Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Michael Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Photoinduced Ru-Yb energy transfer and sensitised near-infrared luminescence in a coordination polymer containing co-crystallised [Ru(bipy)(CN)4]2- and Yb(III) units ; loop_ _publ_author_name 'Michael Ward' 'H. Adams' 'Stephen Faulkner' 'John C. Jeffery' 'Thomas A. Miller' 'Simon J. A. Pope' data_ladystam _database_code_depnum_ccdc_archive 'CCDC 235083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 K N12 O15 Ru2 Yb' _chemical_formula_weight 1205.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.18400(10) _cell_length_b 29.2773(2) _cell_length_c 17.17470(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8640.61(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4760 _exptl_absorpt_coefficient_mu 10.979 _exptl_absorpt_correction_T_min 0.105 _exptl_absorpt_correction_T_max 0.337 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68391 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 70.17 _reflns_number_total 15484 _reflns_number_gt 14947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^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 0.213(5) _refine_ls_number_reflns 15484 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.006 _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 0.73737(2) 0.865412(11) 0.501740(19) 0.01069(7) Uani 1 1 d . . . Ru2 Ru 0.74897(2) 1.137353(11) 0.471030(19) 0.01038(7) Uani 1 1 d . . . Ru4 Ru 0.98927(2) 0.629996(11) 0.829943(17) 0.01021(7) Uani 1 1 d . . . Ru3 Ru 0.99770(2) 0.358956(11) 0.845449(19) 0.01073(7) Uani 1 1 d . . . N16 N 0.8537(3) 0.60877(15) 0.9515(3) 0.0197(9) Uani 1 1 d . . . N15 N 1.1046(3) 0.57021(15) 0.9271(2) 0.0202(9) Uani 1 1 d . . . C16 C 0.9023(3) 0.61600(16) 0.9071(3) 0.0144(10) Uani 1 1 d . . . N14 N 1.1179(2) 0.65110(14) 0.7001(2) 0.0173(9) Uani 1 1 d . . . C15 C 1.0622(3) 0.59247(17) 0.8914(3) 0.0152(10) Uani 1 1 d . . . C14 C 1.0735(3) 0.64430(16) 0.7493(3) 0.0144(10) Uani 1 1 d . . . N13 N 0.9493(3) 0.54361(14) 0.7295(2) 0.0183(9) Uani 1 1 d . . . C13 C 0.9643(3) 0.57525(17) 0.7677(3) 0.0148(10) Uani 1 1 d . . . N12 N 0.8592(3) 0.38607(15) 0.9608(2) 0.0188(9) Uani 1 1 d . . . C12 C 0.9090(3) 0.37546(17) 0.9189(3) 0.0150(10) Uani 1 1 d . . . N11 N 1.1053(3) 0.42526(16) 0.9388(2) 0.0217(10) Uani 1 1 d . . . C11 C 1.0669(3) 0.39959(17) 0.9058(3) 0.0158(10) Uani 1 1 d . . . N10 N 1.1385(3) 0.34049(14) 0.7286(2) 0.0194(9) Uani 1 1 d . . . C10 C 1.0879(3) 0.34540(15) 0.7717(3) 0.0144(9) Uani 1 1 d . . . N9 N 0.9587(3) 0.44287(15) 0.7408(2) 0.0180(9) Uani 1 1 d . . . C9 C 0.9729(3) 0.41168(16) 0.7801(3) 0.0137(9) Uani 1 1 d . . . N8 N 0.8862(3) 1.15826(15) 0.5913(3) 0.0202(9) Uani 1 1 d . . . C8 C 0.8367(3) 1.15212(15) 0.5471(3) 0.0128(9) Uani 1 1 d . . . N7 N 0.6104(3) 1.11107(15) 0.3559(2) 0.0198(9) Uani 1 1 d . . . C7 C 0.6614(3) 1.12097(16) 0.3966(3) 0.0123(9) Uani 1 1 d . . . N6 N 0.8670(3) 1.07532(16) 0.3797(3) 0.0225(10) Uani 1 1 d . . . C6 C 0.8228(3) 1.09869(16) 0.4122(2) 0.0142(10) Uani 1 1 d . . . N5 N 0.7075(3) 1.05195(14) 0.5730(2) 0.0166(9) Uani 1 1 d . . . C5 C 0.7238(3) 1.08283(16) 0.5347(2) 0.0141(10) Uani 1 1 d . . . N4 N 0.8648(3) 0.84613(14) 0.6342(2) 0.0205(9) Uani 1 1 d . . . C4 C 0.8211(3) 0.85215(16) 0.5841(3) 0.0147(9) Uani 1 1 d . . . N3 N 0.6025(3) 0.88791(16) 0.3791(3) 0.0216(10) Uani 1 1 d . . . C3 C 0.6512(3) 0.87969(16) 0.4231(3) 0.0133(10) Uani 1 1 d . . . N2 N 0.8575(3) 0.92300(16) 0.4051(2) 0.0213(10) Uani 1 1 d . . . C2 C 0.8129(3) 0.90139(16) 0.4395(2) 0.0133(9) Uani 1 1 d . . . N1 N 0.6960(3) 0.95333(13) 0.5981(2) 0.0154(8) Uani 1 1 d . . . C1 C 0.7121(3) 0.92128(17) 0.5616(2) 0.0135(10) Uani 1 1 d . . . C26 C 0.7163(3) 0.76537(16) 0.4777(3) 0.0145(9) Uani 1 1 d . . . C25 C 0.7234(3) 0.72229(17) 0.4465(3) 0.0203(10) Uani 1 1 d . . . H25 H 0.6969 0.6973 0.4698 0.024 Uiso 1 1 calc R . . C24 C 0.7694(3) 0.71523(18) 0.3806(3) 0.0232(11) Uani 1 1 d . . . H24 H 0.7754 0.6855 0.3593 0.028 Uiso 1 1 calc R . . C23 C 0.8060(3) 0.75214(18) 0.3471(3) 0.0207(10) Uani 1 1 d . . . H23 H 0.8366 0.7485 0.3015 0.025 Uiso 1 1 calc R . . C22 C 0.7973(3) 0.79470(17) 0.3810(3) 0.0160(10) Uani 1 1 d . . . H22 H 0.8229 0.8201 0.3578 0.019 Uiso 1 1 calc R . . N21 N 0.7542(2) 0.80181(13) 0.4454(2) 0.0141(8) Uani 1 1 d . . . N32 N 0.6634(2) 0.82108(14) 0.5656(2) 0.0140(8) Uani 1 1 d . . . C31 C 0.6184(3) 0.83329(17) 0.6254(3) 0.0176(10) Uani 1 1 d . . . H31 H 0.6173 0.8645 0.6404 0.021 Uiso 1 1 calc R . . C30 C 0.5731(3) 0.80234(17) 0.6666(3) 0.0213(10) Uani 1 1 d . . . H30 H 0.5397 0.8123 0.7073 0.026 Uiso 1 1 calc R . . C29 C 0.5779(3) 0.75655(17) 0.6470(3) 0.0223(10) Uani 1 1 d . . . H29 H 0.5488 0.7344 0.6749 0.027 Uiso 1 1 calc R . . C28 C 0.6251(3) 0.74379(18) 0.5869(3) 0.0189(11) Uani 1 1 d . . . H28 H 0.6292 0.7124 0.5731 0.023 Uiso 1 1 calc R . . C27 C 0.6672(3) 0.77636(16) 0.5456(3) 0.0156(9) Uani 1 1 d . . . N52 N 0.6769(2) 1.18352(13) 0.5330(2) 0.0115(8) Uani 1 1 d . . . C51 C 0.6314(3) 1.17332(18) 0.5940(3) 0.0161(10) Uani 1 1 d . . . H51 H 0.6281 1.1423 0.6101 0.019 Uiso 1 1 calc R . . C50 C 0.5893(3) 1.20532(17) 0.6343(3) 0.0178(10) Uani 1 1 d . . . H50 H 0.5578 1.1966 0.6772 0.021 Uiso 1 1 calc R . . C49 C 0.5935(3) 1.25019(17) 0.6114(3) 0.0179(10) Uani 1 1 d . . . H49 H 0.5647 1.2729 0.6384 0.022 Uiso 1 1 calc R . . C48 C 0.6401(3) 1.26208(17) 0.5486(3) 0.0172(10) Uani 1 1 d . . . H48 H 0.6440 1.2930 0.5321 0.021 Uiso 1 1 calc R . . C47 C 0.6811(3) 1.22769(15) 0.5100(3) 0.0126(9) Uani 1 1 d . . . C46 C 0.7312(3) 1.23692(16) 0.4416(3) 0.0124(9) Uani 1 1 d . . . C45 C 0.7393(3) 1.27986(16) 0.4081(3) 0.0173(10) Uani 1 1 d . . . H45 H 0.7122 1.3053 0.4293 0.021 Uiso 1 1 calc R . . C44 C 0.7866(3) 1.28551(17) 0.3439(3) 0.0183(10) Uani 1 1 d . . . H44 H 0.7929 1.3147 0.3206 0.022 Uiso 1 1 calc R . . C43 C 0.8251(3) 1.24758(17) 0.3141(3) 0.0189(10) Uani 1 1 d . . . H43 H 0.8583 1.2505 0.2702 0.023 Uiso 1 1 calc R . . C42 C 0.8142(3) 1.20560(17) 0.3492(3) 0.0156(10) Uani 1 1 d . . . H42 H 0.8402 1.1797 0.3283 0.019 Uiso 1 1 calc R . . N41 N 0.7685(2) 1.19986(13) 0.4117(2) 0.0128(8) Uani 1 1 d . . . C65 C 0.8920(3) 0.23235(17) 0.7710(3) 0.0184(10) Uani 1 1 d . . . H65 H 0.8961 0.2017 0.7886 0.022 Uiso 1 1 calc R . . C64 C 0.8464(3) 0.24278(18) 0.7072(3) 0.0201(10) Uani 1 1 d . . . H64 H 0.8189 0.2193 0.6806 0.024 Uiso 1 1 calc R . . C63 