.091(4) 0.074(4) 0.000(3) 0.003(3) -0.008(3) C69 0.048(3) 0.083(4) 0.079(4) 0.018(3) 0.019(3) -0.024(3) C70 0.068(3) 0.075(3) 0.067(3) 0.032(3) 0.021(3) -0.005(3) C71 0.079(4) 0.097(4) 0.074(4) 0.047(3) 0.016(3) -0.001(4) C72 0.056(4) 0.141(5) 0.103(4) 0.079(4) -0.004(4) -0.004(4) C73 0.036(3) 0.114(4) 0.095(4) 0.048(4) 0.002(3) 0.004(3) N74 0.024(2) 0.076(3) 0.053(2) 0.022(2) 0.000(2) 0.003(2) C75 0.048(3) 0.070(3) 0.034(3) 0.008(2) 0.013(2) 0.004(3) C76 0.041(3) 0.052(3) 0.031(3) 0.004(2) 0.002(2) 0.004(2) C77 0.032(3) 0.062(3) 0.051(3) 0.005(2) 0.001(2) 0.003(3) C78 0.048(3) 0.071(3) 0.048(3) 0.025(3) 0.010(3) 0.008(3) N79 0.036(2) 0.071(3) 0.048(2) 0.010(2) -0.003(2) 0.002(2) C80 0.048(3) 0.082(4) 0.054(3) 0.000(3) -0.003(3) -0.002(3) C81 0.069(4) 0.088(4) 0.059(3) -0.010(3) 0.005(3) -0.003(3) C82 0.068(4) 0.089(4) 0.063(4) -0.006(3) -0.013(3) -0.013(4) C83 0.077(4) 0.075(4) 0.076(4) 0.022(3) -0.026(3) -0.017(3) C84 0.038(3) 0.084(4) 0.106(5) 0.039(4) -0.032(3) -0.014(3) C85 0.035(3) 0.122(5) 0.093(5) 0.039(4) -0.012(3) -0.005(3) C86 0.045(3) 0.126(5) 0.077(4) 0.033(4) 0.021(3) 0.028(4) C87 0.044(3) 0.095(4) 0.070(3) 0.029(3) 0.011(3) 0.020(3) N88 0.045(2) 0.067(3) 0.052(2) 0.032(2) 0.010(2) 0.012(2) C89 0.040(3) 0.057(3) 0.059(3) 0.024(3) -0.007(3) -0.002(3) C90 0.040(3) 0.067(3) 0.051(3) 0.022(3) -0.009(3) -0.006(3) C91 0.056(3) 0.066(3) 0.060(3) 0.013(3) -0.027(3) -0.010(3) C92 0.034(3) 0.079(4) 0.082(4) 0.030(3) -0.004(3) 0.004(3) Ru93 0.0376(2) 0.0587(2) 0.0440(2) 0.0121(2) 0.00338(19) 0.0025(2) P1 0.0475(8) 0.0611(9) 0.0699(10) 0.0079(7) -0.0006(8) 0.0051(8) F2 0.119(2) 0.0814(18) 0.103(2) 0.0169(18) -0.005(2) 0.0417(18) F3 0.067(2) 0.147(3) 0.212(4) 0.105(3) 0.026(2) -0.010(2) F4 0.162(3) 0.124(2) 0.082(2) -0.0096(18) -0.051(2) -0.008(2) F5 0.124(3) 0.0799(19) 0.106(2) 0.0004(17) 0.026(2) 0.0419(19) F6 0.0583(18) 0.124(2) 0.133(3) 0.046(2) 0.0071(18) -0.0021(18) F7 0.149(3) 0.085(2) 0.123(3) 0.0065(19) -0.067(2) 0.009(2) P11 0.0602(10) 0.0932(13) 0.1120(15) -0.0105(12) 0.0077(11) 0.0048(11) F12 0.109(3) 0.167(3) 0.190(4) -0.072(3) -0.012(3) -0.024(3) F13 0.108(3) 0.162(3) 0.172(4) 0.048(3) 0.000(3) 0.014(2) F14 0.126(3) 0.161(3) 0.155(3) -0.069(3) 0.068(3) -0.036(3) F15 0.123(3) 0.158(3) 0.174(4) -0.048(3) 0.024(3) -0.065(2) F16 0.155(4) 0.174(4) 0.263(5) 0.065(4) -0.016(4) 0.083(3) F17 0.156(3) 0.176(4) 0.132(3) 0.012(3) 0.062(3) 0.023(3) P21 0.0607(10) 0.1304(15) 0.0821(12) 0.0253(11) -0.0079(10) -0.0140(11) F22 0.095(3) 0.157(3) 0.178(4) 0.009(3) -0.040(3) -0.011(2) F23 0.108(3) 0.172(3) 0.241(5) 0.094(3) -0.079(3) -0.010(3) F24 0.195(4) 0.248(4) 0.119(3) 0.025(3) 0.080(3) 0.005(4) F25 0.194(4) 0.159(3) 0.147(3) -0.004(3) -0.070(3) -0.067(3) F26 0.098(3) 0.164(3) 0.127(3) 0.021(2) -0.003(2) 0.029(2) F27 0.118(3) 0.185(4) 0.140(3) 0.026(3) 0.034(3) -0.003(3) P31 0.0876(12) 0.0797(11) 0.0624(10) -0.0025(9) 0.0058(9) 0.0211(10) F32 0.161(3) 0.089(2) 0.161(3) -0.041(2) 0.007(3) -0.014(2) F33 0.318(6) 0.112(3) 0.123(3) 0.022(2) 0.124(3) 0.021(3) F34 0.193(4) 0.144(3) 0.183(4) -0.021(3) -0.104(3) 0.073(3) F35 0.177(3) 0.089(2) 0.095(2) -0.0170(19) 0.014(2) 0.010(2) F36 0.125(3) 0.168(3) 0.066(2) -0.0234(19) 0.0188(19) -0.035(2) F37 0.082(2) 0.136(3) 0.260(5) 0.037(3) -0.016(3) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.304(5) . ? N1 C12 1.374(5) . ? N1 Ru43 2.047(3) . ? C2 C3 1.405(6) . ? C3 C4 1.352(6) . ? C4 C13 1.401(6) . ? C5 C6 1.307(6) . ? C5 C13 1.428(6) . ? C6 C14 1.438(6) . ? C7 C8 1.361(5) . ? C7 C14 1.404(5) . ? C8 C9 1.385(5) . ? C9 N10 1.311(5) . ? N10 C11 1.372(5) . ? N10 Ru43 2.059(3) . ? C11 C14 1.403(5) . ? C11 C12 1.413(5) . ? C12 C13 1.396(5) . ? N15 C16 1.322(4) . ? N15 C26 1.367(5) . ? N15 Ru43 2.063(3) . ? C16 C17 1.387(5) . ? C17 C18 1.352(6) . ? C18 C27 1.387(6) . ? C19 C20 1.335(6) . ? C19 C27 1.428(6) . ? C20 C28 1.418(5) . ? C21 C22 1.373(5) . ? C21 C28 1.398(5) . ? C22 C23 1.392(5) . ? C23 N24 1.319(4) . ? N24 C25 1.378(4) . ? N24 Ru43 2.069(3) . ? C25 C28 1.391(5) . ? C25 C26 1.438(5) . ? C26 C27 1.396(5) . ? N29 C30 1.327(5) . ? N29 C40 1.355(5) . ? N29 Ru43 2.072(3) . ? C30 C31 1.411(6) . ? C31 C32 1.354(6) . ? C32 C41 1.398(6) . ? C33 C34 1.320(6) . ? C33 C41 1.414(6) . ? C34 C42 1.442(6) . ? C35 C36 1.345(6) . ? C35 C42 1.366(6) . ? C36 C37 1.424(5) . ? C37 N38 1.315(5) . ? N38 C39 1.380(5) . ? N38 Ru43 2.053(3) . ? C39 C40 1.399(5) . ? C39 C42 1.417(6) . ? C40 C41 1.410(6) . ? N51 C52 1.305(4) . ? N51 C62 1.384(5) . ? N51 Ru93 2.061(3) . ? C52 C53 1.407(5) . ? C53 C54 1.368(6) . ? C54 C63 1.387(6) . ? C55 C56 1.338(6) . ? C55 C63 1.421(6) . ? C56 C64 1.419(7) . ? C57 C58 1.356(7) . ? C57 C64 1.385(6) . ? C58 C59 1.399(6) . ? C59 N60 1.318(5) . ? N60 C61 1.367(5) . ? N60 Ru93 2.060(3) . ? C61 C64 1.391(6) . ? C61 C62 1.425(5) . ? C62 C63 1.409(5) . ? N65 C66 1.330(4) . ? N65 C76 1.359(5) . ? N65 Ru93 2.066(3) . ? C66 C67 1.382(5) . ? C67 C68 1.373(6) . ? C68 C77 1.408(6) . ? C69 C70 1.339(6) . ? C69 C77 1.426(5) . ? C70 C78 1.430(6) . ? C71 C72 1.346(6) . ? C71 C78 1.393(6) . ? C72 C73 1.431(6) . ? C73 N74 1.300(5) . ? N74 C75 1.363(5) . ? N74 Ru93 2.053(3) . ? C75 C78 1.404(5) . ? C75 C76 1.408(5) . ? C76 C77 1.373(5) . ? N79 C80 1.321(5) . ? N79 C90 1.370(5) . ? N79 Ru93 2.065(3) . ? C80 C81 1.410(6) . ? C81 C82 1.345(6) . ? C82 C91 1.387(6) . ? C83 C84 1.345(6) . ? C83 C91 1.450(6) . ? C84 C92 1.407(6) . ? C85 C86 1.360(7) . ? C85 C92 1.380(7) . ? C86 C87 1.401(6) . ? C87 N88 1.328(5) . ? N88 C89 1.387(5) . ? N88 Ru93 2.072(3) . ? C89 C92 1.405(6) . ? C89 C90 1.407(6) . ? C90 C91 1.399(6) . ? P1 F3 1.533(3) . ? P1 F4 1.535(3) . ? P1 F5 1.558(3) . ? P1 F6 1.565(3) . ? P1 F2 1.587(3) . ? P1 F7 1.598(3) . ? P11 F16 1.507(4) . ? P11 F15 1.541(3) . ? P11 F14 1.542(3) . ? P11 F17 1.557(4) . ? P11 F12 1.565(3) . ? P11 F13 1.576(4) . ? P21 F24 1.523(4) . ? P21 F25 1.547(4) . ? P21 F23 1.556(4) . ? P21 F27 1.559(4) . ? P21 F26 1.560(3) . ? P21 F22 1.597(3) . ? P31 F33 1.535(3) . ? P31 F34 1.528(4) . ? P31 F37 1.541(4) . ? P31 F32 1.555(3) . ? P31 F36 1.555(3) . ? P31 F35 1.576(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C12 117.4(3) . . ? C2 N1 Ru43 130.2(3) . . ? C12 N1 Ru43 112.2(3) . . ? N1 C2 C3 123.4(4) . . ? C4 C3 C2 119.4(5) . . ? C3 C4 C13 119.4(4) . . ? C6 C5 C13 122.8(5) . . ? C5 C6 C14 121.1(5) . . ? C8 C7 C14 120.2(4) . . ? C7 C8 C9 118.5(4) . . ? N10 C9 C8 124.3(4) . . ? C9 N10 C11 117.5(4) . . ? C9 N10 Ru43 130.1(3) . . ? C11 N10 Ru43 112.3(3) . . ? N10 C11 C14 122.4(4) . . ? N10 C11 C12 116.7(4) . . ? C14 C11 C12 120.9(4) . . ? N1 C12 C13 122.8(4) . . ? N1 C12 C11 117.4(4) . . ? C13 C12 C11 119.8(4) . . ? C12 C13 C4 117.4(4) . . ? C12 C13 C5 117.8(4) . . ? C4 C13 C5 124.7(4) . . ? C11 C14 C7 117.0(4) . . ? C11 C14 C6 117.5(4) . . ? C7 C14 C6 125.5(4) . . ? C16 N15 C26 117.5(3) . . ? C16 N15 Ru43 128.7(3) . . ? C26 N15 Ru43 113.8(3) . . ? N15 C16 C17 122.4(4) . . ? C18 C17 C16 119.6(4) . . ? C17 C18 C27 120.6(4) . . ? C20 C19 C27 122.1(4) . . ? C19 C20 C28 121.2(4) . . ? C22 C21 C28 120.1(4) . . ? C21 C22 C23 119.1(4) . . ? N24 C23 C22 123.5(4) . . ? C23 N24 C25 116.9(3) . . ? C23 N24 Ru43 129.9(3) . . ? C25 N24 Ru43 113.2(3) . . ? N24 C25 C28 123.9(4) . . ? N24 C25 C26 116.4(4) . . ? C28 C25 C26 119.7(4) . . ? N15 C26 C27 123.4(4) . . ? N15 C26 C25 116.4(4) . . ? C27 C26 C25 120.2(4) . . ? C18 C27 C26 116.4(4) . . ? C18 C27 C19 125.9(5) . . ? C26 C27 C19 117.7(4) . . ? C25 C28 C21 116.7(4) . . ? C25 C28 C20 118.9(4) . . ? C21 C28 C20 124.4(4) . . ? C30 N29 C40 118.3(4) . . ? C30 N29 Ru43 128.7(3) . . ? C40 N29 Ru43 112.9(3) . . ? N29 C30 C31 121.9(5) . . ? C32 C31 C30 120.0(5) . . ? C31 C32 C41 119.6(5) . . ? C34 C33 C41 121.7(5) . . ? C33 C34 C42 123.1(5) . . ? C36 C35 C42 120.9(5) . . ? C35 C36 C37 119.2(4) . . ? N38 C37 C36 122.2(4) . . ? C37 N38 C39 118.1(4) . . ? C37 N38 Ru43 128.7(3) . . ? C39 N38 Ru43 113.2(3) . . ? N38 C39 C40 116.4(4) . . ? N38 C39 C42 121.6(4) . . ? C40 C39 C42 122.0(4) . . ? N29 C40 C39 117.5(4) . . ? N29 C40 C41 122.8(4) . . ? C39 C40 C41 119.8(5) . . ? C32 C41 C40 117.4(5) . . ? C32 C41 C33 124.5(5) . . ? C40 C41 C33 118.1(5) . . ? C35 C42 C39 118.0(4) . . ? C35 C42 C34 126.8(5) . . ? C39 C42 C34 115.2(5) . . ? N1 Ru43 N38 92.63(12) . . ? N1 Ru43 N10 80.86(14) . . ? N38 