Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_total _journal_coden_Cambridge 182 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Kay Severin' _publ_contact_author_address ; Institut de Chimie Moleculaire et Biologique Ecole Polytechnique Federale de Lausanne 1015 Lausanne Switzerland ; _publ_contact_author_email 'kay.severin@epfl.ch' _publ_contact_author_fax '+41 21 693 9305' _publ_contact_author_phone '+41 21 693 9302' _publ_section_title ; Encapsulation of molecular Na2SiF6 by two metallacrown complexes ; loop_ _publ_author_name _publ_author_address 'Lehaire, Marie-Line' ; Institut de Chimie Moleculaire et Biologique Ecole Polytechnique Federale de Lausanne 1015 Lausanne Switzerland ; 'Scopelliti, Rosario' ; Institut de Chimie Moleculaire et Biologique Ecole Polytechnique Federale de Lausanne 1015 Lausanne Switzerland ; 'Severin, Kay' ; Institut de Chimie Moleculaire et Biologique Ecole Polytechnique Federale de Lausanne 1015 Lausanne Switzerland ; data_2 _database_code_CSD 193869 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H51 B F4 N3 Na O6 Ru3, 2(C6 H6), 0.5(C5 H12)' _chemical_formula_sum 'C59.50 H69 B F4 N3 Na O6 Ru3' _chemical_formula_weight 1335.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6792(5) _cell_length_b 14.5923(8) _cell_length_c 19.1853(11) _cell_angle_alpha 104.577(5) _cell_angle_beta 90.350(4) _cell_angle_gamma 93.685(4) _cell_volume 2886.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 7765 _cell_measurement_theta_min 2.06635 _cell_measurement_theta_max 27.70905 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1358 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7825 _exptl_absorpt_correction_T_max 0.9185 _exptl_absorpt_process_details ? _exptl_special_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_ambient_temperature 143(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 detector Kuma4CCD/Sapphire' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17183 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8932 _reflns_number_gt 7460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8932 _refine_ls_number_parameters 711 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.099 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.09836(3) 0.30883(2) 0.347276(17) 0.01898(11) Uani 1 1 d . . . Ru2 Ru 0.41655(3) 0.16581(2) 0.132526(17) 0.01895(11) Uani 1 1 d . . . Ru3 Ru 0.50739(3) 0.12606(2) 0.399287(17) 0.01785(11) Uani 1 1 d . . . Na1 Na 0.41491(15) 0.28612(11) 0.30983(9) 0.0218(4) Uani 1 1 d . . . F1 F 0.6230(3) 0.36817(19) 0.31286(15) 0.0354(7) Uani 1 1 d . . . F2 F 0.4561(3) 0.4524(2) 0.3324(2) 0.0712(12) Uani 1 1 d . . . F3 F 0.6405(4) 0.5235(3) 0.3101(2) 0.0743(12) Uani 1 1 d . . . F4 F 0.6146(5) 0.4870(3) 0.4141(2) 0.0953(16) Uani 1 1 d . . . O1 O 0.2177(2) 0.2571(2) 0.26095(14) 0.0198(6) Uani 1 1 d . . . O2 O -0.0247(2) 0.2141(2) 0.27881(14) 0.0205(6) Uani 1 1 d . . . O3 O 0.4604(3) 0.14719(19) 0.23417(15) 0.0201(6) Uani 1 1 d . . . O4 O 0.4190(3) 0.0203(2) 0.10874(15) 0.0222(7) Uani 1 1 d . . . O5 O 0.3515(2) 0.2052(2) 0.39070(15) 0.0197(6) Uani 1 1 d . . . O6 O 0.3704(3) 0.0519(2) 0.44118(15) 0.0234(7) Uani 1 1 d . . . N1 N 0.2253(3) 0.1352(3) 0.15740(18) 0.0211(8) Uani 1 1 d . . . N2 N 0.4417(3) 0.0327(2) 0.29858(18) 0.0196(8) Uani 1 1 d . . . N3 N 0.1342(3) 0.1862(2) 0.38464(18) 0.0194(8) Uani 1 1 d . . . C1 C 0.1622(4) 0.1845(3) 0.2138(2) 0.0182(9) Uani 1 1 d . . . C2 C 0.0322(4) 0.1599(3) 0.2232(2) 0.0186(9) Uani 1 1 d . . . C3 C -0.0277(4) 0.0842(3) 0.1746(2) 0.0259(10) Uani 1 1 d . . . H3 H -0.1133 0.0660 0.1804 0.031 Uiso 1 1 calc R . . C4 C 0.0399(4) 0.0341(4) 0.1160(3) 0.0342(12) Uani 1 1 d . . . H4 H -0.0003 -0.0178 0.0813 0.041 Uiso 1 1 calc R . . C5 C 0.1630(4) 0.0603(3) 0.1093(2) 0.0285(11) Uani 1 1 d . . . H5 H 0.2075 0.0253 0.0697 0.034 Uiso 1 1 calc R . . C6 C 0.4386(4) 0.0578(3) 0.2358(2) 0.0184(9) Uani 1 1 d . . . C7 C 0.4175(4) -0.0114(3) 0.1682(2) 0.0209(9) Uani 1 1 d . . . C8 C 0.4005(5) -0.1057(3) 0.1685(2) 0.0313(11) Uani 1 1 d . . . H8 H 0.3882 -0.1534 0.1246 0.038 Uiso 1 1 calc R . . C9 C 0.4016(5) -0.1302(3) 0.2347(3) 0.0368(12) Uani 1 1 d . . . H9 H 0.3895 -0.1948 0.2360 0.044 Uiso 1 1 calc R . . C10 C 0.4200(4) -0.0614(3) 0.2965(2) 0.0283(10) Uani 1 1 d . . . H10 H 0.4177 -0.0793 0.3408 0.034 Uiso 1 1 calc R . . C11 C 0.2461(4) 0.1574(3) 0.3995(2) 0.0187(9) Uani 1 1 d . . . C12 C 0.2549(4) 0.0760(3) 0.4270(2) 0.0214(10) Uani 1 1 d . . . C13 C 0.1473(4) 0.0251(4) 0.4386(2) 0.0294(11) Uani 1 1 d . . . H13 H 0.1515 -0.0300 0.4562 0.035 Uiso 1 1 calc R . . C14 C 0.0302(4) 0.0572(4) 0.4237(3) 0.0317(12) Uani 1 1 d . . . H14 H -0.0457 0.0245 0.4322 0.038 Uiso 1 1 calc R . . C15 C 0.0270(4) 0.1350(3) 0.3971(2) 0.0247(10) Uani 1 1 d . . . H15 H -0.0523 0.1551 0.3867 0.030 Uiso 1 1 calc R . . C16 C 0.1036(5) 0.3920(3) 0.4603(2) 0.0336(12) Uani 1 1 d . . . C17 C -0.0197(4) 0.3819(3) 0.4321(2) 0.0301(11) Uani 1 1 d . . . H17 H -0.0856 0.3581 0.4571 0.036 Uiso 1 1 calc R . . C18 C -0.0479(4) 0.4068(3) 0.3666(2) 0.0277(11) Uani 1 1 d . . . H18 H -0.1320 0.3985 0.3485 0.033 Uiso 1 1 calc R . . C19 C 0.0477(4) 0.4438(3) 0.3280(2) 0.0249(10) Uani 1 1 d . . . C20 C 0.1718(4) 0.4528(3) 0.3580(3) 0.0294(11) Uani 1 1 d . . . H20 H 0.2384 0.4756 0.3329 0.035 Uiso 1 1 calc R . . C21 C 0.2005(4) 0.4296(3) 0.4231(2) 0.0309(11) Uani 1 1 d . . . H21 H 0.2841 0.4391 0.4419 0.037 Uiso 1 1 calc R . . C22 C 0.1334(6) 0.3582(4) 0.5267(3) 0.0472(15) Uani 1 1 d . . . H22A H 0.2218 0.3440 0.5267 0.071 Uiso 1 1 calc R . . H22B H 0.0802 0.3008 0.5264 0.071 Uiso 1 1 calc R . . H22C H 0.1174 0.4079 0.5700 0.071 Uiso 1 1 calc R . . C23 C 0.0217(5) 0.4689(3) 0.2574(2) 0.0309(11) Uani 1 1 d . . . H23 H 0.1020 0.4645 0.2306 0.037 Uiso 1 1 calc R . . C24 C -0.0135(6) 0.5722(4) 0.2718(3) 0.0490(15) Uani 1 1 d . . . H24A H -0.0965 0.5780 0.2933 0.074 Uiso 1 1 calc R . . H24B H -0.0152 0.5912 0.2263 0.074 Uiso 1 1 calc R . . H24C H 0.0488 0.6135 0.3049 0.074 Uiso 1 1 calc R . . C25 C -0.0764(6) 0.4027(4) 0.2086(3) 0.0484(15) Uani 1 1 d . . . H25A H -0.0602 0.3368 0.2065 0.073 Uiso 1 1 calc R . . H25B H -0.0720 0.4129 0.1600 0.073 Uiso 1 1 calc R . . H25C H -0.1600 0.4159 0.2277 0.073 Uiso 1 1 calc R . . C26 C 0.3547(5) 0.2822(4) 0.0902(3) 0.0346(12) Uani 1 1 d . . . C27 C 0.3853(4) 0.2037(4) 0.0316(2) 0.0317(11) Uani 1 1 d . . . H27 H 0.3261 0.1785 -0.0066 0.038 Uiso 1 1 calc R . . C28 C 0.5023(4) 0.1642(3) 0.0308(2) 0.0249(10) Uani 1 1 d . . . H28 H 0.5195 0.1113 -0.0074 0.030 Uiso 1 1 calc R . . C29 C 0.5956(4) 0.2013(3) 