C 0.8409(3) 0.28762(18) 0.6824(3) 0.0195(10) Uani 1 1 d . . . H63 H 0.8091 0.2955 0.6392 0.023 Uiso 1 1 calc R . . C62 C 0.8831(3) 0.32094(18) 0.7223(3) 0.0159(10) Uani 1 1 d . . . H62 H 0.8802 0.3517 0.7049 0.019 Uiso 1 1 calc R . . N61 N 0.9277(2) 0.31102(13) 0.7843(2) 0.0134(8) Uani 1 1 d . . . C66 C 0.9318(3) 0.26692(16) 0.8091(3) 0.0147(9) Uani 1 1 d . . . C67 C 0.9819(3) 0.25946(16) 0.8787(3) 0.0153(9) Uani 1 1 d . . . C68 C 0.9915(3) 0.21672(18) 0.9123(3) 0.0159(10) Uani 1 1 d . . . H68 H 0.9674 0.1906 0.8901 0.019 Uiso 1 1 calc R . . C69 C 1.0369(3) 0.21280(17) 0.9789(3) 0.0196(10) Uani 1 1 d . . . H69 H 1.0443 0.1839 1.0030 0.024 Uiso 1 1 calc R . . C70 C 1.0710(3) 0.25143(16) 1.0095(3) 0.0177(9) Uani 1 1 d . . . H70 H 1.1016 0.2496 1.0554 0.021 Uiso 1 1 calc R . . C71 C 1.0601(3) 0.29293(17) 0.9726(3) 0.0171(10) Uani 1 1 d . . . H71 H 1.0842 0.3194 0.9936 0.021 Uiso 1 1 calc R . . N72 N 1.0163(2) 0.29704(14) 0.9077(2) 0.0126(8) Uani 1 1 d . . . C91 C 1.0514(3) 0.69977(17) 0.9517(3) 0.0158(10) Uani 1 1 d . . . H91 H 1.0786 0.6744 0.9730 0.019 Uiso 1 1 calc R . . C90 C 1.0591(3) 0.74166(19) 0.9872(3) 0.0219(11) Uani 1 1 d . . . H90 H 1.0910 0.7451 1.0321 0.026 Uiso 1 1 calc R . . C89 C 1.0199(3) 0.77863(18) 0.9567(3) 0.0222(11) Uani 1 1 d . . . H89 H 1.0244 0.8078 0.9803 0.027 Uiso 1 1 calc R . . C88 C 0.9740(3) 0.77283(18) 0.8915(3) 0.0194(10) Uani 1 1 d . . . H88 H 0.9468 0.7980 0.8695 0.023 Uiso 1 1 calc R . . C87 C 0.9682(3) 0.72930(16) 0.8581(3) 0.0149(9) Uani 1 1 d . . . C86 C 0.9175(3) 0.71936(17) 0.7905(2) 0.0144(9) Uani 1 1 d . . . C85 C 0.8734(3) 0.75297(17) 0.7534(3) 0.0165(10) Uani 1 1 d . . . H85 H 0.8771 0.7840 0.7689 0.020 Uiso 1 1 calc R . . C84 C 0.8235(3) 0.73985(18) 0.6929(3) 0.0219(11) Uani 1 1 d . . . H84 H 0.7912 0.7617 0.6678 0.026 Uiso 1 1 calc R . . C83 C 0.8220(3) 0.69473(17) 0.6703(3) 0.0194(10) Uani 1 1 d . . . H83 H 0.7888 0.6851 0.6291 0.023 Uiso 1 1 calc R . . C82 C 0.8693(3) 0.66350(18) 0.7080(3) 0.0180(10) Uani 1 1 d . . . H82 H 0.8691 0.6326 0.6910 0.022 Uiso 1 1 calc R . . N92 N 1.0072(2) 0.69325(13) 0.8882(2) 0.0124(8) Uani 1 1 d . . . N81 N 0.9154(2) 0.67531(13) 0.7679(2) 0.0135(8) Uani 1 1 d . . . Yb1 Yb 0.619893(13) 1.011860(8) 0.655173(12) 0.01087(5) Uani 1 1 d . . . O11 O 0.6729(2) 1.07441(15) 0.7195(2) 0.0339(10) Uani 1 1 d . . . H102 H 0.6702 1.0756 0.7679 0.051 Uiso 1 1 d . . . H103 H 0.7211 1.0749 0.7102 0.051 Uiso 1 1 d . . . O12 O 0.5179(2) 1.06263(11) 0.63607(18) 0.0192(7) Uani 1 1 d . . . O13 O 0.5707(3) 1.00380(12) 0.5274(2) 0.0201(9) Uani 1 1 d . . . O14 O 0.5554(2) 1.01867(11) 0.77549(17) 0.0163(7) Uani 1 1 d . . . H106 H 0.5773 1.0170 0.8174 0.024 Uiso 1 1 d . . . H107 H 0.5109 1.0078 0.7810 0.024 Uiso 1 1 d . . . O15 O 0.52662(18) 0.95509(10) 0.66087(18) 0.0151(6) Uani 1 1 d . . . O16 O 0.6929(3) 0.9753(2) 0.7497(2) 0.069(2) Uani 1 1 d . . . Yb2 Yb 0.871437(13) 0.486963(8) 0.666047(11) 0.01043(5) Uani 1 1 d . . . O21 O 0.9264(2) 0.42630(14) 0.5926(2) 0.0282(9) Uani 1 1 d . . . O22 O 0.9392(2) 0.52704(15) 0.57443(19) 0.0281(9) Uani 1 1 d . . . H111 H 0.9212 0.5382 0.5327 0.042 Uiso 1 1 d . . . H112 H 0.9732 0.5470 0.5865 0.042 Uiso 1 1 d . . . O23 O 0.80551(19) 