Ru43 N10 95.93(13) . . ? N1 Ru43 N15 92.45(13) . . ? N38 Ru43 N15 173.03(13) . . ? N10 Ru43 N15 89.58(12) . . ? N1 Ru43 N24 170.70(13) . . ? N38 Ru43 N24 95.26(12) . . ? N10 Ru43 N24 93.42(13) . . ? N15 Ru43 N24 80.12(13) . . ? N1 Ru43 N29 96.87(14) . . ? N38 Ru43 N29 79.48(14) . . ? N10 Ru43 N29 174.82(13) . . ? N15 Ru43 N29 95.17(13) . . ? N24 Ru43 N29 89.42(12) . . ? C52 N51 C62 118.4(4) . . ? C52 N51 Ru93 129.6(3) . . ? C62 N51 Ru93 112.0(3) . . ? N51 C52 C53 122.5(4) . . ? C54 C53 C52 119.3(4) . . ? C53 C54 C63 120.4(4) . . ? C56 C55 C63 121.1(5) . . ? C55 C56 C64 122.9(5) . . ? C58 C57 C64 120.0(6) . . ? C57 C58 C59 119.2(5) . . ? N60 C59 C58 123.1(5) . . ? C59 N60 C61 117.0(4) . . ? C59 N60 Ru93 129.4(3) . . ? C61 N60 Ru93 113.5(3) . . ? N60 C61 C64 123.3(4) . . ? N60 C61 C62 115.9(4) . . ? C64 C61 C62 120.8(4) . . ? N51 C62 C63 122.4(4) . . ? N51 C62 C61 117.5(4) . . ? C63 C62 C61 120.0(4) . . ? C54 C63 C62 116.9(5) . . ? C54 C63 C55 125.3(5) . . ? C62 C63 C55 117.8(4) . . ? C57 C64 C61 117.3(5) . . ? C57 C64 C56 125.3(6) . . ? C61 C64 C56 117.4(5) . . ? C66 N65 C76 117.3(3) . . ? C66 N65 Ru93 128.2(3) . . ? C76 N65 Ru93 114.5(3) . . ? N65 C66 C67 122.8(4) . . ? C68 C67 C66 119.6(4) . . ? C67 C68 C77 118.9(4) . . ? C70 C69 C77 121.0(4) . . ? C69 C70 C78 121.3(4) . . ? C72 C71 C78 121.1(4) . . ? C71 C72 C73 117.7(5) . . ? N74 C73 C72 123.3(4) . . ? C73 N74 C75 118.4(4) . . ? C73 N74 Ru93 127.7(3) . . ? C75 N74 Ru93 113.9(3) . . ? N74 C75 C78 122.3(4) . . ? N74 C75 C76 117.2(4) . . ? C78 C75 C76 120.4(4) . . ? N65 C76 C77 124.0(4) . . ? N65 C76 C75 115.5(4) . . ? C77 C76 C75 120.5(4) . . ? C76 C77 C68 117.3(4) . . ? C76 C77 C69 119.1(4) . . ? C68 C77 C69 123.6(4) . . ? C71 C78 C75 117.2(4) . . ? C71 C78 C70 125.0(4) . . ? C75 C78 C70 117.8(4) . . ? C80 N79 C90 117.0(4) . . ? C80 N79 Ru93 128.2(3) . . ? C90 N79 Ru93 114.8(3) . . ? N79 C80 C81 123.1(4) . . ? C82 C81 C80 119.6(5) . . ? C81 C82 C91 119.4(5) . . ? C84 C83 C91 119.6(5) . . ? C83 C84 C92 124.3(5) . . ? C86 C85 C92 119.2(5) . . ? C85 C86 C87 121.3(5) . . ? N88 C87 C86 121.1(5) . . ? C87 N88 C89 118.0(4) . . ? C87 N88 Ru93 128.9(3) . . ? C89 N88 Ru93 113.0(3) . . ? N88 C89 C92 122.3(5) . . ? N88 C89 C90 117.2(4) . . ? C92 C89 C90 120.4(5) . . ? N79 C90 C91 122.6(5) . . ? N79 C90 C89 115.7(4) . . ? C91 C90 C89 121.8(5) . . ? C82 C91 C90 118.3(4) . . ? C82 C91 C83 124.6(5) . . ? C90 C91 C83 117.1(5) . . ? C85 C92 C89 118.0(5) . . ? C85 C92 C84 125.3(5) . . ? C89 C92 C84 116.7(5) . . ? N74 Ru93 N51 172.27(14) . . ? N74 Ru93 N60 93.33(13) . . ? N51 Ru93 N60 80.45(13) . . ? N74 Ru93 N79 89.14(13) . . ? N51 Ru93 N79 97.57(13) . . ? N60 Ru93 N79 172.99(15) . . ? N74 Ru93 N65 78.90(13) . . ? N51 Ru93 N65 96.61(13) . . ? N60 Ru93 N65 91.91(13) . . ? N79 Ru93 N65 95.01(13) . . ? N74 Ru93 N88 97.18(13) . . ? N51 Ru93 N88 87.89(13) . . ? N60 Ru93 N88 93.99(15) . . ? N79 Ru93 N88 79.18(15) . . ? N65 Ru93 N88 173.11(14) . . ? F3 P1 F4 92.3(2) . . ? F3 P1 F5 91.70(18) . . ? F4 P1 F5 94.13(18) . . ? F3 P1 F6 175.4(2) . . ? F4 P1 F6 92.05(18) . . ? F5 P1 F6 89.40(16) . . ? F3 P1 F2 89.25(17) . . ? F4 P1 F2 88.89(17) . . ? F5 P1 F2 176.80(19) . . ? F6 P1 F2 89.41(16) . . ? F3 P1 F7 89.20(19) . . ? F4 P1 F7 178.2(2) . . ? F5 P1 F7 86.94(16) . . ? F6 P1 F7 86.45(17) . . ? F2 P1 F7 90.02(17) . . ? F16 P11 F15 91.0(2) . . ? F16 P11 F14 90.2(2) . . ? F15 P11 F14 92.3(2) . . ? F16 P11 F17 90.7(3) . . ? F15 P11 F17 88.9(2) . . ? F14 P11 F17 178.5(2) . . ? F16 P11 F12 91.0(2) . . ? F15 P11 F12 177.8(2) . . ? F14 P11 F12 88.7(2) . . ? F17 P11 F12 90.1(2) . . ? F16 P11 F13 176.7(3) . . ? F15 P11 F13 91.2(2) . . ? F14 P11 F13 92.2(2) . . ? F17 P11 F13 86.8(2) . . ? F12 P11 F13 86.8(2) . . ? F24 P21 F25 94.1(3) . . ? F24 P21 F23 89.3(2) . . ? F25 P21 F23 89.9(2) . . ? F24 P21 F27 178.1(3) . . ? F25 P21 F27 87.7(2) . . ? F23 P21 F27 91.4(2) . . ? F24 P21 F26 90.8(2) . . ? F25 P21 F26 91.0(2) . . ? F23 P21 F26 179.2(2) . . ? F27 P21 F26 88.5(2) . . ? F24 P21 F22 89.5(2) . . ? F25 P21 F22 176.2(3) . . ? F23 P21 F22 88.9(2) . . ? F27 P21 F22 88.7(2) . . ? F26 P21 F22 90.30(19) . . ? F33 P31 F34 92.5(3) . . ? F33 P31 F37 89.4(2) . . ? F34 P31 F37 178.0(3) . . ? F33 P31 F32 89.6(2) . . ? F34 P31 F32 90.9(2) . . ? F37 P31 F32 89.8(2) . . ? F33 P31 F36 177.6(3) . . ? F34 P31 F36 89.9(2) . . ? F37 P31 F36 88.3(2) . . ? F32 P31 F36 89.79(19) . . ? F33 P31 F35 92.1(2) . . ? F34 P31 F35 89.4(2) . . ? F37 P31 F35 89.8(2) . . ? F32 P31 F35 178.3(2) . . ? F36 P31 F35 88.57(17) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.050 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.055 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 249784' # data_481601a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 F12 N6 P2 Ru' _chemical_formula_weight 931.62 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' 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 37.042(3) _cell_length_b 16.0714(14) _cell_length_c 12.0759(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.023(2) _cell_angle_gamma 90.00 _cell_volume 7056.4(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8101 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 27.92 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9104 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21581 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.92 _reflns_number_total 8101 _reflns_number_gt 5674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0664P)^2^+8.7856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8101 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 N1 N 0.39170(8) 0.1096(2) 0.0653(3) 0.0407(7) Uani 1 1 d . . . C2 C 0.41225(11) 0.0909(3) -0.0113(4) 0.0501(10) Uani 1 1 d . . . H2 H 0.4214 0.1338 -0.0497 0.060 Uiso 1 1 calc R . . C3 C 0.42029(13) 0.0090(3) -0.0352(4) 0.0621(13) Uani 1 1 d . . . H3 H 0.4349 -0.0022 -0.0880 0.075 Uiso 1 1 calc R . . C4 C 0.40670(15) -0.0549(3) 0.0193(5) 0.0720(16) Uani 1 1 d . . . H4 H 0.4118 -0.1097 0.0029 0.086 Uiso 1 1 calc R . . C5 C 0.36941(17) -0.0998(3) 0.1629(6) 0.0828(18) Uani 1 1 d . . . H5 H 0.3738 -0.1559 0.1517 0.099 Uiso 1 1 calc R . . C6 C 0.34881(17) -0.0783(4) 0.2372(5) 0.085(2) Uani 1 1 d . . . H6 H 0.3387 -0.1201 0.2749 0.102 Uiso 1 1 calc R . . C7 C 0.32001(14) 0.0324(4) 0.3377(4) 0.0768(18) Uani 1 1 d . . . H7 H 0.3085 -0.0065 0.3761 0.092 Uiso 1 1 calc R . . C8 C 0.31570(14) 0.1143(5) 0.3559(4) 0.0781(17) Uani 1 1 d . . . H8 H 0.3019 0.1319 0.4083 0.094 Uiso 1 1 calc R . . C9 C 0.33212(12) 0.1723(4) 0.2955(4) 0.0627(13) Uani 1 1 d . . . H9 H 0.3288 0.2286 0.3084 0.075 Uiso 1 1 calc R . . N10 N 0.35242(9) 0.1505(2) 0.2197(3) 0.0467(8) Uani 1 1 d . . . C11 C 0.35697(11) 0.0676(3) 0.2026(3) 0.0490(11) Uani 1 1 d . . . C12 C 0.34167(13) 0.0056(3) 0.2612(4) 0.0655(14) Uani 1 1 d . . . C13 C 0.38516(13) -0.0378(3) 0.0992(4) 0.0629(13) Uani 1 1 d . . . C14 C 0.37829(10) 0.0449(3) 0.1202(3) 0.0466(10) Uani 1 1 d . . . N21 N 0.33325(8) 0.22950(19) -0.0103(3) 0.0400(7) Uani 1 1 d . . . C22 C 0.29988(11) 0.1961(3) -0.0160(4) 0.0526(10) Uani 1 1 d . . . H22 H 0.2946 0.1690 0.0471 0.063 Uiso 1 1 calc R . . C23 C 0.27279(12) 0.2005(3) -0.1134(4) 0.0641(13) Uani 1 1 d . . . H23 H 0.2499 0.1764 -0.1140 0.077 Uiso 1 1 calc R . . C24 C 0.27937(13) 0.2393(3) -0.2072(4) 0.0610(13) Uani 1 1 d . . . H24 H 0.2611 0.2427 -0.2715 0.073 Uiso 1 1 calc R . . C25 C 0.32504(15) 0.3124(3) -0.2999(4) 0.0652(13) Uani 1 1 d . . . H25 H 0.3081 0.3167 -0.3671 0.078 Uiso 1 1 calc R . . C26 C 0.35931(16) 0.3426(3) -0.2946(4) 0.0677(14) Uani 1 1 d . . . H26 H 0.3656 0.3668 -0.3583 0.081 Uiso 1 1 calc R . . C27 C 0.42199(13) 0.3724(3) -0.1780(4) 0.0582(12) Uani 1 1 d . . . H27 H 0.4297 0.3993 -0.2376 0.070 Uiso 1 1 calc R . . C28 C 0.44479(12) 0.3656(3) -0.0764(4) 0.0549(11) Uani 1 1 d . . . H28 H 0.4683 0.3884 -0.0661 0.066 Uiso 1 1 calc R . . C29 C 0.43351(11) 0.3250(2) 0.0124(3) 0.0436(9) Uani 1 1 d . . . H29 H 0.4498 0.3209 0.0810 0.052 Uiso 1 1 calc R . . N30 N 0.40005(8) 0.29163(18) 0.0030(2) 0.0355(7) Uani 1 1 d . . . C31 C 0.37631(11) 0.2997(2) -0.0986(3) 0.0386(8) Uani 1 1 d . . . C32 C 0.38635(12) 0.3379(3) -0.1920(3) 0.0497(10) Uani 1 1 d . . . C33 C 0.31435(12) 0.2746(3) -0.2058(3) 0.0499(10) Uani 1 1 d . . . C34 C 0.34033(10) 