0.0857(2) 0.0259(10) Uani 1 1 d . . . C30 C 0.5637(5) 0.2786(3) 0.1424(2) 0.0296(11) Uani 1 1 d . . . H30 H 0.6229 0.3038 0.1807 0.036 Uiso 1 1 calc R . . C31 C 0.4469(5) 0.3196(3) 0.1441(3) 0.0350(12) Uani 1 1 d . . . H31 H 0.4307 0.3731 0.1821 0.042 Uiso 1 1 calc R . . C32 C 0.2243(6) 0.3193(5) 0.0932(3) 0.0582(18) Uani 1 1 d . . . H32A H 0.2000 0.3409 0.1435 0.087 Uiso 1 1 calc R . . H32B H 0.1640 0.2684 0.0675 0.087 Uiso 1 1 calc R . . H32C H 0.2250 0.3724 0.0705 0.087 Uiso 1 1 calc R . . C33 C 0.7212(4) 0.1563(3) 0.0859(2) 0.0293(11) Uani 1 1 d . . . H33 H 0.7600 0.1802 0.1352 0.035 Uiso 1 1 calc R . . C34 C 0.7063(4) 0.0487(4) 0.0695(3) 0.0350(12) Uani 1 1 d . . . H34A H 0.6526 0.0298 0.1054 0.053 Uiso 1 1 calc R . . H34B H 0.7889 0.0235 0.0710 0.053 Uiso 1 1 calc R . . H34C H 0.6678 0.0233 0.0214 0.053 Uiso 1 1 calc R . . C35 C 0.8087(5) 0.1906(4) 0.0329(3) 0.0477(15) Uani 1 1 d . . . H35A H 0.7757 0.1646 -0.0164 0.072 Uiso 1 1 calc R . . H35B H 0.8928 0.1689 0.0371 0.072 Uiso 1 1 calc R . . H35C H 0.8135 0.2601 0.0442 0.072 Uiso 1 1 calc R . . C36 C 0.6966(4) 0.0926(3) 0.3638(2) 0.0277(11) Uani 1 1 d . . . C37 C 0.6696(4) 0.0601(3) 0.4264(2) 0.0252(10) Uani 1 1 d . . . H37 H 0.6803 -0.0041 0.4260 0.030 Uiso 1 1 calc R . . C38 C 0.6271(4) 0.1226(3) 0.4892(2) 0.0216(9) Uani 1 1 d . . . H38 H 0.6087 0.0992 0.5302 0.026 Uiso 1 1 calc R . . C39 C 0.6111(4) 0.2190(3) 0.4925(2) 0.0253(10) Uani 1 1 d . . . C40 C 0.6392(4) 0.2499(3) 0.4296(2) 0.0262(10) Uani 1 1 d . . . H40 H 0.6282 0.3142 0.4303 0.031 Uiso 1 1 calc R . . C41 C 0.6831(4) 0.1894(4) 0.3655(3) 0.0290(11) Uani 1 1 d . . . H41 H 0.7028 0.2132 0.3248 0.035 Uiso 1 1 calc R . . C42 C 0.7331(5) 0.0255(4) 0.2948(3) 0.0419(14) Uani 1 1 d . . . H42A H 0.7052 0.0482 0.2537 0.063 Uiso 1 1 calc R . . H42B H 0.6933 -0.0379 0.2916 0.063 Uiso 1 1 calc R . . H42C H 0.8245 0.0225 0.2941 0.063 Uiso 1 1 calc R . . C43 C 0.5637(5) 0.2877(4) 0.5596(3) 0.0381(12) Uani 1 1 d . . . H43 H 0.5423 0.3469 0.5463 0.046 Uiso 1 1 calc R . . C44 C 0.6732(6) 0.3133(5) 0.6159(3) 0.0592(18) Uani 1 1 d . . . H44A H 0.6456 0.3572 0.6598 0.089 Uiso 1 1 calc R . . H44B H 0.7443 0.3436 0.5962 0.089 Uiso 1 1 calc R . . H44C H 0.6989 0.2555 0.6274 0.089 Uiso 1 1 calc R . . C45 C 0.4477(5) 0.2476(4) 0.5903(3) 0.0460(14) Uani 1 1 d . . . H45A H 0.3834 0.2251 0.5521 0.069 Uiso 1 1 calc R . . H45B H 0.4150 0.2973 0.6289 0.069 Uiso 1 1 calc R . . H45C H 0.4699 0.1946 0.6097 0.069 Uiso 1 1 calc R . . B1 B 0.5833(5) 0.4605(4) 0.3419(3) 0.0355(14) Uani 1 1 d . . . C46 C 0.4317(12) -0.4231(5) 0.1816(4) 0.177(7) Uani 1 1 d GU . . H46 H 0.4419 -0.4421 0.2251 0.080 Uiso 1 1 calc R . . C47 C 0.3170(10) -0.3931(6) 0.1646(5) 0.164(6) Uani 1 1 d GU . . H47 H 0.2490 -0.3916 0.1964 0.080 Uiso 1 1 calc R . . C48 C 0.3021(9) -0.3654(6) 0.1010(5) 0.171(5) Uani 1 1 d GU . . H48 H 0.2237 -0.3449 0.0894 0.080 Uiso 1 1 calc R . . C49 C 0.4017(11) -0.3677(7) 0.0544(4) 0.167(6) Uani 1 1 d GU . . H49 H 0.3914 -0.3487 0.0110 0.080 Uiso 1 1 calc R . . C50 C 0.5163(9) -0.3977(7) 0.0715(5) 0.205(8) Uani 1 1 d GU . . H50 H 0.5844 -0.3992 0.0396 0.080 Uiso 1 1 calc R . . C51 C 0.5313(9) -0.4254(7) 0.1351(6) 0.183(6) Uani 1 1 d GU . . H51 H 0.6096 -0.4459 0.1467 0.080 Uiso 1 1 calc R . . C52A C 0.2154(18) 0.2274(15) 0.7586(12) 0.230(19) Uani 0.556(19) 1 d PGU A 1 H52A H 0.2926 0.2497 0.7423 0.080 Uiso 0.556(19) 1 calc PR A 1 C53A C 0.114(2) 0.1977(14) 0.7110(10) 0.179(15) Uani 0.556(19) 1 d PGU A 1 H53A H 0.1214 0.1996 0.6620 0.080 Uiso 0.556(19) 1 calc PR A 1 C54A C 0.0009(18) 0.1651(13) 0.7348(12) 0.190(16) Uani 0.556(19) 1 d PGU A 1 H54A H -0.0686 0.1447 0.7022 0.080 Uiso 0.556(19) 1 calc PR A 1 C55A C -0.0103(16) 0.1622(16) 0.8064(14) 0.211(19) Uani 0.556(19) 1 d PGU A 1 H55A H -0.0875 0.1399 0.8227 0.080 Uiso 0.556(19) 1 calc PR A 1 C56A C 0.091(2) 0.1920(14) 0.8541(10) 0.224(19) Uani 0.556(19) 1 d PGU A 1 H56A H 0.0837 0.1900 0.9030 0.080 Uiso 0.556(19) 1 calc PR A 1 C57A C 0.2042(17) 0.2246(13) 0.8302(11) 0.179(12) Uani 0.556(19) 1 d PGU A 1 H57A H 0.2737 0.2449 0.8628 0.080 Uiso 0.556(19) 1 calc PR A 1 C52B C 0.0336(19) 0.1807(14) 0.6606(11) 0.109(8) Uani 0.444(19) 1 d PGU A 2 H52B H 0.0044 0.1737 0.6125 0.080 Uiso 0.444(19) 1 calc PR A 2 C53B C -0.0470(16) 0.1577(16) 0.7111(14) 0.151(14) Uani 0.444(19) 1 d PGU A 2 H53B H -0.1313 0.1350 0.6976 0.080 Uiso 0.444(19) 1 calc PR A 2 C54B C -0.004(3) 0.1679(17) 0.7814(12) 0.19(2) Uani 0.444(19) 1 d PGU A 2 H54B H -0.0594 0.1521 0.8160 0.080 Uiso 0.444(19) 1 calc PR A 2 C55B C 0.119(3) 0.2011(14) 0.8012(11) 0.172(15) Uani 0.444(19) 1 d PGU A 2 H55B H 0.1482 0.2080 0.8492 0.080 Uiso 0.444(19) 1 calc PR A 2 C56B C 0.1996(17) 0.2241(13) 0.7506(15) 0.157(16) Uani 0.444(19) 1 d PGU A 2 H56B H 0.2839 0.2468 0.7641 0.080 Uiso 0.444(19) 1 calc PR A 2 C57B C 0.1569(17) 0.2139(14) 0.6803(14) 0.129(11) Uani 0.444(19) 1 d PGU A 2 H57B H 0.2120 0.2296 0.6457 0.080 Uiso 0.444(19) 1 calc PR A 2 C58 C -0.158(6) 0.461(6) 0.017(5) 0.44(5) Uiso 0.50 1 d PD . . C59 C -0.039(4) 0.531(3) 0.0346(18) 0.345(16) Uiso 1 1 d D . . C61 C -0.171(4) 0.553(5) 0.066(3) 0.31(3) Uiso 0.50 1 d PD . . C60 C 0.076(5) 0.598(3) 0.070(3) 0.26(2) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01601(19) 0.0218(2) 0.01761(17) 0.00116(14) 0.00264(13) 0.00534(13) Ru2 0.01989(19) 0.0213(2) 0.01600(17) 0.00460(14) 0.00607(13) 0.00379(14) Ru3 0.01388(19) 0.0218(2) 0.01888(18) 0.00707(14) 0.00022(13) 0.00100(13) Na1 0.0191(8) 0.0211(9) 0.0235(8) 0.0026(7) 0.0032(7) -0.0004(7) F1 0.0337(15) 0.0308(15) 0.0396(15) 0.0039(13) 0.0056(12) 0.0058(12) F2 0.0267(17) 0.043(2) 0.135(4) 0.006(2) 0.006(2) 0.0025(14) F3 0.071(3) 0.048(2) 0.114(3) 0.040(2) 0.027(2) -0.0005(18) F4 0.147(4) 0.070(3) 0.052(2) -0.017(2) -0.028(3) 0.015(3) O1 0.0172(14) 0.0217(16) 0.0185(14) 0.0011(12) 0.0047(11) 0.0012(12) O2 0.0159(14) 0.0255(16) 0.0187(14) 0.0024(13) 0.0031(11) 0.0043(12) O3 0.0199(15) 0.0183(15) 0.0210(14) 0.0029(12) 0.0021(11) 0.0006(11) O4 0.0225(15) 0.0246(16) 0.0183(14) 0.0027(13) 0.0038(12) 0.0035(12) O5 0.0134(14) 0.0242(16) 0.0223(14) 0.0069(13) 0.0020(11) 0.0024(11) O6 0.0219(16) 0.0281(17) 0.0261(15) 0.0172(14) 0.0014(12) 0.0028(13) N1 0.0194(18) 0.027(2) 0.0165(16) 0.0040(15) 0.0018(14) 0.0040(15) N2 0.0170(18) 0.0227(19) 0.0206(17) 0.0079(15) 0.0010(14) 0.0018(14) N3 0.0155(18) 0.0236(19) 0.0179(16) 0.0022(15) 0.0022(14) 0.0039(14) C1 0.020(2) 0.021(2) 0.0147(18) 0.0058(17) 0.0026(16) 0.0047(17) C2 0.020(2) 0.022(2) 0.0165(19) 0.0078(18) 0.0007(16) 0.0071(17) C3 0.016(2) 0.034(3) 0.024(2) 0.001(2) 