0.47950(12) 0.54629(18) 0.0169(7) Uani 1 1 d . . . H113 H 0.7621 0.4885 0.5315 0.025 Uiso 1 1 d . . . H114 H 0.8209 0.4616 0.5117 0.025 Uiso 1 1 d . . . O24 O 0.7740(2) 0.43555(11) 0.68706(17) 0.0178(7) Uani 1 1 d . . . H115 H 0.7632 0.4169 0.6517 0.027 Uiso 1 1 d . . . H116 H 0.7681 0.4224 0.7278 0.027 Uiso 1 1 d . . . O25 O 0.8264(2) 0.49510(12) 0.7946(2) 0.0180(8) Uani 1 1 d . . . H117 H 0.7804 0.4964 0.8100 0.027 Uiso 1 1 d . . . H118 H 0.8532 0.4995 0.8331 0.027 Uiso 1 1 d . . . O26 O 0.77777(18) 0.54431(11) 0.66403(18) 0.0155(6) Uani 1 1 d . . . H105 H 0.7766 0.5646 0.6287 0.023 Uiso 1 1 d . . . H104 H 0.7793 0.5617 0.7043 0.023 Uiso 1 1 d . . . K1 K 1.11747(8) 0.49161(4) 0.67658(7) 0.0247(3) Uani 1 1 d . . . K2 K 0.36792(8) 0.99824(4) 0.64710(8) 0.0250(3) Uani 1 1 d . . . O101 O 0.4999(2) 0.10330(12) 0.49727(19) 0.0224(7) Uani 1 1 d . . . H120 H 0.4596 0.0928 0.4761 0.034 Uiso 1 1 d . . . H121 H 0.5351 0.0965 0.4652 0.034 Uiso 1 1 d . . . O102 O 0.4885(2) 0.13166(12) 0.73730(18) 0.0193(7) Uani 1 1 d . . . H122 H 0.4504 0.1424 0.7116 0.029 Uiso 1 1 d . . . H123 H 0.4680 0.1262 0.7805 0.029 Uiso 1 1 d . . . O103 O 0.3292(2) 0.91017(13) 0.7008(2) 0.0253(8) Uani 1 1 d . . . H109 H 0.3422 0.9056 0.7471 0.038 Uiso 1 1 d . . . H108 H 0.3535 0.8907 0.6758 0.038 Uiso 1 1 d . . . O104 O 1.23915(19) 0.63540(11) 0.59265(19) 0.0176(7) Uani 1 1 d . . . O105 O 0.7467(2) 0.39750(13) 0.8282(2) 0.0236(8) Uani 1 1 d . . . H144 H 0.7058 0.4079 0.8497 0.035 Uiso 1 1 d . . . H126 H 0.7781 0.3955 0.8652 0.035 Uiso 1 1 d . . . O106 O 1.1695(3) 0.49630(11) 0.8297(2) 0.0199(8) Uani 1 1 d . . . H127 H 1.1530 0.5183 0.8563 0.030 Uiso 1 1 d . . . H128 H 1.1563 0.4734 0.8564 0.030 Uiso 1 1 d . . . O107 O 0.9470(3) 0.49399(12) 0.9091(2) 0.0227(9) Uani 1 1 d . . . H129 H 0.9715 0.4703 0.8966 0.034 Uiso 1 1 d . . . H130 H 0.9766 0.5152 0.8967 0.034 Uiso 1 1 d . . . O108 O 0.7476(2) 0.59252(12) 0.7929(2) 0.0229(8) Uani 1 1 d . . . O109 O 0.7828(2) 0.60653(12) 0.54885(19) 0.0228(7) Uani 1 1 d . . . H132 H 0.7441 0.6065 0.5185 0.034 Uiso 1 1 d . . . H133 H 0.8195 0.5989 0.5183 0.034 Uiso 1 1 d . . . O110 O 1.1631(2) 0.48540(13) 0.5186(2) 0.0226(8) Uani 1 1 d . . . H145 H 1.1262 0.4984 0.4965 0.034 Uiso 1 1 d . . . H134 H 1.1638 0.4584 0.5038 0.034 Uiso 1 1 d . . . O111 O 1.0807(2) 0.40354(13) 0.6116(2) 0.0271(8) Uani 1 1 d . . . O112 O 1.0748(2) 0.57141(13) 0.6004(2) 0.0239(8) Uani 1 1 d . . . O113 O 0.4162(3) 0.99753(12) 0.4916(2) 0.0214(9) Uani 1 1 d . . . O114 O 0.4100(2) 0.98694(14) 0.8055(2) 0.0270(8) Uani 1 1 d . . . O115 O 0.7012(3) 0.99261(15) 0.4152(3) 0.0382(12) Uani 1 1 d . . . H146 H 0.7211 1.0125 0.3863 0.057 Uiso 1 1 d . . . H139 H 0.7381 0.9734 0.4188 0.057 Uiso 1 1 d . . . O116 O 0.5383(2) 0.89511(12) 0.77936(19) 0.0225(7) Uani 1 1 d . . . O117 O 0.4995(2) 0.90769(13) 0.5318(2) 0.0253(8) Uani 1 1 d . . . H140 H 0.5234 0.9044 0.4905 0.038 Uiso 1 1 d . . . H141 H 0.4674 0.8864 0.5348 0.038 Uiso 1 1 d . . . O118 O 0.3205(2) 1.07536(14) 0.7359(2) 0.0298(9) Uani 1 1 d . . . H142 H 0.3316 1.0986 0.7076 0.045 Uiso 1 1 d . . . H143 H 0.2742 1.0831 0.7505 0.045 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01078(17) 0.01156(16) 