0.2671(2) -0.1050(3) 0.0388(8) Uani 1 1 d . . . N41 N 0.36719(9) 0.3340(2) 0.1993(3) 0.0427(7) Uani 1 1 d . . . C42 C 0.33948(12) 0.3880(3) 0.1692(4) 0.0545(11) Uani 1 1 d . . . H42 H 0.3236 0.3814 0.1001 0.065 Uiso 1 1 calc R . . C43 C 0.33388(13) 0.4536(3) 0.2383(5) 0.0653(13) Uani 1 1 d . . . H43 H 0.3141 0.4892 0.2157 0.078 Uiso 1 1 calc R . . C44 C 0.35686(14) 0.4665(3) 0.3386(4) 0.0648(13) Uani 1 1 d . . . H44 H 0.3528 0.5106 0.3845 0.078 Uiso 1 1 calc R . . C45 C 0.41298(15) 0.4209(4) 0.4762(4) 0.0679(14) Uani 1 1 d . . . H45 H 0.4110 0.4648 0.5247 0.081 Uiso 1 1 calc R . . C46 C 0.44050(14) 0.3655(3) 0.5044(4) 0.0643(14) Uani 1 1 d . . . H46 H 0.4569 0.3716 0.5725 0.077 Uiso 1 1 calc R . . C47 C 0.47305(13) 0.2366(3) 0.4572(4) 0.0610(13) Uani 1 1 d . . . H47 H 0.4899 0.2384 0.5250 0.073 Uiso 1 1 calc R . . C48 C 0.47506(12) 0.1758(3) 0.3819(4) 0.0581(12) Uani 1 1 d . . . H48 H 0.4935 0.1358 0.3977 0.070 Uiso 1 1 calc R . . C49 C 0.44965(11) 0.1724(3) 0.2800(3) 0.0473(10) Uani 1 1 d . . . H49 H 0.4519 0.1301 0.2291 0.057 Uiso 1 1 calc R . . N50 N 0.42234(8) 0.2275(2) 0.2531(3) 0.0399(7) Uani 1 1 d . . . C51 C 0.42035(11) 0.2898(3) 0.3291(3) 0.0414(9) Uani 1 1 d . . . C52 C 0.44499(12) 0.2980(3) 0.4325(3) 0.0499(10) Uani 1 1 d . . . C53 C 0.38653(12) 0.4134(3) 0.3720(4) 0.0520(11) Uani 1 1 d . . . C54 C 0.39093(11) 0.3471(3) 0.2998(3) 0.0435(9) Uani 1 1 d . . . Ru Ru 0.378034(8) 0.225101(19) 0.12060(2) 0.03439(11) Uani 1 1 d . . . P1 P 0.24077(4) -0.04100(15) 0.05506(12) 0.0907(6) Uani 1 1 d . . . F11 F 0.24519(11) -0.0432(3) 0.1851(3) 0.1196(14) Uani 1 1 d . . . F12 F 0.26632(18) -0.1194(4) 0.0603(5) 0.191(3) Uani 1 1 d . . . F13 F 0.27670(12) 0.0095(3) 0.0611(4) 0.1392(17) Uani 1 1 d . . . F14 F 0.23762(11) -0.0459(5) -0.0748(3) 0.193(3) Uani 1 1 d . . . F15 F 0.21588(18) 0.0333(5) 0.0515(5) 0.213(3) Uani 1 1 d . . . F16 F 0.20622(15) -0.0937(6) 0.0446(5) 0.255(5) Uani 1 1 d . . . P2 P 0.5000 0.46075(9) 0.2500 0.0395(3) Uani 1 2 d S . . F21 F 0.5000 0.3605(2) 0.2500 0.0604(9) Uani 1 2 d S . . F22 F 0.45632(7) 0.46078(17) 0.2157(2) 0.0656(7) Uani 1 1 d . . . F23 F 0.5000 0.5608(2) 0.2500 0.0602(9) Uani 1 2 d S . . F24 F 0.50258(8) 0.46074(19) 0.1209(2) 0.0726(8) Uani 1 1 d . . . P3 P 0.5000 -0.08459(13) 0.2500 0.0718(6) Uani 1 2 d S . . F31 F 0.46906(13) -0.0167(3) 0.2347(4) 0.1393(17) Uani 1 1 d . . . F32 F 0.47019(14) -0.1521(3) 0.2251(5) 0.183(2) Uani 1 1 d . . . F33 F 0.50023(14) -0.0842(3) 0.3783(3) 0.1546(19) 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 N1 0.0374(17) 0.0382(18) 0.0437(18) 0.0006(14) 0.0005(14) -0.0034(14) C2 0.046(2) 0.051(3) 0.051(2) -0.005(2) 0.0039(19) 0.0024(19) C3 0.054(3) 0.059(3) 0.068(3) -0.012(2) -0.001(2) 0.012(2) C4 0.066(3) 0.044(3) 0.091(4) -0.011(3) -0.022(3) 0.010(2) C5 0.086(4) 0.040(3) 0.106(5) 0.020(3) -0.022(3) -0.012(3) C6 0.086(4) 0.064(4) 0.092(4) 0.039(3) -0.018(3) -0.031(3) C7 0.062(3) 0.107(5) 0.057(3) 0.038(3) -0.001(2) -0.036(3) C8 0.059(3) 0.129(5) 0.050(3) 0.014(3) 0.017(2) -0.026(3) C9 0.054(3) 0.084(4) 0.053(3) 0.009(2) 0.017(2) -0.012(2) N10 0.0403(18) 0.062(2) 0.0378(17) 0.0088(16) 0.0070(14) -0.0116(16) C11 0.040(2) 0.055(3) 0.046(2) 0.017(2) -0.0094(18) -0.0185(19) C12 0.052(3) 0.076(4) 0.059(3) 0.030(3) -0.014(2) -0.027(2) C13 0.057(3) 0.046(3) 0.073(3) 0.010(2) -0.022(2) -0.002(2) C14 0.042(2) 0.040(2) 0.050(2) 0.0107(19) -0.0101(18) -0.0099(18) N21 0.0358(16) 0.0416(18) 0.0425(17) -0.0050(15) 0.0073(13) -0.0026(14) C22 0.040(2) 0.060(3) 0.057(3) -0.011(2) 0.0079(19) -0.006(2) C23 0.036(2) 0.077(3) 0.075(3) -0.025(3) 0.001(2) -0.005(2) C24 0.050(3) 0.063(3) 0.060(3) -0.013(2) -0.014(2) 0.008(2) C25 0.089(4) 0.052(3) 0.046(3) 0.008(2) -0.010(2) 0.009(3) C26 0.103(4) 0.055(3) 0.040(2) 0.012(2) 0.002(2) 0.000(3) C27 0.080(3) 0.048(3) 0.051(3) 0.010(2) 0.025(2) -0.009(2) C28 0.058(3) 0.051(3) 0.061(3) 0.003(2) 0.024(2) -0.014(2) C29 0.044(2) 0.041(2) 0.046(2) 0.0019(18) 0.0090(17) -0.0070(17) N30 0.0428(17) 0.0289(16) 0.0350(16) 0.0022(12) 0.0082(13) -0.0040(13) C31 0.049(2) 0.0268(18) 0.038(2) 0.0022(15) 0.0046(16) 0.0011(15) C32 0.069(3) 0.038(2) 0.041(2) 0.0052(18) 0.0106(19) 0.000(2) C33 0.054(3) 0.041(2) 0.048(2) -0.0072(19) -0.0079(19) 0.0080(19) C34 0.046(2) 0.032(2) 0.0362(19) -0.0024(16) 0.0010(16) 0.0064(16) N41 0.0426(18) 0.0433(19) 0.0433(18) 0.0004(15) 0.0111(14) -0.0041(15) C42 0.045(2) 0.050(3) 0.068(3) 0.002(2) 0.010(2) 0.002(2) C43 0.057(3) 0.053(3) 0.089(4) -0.007(3) 0.024(3) 0.007(2) C44 0.070(3) 0.055(3) 0.077(3) -0.019(3) 0.035(3) -0.011(2) C45 0.084(4) 0.077(4) 0.049(3) -0.023(3) 0.030(3) -0.030(3) C46 0.067(3) 0.087(4) 0.040(2) -0.013(2) 0.013(2) -0.032(3) C47 0.053(3) 0.082(4) 0.044(2) 0.014(2) -0.002(2) -0.020(3) C48 0.044(2) 0.069(3) 0.058(3) 0.021(2) -0.001(2) -0.004(2) C49 0.043(2) 0.050(3) 0.048(2) 0.0118(19) 0.0066(18) 0.0009(19) N50 0.0420(18) 0.0421(19) 0.0359(16) 0.0040(14) 0.0082(13) -0.0086(15) C51 0.042(2) 0.051(3) 0.0315(18) 0.0050(17) 0.0088(15) -0.0164(17) C52 0.047(2) 0.065(3) 0.037(2) 0.007(2) 0.0083(18) -0.018(2) C53 0.057(3) 0.054(3) 0.051(2) -0.007(2) 0.026(2) -0.014(2) C54 0.048(2) 0.050(2) 0.036(2) -0.0022(17) 0.0156(17) -0.0109(19) Ru 0.03339(17) 0.03782(18) 0.03182(16) 0.00227(13) 0.00590(11) -0.00421(13) P1 0.0521(8) 0.1660(19) 0.0535(8) -0.0141(9) 0.0085(6) -0.0089(10) F11 0.120(3) 0.178(4) 0.063(2) -0.006(2) 0.0237(19) -0.012(3) F12 0.228(6) 0.179(6) 0.203(6) 0.009(4) 0.136(5) 0.037(5) F13 0.111(3) 0.189(5) 0.114(3) 0.021(3) 0.011(2) -0.063(3) F14 0.077(3) 0.439(10) 0.063(2) -0.015(4) 0.0095(19) -0.006(4) F15 0.204(6) 0.262(8) 0.172(5) 0.060(5) 0.031(4) 0.141(6) F16 0.162(5) 0.443(12) 0.192(5) -0.205(7) 0.114(4) -0.186(6) P2 0.0463(8) 0.0383(8) 0.0352(7) 0.000 0.0106(6) 0.000 F21 0.070(2) 0.0354(19) 0.075(2) 0.000 0.0122(19) 0.000 F22 0.0457(14) 0.0632(17) 0.0869(19) -0.0080(14) 0.0099(13) 0.0007(12) F23 0.075(2) 0.0372(19) 0.068(2) 0.000 0.0132(19) 0.000 F24 0.100(2) 0.083(2) 0.0396(14) -0.0011(13) 0.0244(14) 0.0049(17) P3 0.0754(13) 0.0582(12) 0.0710(12) 0.000 -0.0132(10) 0.000 F31 0.151(4) 0.124(4) 0.122(3) -0.008(3) -0.027(3) 0.065(3) F32 0.152(4) 0.133(4) 0.253(6) -0.011(4) 0.012(4) -0.074(3) F33 0.175(5) 0.201(5) 0.082(3) 0.044(3) 0.009(3) 0.043(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.340(5) . ? N1 C14 1.377(5) . ? N1 Ru 2.068(3) . ? C2 C3 1.391(6) . ? C3 C4 1.366(7) . ? C4 C13 1.392(7) . ? C5 C6 1.330(9) . ? C5 C13 1.448(8) . ? C6 C12 1.416(8) . ? C7 C8 1.348(8) . ? C7 C12 1.401(8) . ? C8 C9 1.393(7) . ? C9 N10 1.337(5) . ? N10 C11 1.363(6) . ? N10 Ru 2.051(3) . ? C11 C12 1.403(6) . ? C11 C14 1.431(6) . ? C13 C14 1.387(6) . ? N21 C22 1.337(5) . ? N21 C34 1.362(5) . ? N21 Ru 2.062(3) . ? C22 C23 1.395(6) . ? C23 C24 1.355(7) . ? C24 C33 1.411(7) . ? C25 C26 1.349(7) . ? C25 C33 1.410(6) . ? C26 C32 1.439(6) . ? C27 C28 1.354(6) . ? C27 C32 1.412(6) . ? C28 C29 1.386(5) . ? C29 N30 1.335(5) . ? N30 C31 1.373(4) . ? N30 Ru 2.066(3) . ? C31 C32 1.395(5) . ? C31 C34 1.421(5) . ? C33 C34 1.406(5) . ? N41 C42 1.341(5) . ? N41 C54 1.373(5) . ? N41 Ru 2.067(3) . ? C42 C43 1.384(6) . ? C43 C44 1.356(7) . ? C44 C53 1.389(6) . ? C45 C46 1.347(7) . ? C45 C53 1.444(7) . ? C46 C52 1.419(7) . ? C47 C48 1.346(7) . ? C47 C52 1.423(7) . ? C48 C49 1.400(6) . ? C49 N50 1.337(5) . ? N50 C51 1.370(5) . ? N50 Ru 2.062(3) . ? C51 C52 1.404(5) . ? C51 C54 1.418(6) . ? C53 C54 1.405(6) . ? P1 F15 1.504(6) . ? P1 F16 1.519(5) . ? P1 F11 1.548(3) . ? P1 F13 1.549(4) . ? P1 F14 1.552(4) . ? P1 F12 1.570(6) . ? P2 F24 1.580(2) . ? P2 F24 1.580(2) 2_655 ? P2 F22 1.591(2) 2_655 ? P2 F22 1.591(2) . ? P2 F21 1.612(4) . ? P2 F23 1.609(4) . ? P3 F32 1.536(4) . ? P3 F32 1.536(4) 2_655 ? P3 F33 1.548(4) 2_655 ? P3 F33 1.548(4) . ? P3 F31 1.567(4) 2_655 ? P3 F31 1.567(4) . ? 