0.0012(17) -0.0002(18) C4 0.024(2) 0.040(3) 0.028(2) -0.010(2) -0.0023(19) -0.001(2) C5 0.024(2) 0.036(3) 0.020(2) -0.005(2) -0.0001(18) 0.005(2) C6 0.015(2) 0.019(2) 0.023(2) 0.0060(18) 0.0029(16) 0.0037(16) C7 0.021(2) 0.023(2) 0.019(2) 0.0060(18) 0.0037(17) 0.0014(17) C8 0.041(3) 0.023(2) 0.025(2) -0.001(2) 0.001(2) 0.000(2) C9 0.057(3) 0.021(3) 0.033(3) 0.009(2) 0.002(2) -0.003(2) C10 0.039(3) 0.026(2) 0.024(2) 0.013(2) -0.0017(19) 0.001(2) C11 0.020(2) 0.021(2) 0.0137(18) 0.0032(17) 0.0033(16) 0.0018(17) C12 0.016(2) 0.032(3) 0.0171(19) 0.0069(19) 0.0020(16) 0.0047(18) C13 0.021(2) 0.041(3) 0.032(2) 0.021(2) 0.0042(19) 0.000(2) C14 0.021(2) 0.044(3) 0.034(2) 0.019(2) 0.006(2) -0.005(2) C15 0.016(2) 0.034(3) 0.028(2) 0.012(2) 0.0046(18) 0.0043(18) C16 0.046(3) 0.025(3) 0.024(2) -0.009(2) 0.003(2) 0.012(2) C17 0.032(3) 0.027(2) 0.029(2) -0.001(2) 0.010(2) 0.0104(19) C18 0.024(2) 0.026(2) 0.032(2) 0.002(2) 0.0081(19) 0.0114(18) C19 0.022(2) 0.024(2) 0.027(2) -0.0007(19) 0.0021(18) 0.0096(18) C20 0.027(2) 0.020(2) 0.037(3) -0.002(2) 0.006(2) 0.0025(19) C21 0.027(2) 0.030(3) 0.029(2) -0.007(2) -0.0046(19) 0.007(2) C22 0.072(4) 0.044(3) 0.023(2) 0.000(2) -0.005(2) 0.022(3) C23 0.035(3) 0.035(3) 0.026(2) 0.011(2) 0.001(2) 0.012(2) C24 0.067(4) 0.039(3) 0.044(3) 0.012(3) -0.004(3) 0.014(3) C25 0.066(4) 0.043(3) 0.038(3) 0.013(3) -0.012(3) 0.002(3) C26 0.049(3) 0.031(3) 0.035(3) 0.025(2) 0.018(2) 0.018(2) C27 0.030(3) 0.045(3) 0.023(2) 0.014(2) 0.0047(19) 0.006(2) C28 0.031(2) 0.030(2) 0.016(2) 0.0088(19) 0.0101(18) 0.0036(19) C29 0.026(2) 0.028(2) 0.023(2) 0.0069(19) 0.0084(18) -0.0033(19) C30 0.037(3) 0.025(2) 0.024(2) 0.005(2) 0.009(2) -0.007(2) C31 0.054(3) 0.021(2) 0.032(3) 0.008(2) 0.017(2) 0.005(2) C32 0.061(4) 0.072(5) 0.055(4) 0.031(3) 0.026(3) 0.041(3) C33 0.021(2) 0.039(3) 0.025(2) 0.002(2) 0.0037(18) -0.005(2) C34 0.024(2) 0.049(3) 0.026(2) -0.004(2) -0.0010(19) 0.006(2) C35 0.033(3) 0.060(4) 0.050(3) 0.014(3) 0.015(2) -0.001(3) C36 0.015(2) 0.036(3) 0.030(2) 0.004(2) 0.0022(18) 0.0004(19) C37 0.014(2) 0.027(2) 0.035(2) 0.008(2) -0.0068(18) 0.0060(17) C38 0.019(2) 0.026(2) 0.024(2) 0.0136(19) -0.0095(17) 0.0020(17) C39 0.025(2) 0.026(2) 0.026(2) 0.009(2) -0.0101(18) -0.0003(18) C40 0.018(2) 0.026(2) 0.035(2) 0.010(2) -0.0044(19) -0.0059(18) C41 0.013(2) 0.042(3) 0.032(2) 0.011(2) 0.0007(18) -0.0072(19) C42 0.024(3) 0.050(3) 0.045(3) -0.001(3) 0.013(2) 0.006(2) C43 0.055(3) 0.026(3) 0.031(3) 0.001(2) -0.002(2) 0.004(2) C44 0.080(5) 0.054(4) 0.031(3) -0.007(3) -0.009(3) -0.018(3) C45 0.058(4) 0.034(3) 0.041(3) -0.003(2) 0.011(3) 0.012(3) B1 0.031(3) 0.028(3) 0.043(3) 0.001(3) 0.002(2) -0.004(2) C46 0.35(2) 0.069(7) 0.115(10) 0.024(7) 0.015(10) 0.005(12) C47 0.303(16) 0.077(8) 0.110(9) 0.024(6) 0.060(11) -0.012(10) C48 0.232(13) 0.136(11) 0.153(12) 0.054(10) 0.032(10) -0.014(11) C49 0.245(16) 0.143(12) 0.120(10) 0.052(9) 0.031(9) -0.019(12) C50 0.244(15) 0.219(19) 0.181(15) 0.103(14) 0.042(14) 0.013(16) C51 0.277(15) 0.139(12) 0.126(11) 0.033(10) -0.015(10) -0.035(12) C52A 0.24(3) 0.27(5) 0.26(3) 0.21(4) -0.01(2) 0.00(3) C53A 0.28(3) 0.14(3) 0.150(19) 0.058(18) -0.002(18) 0.17(3) C54A 0.22(2) 0.057(16) 0.25(3) -0.06(2) -0.07(2) 0.095(17) C55A 0.15(2) 0.15(3) 0.38(5) 0.17(4) -0.03(2) -0.03(2) C56A 0.29(4) 0.17(3) 0.22(3) 0.09(3) -0.02(2) -0.15(3) C57A 0.22(2) 0.119(19) 0.17(2) 0.026(18) -0.048(18) -0.11(2) C52B 0.113(16) 0.053(12) 0.16(2) 0.029(16) 0.007(13) 0.012(12) C53B 0.14(2) 0.10(2) 0.18(2) 0.00(2) 0.037(17) -0.04(2) C54B 0.30(4) 0.07(3) 0.144(19) -0.03(2) 0.05(2) -0.04(3) C55B 0.30(4) 0.06(2) 0.14(2) -0.027(17) -0.04(2) 0.07(3) C56B 0.14(2) 0.057(17) 0.24(3) -0.04(2) -0.032(18) 0.063(15) C57B 0.110(15) 0.057(14) 0.23(3) 0.06(2) 0.035(17) -0.002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O2 2.048(3) . ? Ru1 O1 2.111(3) . ? Ru1 N3 2.143(4) . ? Ru1 C18 2.156(4) . ? Ru1 C20 2.154(5) . ? Ru1 C17 2.168(4) . ? Ru1 C19 2.192(5) . ? Ru1 C16 2.201(4) . ? Ru1 C21 2.203(4) . ? Ru1 Na1 3.4796(16) . ? Ru2 O4 2.058(3) . ? Ru2 O3 2.090(3) . ? Ru2 N1 2.145(3) . ? Ru2 C28 2.156(4) . ? Ru2 C27 2.172(5) . ? Ru2 C30 2.173(4) . ? Ru2 C26 2.194(5) . ? Ru2 C31 2.202(5) . ? Ru2 C29 2.205(4) . ? Ru2 Na1 3.4136(16) . ? Ru3 O6 2.050(3) . ? Ru3 O5 2.114(3) . ? Ru3 N2 2.148(3) . ? Ru3 C38 2.153(4) . ? Ru3 C37 2.157(4) . ? Ru3 C40 2.172(4) . ? Ru3 C36 2.182(4) . ? Ru3 C39 2.197(4) . ? Ru3 C41 2.211(4) . ? Ru3 Na1 3.4161(18) . ? Na1 O5 2.257(3) . ? Na1 O3 2.260(3) . ? Na1 O1 2.271(3) . ? Na1 F2 2.366(4) . ? Na1 F1 2.449(3) . ? Na1 B1 2.949(6) . ? F1 B1 1.415(6) . ? F2 B1 1.363(7) . ? F3 B1 1.344(7) . ? F4 B1 1.374(7) . ? O1 C1 1.312(5) . ? O2 C2 1.333(5) . ? O3 C6 1.319(5) . ? O4 C7 1.335(5) . ? O5 C11 1.320(5) . ? O6 C12 1.349(5) . ? N1 C1 1.350(5) . ? N1 C5 1.371(5) . ? N2 C6 1.345(5) . ? N2 C10 1.369(6) . ? N3 C11 1.344(6) . ? N3 C15 1.381(5) . ? C1 C2 1.436(5) . ? C2 C3 1.372(6) . ? C3 C4 1.409(6) . ? C4 C5 1.361(6) . ? C6 C7 1.434(6) . ? C7 C8 1.378(6) . ? C8 C9 1.403(7) . ? C9 C10 1.351(6) . ? C11 C12 1.424(6) . ? C12 C13 1.378(6) . ? C13 C14 1.415(7) . ? C14 C15 1.359(7) . ? C16 C17 1.405(7) . ? C16 C21 1.419(7) . ? C16 C22 1.517(7) . ? C17 C18 1.429(7) . ? C18 C19 1.421(6) . ? C19 C20 1.427(7) . ? C19 C23 1.519(7) . ? C20 C21 1.410(7) . ? C23 C25 1.519(7) . ? C23 C24 1.534(7) . ? C26 C31 1.404(8) . ? C26 C27 1.445(7) . ? C26 C32 1.521(7) . ? C27 C28 1.408(7) . ? C28 C29 1.423(6) . ? C29 C30 1.418(6) . ? C29 C33 1.531(7) . ? C30 C31 1.415(7) . ? C33 C34 1.520(7) . ? C33 C35 1.538(6) . ? C36 C41 1.421(7) . ? C36 C37 1.423(7) . ? C36 C42 1.505(6) . ? C37 C38 1.412(6) . ? C38 C39 1.414(6) . ? C39 C40 1.417(6) . ? C39 C43 1.530(6) . ? C40 C41 1.424(6) . ? C43 C45 1.521(7) . ? C43 C44 1.549(8) . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C52A C53A 1.3900 . ? C52A C57A 1.3900 . ? C53A C54A 1.3900 . ? C54A C55A 1.3900 . ? C55A C56A 1.3900 . ? C56A C57A 1.3900 . ? C52B C53B 1.3900 . ? C52B C57B 1.3900 . ? C53B C54B 1.3900 . ? C54B C55B 1.3900 . ? C55B C56B 1.3900 . ? C56B C57B 1.3900 . ? C58 C61 1.44(10) . ? C58 C59 1.56(2) . ? C58 C60 1.92(9) 2_565 ? C59 C61 1.55(2) . ? C59 C60 1.562(19) . ? C59 C59 1.67(6) 2_565 ? C60 C58 1.92(9) 2_565 ? 