0.00973(14) -0.00089(11) -0.00004(12) 0.00063(12) Ru2 0.01170(17) 0.01035(15) 0.00910(14) 0.00035(11) 0.00097(12) -0.00012(12) Ru4 0.01096(17) 0.01084(16) 0.00882(14) 0.00006(11) -0.00084(12) -0.00054(12) Ru3 0.01085(17) 0.01148(16) 0.00987(14) 0.00064(11) -0.00056(12) 0.00015(12) N16 0.018(2) 0.022(2) 0.019(2) 0.0026(16) 0.0028(17) -0.0001(17) N15 0.022(2) 0.025(2) 0.0138(19) 0.0024(16) 0.0017(17) 0.0045(18) C16 0.015(3) 0.013(2) 0.015(2) 0.0003(17) -0.0034(18) 0.0005(18) N14 0.018(2) 0.017(2) 0.017(2) 0.0001(15) 0.0043(16) -0.0025(16) C15 0.018(3) 0.016(2) 0.012(2) -0.0029(17) 0.0038(18) 0.0014(19) C14 0.018(3) 0.010(2) 0.015(2) -0.0015(16) -0.0074(18) -0.0013(18) N13 0.024(2) 0.018(2) 0.0133(18) -0.0003(15) -0.0013(15) -0.0078(17) C13 0.012(3) 0.020(3) 0.013(2) 0.0071(18) 0.0005(17) -0.0028(19) N12 0.019(2) 0.023(2) 0.015(2) -0.0009(16) -0.0012(17) -0.0006(17) C12 0.015(3) 0.015(2) 0.015(2) -0.0018(17) -0.0032(18) -0.0006(18) N11 0.024(2) 0.025(2) 0.0157(19) -0.0008(16) -0.0020(17) -0.0078(18) C11 0.016(3) 0.019(3) 0.012(2) 0.0062(18) 0.0032(17) 0.0004(19) N10 0.018(2) 0.021(2) 0.019(2) -0.0007(16) 0.0039(17) 0.0009(17) C10 0.016(3) 0.011(2) 0.016(2) 0.0005(17) -0.0042(19) 0.0005(17) N9 0.027(3) 0.014(2) 0.0127(18) 0.0000(15) -0.0027(15) 0.0074(17) C9 0.013(2) 0.017(2) 0.0114(19) -0.0073(17) 0.0024(16) 0.0028(18) N8 0.019(2) 0.019(2) 0.023(2) 0.0009(16) 0.0023(18) -0.0012(17) C8 0.011(2) 0.014(2) 0.013(2) -0.0006(16) 0.0032(17) 0.0001(17) N7 0.019(2) 0.023(2) 0.017(2) -0.0031(16) -0.0002(17) 0.0003(17) C7 0.013(3) 0.011(2) 0.013(2) 0.0015(16) 0.0030(17) 0.0021(17) N6 0.025(3) 0.025(2) 0.017(2) -0.0031(17) -0.0010(17) 0.0095(18) C6 0.017(3) 0.013(2) 0.012(2) 0.0003(17) -0.0005(17) 0.0011(19) N5 0.020(2) 0.014(2) 0.0153(19) -0.0020(15) 0.0048(15) -0.0039(17) C5 0.015(2) 0.015(2) 0.012(2) -0.0060(17) 0.0007(16) 0.0008(18) N4 0.024(2) 0.020(2) 0.017(2) 0.0003(15) -0.0013(16) 0.0017(17) C4 0.012(2) 0.013(2) 0.018(2) -0.0012(17) 0.0002(18) 0.0012(18) N3 0.020(2) 0.026(2) 0.018(2) -0.0005(16) -0.0026(18) -0.0014(18) C3 0.014(3) 0.013(2) 0.013(2) -0.0016(16) 0.0010(18) -0.0018(18) N2 0.020(2) 0.029(2) 0.0143(19) -0.0008(16) -0.0009(16) -0.0066(19) C2 0.012(2) 0.015(2) 0.013(2) -0.0016(17) -0.0007(17) 0.0010(18) N1 0.019(2) 0.008(2) 0.0187(19) -0.0017(14) 0.0004(15) 0.0032(16) C1 0.013(3) 0.016(2) 0.012(2) 0.0043(17) -0.0014(16) 0.0009(18) C26 0.008(2) 0.017(2) 0.019(2) -0.0002(17) -0.0046(17) 0.0012(17) C25 0.019(3) 0.017(3) 0.025(2) -0.0045(19) -0.0004(19) 0.0002(19) C24 0.024(3) 0.018(2) 0.028(3) -0.011(2) -0.002(2) 0.002(2) C23 0.016(3) 0.026(3) 0.020(2) -0.0075(19) 0.0004(19) 0.0063(19) C22 0.014(3) 0.019(2) 0.014(2) -0.0013(17) -0.0040(18) -0.0009(18) N21 0.014(2) 0.016(2) 0.0117(16) -0.0029(14) -0.0037(14) 0.0047(15) N32 0.014(2) 0.013(2) 0.0148(19) 0.0015(14) -0.0011(14) 0.0016(15) C31 0.016(3) 0.018(3) 0.019(2) 0.0006(18) 0.0033(18) 0.0040(18) C30 0.019(3) 0.023(3) 0.021(2) 0.0033(19) 0.0055(19) 0.0019(18) C29 0.018(3) 0.023(3) 0.026(2) 0.008(2) -0.0021(19) -0.0023(19) C28 0.019(3) 0.015(2) 0.022(2) 0.0004(18) -0.0013(19) -0.0023(19) C27 0.014(2) 0.017(2) 0.015(2) -0.0012(17) -0.0065(17) 0.0042(18) N52 0.010(2) 0.0111(19) 0.0134(17) -0.0011(14) 