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 C2 N1 C14 117.9(4) . . ? C2 N1 Ru 129.2(3) . . ? C14 N1 Ru 112.9(3) . . ? N1 C2 C3 121.9(4) . . ? C4 C3 C2 119.9(5) . . ? C3 C4 C13 119.9(5) . . ? C6 C5 C13 121.4(6) . . ? C5 C6 C12 122.7(5) . . ? C8 C7 C12 120.5(5) . . ? C7 C8 C9 119.3(5) . . ? N10 C9 C8 122.8(5) . . ? C9 N10 C11 117.5(4) . . ? C9 N10 Ru 129.0(3) . . ? C11 N10 Ru 113.5(3) . . ? N10 C11 C12 123.0(5) . . ? N10 C11 C14 117.1(3) . . ? C12 C11 C14 119.9(5) . . ? C7 C12 C11 116.8(5) . . ? C7 C12 C6 125.5(5) . . ? C11 C12 C6 117.6(5) . . ? C14 C13 C4 117.8(5) . . ? C14 C13 C5 117.1(6) . . ? C4 C13 C5 125.1(5) . . ? N1 C14 C13 122.7(4) . . ? N1 C14 C11 116.1(4) . . ? C13 C14 C11 121.2(4) . . ? C22 N21 C34 117.4(3) . . ? C22 N21 Ru 128.7(3) . . ? C34 N21 Ru 113.7(2) . . ? N21 C22 C23 122.1(4) . . ? C24 C23 C22 120.9(4) . . ? C23 C24 C33 119.1(4) . . ? C26 C25 C33 121.6(4) . . ? C25 C26 C32 121.0(4) . . ? C28 C27 C32 118.9(4) . . ? C27 C28 C29 120.7(4) . . ? N30 C29 C28 122.4(4) . . ? C29 N30 C31 117.6(3) . . ? C29 N30 Ru 129.2(3) . . ? C31 N30 Ru 113.2(2) . . ? N30 C31 C32 122.7(4) . . ? N30 C31 C34 116.6(3) . . ? C32 C31 C34 120.7(3) . . ? C31 C32 C27 117.6(4) . . ? C31 C32 C26 118.0(4) . . ? C27 C32 C26 124.3(4) . . ? C34 C33 C24 116.8(4) . . ? C34 C33 C25 118.9(4) . . ? C24 C33 C25 124.2(4) . . ? N21 C34 C33 123.7(4) . . ? N21 C34 C31 116.6(3) . . ? C33 C34 C31 119.7(4) . . ? C42 N41 C54 117.9(4) . . ? C42 N41 Ru 129.0(3) . . ? C54 N41 Ru 112.9(3) . . ? N41 C42 C43 121.6(4) . . ? C44 C43 C42 121.0(5) . . ? C43 C44 C53 119.5(4) . . ? C46 C45 C53 121.3(4) . . ? C45 C46 C52 121.5(4) . . ? C48 C47 C52 119.6(4) . . ? C47 C48 C49 120.5(4) . . ? N50 C49 C48 122.5(4) . . ? C49 N50 C51 117.2(3) . . ? C49 N50 Ru 129.0(3) . . ? C51 N50 Ru 113.4(3) . . ? N50 C51 C52 123.7(4) . . ? N50 C51 C54 116.4(3) . . ? C52 C51 C54 119.9(4) . . ? C51 C52 C47 116.5(4) . . ? C51 C52 C46 118.9(4) . . ? C47 C52 C46 124.6(4) . . ? C44 C53 C54 117.7(4) . . ? C44 C53 C45 124.7(4) . . ? C54 C53 C45 117.6(4) . . ? N41 C54 C53 122.3(4) . . ? N41 C54 C51 116.9(3) . . ? C53 C54 C51 120.8(4) . . ? N10 Ru N50 86.91(12) . . ? N10 Ru N21 94.20(12) . . ? N50 Ru N21 176.87(12) . . ? N10 Ru N30 172.50(12) . . ? N50 Ru N30 99.42(11) . . ? N21 Ru N30 79.69(12) . . ? N10 Ru N1 80.38(14) . . ? N50 Ru N1 93.42(12) . . ? N21 Ru N1 89.66(12) . . ? N30 Ru N1 95.13(12) . . ? N10 Ru N41 94.26(13) . . ? N50 Ru N41 79.82(13) . . ? N21 Ru N41 97.17(12) . . ? N30 Ru N41 90.85(12) . . ? N1 Ru N41 171.65(12) . . ? F15 P1 F16 86.4(4) . . ? F15 P1 F11 89.6(3) . . ? F16 P1 F11 89.8(3) . . ? F15 P1 F13 95.8(4) . . ? F16 P1 F13 176.9(3) . . ? F11 P1 F13 92.3(2) . . ? F15 P1 F14 94.8(3) . . ? F16 P1 F14 89.3(3) . . ? F11 P1 F14 175.4(4) . . ? F13 P1 F14 88.4(3) . . ? F15 P1 F12 178.9(4) . . ? F16 P1 F12 92.8(4) . . ? F11 P1 F12 89.7(3) . . ? F13 P1 F12 85.0(3) . . ? F14 P1 F12 85.9(3) . . ? F24 P2 F24 180.0(3) . 2_655 ? F24 P2 F22 90.37(15) . 2_655 ? F24 P2 F22 89.63(15) 2_655 2_655 ? F24 P2 F22 89.63(15) . . ? F24 P2 F22 90.37(15) 2_655 . ? F22 P2 F22 180.0(3) 2_655 . ? F24 P2 F21 89.99(12) . . ? F24 P2 F21 89.99(12) 2_655 . ? F22 P2 F21 90.02(11) 2_655 . ? F22 P2 F21 90.02(11) . . ? F24 P2 F23 90.01(12) . . ? F24 P2 F23 90.01(12) 2_655 . ? F22 P2 F23 89.98(11) 2_655 . ? F22 P2 F23 89.98(11) . . ? F21 P2 F23 180.000(1) . . ? F32 P3 F32 90.1(5) . 2_655 ? F32 P3 F33 86.6(3) . 2_655 ? F32 P3 F33 93.7(3) 2_655 2_655 ? F32 P3 F33 93.7(3) . . ? F32 P3 F33 86.6(3) 2_655 . ? F33 P3 F33 179.5(5) 2_655 . ? F32 P3 F31 175.3(3) . 2_655 ? F32 P3 F31 89.2(3) 2_655 2_655 ? F33 P3 F31 88.8(3) 2_655 2_655 ? F33 P3 F31 90.9(3) . 2_655 ? F32 P3 F31 89.2(3) . . ? F32 P3 F31 175.3(3) 2_655 . ? F33 P3 F31 90.9(3) 2_655 . ? F33 P3 F31 88.8(3) . . ? F31 P3 F31 91.8(4) 2_655 . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.032 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.094 data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 249785' # data_481604a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H48 F24 N12 Os2 P4' _chemical_formula_weight 2041.50 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' 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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.1878(13) _cell_length_b 17.9354(16) _cell_length_c 32.058(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7582.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 27.93 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 3.543 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5376 _exptl_absorpt_correction_T_max 0.9011 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47279 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.1274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.93 _reflns_number_total 17377 _reflns_number_gt 11599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(7) _refine_ls_number_reflns 17377 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 N1 N -0.1228(5) 0.4306(3) 0.5294(2) 0.0450(16) Uiso 1 1 d . . . C2 C -0.1987(7) 0.4591(5) 0.5514(3) 0.055(2) Uiso 1 1 d . . . H2 H -0.1842 0.4969 0.5703 0.066 Uiso 1 1 calc R . . C3 C -0.2991(8) 0.4356(5) 0.5476(3) 0.066(3) Uiso 1 1 d . . . H3 H -0.3500 0.4562 0.5640 0.079 Uiso 1 1 calc R . . C4 C -0.3204(8) 0.3806(5) 0.5187(3) 0.058(2) Uiso 1 1 d . . . H4 H -0.3868 0.3642 0.5154 0.069 Uiso 1 1 calc R . . C5 C -0.2582(8) 0.2931(5) 0.4627(3) 0.063(3) Uiso 1 1 d . . . H5 H -0.3230 0.2749 0.4572 0.076 Uiso 1 1 calc R . . C6 C -0.1824(9) 0.2683(6) 0.4421(3) 0.074(3) Uiso 1 1 d . . . H6 H -0.1949 0.2329 0.4216 0.089 Uiso 1 1 calc R . . C7 C 0.0078(8) 0.2654(6) 0.4265(3) 0.074(3) Uiso 1 1 d . . . H7 H 0.0006 0.2298 0.4056 0.089 Uiso 1 1 calc R . . C8 C 0.1011(9) 0.2937(5) 0.4363(3) 0.069(3) Uiso 1 1 d . . . H8 H 0.1581 0.2766 0.4221 0.083 Uiso 1 1 calc R . . C9 C 0.1120(8) 0.3477(5) 0.4674(3) 0.060(2) Uiso 1 1 d . . . H9 H 0.1765 0.3661 0.4732 0.072 Uiso 1 1 calc R . . N10 N 0.0331(6) 0.3739(3) 0.48897(19) 0.0446(16) Uiso 1 1 d . . . C11 C -0.0607(6) 0.3459(4) 0.4789(2) 0.045(2) Uiso 1 1 d . . . C12 C -0.0774(8) 0.2916(5) 0.4487(3) 0.060(3) Uiso 1 1 d . . . C13 C -0.2436(7) 0.3495(4) 0.4947(3) 0.050(2) Uiso 1 1 d . . . C14 C -0.1461(7) 0.3741(4) 0.5016(3) 0.043(2) Uiso 1 1 d . . . N21 N 0.0024(5) 0.5580(3) 0.56459(19) 0.0387(16) Uiso 1 1 d . . . C22 C 0.0055(7) 0.5679(5) 0.6055(3) 0.049(2) Uiso 1 1 d . . . H22 H 0.0239 0.5275 0.6220 0.058 Uiso 1 1 calc R . . C23 C -0.0170(8) 0.6347(5) 0.6251(3) 0.064(3) Uiso 1 1 d . . . H23 H -0.0128 0.6382 0.6540 0.077 Uiso 1 1 calc R . . C24 C -0.0461(8) 0.6971(5) 0.6016(3) 0.061(3) Uiso 1 1 d . . . H24 H -0.0644 0.7419 0.6141 0.073 Uiso 1 1 calc R . . C25 C -0.0697(7) 0.7486(5) 0.5302(3) 0.058(2) Uiso 1 1 d . . . H25 H -0.0865 0.7950 0.5411 0.069 Uiso 1 1 calc R . . C26 C -0.0682(8) 0.7397(6) 0.4900(3) 0.069(3) Uiso 1 1 d . . . H26 H -0.0808 0.7808 0.4731 0.082 Uiso 1 1 calc R . . C27 C -0.0498(8) 0.6539(5) 0.4276(3) 0.066(3) Uiso 1 1 d . . . H27 H -0.0656 0.6920 0.4091 0.079 Uiso 1 1 calc R . . C28 C -0.0291(9) 0.5847(5) 0.4129(3) 0.070(3) Uiso 1 1 d . . . H28 H -0.0280 0.5755 0.3843 0.084 Uiso 1 1 calc R . . C29 C -0.0095(7) 0.5274(5) 0.4413(3) 0.062(3) Uiso 1 1 d . . . H29 H 0.0009 0.4794 0.4312 0.074 Uiso 1 1 calc R . . N30 N -0.0051(5) 0.5389(4) 0.4831(2) 0.0470(17) Uiso 1 1 d . . . C31 C -0.0248(7) 0.6096(4) 0.4956(2) 0.046(2) Uiso 1 1 d . . . C32 C -0.0477(7) 0.6686(5) 0.4704(3) 0.056(2) Uiso 1 1 d . . . C33 C -0.0461(7) 0.6886(4) 0.5581(3) 0.052(2) Uiso 1 1 d . . . C34 C -0.0230(6) 0.6200(4) 0.5409(2) 0.0376(18) Uiso 1 1 d . . . N41 N 0.0737(5) 0.3972(3) 0.5790(2) 0.0420(16) Uiso 1 1 d . . . C42 C 0.0188(8) 0.3496(5) 0.6020(3) 0.054(2) Uiso 1 1 d . . . H42 H -0.0486 0.3418 0.5946 0.065 Uiso 1 1 calc R . . C43 C 0.0573(8) 0.3109(5) 0.6365(3) 0.065(3) Uiso 1 1 d . . . H43 H 0.0173 0.2780 0.6517 0.078 Uiso 1 1 calc R . . C44 C 0.1568(8) 0.3239(5) 0.6469(3) 0.067(3) Uiso 1 1 d . . . H44 H 0.1844 0.2990 0.6697 0.080 Uiso 1 1 calc R . . C45 C 0.3220(8) 0.3891(5) 0.6337(3) 0.067(3) Uiso 1 1 d . . . H45 H 0.3526 0.3692 0.6573 0.081 Uiso 1 1 calc R . . C46 C 0.3757(9) 0.4318(5) 0.6093(3) 0.066(3) Uiso 1 1 d . . . H46 H 0.4435 0.4399 0.6159 0.079 Uiso 1 1 calc R . . C47 C 0.3874(9) 0.5118(5) 0.5447(3) 0.071(3) Uiso 1 1 d . . . H47 H 0.4556 0.5225 0.5491 0.086 Uiso 1 1 calc R . . C48 C 0.3400(9) 0.5396(6) 0.5113(3) 0.074(3) Uiso 1 1 d . . . H48 H 0.3763 0.5683 0.4923 0.089 Uiso 1 1 calc R . . C49 C 0.2369(8) 0.5263(5) 0.5043(3) 0.059(2) Uiso 1 1 d . . . H49 H 0.2059 0.5467 0.4808 0.070 Uiso 1 1 calc R . . N50 N 0.1820(5) 0.4851(3) 0.5305(2) 0.0462(17) Uiso 1 1 d . . . C51 C 0.2294(7) 0.4540(5) 0.5645(3) 0.048(2) Uiso 1 1 d . . . C52 C 0.3350(7) 0.4667(5) 0.5731(3) 0.056(2) Uiso 1 1 d . . . C53 C 