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 O2 Ru1 O1 79.81(10) . . ? O2 Ru1 N3 82.42(12) . . ? O1 Ru1 N3 87.40(12) . . ? O2 Ru1 C18 87.86(15) . . ? O1 Ru1 C18 135.17(15) . . ? N3 Ru1 C18 133.67(15) . . ? O2 Ru1 C20 136.21(16) . . ? O1 Ru1 C20 91.78(14) . . ? N3 Ru1 C20 140.52(16) . . ? C18 Ru1 C20 68.22(17) . . ? O2 Ru1 C17 103.74(15) . . ? O1 Ru1 C17 171.59(16) . . ? N3 Ru1 C17 100.58(16) . . ? C18 Ru1 C17 38.61(18) . . ? C20 Ru1 C17 80.37(18) . . ? O2 Ru1 C19 101.47(14) . . ? O1 Ru1 C19 102.53(14) . . ? N3 Ru1 C19 169.80(14) . . ? C18 Ru1 C19 38.14(16) . . ? C20 Ru1 C19 38.31(18) . . ? C17 Ru1 C19 69.40(18) . . ? O2 Ru1 C16 137.40(15) . . ? O1 Ru1 C16 141.42(15) . . ? N3 Ru1 C16 88.38(17) . . ? C18 Ru1 C16 69.08(18) . . ? C20 Ru1 C16 68.31(19) . . ? C17 Ru1 C16 37.51(19) . . ? C19 Ru1 C16 82.39(18) . . ? O2 Ru1 C21 168.70(15) . . ? O1 Ru1 C21 107.92(14) . . ? N3 Ru1 C21 105.77(16) . . ? C18 Ru1 C21 80.85(18) . . ? C20 Ru1 C21 37.73(18) . . ? C17 Ru1 C21 67.50(17) . . ? C19 Ru1 C21 69.18(17) . . ? C16 Ru1 C21 37.61(18) . . ? O2 Ru1 Na1 115.85(8) . . ? O1 Ru1 Na1 39.06(8) . . ? N3 Ru1 Na1 78.47(9) . . ? C18 Ru1 Na1 144.26(13) . . ? C20 Ru1 Na1 76.38(12) . . ? C17 Ru1 Na1 139.71(13) . . ? C19 Ru1 Na1 107.73(12) . . ? C16 Ru1 Na1 102.67(14) . . ? C21 Ru1 Na1 74.01(12) . . ? O4 Ru2 O3 79.62(11) . . ? O4 Ru2 N1 82.22(12) . . ? O3 Ru2 N1 85.55(12) . . ? O4 Ru2 C28 89.39(15) . . ? O3 Ru2 C28 140.56(15) . . ? N1 Ru2 C28 130.64(15) . . ? O4 Ru2 C27 107.14(16) . . ? O3 Ru2 C27 172.20(15) . . ? N1 Ru2 C27 99.07(16) . . ? C28 Ru2 C27 37.97(17) . . ? O4 Ru2 C30 132.71(15) . . ? O3 Ru2 C30 92.23(15) . . ? N1 Ru2 C30 144.03(16) . . ? C28 Ru2 C30 67.90(16) . . ? C27 Ru2 C30 80.34(19) . . ? O4 Ru2 C26 142.58(16) . . ? O3 Ru2 C26 135.97(15) . . ? N1 Ru2 C26 88.74(17) . . ? C28 Ru2 C26 69.41(17) . . ? C27 Ru2 C26 38.63(18) . . ? C30 Ru2 C26 68.3(2) . . ? O4 Ru2 C31 168.51(14) . . ? O3 Ru2 C31 104.83(16) . . ? N1 Ru2 C31 108.50(16) . . ? C28 Ru2 C31 80.48(17) . . ? C27 Ru2 C31 67.80(19) . . ? C30 Ru2 C31 37.74(19) . . ? C26 Ru2 C31 37.3(2) . . ? O4 Ru2 C29 100.08(14) . . ? O3 Ru2 C29 106.57(14) . . ? N1 Ru2 C29 167.87(15) . . ? C28 Ru2 C29 38.07(16) . . ? C27 Ru2 C29 68.84(18) . . ? C30 Ru2 C29 37.78(16) . . ? C26 Ru2 C29 82.23(18) . . ? C31 Ru2 C29 68.57(17) . . ? O4 Ru2 Na1 117.71(8) . . ? O3 Ru2 Na1 40.11(8) . . ? N1 Ru2 Na1 79.63(9) . . ? C28 Ru2 Na1 143.76(12) . . ? C27 Ru2 Na1 134.32(14) . . ? C30 Ru2 Na1 75.90(12) . . ? C26 Ru2 Na1 95.94(13) . . ? C31 Ru2 Na1 69.52(13) . . ? C29 Ru2 Na1 109.26(11) . . ? O6 Ru3 O5 79.70(11) . . ? O6 Ru3 N2 83.41(12) . . ? O5 Ru3 N2 86.14(12) . . ? O6 Ru3 C38 88.13(14) . . ? O5 Ru3 C38 132.14(14) . . ? N2 Ru3 C38 138.46(15) . . ? O6 Ru3 C37 99.28(15) . . ? O5 Ru3 C37 170.31(14) . . ? N2 Ru3 C37 103.36(15) . . ? C38 Ru3 C37 38.26(16) . . ? O6 Ru3 C40 141.51(14) . . ? O5 Ru3 C40 94.38(15) . . ? N2 Ru3 C40 134.51(15) . . ? C38 Ru3 C40 67.74(17) . . ? C37 Ru3 C40 80.38(18) . . ? O6 Ru3 C36 131.83(16) . . ? O5 Ru3 C36 146.43(16) . . ? N2 Ru3 C36 86.75(15) . . ? C38 Ru3 C36 69.22(17) . . ? C37 Ru3 C36 38.28(17) . . ? C40 Ru3 C36 68.26(17) . . ? O6 Ru3 C39 105.74(14) . . ? O5 Ru3 C39 101.83(14) . . ? N2 Ru3 C39 168.70(15) . . ? C38 Ru3 C39 37.92(17) . . ? C37 Ru3 C39 69.05(17) . . ? C40 Ru3 C39 37.84(17) . . ? C36 Ru3 C39 82.19(17) . . ? O6 Ru3 C41 167.54(16) . . ? O5 Ru3 C41 112.21(16) . . ? N2 Ru3 C41 100.56(15) . . ? C38 Ru3 C41 81.08(17) . . ? C37 Ru3 C41 68.36(18) . . ? C40 Ru3 C41 37.89(17) . . ? C36 Ru3 C41 37.75(18) . . ? C39 Ru3 C41 69.11(17) . . ? O6 Ru3 Na1 117.73(9) . . ? O5 Ru3 Na1 40.11(8) . . ? N2 Ru3 Na1 79.19(10) . . ? C38 Ru3 Na1 138.95(12) . . ? C37 Ru3 Na1 142.84(13) . . ? C40 Ru3 Na1 72.83(13) . . ? C36 Ru3 Na1 106.32(14) . . ? C39 Ru3 Na1 101.66(13) . . ? C41 Ru3 Na1 74.70(14) . . ? O5 Na1 O3 88.74(12) . . ? O5 Na1 O1 87.81(11) . . ? O3 Na1 O1 86.79(11) . . ? O5 Na1 F2 126.48(15) . . ? O3 Na1 F2 142.47(14) . . ? O1 Na1 F2 105.04(13) . . ? O5 Na1 F1 123.85(12) . . ? O3 Na1 F1 97.19(11) . . ? O1 Na1 F1 148.04(13) . . ? F2 Na1 F1 54.61(10) . . ? O5 Na1 B1 125.30(16) . . ? O3 Na1 B1 124.39(14) . . ? O1 Na1 B1 130.70(16) . . ? F2 Na1 B1 26.97(15) . . ? F1 Na1 B1 28.52(13) . . ? O5 Na1 Ru2 118.12(9) . . ? O3 Na1 Ru2 36.57(8) . . ? O1 Na1 Ru2 68.51(7) . . ? F2 Na1 Ru2 114.88(13) . . ? F1 Na1 Ru2 96.28(8) . . ? B1 Na1 Ru2 112.43(13) . . ? O5 Na1 Ru3 37.13(8) . . ? O3 Na1 Ru3 67.52(9) . . ? O1 Na1 Ru3 115.41(9) . . ? F2 Na1 Ru3 131.71(12) . . ? F1 Na1 Ru3 95.15(9) . . ? B1 Na1 Ru3 111.92(14) . . ? Ru2 Na1 Ru3 104.03(4) . . ? O5 Na1 Ru1 68.42(8) . . ? O3 Na1 Ru1 115.24(9) . . ? O1 Na1 Ru1 35.87(7) . . ? F2 Na1 Ru1 92.25(9) . . ? F1 Na1 Ru1 146.33(9) . . ? B1 Na1 Ru1 117.81(12) . . ? Ru2 Na1 Ru1 104.31(4) . . ? Ru3 Na1 Ru1 105.11(4) . . ? B1 F1 Na1 95.8(3) . . ? B1 F2 Na1 101.1(3) . . ? C1 O1 Ru1 110.9(2) . . ? C1 O1 Na1 132.8(3) . . ? Ru1 O1 Na1 105.08(11) . . ? C2 O2 Ru1 112.5(2) . . ? C6 O3 Ru2 110.9(2) . . ? C6 O3 Na1 133.1(2) . . ? Ru2 O3 Na1 103.33(13) . . ? C7 O4 Ru2 111.7(2) . . ? C11 O5 Ru3 110.4(3) . . ? C11 O5 Na1 133.9(3) . . ? Ru3 O5 Na1 102.76(11) . . ? C12 O6 Ru3 111.5(3) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Ru2 125.9(3) . . ? C5 N1 Ru2 115.4(3) . . ? C6 N2 C10 117.8(3) . . ? C6 N2 Ru3 124.2(3) . . ? C10 N2 Ru3 117.2(3) . . ? C11 N3 C15 118.3(4) . . ? C11 N3 Ru1 127.6(3) . . ? C15 N3 Ru1 114.0(3) . . ? O1 C1 N1 120.8(3) . . ? O1 C1 C2 118.2(3) . . ? N1 C1 C2 120.9(3) . . ? O2 C2 C3 123.4(4) . . ? O2 C2 C1 117.3(3) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 118.8(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 N1 122.6(4) . . ? O3 C6 N2 120.6(3) . . ? O3 C6 C7 117.6(4) . . ? N2 C6 C7 121.7(4) . . ? O4 C7 C8 124.3(4) . . ? O4 C7 C6 117.2(4) . . ? C8 C7 C6 118.5(4) . . ? C7 C8 C9 119.0(4) . . ? C10 C9 C8 119.6(4) . . ? C9 C10 N2 123.4(4) . . ? O5 C11 N3 121.0(4) . . ? O5 C11 C12 117.8(4) . . ? N3 C11 C12 121.2(4) . . ? O6 C12 C13 122.2(4) . . ? O6 C12 C11 117.8(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C14 118.1(5) . . ? C15 C14 C13 119.6(4) . . ? C14 C15 N3 122.8(4) . . ? C17 C16 C21 118.6(5) . . ? C17 C16 C22 120.6(5) . . ? C21 C16 C22 120.7(5) . . ? C17 C16 Ru1 70.0(3) . . ? C21 C16 Ru1 71.3(2) . . ? C22 C16 Ru1 127.6(3) . . ? C16 C17 C18 121.3(4) . . ? C16 C17 Ru1 72.5(2) . . ? C18 C17 Ru1 70.3(2) . . ? C19 C18 C17 121.1(4) . . ? C19 C18 Ru1 72.3(3) . . ? C17 C18 Ru1 71.1(3) . . ? C18 C19 C20 116.1(4) . . ? C18 C19 C23 122.5(4) . . ? C20 C19 C23 121.3(4) . . ? C18 C19 Ru1 69.5(3) . . ? C20 C19 Ru1 69.4(3) . . ? C23 C19 Ru1 129.6(3) . . ? C21 C20 C19 123.2(4) . . ? C21 C20 Ru1 73.0(3) . . ? C19 C20 Ru1 72.3(3) . . ? C20 C21 C16 119.6(4) . . ? C20 C21 Ru1 69.2(2) . . ? C16 C21 Ru1 71.1(3) . . ? C25 C23 C19 114.6(4) . . ? C25 C23 C24 110.6(5) . . ? C19 C23 C24 110.2(4) . . ? C31 C26 C27 117.8(4) . . ? C31 C26 C32 122.3(5) . . ? C27 C26 C32 119.9(5) . . ? C31 C26 Ru2 