0.0011(14) -0.0015(14) C51 0.016(3) 0.015(3) 0.017(2) 0.0016(18) -0.0015(18) -0.0029(18) C50 0.016(3) 0.024(3) 0.014(2) -0.0022(17) -0.0012(17) -0.0038(19) C49 0.015(3) 0.021(3) 0.018(2) -0.0075(18) 0.0010(18) 0.0015(19) C48 0.019(3) 0.016(2) 0.017(2) -0.0006(18) 0.0034(18) -0.0035(19) C47 0.012(2) 0.011(2) 0.015(2) 0.0003(16) -0.0026(18) -0.0016(16) C46 0.010(2) 0.018(2) 0.0096(19) -0.0003(16) -0.0016(16) -0.0039(18) C45 0.017(3) 0.015(2) 0.020(2) -0.0017(19) -0.0008(19) -0.0004(19) C44 0.020(3) 0.017(2) 0.018(2) 0.0067(18) -0.0019(19) -0.0059(19) C43 0.018(3) 0.019(2) 0.020(2) 0.0041(18) 0.0028(18) -0.0041(19) C42 0.014(2) 0.018(2) 0.015(2) 0.0015(17) 0.0055(17) -0.0024(18) N41 0.015(2) 0.0100(18) 0.0133(17) -0.0013(14) -0.0023(16) -0.0014(14) C65 0.016(3) 0.016(2) 0.024(2) -0.0019(18) 0.0028(19) -0.0010(19) C64 0.018(3) 0.021(3) 0.021(2) -0.0082(19) 0.0008(19) 0.001(2) C63 0.015(3) 0.028(3) 0.015(2) -0.0063(18) -0.0044(17) 0.002(2) C62 0.016(3) 0.019(3) 0.012(2) 0.0011(18) -0.0019(17) 0.0020(18) N61 0.013(2) 0.013(2) 0.0138(18) -0.0024(14) 0.0012(14) 0.0012(15) C66 0.012(2) 0.018(2) 0.014(2) 0.0023(17) 0.0025(17) 0.0015(18) C67 0.013(2) 0.017(2) 0.016(2) -0.0020(17) 0.0016(18) 0.0002(18) C68 0.015(3) 0.015(2) 0.017(2) 0.0018(17) 0.0024(19) 0.0030(18) C69 0.017(3) 0.019(2) 0.023(2) 0.0060(19) 0.0038(19) 0.0010(19) C70 0.016(2) 0.023(2) 0.015(2) 0.0046(19) -0.0020(18) 0.0005(19) C71 0.018(3) 0.020(2) 0.014(2) -0.0016(18) -0.0005(18) -0.0003(19) N72 0.012(2) 0.014(2) 0.0116(17) 0.0019(14) -0.0005(15) 0.0012(16) C91 0.011(2) 0.020(2) 0.017(2) 0.0002(17) -0.0016(17) -0.0003(18) C90 0.017(3) 0.030(3) 0.019(2) -0.0053(19) -0.0017(17) -0.005(2) C89 0.024(3) 0.019(3) 0.023(2) -0.0093(19) 0.002(2) -0.006(2) C88 0.013(3) 0.021(3) 0.024(2) -0.0034(19) 0.0013(19) -0.0001(19) C87 0.012(2) 0.017(2) 0.016(2) -0.0012(17) 0.0037(17) -0.0010(17) C86 0.010(2) 0.020(2) 0.013(2) 0.0009(16) 0.0031(16) -0.0018(18) C85 0.018(3) 0.014(2) 0.018(2) 0.0019(17) 0.0019(17) 0.0005(19) C84 0.017(3) 0.028(3) 0.020(2) 0.0069(19) -0.0013(18) 0.002(2) C83 0.017(2) 0.024(3) 0.018(2) 0.0055(19) -0.0047(17) -0.0035(18) C82 0.021(3) 0.018(3) 0.014(2) 0.0026(18) -0.0018(18) -0.0058(19) N92 0.009(2) 0.015(2) 0.0129(17) -0.0018(14) 0.0006(14) -0.0010(14) N81 0.011(2) 0.016(2) 0.0135(17) 0.0031(15) -0.0004(14) -0.0020(15) Yb1 0.00946(12) 0.01438(11) 0.00878(11) -0.00071(9) 0.00010(8) -0.00006(9) O11 0.034(2) 0.050(3) 0.0169(16) -0.0163(16) 0.0083(15) -0.0255(19) O12 0.0203(18) 0.0217(18) 0.0158(15) -0.0015(12) -0.0016(12) 0.0069(14) O13 0.019(2) 0.032(2) 0.0091(16) -0.0033(12) 0.0007(13) 0.0006(14) O14 0.0183(18) 0.0211(19) 0.0096(14) -0.0016(12) 0.0011(12) -0.0059(13) O15 0.0144(15) 0.0153(15) 0.0156(14) -0.0025(12) 0.0009(12) -0.0023(12) O16 0.079(4) 0.115(5) 0.0138(18) -0.010(2) -0.014(2) 0.080(4) Yb2 0.00942(12) 0.01392(11) 0.00793(11) -0.00018(9) -0.00034(8) 0.00016(9) O21 0.032(2) 0.035(2) 0.0168(16) -0.0088(14) -0.0043(14) 0.0157(17) O22 0.024(2) 0.045(2) 0.0148(17) 0.0088(15) -0.0040(13) -0.0191(17) O23 0.0148(18) 0.0240(19) 0.0120(14) -0.0040(12) -0.0008(12) 0.0048(14) O24 0.0216(18) 0.0201(18) 0.0116(14) -0.0003(12) 0.0020(12) -0.0118(14) O25 0.010(2) 