0.2152(7) 0.3710(5) 0.6255(3) 0.049(2) Uiso 1 1 d . . . C54 C 0.1739(7) 0.4085(4) 0.5908(3) 0.044(2) Uiso 1 1 d . . . N61 N 0.2197(6) 0.9098(4) 0.6558(2) 0.0530(19) Uiso 1 1 d . . . C62 C 0.2179(9) 0.9845(5) 0.6576(3) 0.072(3) Uiso 1 1 d . . . H62 H 0.2260 1.0075 0.6834 0.087 Uiso 1 1 calc R . . C63 C 0.2044(9) 1.0289(7) 0.6226(4) 0.087(3) Uiso 1 1 d . . . H63 H 0.2061 1.0805 0.6251 0.104 Uiso 1 1 calc R . . C64 C 0.1889(9) 0.9977(6) 0.5851(4) 0.087(4) Uiso 1 1 d . . . H64 H 0.1772 1.0275 0.5618 0.105 Uiso 1 1 calc R . . C65 C 0.1799(9) 0.8799(6) 0.5438(3) 0.074(3) Uiso 1 1 d . . . H65 H 0.1677 0.9064 0.5194 0.089 Uiso 1 1 calc R . . C66 C 0.1866(8) 0.8055(5) 0.5417(3) 0.070(3) Uiso 1 1 d . . . H66 H 0.1784 0.7820 0.5160 0.084 Uiso 1 1 calc R . . C67 C 0.2231(8) 0.6846(5) 0.5799(3) 0.064(3) Uiso 1 1 d . . . H67 H 0.2215 0.6573 0.5552 0.077 Uiso 1 1 calc R . . C68 C 0.2415(8) 0.6496(5) 0.6161(3) 0.066(3) Uiso 1 1 d . . . H68 H 0.2508 0.5982 0.6166 0.080 Uiso 1 1 calc R . . C69 C 0.2465(7) 0.6901(5) 0.6529(3) 0.057(2) Uiso 1 1 d . . . H69 H 0.2609 0.6653 0.6777 0.068 Uiso 1 1 calc R . . N70 N 0.2311(5) 0.7641(3) 0.65370(19) 0.0419(16) Uiso 1 1 d . . . C71 C 0.2132(7) 0.8004(4) 0.6167(3) 0.047(2) Uiso 1 1 d . . . C72 C 0.2066(8) 0.7603(5) 0.5786(3) 0.063(3) Uiso 1 1 d . . . C73 C 0.1906(8) 0.9197(5) 0.5812(3) 0.065(3) Uiso 1 1 d . . . C74 C 0.2078(7) 0.8772(5) 0.6177(3) 0.052(2) Uiso 1 1 d . . . N81 N 0.3831(5) 0.8496(3) 0.7086(2) 0.0428(16) Uiso 1 1 d . . . C82 C 0.4585(7) 0.8137(4) 0.6879(3) 0.049(2) Uiso 1 1 d . . . H82 H 0.4408 0.7764 0.6691 0.059 Uiso 1 1 calc R . . C83 C 0.5602(7) 0.8295(5) 0.6934(3) 0.059(3) Uiso 1 1 d . . . H83 H 0.6086 0.8025 0.6787 0.071 Uiso 1 1 calc R . . C84 C 0.5898(8) 0.8840(5) 0.7200(3) 0.061(3) Uiso 1 1 d . . . H84 H 0.6582 0.8955 0.7229 0.073 Uiso 1 1 calc R . . C85 C 0.5378(9) 0.9812(5) 0.7727(3) 0.064(3) Uiso 1 1 d . . . H85 H 0.6046 0.9949 0.7779 0.077 Uiso 1 1 calc R . . C86 C 0.4615(8) 1.0157(5) 0.7928(3) 0.069(3) Uiso 1 1 d . . . H86 H 0.4774 1.0537 0.8113 0.083 Uiso 1 1 calc R . . C87 C 0.2736(10) 1.0317(6) 0.8058(3) 0.084(3) Uiso 1 1 d . . . H87 H 0.2848 1.0713 0.8239 0.101 Uiso 1 1 calc R . . C88 C 0.1780(10) 1.0090(6) 0.7982(4) 0.091(4) Uiso 1 1 d . . . H88 H 0.1235 1.0319 0.8114 0.109 Uiso 1 1 calc R . . C89 C 0.1616(9) 0.9496(6) 0.7696(3) 0.071(3) Uiso 1 1 d . . . H89 H 0.0956 0.9335 0.7647 0.086 Uiso 1 1 calc R . . N90 N 0.2374(6) 0.9164(4) 0.7498(2) 0.0540(19) Uiso 1 1 d . . . C91 C 0.3357(7) 0.9391(4) 0.7576(3) 0.047(2) Uiso 1 1 d . . . C92 C 0.3566(8) 0.9965(5) 0.7869(3) 0.063(3) Uiso 1 1 d . . . C93 C 0.5163(7) 0.9233(5) 0.7432(3) 0.048(2) Uiso 1 1 d . . . C94 C 0.4138(7) 0.9039(5) 0.7363(3) 0.046(2) Uiso 1 1 d . . . N101 N 0.0756(5) 0.8182(4) 0.7082(2) 0.0499(18) Uiso 1 1 d . . . C102 C 0.0010(8) 0.8502(5) 0.6855(3) 0.064(3) Uiso 1 1 d . . . H102 H 0.0161 0.8876 0.6664 0.076 Uiso 1 1 calc R . . C103 C -0.1002(9) 0.8264(6) 0.6910(3) 0.071(3) Uiso 1 1 d . . . H103 H -0.1508 0.8484 0.6749 0.086 Uiso 1 1 calc R . . C104 C -0.1255(9) 0.7750(6) 0.7177(3) 0.074(3) Uiso 1 1 d . . . H104 H -0.1933 0.7611 0.7199 0.088 Uiso 1 1 calc R . . C105 C -0.0694(9) 0.6858(6) 0.7736(3) 0.075(3) Uiso 1 1 d . . . H105 H -0.1353 0.6688 0.7775 0.090 Uiso 1 1 calc R . . C106 C 0.0017(8) 0.6562(5) 0.7974(3) 0.065(3) Uiso 1 1 d . . . H106 H -0.0154 0.6205 0.8172 0.078 Uiso 1 1 calc R . . C107 C 0.1887(8) 0.6543(6) 0.8151(3) 0.069(3) Uiso 1 1 d . . . H107 H 0.1781 0.6197 0.8362 0.083 Uiso 1 1 calc R . . C108 C 0.2843(8) 0.6784(5) 0.8072(3) 0.063(3) Uiso 1 1 d . . . H108 H 0.3383 0.6621 0.8234 0.075 Uiso 1 1 calc R . . C109 C 0.3006(8) 0.7281(5) 0.7743(3) 0.057(3) Uiso 1 1 d . . . H109 H 0.3667 0.7423 0.7681 0.069 Uiso 1 1 calc R . . N110 N 0.2246(6) 0.7560(4) 0.7516(2) 0.0481(17) Uiso 1 1 d . . . C111 C 0.1258(7) 0.7328(5) 0.7609(3) 0.053(2) Uiso 1 1 d . . . C112 C 0.1075(7) 0.6796(5) 0.7925(3) 0.055(2) Uiso 1 1 d . . . C113 C -0.0550(8) 0.7408(5) 0.7427(3) 0.064(3) Uiso 1 1 d . . . C114 C 0.0487(7) 0.7653(5) 0.7353(3) 0.056(2) Uiso 1 1 d . . . Os1 Os 0.02805(3) 0.463023(17) 0.529398(10) 0.03986(9) Uani 1 1 d . . . Os2 Os 0.22992(3) 0.835425(19) 0.704545(10) 0.04331(9) Uani 1 1 d . . . P1 P 0.8603(2) 0.00280(15) 0.78060(8) 0.0559(7) Uani 1 1 d . . . F11 F 0.7777(6) 0.0502(4) 0.7598(3) 0.139(3) Uani 1 1 d . . . F12 F 0.8036(6) 0.0132(3) 0.8243(2) 0.111(3) Uani 1 1 d . . . F13 F 0.9190(5) 0.0786(3) 0.7887(2) 0.096(2) Uani 1 1 d . . . F14 F 0.9446(5) -0.0407(4) 0.8054(2) 0.107(2) Uani 1 1 d . . . F15 F 0.9210(7) -0.0060(4) 0.7395(2) 0.117(3) Uani 1 1 d . . . F16 F 0.7988(6) -0.0720(3) 0.7751(2) 0.096(2) Uani 1 1 d . . . P2 P 0.9195(3) 0.1423(2) 0.55953(10) 0.0857(10) Uani 1 1 d . . . F21 F 0.8425(8) 0.0856(5) 0.5769(3) 0.161(4) Uani 1 1 d . . . F22 F 0.8544(7) 0.2082(5) 0.5787(3) 0.167(4) Uani 1 1 d . . . F23 F 0.9827(9) 0.1422(6) 0.6003(3) 0.178(4) Uani 1 1 d . . . F24 F 0.9915(6) 0.2043(4) 0.5396(3) 0.131(3) Uani 1 1 d . . . F25 F 0.9871(6) 0.0773(5) 0.5410(3) 0.130(3) Uani 1 1 d . . . F26 F 0.8568(7) 0.1411(5) 0.5181(2) 0.130(3) Uani 1 1 d . . . P3 P 0.6311(3) 0.65833(18) 0.59130(9) 0.0739(8) Uani 1 1 d . . . F31 F 0.5747(6) 0.6356(5) 0.5503(2) 0.127(3) Uani 1 1 d . . . F32 F 0.5275(8) 0.6858(5) 0.6087(3) 0.163(4) Uani 1 1 d . . . F33 F 0.6535(7) 0.7375(4) 0.5726(3) 0.134(3) Uani 1 1 d . . . F34 F 0.6860(10) 0.6801(4) 0.6316(3) 0.188(5) Uani 1 1 d . . . F35 F 0.7306(7) 0.6282(4) 0.5715(4) 0.162(4) Uani 1 1 d . . . F36 F 0.6049(7) 0.5776(4) 0.6092(2) 0.112(3) Uani 1 1 d . . . P4 P 0.6032(2) 0.67748(19) 0.80370(11) 0.0825(9) Uani 1 1 d . . . F41 F 0.5339(6) 0.6718(5) 0.7655(3) 0.139(3) Uani 1 1 d . . . F42 F 0.5301(7) 0.7426(5) 0.8200(3) 0.142(3) Uani 1 1 d . . . F43 F 0.6679(7) 0.7413(5) 0.7821(3) 0.141(3) Uani 1 1 d . . . F44 F 0.6714(7) 0.6884(4) 0.8436(3) 0.141(3) Uani 1 1 d . . . F45 F 0.6778(7) 0.6164(4) 0.7881(3) 0.140(3) Uani 1 1 d . . . F46 F 0.5396(9) 0.6199(5) 0.8265(4) 0.189(5) 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 Os1 0.03880(18) 0.03880(16) 0.04198(18) -0.00079(16) -0.00323(15) -0.00351(16) Os2 0.03584(17) 0.0538(2) 0.04028(18) -0.01135(17) -0.00269(15) 0.00284(17) P1 0.0436(15) 0.0607(15) 0.0635(17) 0.0103(13) -0.0019(12) -0.0035(12) F11 0.058(4) 0.142(6) 0.217(8) 0.107(6) -0.018(5) 0.008(4) F12 0.154(8) 0.083(4) 0.095(5) 0.007(4) 0.062(5) -0.010(4) F13 0.119(6) 0.082(4) 0.088(5) 0.011(4) 0.010(4) -0.049(4) F14 0.062(4) 0.122(5) 0.135(6) 0.055(5) -0.015(4) -0.005(4) F15 0.158(8) 0.113(5) 0.081(5) -0.005(4) 0.043(5) -0.006(5) F16 0.121(6) 0.075(4) 0.092(5) 0.004(3) -0.032(4) -0.041(4) P2 0.059(2) 0.122(3) 0.076(2) -0.022(2) 0.0058(16) -0.0104(19) F21 0.186(10) 0.142(7) 0.155(8) -0.003(6) 0.055(7) -0.064(7) F22 0.107(7) 0.149(7) 0.245(10) -0.089(7) 0.079(7) -0.025(5) F23 0.175(10) 0.250(11) 0.108(6) -0.020(7) -0.052(6) 0.006(9) F24 0.079(6) 0.153(7) 0.160(7) -0.008(6) 0.042(5) -0.025(5) F25 0.082(6) 0.167(7) 0.142(7) -0.034(6) -0.006(5) 0.041(5) F26 0.119(7) 0.159(7) 0.111(6) -0.016(5) -0.033(5) -0.001(5) P3 0.086(2) 0.0757(19) 0.0602(18) 0.0037(16) -0.0043(15) 0.0260(17) F31 0.124(7) 0.179(7) 0.078(5) 0.027(5) -0.019(4) -0.034(6) F32 0.167(9) 0.151(7) 0.171(8) 0.025(6) 0.087(7) 0.057(7) F33 0.146(8) 0.086(5) 0.170(8) 0.030(5) 0.004(6) -0.012(5) F34 0.353(16) 0.100(5) 0.111(6) -0.011(5) -0.120(8) 0.005(8) F35 0.089(6) 0.121(6) 0.276(11) -0.032(7) 0.027(7) 0.006(5) F36 0.169(8) 0.093(5) 0.073(4) 0.021(4) -0.015(4) 0.014(5) P4 0.0541(18) 0.088(2) 0.105(3) -0.008(2) -0.0083(17) -0.0050(17) F41 0.105(6) 0.158(7) 0.153(7) -0.050(6) -0.064(5) 0.025(6) F42 0.113(7) 0.139(6) 0.175(8) -0.056(6) 0.011(6) 0.027(6) F43 0.106(7) 0.152(7) 0.164(8) 0.038(6) 0.009(6) -0.021(5) F44 0.148(8) 0.146(7) 0.128(6) 0.026(5) -0.062(6) -0.026(6) F45 0.108(7) 0.133(6) 0.178(8) -0.031(6) -0.030(6) 0.054(5) F46 0.142(9) 0.174(8) 0.252(12) 0.053(8) 0.017(8) -0.078(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 N1 C2 1.326(10) . ? N1 C14 1.384(10) . ? N1 Os1 2.073(7) . ? C2 C3 1.394(13) . ? C3 C4 1.382(12) . ? C4 C13 1.390(12) . ? C5 C6 1.278(13) . ? C5 C13 1.452(11) . ? C6 C12 1.463(14) . ? C7 C8 1.368(14) . ? C7 C12 1.410(14) . ? C8 C9 1.398(13) . ? C9 N10 1.335(11) . ? N10 C11 1.374(10) . ? N10 Os1 2.059(6) . ? C11 C12 1.391(11) . ? C11 C14 