71.6(3) . . ? C27 C26 Ru2 69.9(3) . . ? C32 C26 Ru2 127.8(4) . . ? C28 C27 C26 120.5(4) . . ? C28 C27 Ru2 70.4(3) . . ? C26 C27 Ru2 71.5(3) . . ? C27 C28 C29 121.8(4) . . ? C27 C28 Ru2 71.6(2) . . ? C29 C28 Ru2 72.8(2) . . ? C30 C29 C28 116.6(4) . . ? C30 C29 C33 121.6(4) . . ? C28 C29 C33 121.7(4) . . ? C30 C29 Ru2 69.9(2) . . ? C28 C29 Ru2 69.1(2) . . ? C33 C29 Ru2 128.8(3) . . ? C31 C30 C29 122.4(4) . . ? C31 C30 Ru2 72.2(3) . . ? C29 C30 Ru2 72.3(2) . . ? C26 C31 C30 120.7(4) . . ? C26 C31 Ru2 71.1(3) . . ? C30 C31 Ru2 70.0(3) . . ? C34 C33 C29 112.7(4) . . ? C34 C33 C35 112.0(4) . . ? C29 C33 C35 108.8(4) . . ? C41 C36 C37 119.3(4) . . ? C41 C36 C42 119.4(4) . . ? C37 C36 C42 121.3(5) . . ? C41 C36 Ru3 72.2(2) . . ? C37 C36 Ru3 69.9(2) . . ? C42 C36 Ru3 127.3(3) . . ? C38 C37 C36 120.6(4) . . ? C38 C37 Ru3 70.7(2) . . ? C36 C37 Ru3 71.8(3) . . ? C39 C38 C37 121.7(4) . . ? C39 C38 Ru3 72.7(2) . . ? C37 C38 Ru3 71.0(2) . . ? C38 C39 C40 116.8(4) . . ? C38 C39 C43 122.6(4) . . ? C40 C39 C43 120.7(4) . . ? C38 C39 Ru3 69.4(2) . . ? C40 C39 Ru3 70.1(2) . . ? C43 C39 Ru3 130.5(3) . . ? C39 C40 C41 123.3(4) . . ? C39 C40 Ru3 72.0(2) . . ? C41 C40 Ru3 72.5(2) . . ? C36 C41 C40 118.4(4) . . ? C36 C41 Ru3 70.0(2) . . ? C40 C41 Ru3 69.6(2) . . ? C45 C43 C39 113.1(4) . . ? C45 C43 C44 111.1(5) . . ? C39 C43 C44 107.5(4) . . ? F3 B1 F2 113.2(6) . . ? F3 B1 F4 108.5(5) . . ? F2 B1 F4 110.2(5) . . ? F3 B1 F1 111.1(4) . . ? F2 B1 F1 105.4(4) . . ? F4 B1 F1 108.4(5) . . ? F3 B1 Na1 141.7(4) . . ? F2 B1 Na1 51.9(2) . . ? F4 B1 Na1 109.9(4) . . ? F1 B1 Na1 55.7(2) . . ? C47 C46 C51 120.0 . . ? C46 C47 C48 120.0 . . ? C47 C48 C49 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C46 120.0 . . ? C53A C52A C57A 120.0 . . ? C52A C53A C54A 120.0 . . ? C55A C54A C53A 120.0 . . ? C54A C55A C56A 120.0 . . ? C57A C56A C55A 120.0 . . ? C56A C57A C52A 120.0 . . ? C53B C52B C57B 120.0 . . ? C54B C53B C52B 120.0 . . ? C53B C54B C55B 120.0 . . ? C54B C55B C56B 120.0 . . ? C57B C56B C55B 120.0 . . ? C56B C57B C52B 120.0 . . ? C61 C58 C59 62(2) . . ? C61 C58 C60 142(5) . 2_565 ? C59 C58 C60 87(5) . 2_565 ? C61 C59 C58 55(4) . . ? C61 C59 C60 118(4) . . ? C58 C59 C60 167(5) . . ? C61 C59 C59 145(5) . 2_565 ? C58 C59 C59 93(5) . 2_565 ? C60 C59 C59 96(4) . 2_565 ? C58 C61 C59 63(2) . . ? C59 C60 C58 83(4) . 2_565 ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 1.056 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.107 data_3 _database_code_CSD 193870 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H102 F6 N6 Na2 O12 Ru6 Si, 2(H2 O)' _chemical_formula_sum 'C90 H106 F6 N6 Na2 O14 Ru6 Si' _chemical_formula_weight 2290.30 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5292(10) _cell_length_b 29.415(3) _cell_length_c 13.0113(14) _cell_angle_alpha 90.00 _cell_angle_beta 109.567(9) _cell_angle_gamma 90.00 _cell_volume 4518.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 2630 _cell_measurement_theta_min 2.1829 _cell_measurement_theta_max 18.8826 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type 'refdelf' _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.5010 _exptl_absorpt_correction_T_max 0.8410 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction, KM4CCD/SAPPHIRE' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26357 _diffrn_reflns_av_R_equivalents 0.1487 _diffrn_reflns_av_sigmaI/netI 0.2727 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7286 _reflns_number_gt 3248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction, CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction, CrysAlis RED' _computing_data_reduction 'Oxford Diffraction, CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0000P)^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_number_reflns 7286 _refine_ls_number_parameters 572 _refine_ls_number_restraints 415 _refine_ls_R_factor_all 0.2032 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.00788(10) -0.14619(4) -0.26003(10) 0.0265(3) Uani 1 1 d U . . Ru2 Ru -0.19267(10) -0.16102(3) 0.05708(9) 0.0173(3) Uani 1 1 d U . . Ru3 Ru -0.39304(10) -0.05196(3) -0.28815(9) 0.0180(3) Uani 1 1 d U . . Si1 Si 0.0000 0.0000 0.0000 0.0266(14) Uani 1 2 d SU . . Na1 Na -0.1311(4) -0.08177(15) -0.1093(4) 0.0207(10) Uani 1 1 d U . . F1 F 0.0477(6) -0.0541(2) 0.0283(6) 0.0266(16) Uani 1 1 d U . . F2 F -0.0452(6) -0.0131(2) -0.1333(6) 0.0245(17) Uani 1 1 d U . . F3 F -0.1251(6) -0.0170(2) 0.0069(6) 0.0283(17) Uani 1 1 d U . . O1 O -0.0762(7) -0.1539(3) -0.1341(7) 0.0185(17) Uani 1 1 d U . . O2 O -0.0383(7) -0.2155(3) -0.2687(7) 0.024(2) Uani 1 1 d U . . O3 O -0.2764(7) -0.1168(2) -0.0737(7) 0.0178(16) Uani 1 1 d U . . O4 O -0.3528(7) -0.1880(3) 0.0046(7) 0.0202(19) Uani 1 1 d U . . O5 O -0.2401(7) -0.0833(3) -0.2877(7) 0.0193(17) Uani 1 1 d U . . O6 O -0.4436(7) -0.0817(3) -0.4376(7) 0.0196(19) Uani 1 1 d U . . N1 N -0.1718(8) -0.2054(3) -0.0637(8) 0.015(2) Uani 1 1 d U . . N2 N -0.4305(9) -0.1170(3) -0.2347(9) 0.017(2) Uani 1 1 d U . . N3 N -0.1789(9) -0.1428(3) -0.3714(9) 0.023(2) Uani 1 1 d U . . C1 C -0.1176(12) -0.1951(4) -0.1322(10) 0.021(3) Uani 1 1 d U . . C2 C -0.0925(11) -0.2289(4) -0.2022(11) 0.021(3) Uani 1 1 d U . . C3 C -0.1228(11) -0.2736(4) -0.1936(11) 0.023(3) Uani 1 1 d U . . H3 H -0.1043 -0.2967 -0.2357 0.028 Uiso 1 1 calc R . . C4 C -0.1809(13) -0.2841(4) -0.1222(13) 0.039(4) Uani 1 1 d U . . H4 H -0.2036 -0.3145 -0.1163 0.047 Uiso 1 1 calc R . . C5 C -0.2054(12) -0.2499(4) -0.0595(12) 0.031(4) Uani 1 1 d U . . H5 H -0.2466 -0.2574 -0.0124 0.037 Uiso 1 1 calc R . . C6 C -0.3707(12) -0.1351(4) -0.1358(11) 0.016(3) Uani 1 1 d U . . C7 C -0.4187(12) -0.1742(4) -0.0962(11) 0.014(3) Uani 1 1 d U . . C8 C -0.5174(12) -0.1927(4) -0.1562(11) 0.025(3) Uani 1 1 d U . . H8 H -0.5489 -0.2174 -0.1289 0.030 Uiso 1 1 calc R . . C9 C -0.5736(11) -0.1747(4) -0.2607(11) 0.022(3) Uani 1 1 d U . . H9 H -0.6422 -0.1880 -0.3063 0.026 Uiso 1 1 calc R . . C10 C -0.5279(11) -0.1372(4) -0.2967(11) 0.021(3) Uani 1 1 d U . . H10 H -0.5665 -0.1254 -0.3674 0.025 Uiso 1 1 calc R . . C11 C -0.2574(11) -0.1126(4) -0.3650(11) 0.017(3) Uani 1 1 d U . . C12 C -0.3679(11) -0.1130(4) -0.4485(11) 0.016(3) Uani 1 1 d U . . C13 C -0.3923(12) -0.1419(4) -0.5339(10) 0.026(3) Uani 1 1 d U . . H13 H -0.4637 -0.1409 -0.5905 0.031 Uiso 1 1 calc R . . C14 C -0.3081(13) -0.1739(4) -0.5368(11) 0.030(3) Uani 1 1 d U . . H14 H -0.3238 -0.1957 -0.5938 0.035 Uiso 1 1 calc R . . C15 C -0.2053(14) -0.1728(4) -0.4574(12) 0.031(3) Uani 1 1 d U . . H15 H -0.1489 -0.1937 -0.4614 0.038 Uiso 1 1 calc