0.034(2) 0.0106(16) -0.0015(12) 0.0028(13) 0.0007(13) O26 0.0145(16) 0.0184(16) 0.0137(14) 0.0009(12) -0.0020(12) 0.0043(12) K1 0.0235(7) 0.0334(6) 0.0173(6) -0.0002(4) -0.0006(4) 0.0032(5) K2 0.0231(7) 0.0322(7) 0.0197(6) -0.0015(4) 0.0017(4) 0.0031(4) O101 0.0225(19) 0.0262(19) 0.0184(16) 0.0027(14) -0.0010(13) -0.0017(14) O102 0.0184(19) 0.0253(18) 0.0141(15) 0.0005(12) -0.0008(12) 0.0017(14) O103 0.025(2) 0.032(2) 0.0183(16) -0.0029(14) -0.0030(14) 0.0099(16) O104 0.0174(18) 0.0182(17) 0.0172(15) 0.0006(12) -0.0025(13) -0.0008(13) O105 0.0179(19) 0.031(2) 0.0220(17) 0.0029(14) -0.0025(14) -0.0017(14) O106 0.020(2) 0.0172(19) 0.0221(19) -0.0013(13) 0.0049(16) -0.0011(13) O107 0.021(2) 0.026(2) 0.0220(19) -0.0007(14) 0.0025(15) 0.0002(14) O108 0.024(2) 0.0210(19) 0.0234(18) -0.0032(14) 0.0008(14) 0.0030(14) O109 0.0195(18) 0.031(2) 0.0182(16) -0.0001(14) -0.0014(13) 0.0020(15) O110 0.023(2) 0.0216(19) 0.0232(18) -0.0036(14) -0.0083(14) 0.0028(15) O111 0.029(2) 0.032(2) 0.0200(17) 0.0055(14) 0.0053(14) 0.0070(16) O112 0.022(2) 0.029(2) 0.0209(18) -0.0009(14) 0.0037(13) -0.0108(15) O113 0.023(3) 0.023(2) 0.0191(19) -0.0027(13) -0.0019(16) 0.0008(14) O114 0.023(2) 0.030(2) 0.0280(19) -0.0019(16) 0.0007(15) -0.0043(16) O115 0.059(4) 0.031(2) 0.024(2) -0.0041(16) -0.020(2) 0.015(2) O116 0.0247(19) 0.0268(19) 0.0159(15) 0.0006(13) 0.0013(13) 0.0014(15) O117 0.026(2) 0.029(2) 0.0217(17) -0.0058(14) 0.0041(14) -0.0094(15) O118 0.028(2) 0.031(2) 0.030(2) 0.0041(15) -0.0024(15) -0.0038(17) _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 C1 1.980(5) . ? Ru1 C2 1.984(5) . ? Ru1 C3 2.047(5) . ? Ru1 C4 2.055(5) . ? Ru1 N21 2.118(4) . ? Ru1 N32 2.121(4) . ? Ru2 C6 1.977(5) . ? Ru2 C5 1.982(5) . ? Ru2 C7 2.031(5) . ? Ru2 C8 2.042(5) . ? Ru2 N52 2.119(4) . ? Ru2 N41 2.121(4) . ? Ru4 C15 1.973(5) . ? Ru4 C13 1.974(5) . ? Ru4 C16 2.039(5) . ? Ru4 C14 2.046(5) . ? Ru4 N81 2.123(4) . ? Ru4 N92 2.128(4) . ? Ru3 C9 1.955(5) . ? Ru3 C11 1.975(5) . ? Ru3 C12 2.037(5) . ? Ru3 C10 2.041(5) . ? Ru3 N61 2.125(4) . ? Ru3 N72 2.128(4) . ? N16 C16 1.151(7) . ? N15 C15 1.155(7) . ? N14 C14 1.156(7) . ? N13 C13 1.164(7) . ? N13 Yb2 2.394(4) . ? N13 K1 3.390(5) . ? N12 C12 1.161(7) . ? N11 C11 1.150(7) . ? N10 C10 1.150(6) . ? N9 C9 1.162(7) . ? N9 Yb2 2.358(4) . ? N9 K1 3.271(5) . ? N8 C8 1.154(7) . ? N7 C7 1.159(7) . ? N6 C6 1.165(7) . ? N5 C5 1.152(6) . ? N5 Yb1 2.374(4) . ? N5 K2 3.374(5) 3_575 ? N4 C4 1.154(7) . ? N3 C3 1.154(7) . ? N2 C2 1.156(7) . ? N1 C1 1.162(6) . ? N1 Yb1 2.368(4) . ? N1 K2 3.384(5) 3_575 ? C26 N21 1.367(6) . ? C26 C25 1.376(7) . ? C26 C27 1.475(7) . ? C25 C24 1.395(7) . ? C24 C23 1.376(8) . ? C23 C22 1.384(7) . ? C22 N21 1.348(7) . ? N32 C31 1.336(6) . ? N32 C27 1.355(6) . ? C31 C30 1.388(7) . ? C30 C29 1.385(7) . ? C29 C28 1.365(7) . ? C28 C27 1.392(7) . ? N52 C51 1.342(6) . ? N52 C47 1.354(6) . ? C51 C50 1.371(7) . ? C50 C49 1.373(7) . ? C49 C48 1.389(7) . ? C48 C47 1.396(7) . ? C47 C46 1.480(6) . ? C46 N41 1.361(6) . ? C46 C45 1.390(7) . ? C45 C44 1.381(7) . ? C44 C43 1.390(7) . ? C43 C42 1.382(7) . ? C42 N41 1.341(6) . ? C65 C64 1.380(7) . ? C65 C66 1.386(7) . ? C64 C63 1.383(7) . ? C63 C62 1.394(7) . ? C62 N61 1.345(6) . ? N61 