1.433(11) . ? C13 C14 1.378(12) . ? N21 C22 1.324(10) . ? N21 C34 1.387(9) . ? N21 Os1 2.071(6) . ? C22 C23 1.386(11) . ? C23 C24 1.404(12) . ? C24 C33 1.401(12) . ? C25 C26 1.297(12) . ? C25 C33 1.434(12) . ? C26 C32 1.447(13) . ? C27 C28 1.357(13) . ? C27 C32 1.396(12) . ? C28 C29 1.399(12) . ? C29 N30 1.356(11) . ? N30 C31 1.356(10) . ? N30 Os1 2.060(6) . ? C31 C32 1.366(11) . ? C31 C34 1.463(11) . ? C33 C34 1.383(10) . ? N41 C42 1.340(10) . ? N41 C54 1.389(11) . ? N41 Os1 2.070(6) . ? C42 C43 1.402(12) . ? C43 C44 1.374(13) . ? C44 C53 1.334(12) . ? C45 C46 1.303(13) . ? C45 C53 1.469(13) . ? C46 C52 1.424(13) . ? C47 C48 1.337(13) . ? C47 C52 1.401(13) . ? C48 C49 1.398(14) . ? C49 N50 1.334(10) . ? N50 C51 1.373(10) . ? N50 Os1 2.069(7) . ? C51 C54 1.383(11) . ? C51 C52 1.439(13) . ? C53 C54 1.409(11) . ? N61 C62 1.341(11) . ? N61 C74 1.366(10) . ? N61 Os2 2.059(7) . ? C62 C63 1.388(14) . ? C63 C64 1.342(15) . ? C64 C73 1.405(13) . ? C65 C66 1.339(13) . ? C65 C73 1.401(13) . ? C66 C72 1.458(13) . ? C67 C68 1.344(12) . ? C67 C72 1.375(12) . ? C68 C69 1.386(12) . ? C69 N70 1.343(10) . ? N70 C71 1.374(10) . ? N70 Os2 2.072(6) . ? C71 C74 1.378(11) . ? C71 C72 1.419(12) . ? C73 C74 1.413(12) . ? N81 C82 1.358(10) . ? N81 C94 1.379(10) . ? N81 Os2 2.040(7) . ? C82 C83 1.381(13) . ? C83 C84 1.355(12) . ? C84 C93 1.411(12) . ? C85 C86 1.346(13) . ? C85 C93 1.432(12) . ? C86 C92 1.438(14) . ? C87 C88 1.348(16) . ? C87 C92 1.400(15) . ? C88 C89 1.422(14) . ? C89 N90 1.326(12) . ? N90 C91 1.381(11) . ? N90 Os2 2.056(7) . ? C91 C94 1.389(12) . ? C91 C92 1.421(12) . ? C93 C94 1.412(12) . ? N101 C114 1.335(10) . ? N101 C102 1.352(11) . ? N101 Os2 2.061(7) . ? C102 C103 1.412(14) . ? C103 C104 1.302(13) . ? C104 C113 1.373(14) . ? C105 C106 1.320(13) . ? C105 C113 1.409(14) . ? C106 C112 1.467(13) . ? C107 C108 1.356(14) . ? C107 C112 1.370(13) . ? C108 C109 1.395(12) . ? C109 N110 1.336(11) . ? N110 C111 1.400(12) . ? N110 Os2 2.076(7) . ? C111 C112 1.412(12) . ? C111 C114 1.432(13) . ? C113 C114 1.456(14) . ? P1 F11 1.534(7) . ? P1 F15 1.551(7) . ? P1 F14 1.575(7) . ? P1 F16 1.577(6) . ? P1 F13 1.586(6) . ? P1 F12 1.598(6) . ? P2 F21 1.541(9) . ? P2 F23 1.551(9) . ? P2 F26 1.564(8) . ? P2 F25 1.583(8) . ? P2 F22 1.585(9) . ? P2 F24 1.596(8) . ? P3 F34 1.531(8) . ? P3 F35 1.555(9) . ? P3 F32 1.556(9) . ? P3 F31 1.564(8) . ? P3 F33 1.569(8) . ? P3 F36 1.595(7) . ? P4 F46 1.518(9) . ? P4 F41 1.532(8) . ? P4 F45 1.555(8) . ? P4 F44 1.575(8) . ? P4 F43 1.587(9) . ? P4 F42 1.602(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C14 117.2(8) . . ? C2 N1 Os1 128.0(6) . . ? C14 N1 Os1 114.7(5) . . ? N1 C2 C3 123.6(9) . . ? C4 C3 C2 117.8(9) . . ? C3 C4 C13 120.7(9) . . ? C6 C5 C13 120.2(10) . . ? C5 C6 C12 124.6(10) . . ? C8 C7 C12 118.5(10) . . ? C7 C8 C9 120.9(11) . . ? N10 C9 C8 122.2(9) . . ? C9 N10 C11 116.9(7) . . ? C9 N10 Os1 128.6(6) . . ? C11 N10 Os1 113.7(6) . . ? N10 C11 C12 124.2(8) . . ? N10 C11 C14 117.4(7) . . ? C12 C11 C14 118.5(8) . . ? C11 C12 C7 117.4(9) . . ? C11 C12 C6 116.8(9) . . ? C7 C12 C6 125.9(9) . . ? C14 C13 C4 117.5(8) . . ? C14 C13 C5 117.5(8) . . ? C4 C13 C5 125.0(9) . . ? C13 C14 N1 123.1(8) . . ? C13 C14 C11 122.5(8) . . ? N1 C14 C11 114.3(7) . . ? C22 N21 C34 116.3(6) . . ? C22 N21 Os1 130.1(5) . . ? C34 N21 Os1 113.6(5) . . ? N21 C22 C23 124.0(8) . . ? C22 C23 C24 120.2(9) . . ? C33 C24 C23 116.6(9) . . ? C26 C25 C33 121.6(9) . . ? C25 C26 C32 122.9(10) . . ? C28 C27 C32 120.8(10) . . ? C27 C28 C29 118.8(10) . . ? N30 C29 C28 122.7(9) . . ? C31 N30 C29 115.2(7) . . ? C31 N30 Os1 116.4(5) . . ? C29 N30 Os1 128.3(6) . . ? N30 C31 C32 126.3(8) . . ? N30 C31 C34 114.2(7) . . ? C32 C31 C34 119.5(7) . . ? C31 C32 C27 116.1(8) . . ? C31 C32 C26 117.8(8) . . ? C27 C32 C26 126.2(9) . . ? C34 C33 C24 119.6(8) . . ? C34 C33 C25 117.8(8) . . ? C24 C33 C25 122.6(8) . . ? C33 C34 N21 123.2(7) . . ? C33 C34 C31 120.4(7) . . ? N21 C34 C31 116.4(6) . . ? C42 N41 C54 117.2(7) . . ? C42 N41 Os1 128.9(6) . . ? C54 N41 Os1 113.7(5) . . ? N41 C42 C43 123.6(9) . . ? C44 C43 C42 117.0(10) . . ? C53 C44 C43 122.3(10) . . ? C46 C45 C53 123.0(10) . . ? C45 C46 C52 122.8(11) . . ? C48 C47 C52 120.4(11) . . ? C47 C48 C49 121.4(11) . . ? N50 C49 C48 121.3(9) . . ? C49 N50 C51 118.6(8) . . ? C49 N50 Os1 128.9(6) . . ? C51 N50 Os1 112.4(6) . . ? N50 C51 C54 118.9(8) . . ? N50 C51 C52 121.9(8) . . ? C54 C51 C52 119.2(8) . . ? C47 C52 C46 126.7(10) . . ? C47 C52 C51 116.4(9) . . ? C46 C52 C51 116.9(9) . . ? C44 C53 C54 119.0(9) . . ? C44 C53 C45 127.0(9) . . ? C54 C53 C45 114.0(8) . . ? C51 C54 N41 115.0(8) . . ? C51 C54 C53 123.9(8) . . ? N41 C54 C53 120.9(7) . . ? C62 N61 C74 117.7(8) . . ? C62 N61 Os2 128.0(6) . . ? C74 N61 Os2 114.1(5) . . ? N61 C62 C63 122.7(10) . . ? C64 C63 C62 120.4(11) . . ? C63 C64 C73 119.4(12) . . ? C66 C65 C73 123.0(11) . . ? C65 C66 C72 121.6(10) . . ? C68 C67 C72 121.1(9) . . ? C67 C68 C69 119.9(9) . . ? N70 C69 C68 121.9(8) . . ? C69 N70 C71 118.5(7) . . ? C69 N70 Os2 128.8(6) . . ? C71 N70 Os2 112.7(5) . . ? N70 C71 C74 117.5(8) . . ? N70 C71 C72 120.9(7) . . ? C74 C71 C72 121.5(8) . . ? C67 C72 C71 117.7(9) . . ? C67 C72 C66 126.9(9) . . ? C71 C72 C66 115.3(8) . . ? C65 C73 C64 125.5(10) . . ? C65 C73 C74 116.6(9) . . ? C64 C73 C74 117.8(10) . . ? N61 C74 C71 116.3(8) . . ? N61 C74 C73 121.9(8) . . ? C71 C74 C73 121.8(8) . . ? C82 N81 C94 115.7(7) . . ? C82 N81 Os2 129.4(6) . . ? C94 N81 Os2 114.8(5) . . ? N81 C82 C83 123.5(8) . . ? C84 C83 C82 120.5(9) . . ? C83 C84 C93 119.6(10) . . ? C86 C85 C93 120.1(10) . . ? C85 C86 C92 123.2(10) . . ? C88 C87 C92 121.1(11) . . ? C87 C88 C89 119.0(12) . . ? N90 C89 C88 122.0(11) . . ? C89 N90 C91 119.3(8) . . ? C89 N90 Os2 128.3(7) . . ? C91 N90 Os2 112.4(6) . . ? N90 C91 C94 118.3(8) . . ? N90 C91 C92 121.0(8) . . ? C94 C91 C92 120.7(9) . . ? C87 C92 C91 117.5(10) . . ? C87 C92 C86 126.0(10) . . ? C91 C92 C86 116.5(9) . . ? C84 C93 C94 116.9(8) . . ? C84 C93 C85 125.0(9) . . ? C94 C93 C85 118.1(8) . . ? N81 C94 C91 114.8(8) . . ? N81 C94 C93 123.8(8) . . ? C91 C94 C93 121.4(8) . . ? C114 N101 C102 117.3(8) . . ? C114 N101 Os2 113.9(6) . . ? C102 N101 Os2 128.7(6) . . ? N101 C102 C103 119.5(9) . . ? C104 C103 C102 122.6(11) . . ? C103 C104 C113 121.8(12) . . ? C106 C105 C113 126.3(11) . . ? C105 C106 C112 119.9(10) . . ? C108 C107 C112 121.4(10) . . ? C107 C108 C109 119.2(10) . . ? N110 C109 C108 122.3(9) . . ? C109 N110 C111 118.1(7) . . ? C109 N110 Os2 128.9(7) . . ? C111 N110 Os2 113.0(6) . . ? N110 C111 C112 120.8(8) . . ? N110 C111 C114 114.7(8) . . ? C112 C111 C114 124.5(9) . . ? C107 C112 C111 118.0(9) . . ? C107 C112 C106 126.4(9) . . ? C111 C112 C106 115.6(8) . . ? C104 C113 C105 129.2(11) . . ? C104 C113 C114 113.9(9) . . ? C105 C113 C114 116.9(9) . . ? N101 C114 C111 118.3(9) . . ? N101 C114 C113 124.9(9) . . ? C111 C114 C113 116.7(8) . . ? N10 Os1 N30 93.8(3) . . ? N10 Os1 N50 97.3(3) . . ? N30 Os1 N50 95.4(3) . . ? N10 Os1 N41 91.8(2) . . ? N30 Os1 N41 172.6(3) . . ? N50 Os1 N41 79.1(3) . . ? N10 Os1 N21 170.7(3) . . ? N30 Os1 N21 79.3(2) . . ? N50 Os1 N21 89.6(3) . . ? N41 Os1 N21 95.7(2) . . ? N10 Os1 N1 79.3(3) . . ? N30 Os1 N1 88.9(3) . . ? N50 Os1 N1 174.7(2) . . ? N41 Os1 N1 96.8(3) . . ? N21 Os1 N1 94.2(2) . . ? N81 Os2 N90 79.6(3) . . ? N81 Os2 N61 91.8(3) . . ? N90 Os2 N61 94.6(3) . . ? N81 Os2 N101 173.0(3) . . ? N90 Os2 N101 96.5(3) . . ? N61 Os2 N101 94.3(3) . . ? N81 Os2 N70 96.9(3) . . ? N90 Os2 N70 172.4(3) . . ? N61 Os2 N70 78.7(2) . . ? N101 Os2 N70 87.7(3) . . ? N81 Os2 N110 94.2(3) . . ? N90 Os2 N110 88.5(3) . . ? N61 Os2 N110 173.6(3) . . ? N101 Os2 N110 79.8(3) . . ? N70 Os2 N110 98.6(2) . . ? F11 P1 F15 93.1(5) . . ? F11 P1 F14 174.7(5) . . ? F15 P1 F14 90.9(5) . . ? F11 P1 F16 93.3(4) . . ? F15 P1 F16 94.8(4) . . ? F14 P1 F16 89.9(4) . . ? F11 P1 F13 86.7(4) . . ? F15 P1 F13 88.5(4) . . ? F14 P1 F13 89.8(4) . . ? F16 P1 F13 176.7(4) . . ? F11 P1 F12 89.1(5) . . ? F15 P1 F12 176.7(5) . . ? F14 P1 F12 86.8(4) . . ? F16 P1 F12 87.5(4) . . ? F13 P1 F12 89.2(4) . . ? F21 P2 F23 92.8(6) . . ? F21 P2 F26 87.0(5) . . ? F23 P2 F26 178.9(6) . . ? F21 P2 F25 91.2(5) . . ? F23 P2 F25 90.8(5) . . ? F26 P2 F25 88.2(5) . . ? F21 P2 F22 89.7(5) . . ? F23 P2 F22 88.0(6) . . ? F26 P2 F22 