R . . C16 C 0.0484(13) -0.1048(6) -0.3705(14) 0.045(4) Uani 1 1 d U . . C17 C 0.1098(12) -0.1452(5) -0.3483(12) 0.044(3) Uani 1 1 d U . . H17 H 0.1126 -0.1636 -0.4073 0.052 Uiso 1 1 calc R . . C18 C 0.1686(11) -0.1597(5) -0.2392(12) 0.036(3) Uani 1 1 d U . . H18 H 0.2094 -0.1876 -0.2266 0.043 Uiso 1 1 calc R . . C19 C 0.1664(12) -0.1327(5) -0.1493(12) 0.031(3) Uani 1 1 d U . . C20 C 0.1036(11) -0.0914(5) -0.1742(13) 0.033(3) Uani 1 1 d U . . H20 H 0.0998 -0.0727 -0.1159 0.040 Uiso 1 1 calc R . . C21 C 0.0483(12) -0.0775(5) -0.2800(13) 0.040(3) Uani 1 1 d U . . H21 H 0.0095 -0.0492 -0.2929 0.048 Uiso 1 1 calc R . . C22 C -0.0193(14) -0.0916(6) -0.4876(13) 0.074(6) Uani 1 1 d U . . H22A H 0.0226 -0.0686 -0.5131 0.110 Uiso 1 1 calc R . . H22B H -0.0928 -0.0792 -0.4904 0.110 Uiso 1 1 calc R . . H22C H -0.0311 -0.1185 -0.5344 0.110 Uiso 1 1 calc R . . C23 C 0.2187(12) -0.1483(5) -0.0352(12) 0.036(3) Uani 1 1 d U . . H23 H 0.1647 -0.1391 0.0028 0.043 Uiso 1 1 calc R . . C24 C 0.3286(13) -0.1232(5) 0.0239(13) 0.059(5) Uani 1 1 d U . . H24A H 0.3870 -0.1324 -0.0067 0.088 Uiso 1 1 calc R . . H24B H 0.3536 -0.1308 0.1017 0.088 Uiso 1 1 calc R . . H24C H 0.3159 -0.0904 0.0146 0.088 Uiso 1 1 calc R . . C25 C 0.2305(13) -0.1998(5) -0.0212(12) 0.044(4) Uani 1 1 d U . . H25A H 0.1597 -0.2145 -0.0654 0.067 Uiso 1 1 calc R . . H25B H 0.2467 -0.2077 0.0557 0.067 Uiso 1 1 calc R . . H25C H 0.2926 -0.2105 -0.0451 0.067 Uiso 1 1 calc R . . C26 C -0.0333(12) -0.1880(4) 0.1719(11) 0.023(3) Uani 1 1 d U . . C27 C -0.1237(11) -0.1948(4) 0.2133(11) 0.025(3) Uani 1 1 d U . . H27 H -0.1370 -0.2244 0.2354 0.030 Uiso 1 1 calc R . . C28 C -0.1931(11) -0.1592(4) 0.2220(10) 0.024(3) Uani 1 1 d U . . H28 H -0.2529 -0.1654 0.2495 0.028 Uiso 1 1 calc R . . C29 C -0.1780(11) -0.1144(4) 0.1916(10) 0.018(2) Uani 1 1 d U . . C30 C -0.0870(11) -0.1066(4) 0.1511(10) 0.023(2) Uani 1 1 d U . . H30 H -0.0748 -0.0768 0.1291 0.027 Uiso 1 1 calc R . . C31 C -0.0155(11) -0.1418(4) 0.1429(10) 0.023(2) Uani 1 1 d U . . H31 H 0.0460 -0.1353 0.1180 0.027 Uiso 1 1 calc R . . C32 C 0.0395(11) -0.2260(4) 0.1532(12) 0.035(4) Uani 1 1 d U . . H32A H 0.0710 -0.2169 0.0968 0.053 Uiso 1 1 calc R . . H32B H -0.0067 -0.2534 0.1296 0.053 Uiso 1 1 calc R . . H32C H 0.1015 -0.2324 0.2213 0.053 Uiso 1 1 calc R . . C33 C -0.2587(12) -0.0752(5) 0.1849(12) 0.032(4) Uani 1 1 d U . . H33 H -0.2739 -0.0616 0.1109 0.038 Uiso 1 1 calc R . . C34 C -0.3710(12) -0.0900(5) 0.1879(13) 0.041(4) Uani 1 1 d U . . H34A H -0.3905 -0.1195 0.1517 0.062 Uiso 1 1 calc R . . H34B H -0.4286 -0.0675 0.1501 0.062 Uiso 1 1 calc R . . H34C H -0.3680 -0.0927 0.2639 0.062 Uiso 1 1 calc R . . C35 C -0.2041(13) -0.0376(5) 0.2647(13) 0.052(5) Uani 1 1 d U . . H35A H -0.1915 -0.0482 0.3393 0.078 Uiso 1 1 calc R . . H35B H -0.2540 -0.0110 0.2495 0.078 Uiso 1 1 calc R . . H35C H -0.1314 -0.0293 0.2570 0.078 Uiso 1 1 calc R . . C36 C -0.4815(12) -0.0231(4) -0.1847(11) 0.020(3) Uani 1 1 d U . . C37 C -0.5419(11) -0.0124(4) -0.2975(11) 0.019(2) Uani 1 1 d U . . H37 H -0.6192 -0.0206 -0.3305 0.023 Uiso 1 1 calc R . . C38 C -0.4822(11) 0.0111(4) -0.3586(11) 0.020(2) Uani 1 1 d U . . H38 H -0.5223 0.0197 -0.4318 0.024 Uiso 1 1 calc R . . C39 C -0.3661(12) 0.0218(4) -0.3136(11) 0.021(3) Uani 1 1 d U . . C40 C -0.3115(12) 0.0088(4) -0.2043(11) 0.025(3) Uani 1 1 d U . . H40 H -0.2322 0.0136 -0.1725 0.030 Uiso 1 1 calc R . . C41 C -0.3696(12) -0.0110(4) -0.1408(11) 0.022(3) Uani 1 1 d U . . H41 H -0.3307 -0.0162 -0.0654 0.027 Uiso 1 1 calc R . . C42 C -0.5452(11) -0.0483(4) -0.1192(11) 0.031(4) Uani 1 1 d U . . H42A H -0.4905 -0.0610 -0.0527 0.046 Uiso 1 1 calc R . . H42B H -0.5901 -0.0730 -0.1636 0.046 Uiso 1 1 calc R . . H42C H -0.5955 -0.0271 -0.0997 0.046 Uiso 1 1 calc R . . C43 C -0.3043(12) 0.0455(4) -0.3815(12) 0.037(4) Uani 1 1 d U . . H43 H -0.3626 0.0548 -0.4519 0.044 Uiso 1 1 calc R . . C44 C -0.2468(13) 0.0882(5) -0.3256(14) 0.062(6) Uani 1 1 d U . . H44A H -0.3035 0.1089 -0.3149 0.094 Uiso 1 1 calc R . . H44B H -0.2084 0.1031 -0.3710 0.094 Uiso 1 1 calc R . . H44C H -0.1910 0.0805 -0.2547 0.094 Uiso 1 1 calc R . . C45 C -0.2200(12) 0.0143(5) -0.4090(13) 0.043(4) Uani 1 1 d U . . H45A H -0.1900 0.0297 -0.4603 0.064 Uiso 1 1 calc R . . H45B H -0.2585 -0.0138 -0.4423 0.064 Uiso 1 1 calc R . . H45C H -0.1576 0.0069 -0.3422 0.064 Uiso 1 1 calc R . . O7 O 0.1320(9) -0.2611(4) -0.3192(10) 0.079(5) Uani 1 1 d D . . H7A H 0.071(10) -0.240(4) -0.322(15) 0.119 Uiso 1 1 d D . . H7B H 0.098(11) -0.289(4) -0.355(14) 0.119 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0239(8) 0.0326(7) 0.0270(8) 0.0091(6) 0.0140(7) 0.0095(6) Ru2 0.0206(7) 0.0141(6) 0.0170(7) 0.0034(5) 0.0060(6) -0.0014(5) Ru3 0.0204(7) 0.0137(6) 0.0185(7) 0.0008(5) 0.0047(6) 0.0021(5) Si1 0.029(4) 0.018(3) 0.028(3) 0.005(2) 0.003(3) -0.004(2) Na1 0.021(3) 0.016(2) 0.023(3) 0.0051(19) 0.004(2) -0.0023(19) F1 0.022(4) 0.019(4) 0.032(4) 0.004(3) 0.000(3) -0.006(3) F2 0.019(5) 0.024(4) 0.027(4) 0.006(3) 0.002(4) -0.003(3) F3 0.032(5) 0.024(4) 0.027(4) 0.002(3) 0.008(4) -0.007(3) O1 0.013(5) 0.020(3) 0.024(5) 0.000(3) 0.008(4) 0.000(3) O2 0.025(6) 0.030(4) 0.018(6) 0.006(4) 0.010(5) 0.013(4) O3 0.021(5) 0.013(4) 0.019(4) 0.004(3) 0.006(3) 0.000(3) O4 0.020(4) 0.017(5) 0.024(5) 0.003(4) 0.008(4) -0.006(4) O5 0.018(4) 0.019(4) 0.021(4) -0.001(3) 0.007(3) -0.001(3) O6 0.013(5) 0.025(5) 0.019(4) -0.008(3) 0.002(4) -0.001(4) N1 0.016(7) 0.012(4) 0.016(5) 0.006(4) 0.004(5) 0.004(4) N2 0.015(6) 0.011(4) 0.025(6) 0.001(4) 0.006(5) -0.001(4) N3 0.025(4) 0.024(6) 0.023(5) 0.008(4) 0.011(4) 0.011(4) C1 0.031(10) 0.019(5) 0.014(8) 0.001(5) 0.008(7) 0.001(6) C2 0.029(10) 0.019(5) 0.018(8) 0.007(5) 0.011(7) 0.016(6) C3 0.025(10) 0.022(6) 0.013(8) -0.006(6) -0.007(7) 0.008(6) C4 0.060(13) 0.010(7) 0.053(12) -0.006(7) 0.027(10) -0.015(8) C5 0.050(11) 0.010(6) 0.041(10) 0.008(6) 0.026(9) 0.006(7) C6 0.017(7) 0.013(7) 0.024(7) -0.001(5) 0.013(5) 0.006(5) C7 0.020(7) 0.006(6) 0.015(7) -0.006(5) 0.003(5) 0.003(5) C8 0.020(8) 0.028(8) 0.029(8) 0.002(6) 0.010(6) -0.006(6) C9 0.014(8) 0.031(8) 0.017(7) -0.010(6) 0.000(6) -0.014(6) C10 0.013(8) 0.027(7) 0.024(8) 0.003(6) 0.008(6) 0.003(5) C11 0.017(6) 0.021(7) 0.016(7) 0.004(5) 0.007(5) 0.001(5) C12 0.012(7) 0.028(8) 0.013(7) -0.001(5) 0.011(5) -0.003(5) C13 0.042(9) 0.026(8) 0.007(7) -0.004(5) 0.004(6) 0.002(6) C14 0.058(10) 0.022(8) 0.012(8) -0.008(6) 0.017(6) -0.004(7) C15 0.040(8) 0.039(9) 0.022(8) 0.002(6) 0.020(5) 0.011(7) C16 0.019(9) 0.077(9) 0.043(6) 0.031(6) 0.016(6) 0.007(6) C17 0.027(8) 0.077(9) 