93.1(6) . . ? F25 P2 F22 178.5(6) . . ? F21 P2 F24 175.2(6) . . ? F23 P2 F24 91.1(6) . . ? F26 P2 F24 89.1(5) . . ? F25 P2 F24 91.5(5) . . ? F22 P2 F24 87.7(5) . . ? F34 P3 F35 91.9(7) . . ? F34 P3 F32 91.9(6) . . ? F35 P3 F32 176.1(7) . . ? F34 P3 F31 179.6(6) . . ? F35 P3 F31 88.1(5) . . ? F32 P3 F31 88.1(6) . . ? F34 P3 F33 90.1(5) . . ? F35 P3 F33 90.0(5) . . ? F32 P3 F33 90.9(5) . . ? F31 P3 F33 90.2(5) . . ? F34 P3 F36 91.7(4) . . ? F35 P3 F36 90.8(5) . . ? F32 P3 F36 88.2(5) . . ? F31 P3 F36 87.9(4) . . ? F33 P3 F36 178.0(5) . . ? F46 P4 F41 90.6(6) . . ? F46 P4 F45 91.5(6) . . ? F41 P4 F45 94.2(5) . . ? F46 P4 F44 90.5(6) . . ? F41 P4 F44 176.3(5) . . ? F45 P4 F44 89.3(5) . . ? F46 P4 F43 176.3(6) . . ? F41 P4 F43 91.1(5) . . ? F45 P4 F43 91.6(5) . . ? F44 P4 F43 87.6(5) . . ? F46 P4 F42 90.3(6) . . ? F41 P4 F42 87.1(5) . . ? F45 P4 F42 177.8(5) . . ? F44 P4 F42 89.4(5) . . ? F43 P4 F42 86.5(5) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.975 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.129 data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 249786' # data_370801z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 F12 N6 Os P2' _chemical_formula_weight 1020.75 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' 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' Os Os -1.2165 7.6030 '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 36.943(4) _cell_length_b 16.1178(15) _cell_length_c 12.1037(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.993(2) _cell_angle_gamma 90.00 _cell_volume 7074.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8093 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 27.94 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 3.798 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5172 _exptl_absorpt_correction_T_max 0.5172 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21362 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.94 _reflns_number_total 8093 _reflns_number_gt 6898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0371P)^2^+11.9397P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8093 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.89147(9) 0.10938(19) 0.0663(3) 0.0431(7) Uani 1 1 d . . . C2 C 0.91195(11) 0.0907(3) -0.0108(3) 0.0516(10) Uani 1 1 d . . . H2 H 0.9210 0.1337 -0.0493 0.062 Uiso 1 1 calc R . . C3 C 0.92017(13) 0.0088(3) -0.0350(4) 0.0645(12) Uani 1 1 d . . . H3 H 0.9348 -0.0020 -0.0879 0.077 Uiso 1 1 calc R . . C4 C 0.90676(14) -0.0552(3) 0.0190(5) 0.0716(15) Uani 1 1 d . . . H4 H 0.9121 -0.1097 0.0027 0.086 Uiso 1 1 calc R . . C5 C 0.86925(18) -0.1002(3) 0.1616(6) 0.0864(18) Uani 1 1 d . . . H5 H 0.8736 -0.1560 0.1499 0.104 Uiso 1 1 calc R . . C6 C 0.84861(17) -0.0792(4) 0.2361(6) 0.089(2) Uani 1 1 d . . . H6 H 0.8385 -0.1212 0.2734 0.107 Uiso 1 1 calc R . . C7 C 0.81999(15) 0.0308(4) 0.3377(4) 0.0824(19) Uani 1 1 d . . . H7 H 0.8087 -0.0081 0.3767 0.099 Uiso 1 1 calc R . . C8 C 0.81573(14) 0.1135(4) 0.3551(4) 0.0772(16) Uani 1 1 d . . . H8 H 0.8017 0.1311 0.4069 0.093 Uiso 1 1 calc R . . C9 C 0.83221(12) 0.1715(3) 0.2960(4) 0.0634(12) Uani 1 1 d . . . H9 H 0.8291 0.2276 0.3098 0.076 Uiso 1 1 calc R . . N10 N 0.85249(9) 0.1499(2) 0.2197(3) 0.0478(8) Uani 1 1 d . . . C11 C 0.85700(11) 0.0669(3) 0.2026(3) 0.0502(10) Uani 1 1 d . . . C12 C 0.84134(14) 0.0052(3) 0.2610(4) 0.0720(16) Uani 1 1 d . . . C13 C 0.88508(14) -0.0385(3) 0.0986(4) 0.0646(13) Uani 1 1 d . . . C14 C 0.87828(10) 0.0449(2) 0.1210(3) 0.0479(9) Uani 1 1 d . . . N21 N 0.83346(9) 0.22900(18) -0.0105(3) 0.0417(7) Uani 1 1 d . . . C22 C 0.79981(11) 0.1952(3) -0.0152(4) 0.0541(10) Uani 1 1 d . . . H22 H 0.7946 0.1684 0.0480 0.065 Uiso 1 1 calc R . . C23 C 0.77253(13) 0.1992(3) -0.1127(4) 0.0675(13) Uani 1 1 d . . . H23 H 0.7497 0.1747 -0.1135 0.081 Uiso 1 1 calc R . . C24 C 0.77910(14) 0.2392(3) -0.2074(4) 0.0665(13) Uani 1 1 d . . . H24 H 0.7608 0.2431 -0.2715 0.080 Uiso 1 1 calc R . . C25 C 0.82450(15) 0.3128(3) -0.2994(4) 0.0667(13) Uani 1 1 d . . . H25 H 0.8075 0.3173 -0.3664 0.080 Uiso 1 1 calc R . . C26 C 0.85910(17) 0.3434(3) -0.2935(4) 0.0721(14) Uani 1 1 d . . . H26 H 0.8653 0.3680 -0.3569 0.086 Uiso 1 1 calc R . . C27 C 0.92181(14) 0.3724(3) -0.1773(4) 0.0636(12) Uani 1 1 d . . . H27 H 0.9296 0.3990 -0.2369 0.076 Uiso 1 1 calc R . . C28 C 0.94516(13) 0.3657(3) -0.0748(4) 0.0573(11) Uani 1 1 d . . . H28 H 0.9687 0.3885 -0.0643 0.069 Uiso 1 1 calc R . . C29 C 0.93347(11) 0.3248(2) 0.0133(3) 0.0465(9) Uani 1 1 d . . . H29 H 0.9496 0.3211 0.0822 0.056 Uiso 1 1 calc R . . N30 N 0.89998(9) 0.29059(17) 0.0032(2) 0.0367(6) Uani 1 1 d . . . C31 C 0.87638(11) 0.2996(2) -0.0982(3) 0.0407(8) Uani 1 1 d . . . C32 C 0.88629(13) 0.3388(2) -0.1915(3) 0.0535(10) Uani 1 1 d . . . C33 C 0.81392(13) 0.2741(2) -0.2053(4) 0.0544(11) Uani 1 1 d . . . C34 C 0.84029(11) 0.2669(2) -0.1049(3) 0.0416(8) Uani 1 1 d . . . N41 N 0.86726(9) 0.3328(2) 0.2000(3) 0.0444(7) Uani 1 1 d . . . C42 C 0.83990(12) 0.3874(3) 0.1689(4) 0.0557(10) Uani 1 1 d . . . H42 H 0.8243 0.3809 0.0995 0.067 Uiso 1 1 calc R . . C43 C 0.83414(14) 0.4534(3) 0.2371(5) 0.0705(13) Uani 1 1 d . . . H43 H 0.8144 0.4892 0.2137 0.085 Uiso 1 1 calc R . . C44 C 0.85711(14) 0.4661(3) 0.3381(4) 0.0674(13) Uani 1 1 d . . . H44 H 0.8529 0.5101 0.3838 0.081 Uiso 1 1 calc R . . C45 C 0.91309(15) 0.4199(3) 0.4763(4) 0.0698(14) Uani 1 1 d . . . H45 H 0.9111 0.4635 0.5250 0.084 Uiso 1 1 calc R . . C46 C 0.94046(14) 0.3648(3) 0.5045(4) 0.0657(13) Uani 1 1 d . . . H46 H 0.9567 0.3710 0.5729 0.079 Uiso 1 1 calc R . . C47 C 0.97310(14) 0.2357(3) 0.4581(4) 0.0644(13) Uani 1 1 d . . . H47 H 0.9898 0.2370 0.5261 0.077 Uiso 1 1 calc R . . C48 C 0.97501(12) 0.1750(3) 0.3822(4) 0.0620(12) Uani 1 1 d . . . H48 H 0.9934 0.1351 0.3977 0.074 Uiso 1 1 calc R . . C49 C 0.94964(11) 0.1717(3) 0.2807(3) 0.0513(9) Uani 1 1 d . . . H49 H 0.9517 0.1294 0.2300 0.062 Uiso 1 1 calc R . . N50 N 0.92248(9) 0.22731(18) 0.2541(3) 0.0415(7) Uani 1 1 d . . . C51 C 0.92040(11) 0.2897(2) 0.3302(3) 0.0430(9) Uani 1 1 d . . . C52 C 0.94555(12) 0.2968(3) 0.4331(3) 0.0532(10) Uani 1 1 d . . . C53 C 0.88677(13) 0.4132(3) 0.3726(3) 0.0554(10) Uani 1 1 d . . . C54 C 0.89104(11) 0.3468(2) 0.3004(3) 0.0458(9) Uani 1 1 d . . . Os Os 0.878111(4) 0.224654(8) 0.120779(10) 0.03660(6) Uani 1 1 d . . . P1 P 0.74056(4) -0.04024(15) 0.05487(12) 0.0945(6) Uani 1 1 d . . . F11 F 0.77693(12) 0.0094(3) 0.0628(4) 0.1427(18) Uani 1 1 d . . . F12 F 0.71603(19) 0.0351(5) 0.0522(5) 0.211(3) Uani 1 1 d . . . F13 F 0.73737(12) -0.0440(5) -0.0755(3) 0.195(3) Uani 1 1 d . . . F14 F 0.70546(16) -0.0929(6) 0.0429(5) 0.260(5) Uani 1 1 d . . . F15 F 0.76563(19) -0.1191(4) 0.0583(5) 0.195(3) Uani 1 1 d . . . F16 F 0.74474(12) -0.0437(3) 0.1842(3) 0.1227(14) Uani 1 1 d . . . P2 P 1.0000 0.46038(9) 0.2500 0.0420(3) Uani 1 2 d S . . F21 F 0.99695(9) 0.46053(19) 0.3789(2) 0.0766(8) Uani 1 1 d . . . F22 F 1.0000 0.3602(2) 0.2500 0.0634(9) Uani 1 2 d S . . F23 F 0.95625(7) 0.46043(17) 0.2149(2) 0.0682(7) Uani 1 1 d . . . F24 F 1.0000 0.5606(2) 0.2500 0.0622(9) Uani 1 2 d S . . P3 P 1.0000 -0.08426(12) 0.2500 0.0721(5) Uani 1 2 d S . . F31 F 0.99978(15) -0.0842(4) 0.1220(3) 0.156(2) Uani 1 1 d . . . F32 F 0.97020(15) -0.1527(3) 0.2243(5) 0.177(2) Uani 1 1 d . . . F33 F 0.96900(13) -0.0170(3) 0.2332(4) 0.1390(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0401(17) 0.0405(16) 0.0455(17) 0.0026(13) 0.0001(13) -0.0058(13) C2 0.049(2) 0.058(2) 0.047(2) -0.0042(18) 0.0048(17) 0.0023(19) C3 0.058(3) 0.064(3) 0.066(3) -0.016(2) -0.003(2) 0.011(2) C4 0.069(3) 0.043(2) 0.090(4) -0.008(2) -0.017(3) 0.008(2) C5 0.090(4) 0.047(3) 0.108(5) 0.023(3) -0.019(4) -0.015(3) C6 0.081(4) 0.073(4) 0.100(4) 0.044(3) -0.018(3) -0.032(3) C7 0.063(3) 0.123(5) 0.058(3) 0.036(3) 0.003(2) -0.038(3) C8 0.058(3) 0.119(5) 0.058(3) 0.015(3) 0.018(2) -0.023(3) C9 0.053(3) 0.086(3) 0.053(2) 0.004(2) 0.016(2) -0.015(2) N10 0.0417(18) 0.059(2) 0.0419(17) 0.0057(15) 0.0066(13) -0.0121(15) C11 0.041(2) 0.057(2) 0.045(2) 0.0175(18) -0.0106(17) -0.0155(18) C12 0.059(3) 0.081(3) 0.065(3) 0.036(3) -0.016(2) -0.031(3) C13 0.061(3) 0.047(2) 0.074(3) 0.007(2) -0.019(2) -0.003(2) C14 0.042(2) 0.0419(19) 0.052(2) 0.0065(16) -0.0107(17) -0.0109(16) N21 0.0377(16) 