0.035(6) 0.015(6) 0.021(6) 0.006(7) C18 0.017(5) 0.057(8) 0.038(7) 0.011(6) 0.016(6) 0.008(5) C19 0.022(5) 0.037(7) 0.035(6) 0.017(5) 0.013(4) 0.002(5) C20 0.022(8) 0.034(6) 0.047(7) 0.015(5) 0.015(6) 0.001(4) C21 0.015(8) 0.048(5) 0.058(8) 0.031(5) 0.015(6) 0.004(5) C22 0.049(13) 0.113(16) 0.052(8) 0.051(9) 0.009(9) -0.010(10) C23 0.021(8) 0.054(9) 0.034(7) 0.022(7) 0.013(6) 0.010(7) C24 0.051(12) 0.076(12) 0.038(11) 0.006(9) 0.000(8) -0.013(9) C25 0.033(11) 0.059(8) 0.030(11) 0.021(7) -0.004(9) 0.004(8) C26 0.022(6) 0.029(6) 0.014(7) 0.006(5) 0.002(4) 0.004(5) C27 0.035(8) 0.021(6) 0.020(6) 0.012(5) 0.011(5) -0.001(5) C28 0.025(8) 0.028(6) 0.022(5) -0.003(5) 0.013(6) -0.010(5) C29 0.016(7) 0.025(5) 0.007(5) 0.002(4) -0.004(6) 0.001(5) C30 0.027(8) 0.019(5) 0.023(6) -0.001(5) 0.008(6) -0.011(4) C31 0.017(5) 0.037(6) 0.014(7) 0.007(5) 0.003(4) -0.005(4) C32 0.018(9) 0.038(8) 0.042(11) -0.001(7) 0.000(8) 0.005(6) C33 0.035(9) 0.031(8) 0.028(10) -0.004(6) 0.009(9) 0.006(6) C34 0.040(9) 0.031(9) 0.057(12) 0.001(8) 0.022(10) 0.006(7) C35 0.040(11) 0.052(10) 0.051(12) -0.024(8) -0.001(10) 0.005(8) C36 0.029(6) 0.014(6) 0.018(6) -0.004(5) 0.008(5) 0.005(5) C37 0.016(5) 0.012(6) 0.025(6) -0.007(5) 0.000(5) -0.001(4) C38 0.035(6) 0.006(5) 0.012(6) -0.002(4) 0.000(5) 0.000(5) C39 0.024(7) 0.010(4) 0.028(7) 0.001(5) 0.006(6) 0.002(5) C40 0.019(6) 0.015(5) 0.034(7) -0.002(5) 0.000(5) 0.002(4) C41 0.027(6) 0.015(7) 0.016(5) -0.004(4) -0.004(5) 0.003(5) C42 0.042(10) 0.027(8) 0.030(9) 0.000(7) 0.020(8) 0.006(7) C43 0.037(10) 0.024(8) 0.046(10) 0.015(7) 0.010(8) 0.004(6) C44 0.069(14) 0.025(8) 0.098(16) 0.007(8) 0.033(12) -0.025(8) C45 0.028(11) 0.051(10) 0.053(13) 0.010(8) 0.019(10) 0.001(8) O7 0.049(9) 0.113(12) 0.056(10) -0.052(9) -0.009(8) 0.037(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O2 2.070(8) . ? Ru1 O1 2.099(7) . ? Ru1 N3 2.150(11) . ? Ru1 C17 2.151(13) . ? Ru1 C18 2.173(13) . ? Ru1 C16 2.173(14) . ? Ru1 C20 2.181(14) . ? Ru1 C21 2.185(14) . ? Ru1 C19 2.212(15) . ? Ru1 Na1 3.442(5) . ? Ru2 O4 2.049(8) . ? Ru2 O3 2.119(8) . ? Ru2 N1 2.125(10) . ? Ru2 C28 2.149(12) . ? Ru2 C27 2.165(13) . ? Ru2 C30 2.174(12) . ? Ru2 C29 2.183(12) . ? Ru2 C31 2.199(13) . ? Ru2 C26 2.202(13) . ? Ru2 Na1 3.440(5) . ? Ru3 O6 2.030(8) . ? Ru3 O5 2.124(8) . ? Ru3 N2 2.141(9) . ? Ru3 C40 2.163(13) . ? Ru3 C37 2.168(12) . ? Ru3 C36 2.182(12) . ? Ru3 C41 2.200(13) . ? Ru3 C38 2.201(12) . ? Ru3 C39 2.239(12) . ? Ru3 Na1 3.441(5) . ? Si1 F3 1.676(7) 3 ? Si1 F3 1.676(7) . ? Si1 F2 1.680(7) 3 ? Si1 F2 1.680(7) . ? Si1 F1 1.697(7) . ? Si1 F1 1.697(7) 3 ? Si1 Na1 2.990(5) 3 ? Si1 Na1 2.990(5) . ? Na1 O5 2.266(10) . ? Na1 O3 2.271(9) . ? Na1 O1 2.286(9) . ? Na1 F2 2.358(8) . ? Na1 F3 2.419(8) . ? Na1 F1 2.489(8) . ? O1 C1 1.323(13) . ? O2 C2 1.325(13) . ? O3 C6 1.304(14) . ? O4 C7 1.356(14) . ? O5 C11 1.287(13) . ? O6 C12 1.363(13) . ? N1 C1 1.323(13) . ? N1 C5 1.382(14) . ? N2 C10 1.354(15) . ? N2 C6 1.362(15) . ? N3 C11 1.348(14) . ? N3 C15 1.376(16) . ? C1 C2 1.453(16) . ? C2 C3 1.382(16) . ? C3 C4 1.394(16) . ? C4 C5 1.393(16) . ? C6 C7 1.469(15) . ? C7 C8 1.338(16) . ? C8 C9 1.409(17) . ? C9 C10 1.394(15) . ? C11 C12 1.446(17) . ? C12 C13 1.351(16) . ? C13 C14 1.423(17) . ? C14 C15 1.355(18) . ? C16 C17 1.393(19) . ? C16 C21 1.43(2) . ? C16 C22 1.53(2) . ? C17 C18 1.428(18) . ? C18 C19 1.423(18) . ? C19 C20 1.425(17) . ? C19 C23 1.481(18) . ? C20 C21 1.380(19) . ? C23 C24 1.524(19) . ? C23 C25 1.527(17) . ? C26 C27 1.421(16) . ? C26 C31 1.448(16) . ? C26 C32 1.514(16) . ? C27 C28 1.389(16) . ? C28 C29 1.408(16) . ? C29 C30 1.426(15) . ? C29 C33 1.517(16) . ? C30 C31 1.396(16) . ? C33 C34 1.485(16) . ? C33 C35 1.514(17) . ? C36 C41 1.371(16) . ? C36 C37 1.443(17) . ? C36 C42 1.540(15) . ? C37 C38 1.439(15) . ? C38 C39 1.409(16) . ? C39 C40 1.411(18) . ? C39 C43 1.524(16) . ? C40 C41 1.398(16) . ? C43 C44 1.508(18) . ? C43 C45 1.530(16) . ? 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 O2 Ru1 O1 79.6(3) . . ? O2 Ru1 N3 83.4(4) . . ? O1 Ru1 N3 87.5(3) . . ? O2 Ru1 C17 97.5(5) . . ? O1 Ru1 C17 161.7(5) . . ? N3 Ru1 C17 110.3(5) . . ? O2 Ru1 C18 89.3(5) . . ? O1 Ru1 C18 123.2(4) . . ? N3 Ru1 C18 146.7(5) . . ? C17 Ru1 C18 38.6(5) . . ? O2 Ru1 C16 127.6(5) . . ? O1 Ru1 C16 152.1(5) . . ? N3 Ru1 C16 90.0(5) . . ? C17 Ru1 C16 37.6(5) . . ? C18 Ru1 C16 69.1(5) . . ? O2 Ru1 C20 146.2(4) . . ? O1 Ru1 C20 92.2(4) . . ? N3 Ru1 C20 129.4(5) . . ? C17 Ru1 C20 80.1(6) . . ? C18 Ru1 C20 67.7(5) . . ? C16 Ru1 C20 68.3(6) . . ? O2 Ru1 C21 165.0(5) . . ? O1 Ru1 C21 115.1(5) . . ? N3 Ru1 C21 99.5(5) . . ? C17 Ru1 C21 67.6(6) . . ? C18 Ru1 C21 80.2(5) . . ? C16 Ru1 C21 38.2(5) . . ? C20 Ru1 C21 36.9(5) . . ? O2 Ru1 C19 109.6(4) . . ? O1 Ru1 C19 94.7(4) . . ? N3 Ru1 C19 167.0(4) . . ? C17 Ru1 C19 69.0(5) . . ? C18 Ru1 C19 37.9(5) . . ? C16 Ru1 C19 82.1(6) . . ? C20 Ru1 C19 37.8(4) . . ? C21 Ru1 C19 67.9(5) . . ? O2 Ru1 Na1 117.6(2) . . ? O1 Ru1 Na1 40.3(2) . . ? N3 Ru1 Na1 79.8(3) . . ? C17 Ru1 Na1 144.6(4) . . ? C18 Ru1 Na1 131.4(4) . . ? C16 Ru1 Na1 112.0(5) . . ? C20 Ru1 Na1 68.5(4) . . ? C21 Ru1 Na1 77.4(4) . . ? C19 Ru1 Na1 93.6(4) . . ? O4 Ru2 O3 78.7(3) . . ? O4 Ru2 N1 82.3(3) . . ? O3 Ru2 N1 86.2(3) . . ? O4 Ru2 C28 90.7(4) . . ? O3 Ru2 C28 128.4(4) . . ? N1 Ru2 C28 142.7(4) . . ? O4 Ru2 C27 100.0(4) . . ? O3 Ru2 C27 165.9(4) . . ? N1 Ru2 C27 107.6(4) . . ? C28 Ru2 C27 37.6(4) . . ? O4 Ru2 C30 144.7(4) . . ? O3 Ru2 C30 92.5(4) . . ? N1 Ru2 C30 131.7(4) . . ? C28 Ru2 C30 67.9(5) . . ? C27 Ru2 C30 80.4(5) . . ? O4 Ru2 C29 108.7(4) . . ? O3 Ru2 C29 98.3(4) . . ? N1 Ru2 C29 168.7(4) . . ? C28 Ru2 C29 37.9(4) . . ? C27 Ru2 C29 68.6(5) . . ? C30 Ru2 C29 38.2(4) . . ? O4 Ru2 C31 167.9(4) . . ? O3 Ru2 C31 113.2(4) . . ? N1 Ru2 C31 100.4(4) . . ? C28 Ru2 C31 80.0(4) . . ? C27 Ru2 C31 67.9(5) . . ? C30 Ru2 C31 37.2(4) . . ? C29 Ru2 C31 68.4(5) . . ? O4 Ru2 C26 130.6(4) . . ? O3 Ru2 C26 149.1(4) . . ? N1 Ru2 C26 88.4(4) . . ? C28 Ru2 C26 68.7(5) . . ? C27 Ru2 C26 38.0(4) . . ? C30 Ru2 C26 68.9(5) . . ? C29 Ru2 C26 82.4(5) . . ? C31 Ru2 C26 38.4(4) . . ? O4 Ru2 Na1 117.0(3) . . ? O3 Ru2 Na1 40.0(2) . . ? N1 Ru2 Na1 80.9(3) . . ? C28 Ru2 Na1 133.5(3) . . ? C27 Ru2 Na1 143.0(4) . . ? C30 Ru2 Na1 68.4(3) . . ? C29 Ru2 Na1 95.9(3) . . ? C31 Ru2 Na1 75.2(3) . . ? C26 Ru2 Na1 109.1(3) . . ? O6 Ru3 O5 78.9(3) . . ? O6 Ru3 N2 83.9(4) . . ? O5 Ru3 N2 84.7(3) . . ? O6 Ru3 C40 141.5(4) . . ? O5 Ru3 C40 94.8(4) . . ? N2 Ru3 C40 133.8(5) . . ? O6 Ru3 C37 101.0(4) . . ? O5 Ru3 C37 172.6(4) . . ? N2 Ru3 C37 102.7(4) . . ? C40 Ru3 C37 80.6(5) . . ? O6 Ru3 C36 134.3(4) . . ? O5 Ru3 C36 144.2(4) . . ? N2 Ru3 C36 86.3(4) . . ? C40 Ru3 C36 67.6(5) . . ? C37 Ru3 C36 38.7(5) . . ? O6 Ru3 C41 168.1(4) . . ? O5 Ru3 C41 112.2(4) . . ? N2 Ru3 C41 100.7(4) . . ? C40 Ru3 C41 37.4(4) . . ? C37 Ru3 C41 67.4(5) . . ? C36 Ru3 C41 36.5(4) . . ? O6 Ru3 C38 90.7(4) . . ? O5 Ru3 C38 134.3(4) . . ? N2 Ru3 C38 138.8(4) . . ? C40 Ru3 C38 66.6(5) . . ? C37 Ru3 C38 38.4(4) . . ? C36 Ru3 C38 68.7(4) . . ? C41 Ru3 C38 78.6(5) . . ? O6 Ru3 C39 106.9(4) . . ? O5 Ru3 C39 103.9(4) . . ? N2 Ru3 C39 167.2(4) . . ? C40 Ru3 C39 37.3(5) . . ? C37 Ru3 C39 68.9(5) . . ? C36 Ru3 C39 81.2(4) . . ? C41 Ru3 C39 67.4(5) . . ? C38 Ru3 C39 37.0(4) . . ? O6 Ru3 Na1 117.3(2) . . ? O5 Ru3 Na1 39.9(2) . . ? N2 Ru3 Na1 79.4(3) . . ? C40 Ru3 Na1 71.7(4) . . ? C37 Ru3 Na1 141.5(4) . . ? C36 Ru3 Na1 104.4(4) . . ? C41 Ru3 Na1 74.4(4) . . ? C38 Ru3 Na1 137.1(4) . . ? C39 Ru3 Na1 101.0(4) . . ? F3 Si1 F3 180.0(6) 3 . ? F3 Si1 F2 89.4(3) 3 3 ? F3 Si1 F2 90.6(3) . 