0.0421(17) 0.0446(17) -0.0046(13) 0.0060(13) -0.0028(13) C22 0.041(2) 0.061(2) 0.059(2) -0.008(2) 0.0092(18) -0.0073(19) C23 0.040(2) 0.087(3) 0.072(3) -0.018(3) -0.001(2) -0.006(2) C24 0.055(3) 0.068(3) 0.065(3) -0.014(2) -0.018(2) 0.010(2) C25 0.090(4) 0.056(3) 0.044(2) 0.003(2) -0.012(2) 0.007(3) C26 0.110(4) 0.059(3) 0.044(2) 0.017(2) 0.005(2) 0.009(3) C27 0.086(3) 0.055(3) 0.054(2) 0.007(2) 0.024(2) -0.012(2) C28 0.059(3) 0.054(2) 0.063(3) 0.005(2) 0.021(2) -0.011(2) C29 0.050(2) 0.042(2) 0.047(2) 0.0006(16) 0.0092(17) -0.0069(17) N30 0.0439(17) 0.0326(14) 0.0342(14) 0.0009(11) 0.0087(12) -0.0023(12) C31 0.050(2) 0.0323(16) 0.0377(18) 0.0013(14) 0.0028(15) 0.0017(15) C32 0.077(3) 0.042(2) 0.042(2) 0.0036(16) 0.0109(19) -0.002(2) C33 0.060(3) 0.046(2) 0.049(2) -0.0058(17) -0.011(2) 0.0131(18) C34 0.045(2) 0.0352(18) 0.0410(19) -0.0063(15) 0.0002(16) 0.0041(15) N41 0.0426(17) 0.0437(17) 0.0472(17) 0.0018(14) 0.0093(14) -0.0047(14) C42 0.045(2) 0.054(2) 0.068(3) -0.003(2) 0.010(2) 0.0016(19) C43 0.059(3) 0.061(3) 0.096(4) -0.009(3) 0.027(3) 0.004(2) C44 0.075(3) 0.057(3) 0.078(3) -0.022(2) 0.034(3) -0.010(2) C45 0.087(4) 0.082(3) 0.048(2) -0.024(2) 0.031(2) -0.032(3) C46 0.071(3) 0.086(3) 0.039(2) -0.012(2) 0.009(2) -0.031(3) C47 0.054(3) 0.092(4) 0.041(2) 0.018(2) -0.0055(19) -0.016(2) C48 0.048(2) 0.075(3) 0.059(3) 0.020(2) -0.001(2) -0.003(2) C49 0.047(2) 0.054(2) 0.050(2) 0.0127(19) 0.0032(17) -0.0020(19) N50 0.0427(17) 0.0458(18) 0.0357(15) 0.0051(13) 0.0064(13) -0.0089(13) C51 0.045(2) 0.049(2) 0.0358(18) 0.0016(15) 0.0111(15) -0.0133(16) C52 0.054(3) 0.070(3) 0.0363(19) 0.0042(18) 0.0093(17) -0.021(2) C53 0.064(3) 0.058(2) 0.052(2) -0.0094(19) 0.027(2) -0.021(2) C54 0.049(2) 0.053(2) 0.0393(19) -0.0032(16) 0.0167(16) -0.0139(18) Os 0.03525(9) 0.04048(9) 0.03385(8) 0.00241(5) 0.00607(5) -0.00488(5) P1 0.0551(8) 0.1724(19) 0.0552(8) -0.0182(9) 0.0081(6) -0.0120(10) F11 0.111(3) 0.194(5) 0.116(3) 0.024(3) 0.005(3) -0.062(3) F12 0.209(7) 0.249(8) 0.172(5) 0.045(5) 0.025(5) 0.118(6) F13 0.083(3) 0.440(11) 0.060(2) -0.010(4) 0.0090(19) -0.006(4) F14 0.154(5) 0.466(13) 0.189(5) -0.206(7) 0.110(4) -0.182(6) F15 0.240(7) 0.170(5) 0.216(6) 0.001(4) 0.151(6) 0.037(5) F16 0.128(3) 0.180(4) 0.064(2) -0.011(2) 0.026(2) -0.017(3) P2 0.0497(8) 0.0407(7) 0.0369(7) 0.000 0.0118(6) 0.000 F21 0.105(2) 0.087(2) 0.0430(14) 0.0008(13) 0.0275(14) -0.0081(17) F22 0.071(2) 0.0399(17) 0.079(2) 0.000 0.0126(19) 0.000 F23 0.0505(15) 0.0653(16) 0.0873(19) -0.0076(14) 0.0096(13) 0.0022(12) F24 0.075(2) 0.0429(18) 0.070(2) 0.000 0.0158(19) 0.000 P3 0.0751(13) 0.0603(10) 0.0706(12) 0.000 -0.0124(10) 0.000 F31 0.179(5) 0.202(5) 0.082(3) -0.045(3) 0.013(3) -0.045(4) F32 0.150(4) 0.122(4) 0.247(6) -0.010(4) 0.008(4) -0.065(3) F33 0.149(4) 0.122(3) 0.123(3) -0.008(3) -0.033(3) 0.059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.342(5) . ? N1 C14 1.371(5) . ? N1 Os 2.063(3) . ? C2 C3 1.398(6) . ? C3 C4 1.365(7) . ? C4 C13 1.391(7) . ? C5 C6 1.331(9) . ? C5 C13 1.443(8) . ? C6 C12 1.430(9) . ? C7 C8 1.363(9) . ? C7 C12 1.390(8) . ? C8 C9 1.387(7) . ? C9 N10 1.342(5) . ? N10 C11 1.368(6) . ? N10 Os 2.053(3) . ? C11 C12 1.407(6) . ? C11 C14 1.420(6) . ? C13 C14 1.403(6) . ? N21 C22 1.349(5) . ? N21 C34 1.362(5) . ? N21 Os 2.061(3) . ? C22 C23 1.400(6) . ? C23 C24 1.376(8) . ? C24 C33 1.400(7) . ? C25 C26 1.360(7) . ? C25 C33 1.417(7) . ? C26 C32 1.437(6) . ? C27 C28 1.374(6) . ? C27 C32 1.399(6) . ? C28 C29 1.390(5) . ? C29 N30 1.339(5) . ? N30 C31 1.371(4) . ? N30 Os 2.061(3) . ? C31 C32 1.401(5) . ? C31 C34 1.422(5) . ? C33 C34 1.410(5) . ? N41 C42 1.339(5) . ? N41 C54 1.376(5) . ? N41 Os 2.065(3) . ? C42 C43 1.387(6) . ? C43 C44 1.365(7) . ? C44 C53 1.388(7) . ? C45 C46 1.340(7) . ? C45 C53 1.438(6) . ? C46 C52 1.430(7) . ? C47 C48 1.353(7) . ? C47 C52 1.407(7) . ? C48 C49 1.397(5) . ? C49 N50 1.339(5) . ? N50 C51 1.376(5) . ? N50 Os 2.070(3) . ? C51 C52 1.409(5) . ? C51 C54 1.416(6) . ? C53 C54 1.409(6) . ? P1 F12 1.512(6) . ? P1 F14 1.534(5) . ? P1 F16 1.544(4) . ? P1 F11 1.551(4) . ? P1 F13 1.561(4) . ? P1 F15 1.569(6) . ? P2 F21 1.586(2) 2_755 ? P2 F21 1.586(2) . ? P2 F23 1.591(3) . ? P2 F23 1.591(3) 2_755 ? P2 F22 1.614(3) . ? P2 F24 1.615(4) . ? P3 F32 1.547(4) . ? P3 F32 1.547(4) 2_755 ? P3 F31 1.547(4) . ? P3 F31 1.547(4) 2_755 ? P3 F33 1.562(4) 2_755 ? P3 F33 1.562(4) . ? 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 C2 N1 C14 117.7(4) . . ? C2 N1 Os 128.7(3) . . ? C14 N1 Os 113.6(3) . . ? N1 C2 C3 122.0(4) . . ? C4 C3 C2 120.1(5) . . ? C3 C4 C13 119.6(4) . . ? C6 C5 C13 121.7(6) . . ? C5 C6 C12 122.6(5) . . ? C8 C7 C12 119.4(5) . . ? C7 C8 C9 120.2(5) . . ? N10 C9 C8 122.5(5) . . ? C9 N10 C11 117.3(4) . . ? C9 N10 Os 129.0(3) . . ? C11 N10 Os 113.8(3) . . ? N10 C11 C12 122.8(5) . . ? N10 C11 C14 116.7(3) . . ? C12 C11 C14 120.5(5) . . ? C7 C12 C11 117.7(5) . . ? C7 C12 C6 125.2(5) . . ? C11 C12 C6 117.1(6) . . ? C4 C13 C14 117.9(5) . . ? C4 C13 C5 125.3(5) . . ? C14 C13 C5 116.9(6) . . ? N1 C14 C13 122.7(4) . . ? N1 C14 C11 116.2(4) . . ? C13 C14 C11 121.2(4) . . ? C22 N21 C34 117.6(3) . . ? C22 N21 Os 127.9(3) . . ? C34 N21 Os 114.4(2) . . ? N21 C22 C23 121.8(4) . . ? C24 C23 C22 120.7(5) . . ? C23 C24 C33 118.7(4) . . ? C26 C25 C33 121.2(4) . . ? C25 C26 C32 121.5(4) . . ? C28 C27 C32 119.5(4) . . ? C27 C28 C29 119.8(4) . . ? N30 C29 C28 122.8(4) . . ? C29 N30 C31 117.2(3) . . ? C29 N30 Os 128.8(2) . . ? C31 N30 Os 114.0(2) . . ? N30 C31 C32 123.4(4) . . ? N30 C31 C34 116.1(3) . . ? C32 C31 C34 120.5(3) . . ? C27 C32 C31 117.3(4) . . ? C27 C32 C26 124.8(4) . . ? C31 C32 C26 117.9(4) . . ? C24 C33 C34 117.7(4) . . ? C24 C33 C25 123.7(4) . . ? C34 C33 C25 118.5(4) . . ? N21 C34 C33 123.5(4) . . ? N21 C34 C31 116.1(3) . . ? C33 C34 C31 120.3(4) . . ? C42 N41 C54 117.5(4) . . ? C42 N41 Os 128.9(3) . . ? C54 N41 Os 113.6(3) . . ? N41 C42 C43 122.0(4) . . ? C44 C43 C42 120.6(5) . . ? C43 C44 C53 119.8(4) . . ? C46 C45 C53 121.7(4) . . ? C45 C46 C52 122.2(4) . . ? C48 C47 C52 119.3(4) . . ? C47 C48 C49 120.8(4) . . ? N50 C49 C48 122.1(4) . . ? C49 N50 C51 117.6(3) . . ? C49 N50 Os 128.3(3) . . ? C51 N50 Os 113.6(3) . . ? N50 C51 C52 122.6(4) . . ? N50 C51 C54 116.3(3) . . ? C52 C51 C54 121.1(4) . . ? C47 C52 C51 117.5(4) . . ? C47 C52 C46 125.4(4) . . ? C51 C52 C46 117.1(4) . . ? C44 C53 C54 117.1(4) . . ? C44 C53 C45 125.4(4) . . ? C54 C53 C45 117.5(4) . . ? N41 C54 C53 123.0(4) . . ? N41 C54 C51 116.6(3) . . ? C53 C54 C51 120.4(4) . . ? N10 Os N30 172.17(12) . . ? N10 Os N21 94.54(12) . . ? N30 Os N21 79.14(12) . . ? N10 Os N1 79.79(13) . . ? N30 Os N1 95.41(12) . . ? N21 Os N1 89.38(12) . . ? N10 Os N41 94.20(13) . . ? N30 Os N41 91.24(11) . . ? N21 Os N41 97.55(12) . . ? N1 Os N41 171.20(12) . . ? N10 Os N50 86.67(12) . . ? N30 Os N50 99.88(12) . . ? N21 Os N50 176.77(12) . . ? N1 Os N50 93.78(12) . . ? N41 Os N50 79.37(12) . . ? F12 P1 F14 87.1(4) . . ? F12 P1 F16 89.7(3) . . ? F14 P1 F16 89.7(3) . . ? F12 P1 F11 95.5(4) . . ? F14 P1 F11 176.8(4) . . ? F16 P1 F11 92.2(2) . . ? F12 P1 F13 94.6(4) . . ? F14 P1 F13 89.1(3) . . ? F16 P1 F13 175.5(4) . . ? F11 P1 F13 88.9(3) . . ? F12 P1 F15 179.3(4) . . ? F14 P1 F15 92.2(5) . . ? F16 P1 F15 90.0(3) . . ? F11 P1 F15 85.2(3) . . ? F13 P1 F15 85.7(4) . . ? F21 P2 F21 179.8(3) 2_755 . ? F21 P2 F23 89.81(16) 2_755 . ? F21 P2 F23 90.19(16) . . ? F21 P2 F23 90.19(16) 2_755 2_755 ? F21 P2 F23 89.81(16) . 2_755 ? F23 P2 F23 179.9(2) . 2_755 ? F21 P2 F22 90.09(12) 2_755 . ? F21 P2 F22 90.09(12) . . ? F23 P2 F22 90.03(11) . . ? F23 P2 F22 90.03(11) 2_755 . ? F21 P2 F24 89.91(12) 2_755 . ? F21 P2 F24 89.91(12) . . ? F23 P2 F24 89.97(11) . . ? F23 P2 F24 89.97(11) 2_755 . ? F22 P2 F24 180.000(1) . . ? F32 P3 F32 89.1(5) . 2_755 ? F32 P3 F31 86.1(3) . . ? F32 P3 F31 94.0(3) 2_755 . ? F32 P3 F31 94.0(3) . 2_755 ? F32 P3 F31 86.1(3) 2_755 2_755 ? F31 P3 F31 179.9(6) . 2_755 ? F32 P3 F33 175.4(3) . 2_755 ? F32 P3 F33 89.6(3) 2_755 2_755 ? F31 P3 F33 89.6(3) . 2_755 ? F31 P3 F33 90.3(3) 2_755 2_755 ? F32 P3 F33 89.6(3) . . ? F32 P3 F33 175.4(3) 2_755 . ? F31 P3 F33 90.3(3) . . ? F31 P3 F33 89.6(3) 2_755 . ? F33 P3 F33 92.1(4) 2_755 . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.459 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.096