3 ? F3 Si1 F2 90.6(3) 3 . ? F3 Si1 F2 89.4(3) . . ? F2 Si1 F2 180.0(6) 3 . ? F3 Si1 F1 91.3(3) 3 . ? F3 Si1 F1 88.7(3) . . ? F2 Si1 F1 91.1(3) 3 . ? F2 Si1 F1 88.9(3) . . ? F3 Si1 F1 88.7(3) 3 3 ? F3 Si1 F1 91.3(3) . 3 ? F2 Si1 F1 88.9(3) 3 3 ? F2 Si1 F1 91.1(3) . 3 ? F1 Si1 F1 180.0(8) . 3 ? F3 Si1 Na1 53.9(2) 3 3 ? F3 Si1 Na1 126.1(2) . 3 ? F2 Si1 Na1 51.9(2) 3 3 ? F2 Si1 Na1 128.1(2) . 3 ? F1 Si1 Na1 123.7(2) . 3 ? F1 Si1 Na1 56.3(2) 3 3 ? F3 Si1 Na1 126.1(2) 3 . ? F3 Si1 Na1 53.9(2) . . ? F2 Si1 Na1 128.1(2) 3 . ? F2 Si1 Na1 51.9(2) . . ? F1 Si1 Na1 56.3(2) . . ? F1 Si1 Na1 123.7(2) 3 . ? Na1 Si1 Na1 180.00(10) 3 . ? O5 Na1 O3 87.2(3) . . ? O5 Na1 O1 86.8(3) . . ? O3 Na1 O1 84.7(3) . . ? O5 Na1 F2 91.5(3) . . ? O3 Na1 F2 148.0(3) . . ? O1 Na1 F2 127.2(3) . . ? O5 Na1 F3 122.5(3) . . ? O3 Na1 F3 95.1(3) . . ? O1 Na1 F3 150.7(4) . . ? F2 Na1 F3 59.2(3) . . ? O5 Na1 F1 146.3(3) . . ? O3 Na1 F1 126.2(3) . . ? O1 Na1 F1 99.4(3) . . ? F2 Na1 F1 58.3(3) . . ? F3 Na1 F1 57.4(3) . . ? O5 Na1 Si1 123.4(3) . . ? O3 Na1 Si1 128.2(3) . . ? O1 Na1 Si1 132.1(3) . . ? F2 Na1 Si1 34.07(19) . . ? F3 Na1 Si1 34.07(17) . . ? F1 Na1 Si1 34.57(17) . . ? O5 Na1 Ru2 116.5(3) . . ? O3 Na1 Ru2 36.9(2) . . ? O1 Na1 Ru2 66.5(2) . . ? F2 Na1 Ru2 150.7(3) . . ? F3 Na1 Ru2 96.2(2) . . ? F1 Na1 Ru2 96.1(2) . . ? Si1 Na1 Ru2 116.68(16) . . ? O5 Na1 Ru3 36.9(2) . . ? O3 Na1 Ru3 66.8(2) . . ? O1 Na1 Ru3 113.9(3) . . ? F2 Na1 Ru3 93.8(2) . . ? F3 Na1 Ru3 92.6(2) . . ? F1 Na1 Ru3 145.9(2) . . ? Si1 Na1 Ru3 111.36(14) . . ? Ru2 Na1 Ru3 103.54(12) . . ? O5 Na1 Ru1 68.7(2) . . ? O3 Na1 Ru1 114.2(3) . . ? O1 Na1 Ru1 36.40(19) . . ? F2 Na1 Ru1 94.8(2) . . ? F3 Na1 Ru1 149.8(2) . . ? F1 Na1 Ru1 97.0(2) . . ? Si1 Na1 Ru1 115.73(14) . . ? Ru2 Na1 Ru1 102.91(12) . . ? Ru3 Na1 Ru1 105.26(14) . . ? Si1 F1 Na1 89.1(3) . . ? Si1 F2 Na1 94.1(3) . . ? Si1 F3 Na1 92.0(3) . . ? C1 O1 Ru1 112.3(7) . . ? C1 O1 Na1 135.2(7) . . ? Ru1 O1 Na1 103.3(3) . . ? C2 O2 Ru1 112.6(7) . . ? C6 O3 Ru2 110.2(7) . . ? C6 O3 Na1 133.1(8) . . ? Ru2 O3 Na1 103.1(4) . . ? C7 O4 Ru2 114.7(7) . . ? C11 O5 Ru3 111.9(8) . . ? C11 O5 Na1 134.4(8) . . ? Ru3 O5 Na1 103.2(3) . . ? C12 O6 Ru3 112.7(8) . . ? C1 N1 C5 118.3(11) . . ? C1 N1 Ru2 125.2(8) . . ? C5 N1 Ru2 116.0(8) . . ? C10 N2 C6 119.5(11) . . ? C10 N2 Ru3 116.8(9) . . ? C6 N2 Ru3 123.0(9) . . ? C11 N3 C15 119.5(12) . . ? C11 N3 Ru1 124.9(9) . . ? C15 N3 Ru1 115.6(9) . . ? O1 C1 N1 121.0(11) . . ? O1 C1 C2 116.5(11) . . ? N1 C1 C2 122.3(12) . . ? O2 C2 C3 123.5(11) . . ? O2 C2 C1 118.1(11) . . ? C3 C2 C1 118.4(12) . . ? C2 C3 C4 119.0(12) . . ? C5 C4 C3 119.8(12) . . ? N1 C5 C4 122.1(12) . . ? O3 C6 N2 121.4(11) . . ? O3 C6 C7 119.9(12) . . ? N2 C6 C7 118.5(13) . . ? C8 C7 O4 126.0(12) . . ? C8 C7 C6 121.4(13) . . ? O4 C7 C6 112.6(12) . . ? C7 C8 C9 118.4(12) . . ? C10 C9 C8 119.6(13) . . ? N2 C10 C9 122.4(13) . . ? O5 C11 N3 123.7(13) . . ? O5 C11 C12 117.4(11) . . ? N3 C11 C12 118.9(12) . . ? C13 C12 O6 122.5(13) . . ? C13 C12 C11 121.2(12) . . ? O6 C12 C11 116.2(11) . . ? C12 C13 C14 118.2(14) . . ? C15 C14 C13 119.3(13) . . ? C14 C15 N3 122.8(13) . . ? C17 C16 C21 117.6(15) . . ? C17 C16 C22 120.5(17) . . ? C21 C16 C22 121.8(16) . . ? C17 C16 Ru1 70.4(8) . . ? C21 C16 Ru1 71.4(8) . . ? C22 C16 Ru1 127.5(11) . . ? C16 C17 C18 121.8(15) . . ? C16 C17 Ru1 72.1(8) . . ? C18 C17 Ru1 71.5(8) . . ? C19 C18 C17 120.3(14) . . ? C19 C18 Ru1 72.6(8) . . ? C17 C18 Ru1 69.9(8) . . ? C18 C19 C20 116.8(14) . . ? C18 C19 C23 121.8(13) . . ? C20 C19 C23 121.2(14) . . ? C18 C19 Ru1 69.6(8) . . ? C20 C19 Ru1 69.9(8) . . ? C23 C19 Ru1 127.3(9) . . ? C21 C20 C19 122.3(15) . . ? C21 C20 Ru1 71.7(9) . . ? C19 C20 Ru1 72.3(8) . . ? C20 C21 C16 121.2(15) . . ? C20 C21 Ru1 71.4(8) . . ? C16 C21 Ru1 70.5(9) . . ? C19 C23 C24 112.1(12) . . ? C19 C23 C25 114.9(13) . . ? C24 C23 C25 112.7(12) . . ? C27 C26 C31 116.3(12) . . ? C27 C26 C32 123.8(11) . . ? C31 C26 C32 119.9(11) . . ? C27 C26 Ru2 69.6(8) . . ? C31 C26 Ru2 70.7(7) . . ? C32 C26 Ru2 128.0(10) . . ? C28 C27 C26 121.6(12) . . ? C28 C27 Ru2 70.6(7) . . ? C26 C27 Ru2 72.4(7) . . ? C27 C28 C29 122.4(11) . . ? C27 C28 Ru2 71.9(7) . . ? C29 C28 Ru2 72.4(7) . . ? C28 C29 C30 116.9(12) . . ? C28 C29 C33 125.4(11) . . ? C30 C29 C33 117.2(11) . . ? C28 C29 Ru2 69.7(7) . . ? C30 C29 Ru2 70.5(7) . . ? C33 C29 Ru2 123.8(9) . . ? C31 C30 C29 121.6(11) . . ? C31 C30 Ru2 72.4(7) . . ? C29 C30 Ru2 71.3(7) . . ? C30 C31 C26 121.1(11) . . ? C30 C31 Ru2 70.4(7) . . ? C26 C31 Ru2 70.9(7) . . ? C34 C33 C35 114.3(12) . . ? C34 C33 C29 113.2(11) . . ? C35 C33 C29 112.0(12) . . ? C41 C36 C37 118.9(12) . . ? C41 C36 C42 122.8(12) . . ? C37 C36 C42 118.3(13) . . ? C41 C36 Ru3 72.5(7) . . ? C37 C36 Ru3 70.1(7) . . ? C42 C36 Ru3 128.1(8) . . ? C38 C37 C36 118.3(13) . . ? C38 C37 Ru3 72.0(7) . . ? C36 C37 Ru3 71.2(7) . . ? C39 C38 C37 122.2(13) . . ? C39 C38 Ru3 73.0(7) . . ? C37 C38 Ru3 69.5(7) . . ? C38 C39 C40 116.3(12) . . ? C38 C39 C43 121.1(13) . . ? C40 C39 C43 122.7(13) . . ? C38 C39 Ru3 70.0(7) . . ? C40 C39 Ru3 68.4(7) . . ? C43 C39 Ru3 131.3(8) . . ? C41 C40 C39 122.4(14) . . ? C41 C40 Ru3 72.7(7) . . ? C39 C40 Ru3 74.2(8) . . ? C36 C41 C40 121.6(13) . . ? C36 C41 Ru3 71.1(7) . . ? C40 C41 Ru3 69.9(8) . . ? C44 C43 C39 110.8(12) . . ? C44 C43 C45 110.9(12) . . ? C39 C43 C45 112.7(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O2 0.98(10) 1.87(12) 2.780(12) 153(16) . O7 H7B O4 0.98(10) 2.22(16) 2.798(13) 116(12) 4_655 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.593 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.131