C66 1.361(6) . ? C66 C67 1.490(7) . ? C67 N72 1.344(6) . ? C67 C68 1.388(7) . ? C68 C69 1.390(7) . ? C69 C70 1.378(7) . ? C70 C71 1.383(7) . ? C71 N72 1.351(6) . ? C91 N92 1.343(6) . ? C91 C90 1.376(7) . ? C90 C89 1.379(8) . ? C89 C88 1.381(8) . ? C88 C87 1.400(7) . ? C87 N92 1.353(6) . ? C87 C86 1.481(6) . ? C86 N81 1.347(6) . ? C86 C85 1.396(7) . ? C85 C84 1.401(7) . ? C84 C83 1.377(7) . ? C83 C82 1.385(7) . ? C82 N81 1.343(6) . ? Yb1 O15 2.311(3) . ? Yb1 O16 2.314(4) . ? Yb1 O12 2.321(3) . ? Yb1 O11 2.325(4) . ? Yb1 O14 2.354(3) . ? Yb1 O13 2.364(4) . ? Yb1 K2 4.2747(15) 3_575 ? Yb1 K2 4.3503(15) . ? O12 K2 3.199(4) . ? O15 K2 3.015(3) . ? Yb2 O24 2.281(3) . ? Yb2 O22 2.283(3) . ? Yb2 O26 2.326(3) . ? Yb2 O25 2.352(3) . ? Yb2 O23 2.358(3) . ? Yb2 O21 2.375(3) . ? Yb2 K1 4.2338(14) . ? Yb2 K1 4.4128(14) 3_465 ? O26 K1 2.956(3) 3_465 ? K1 O112 2.776(4) . ? K1 O106 2.781(4) . ? K1 O110 2.829(4) . ? K1 O111 2.880(4) . ? K1 O26 2.956(3) 3_565 ? K1 Yb2 4.4128(14) 3_565 ? K2 O113 2.797(4) . ? K2 O103 2.818(4) . ? K2 O114 2.834(4) . ? K2 O118 2.844(4) . ? K2 N5 3.374(5) 3_475 ? K2 N1 3.384(5) 3_475 ? K2 Yb1 4.2747(15) 3_475 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 89.10(19) . . ? C1 Ru1 C3 90.86(19) . . ? C2 Ru1 C3 90.53(19) . . ? C1 Ru1 C4 87.27(19) . . ? C2 Ru1 C4 90.76(19) . . ? C3 Ru1 C4 177.72(18) . . ? C1 Ru1 N21 173.34(18) . . ? C2 Ru1 N21 97.54(17) . . ? C3 Ru1 N21 88.68(17) . . ? C4 Ru1 N21 93.02(17) . . ? C1 Ru1 N32 96.10(17) . . ? C2 Ru1 N32 174.24(18) . . ? C3 Ru1 N32 91.86(17) . . ? C4 Ru1 N32 87.04(17) . . ? N21 Ru1 N32 77.28(16) . . ? C6 Ru2 C5 87.76(19) . . ? C6 Ru2 C7 91.05(19) . . ? C5 Ru2 C7 89.72(19) . . ? C6 Ru2 C8 88.52(19) . . ? C5 Ru2 C8 88.79(19) . . ? C7 Ru2 C8 178.47(18) . . ? C6 Ru2 N52 175.00(18) . . ? C5 Ru2 N52 96.27(17) . . ? C7 Ru2 N52 91.93(17) . . ? C8 Ru2 N52 88.60(16) . . ? C6 Ru2 N41 98.47(17) . . ? C5 Ru2 N41 173.71(17) . . ? C7 Ru2 N41 91.06(16) . . ? C8 Ru2 N41 90.45(16) . . ? N52 Ru2 N41 77.47(15) . . ? C15 Ru4 C13 88.60(19) . . ? C15 Ru4 C16 90.3(2) . . ? C13 Ru4 C16 91.71(19) . . ? C15 Ru4 C14 91.55(19) . . ? C13 Ru4 C14 87.32(18) . . ? C16 Ru4 C14 177.87(19) . . ? C15 Ru4 N81 175.18(18) . . ? C13 Ru4 N81 96.06(18) . . ? C16 Ru4 N81 90.78(17) . . ? C14 Ru4 N81 87.45(17) . . ? C15 Ru4 N92 98.12(18) . . ? C13 Ru4 N92 173.27(18) . . ? C16 Ru4 N92 88.56(17) . . ? C14 Ru4 N92 92.18(16) . . ? N81 Ru4 N92 77.21(15) . . ? C9 Ru3 C11 87.5(2) . . ? C9 Ru3 C12 90.30(19) . . ? C11 Ru3 C12 88.99(19) . . ? C9 Ru3 C10 87.87(18) . . ? C11 Ru3 C10 89.16(19) . . ? C12 Ru3 C10 177.5(2) . . ? C9 Ru3 N61 96.59(17) . . ? C11 Ru3 N61 175.71(18) . . ? C12 Ru3 N61 92.26(17) . . ? C10 Ru3 N61 89.70(17) . . ? C9 Ru3 N72 173.33(18) . . ? C11 Ru3 N72 99.16(17) . . ? C12 Ru3 N72 90.19(18) . . ? C10 Ru3 N72 91.83(17) . . ? N61 Ru3 N72 76.74(15) . . ? N16 C16 Ru4 178.8(5) . . ? N15 C15 Ru4 179.5(5) . . ? N14 C14 Ru4 175.5(4) . . ? C13 N13 Yb2 158.7(4) . . ? C13 N13 K1 108.7(4) . . ? Yb2 N13 K1 92.48(13) . . ? N13 C13 Ru4 178.5(4) . . ? N12 C12 Ru3 178.2(5) . . ? N11 C11 Ru3 176.2(5) . . ? N10 C10 Ru3 175.8(4) . . ? C9 N9 Yb2 151.7(4) . . ? C9 N9 K1 111.3(4) . . ? Yb2 N9 K1 96.19(14) . . ? N9 C9 Ru3 179.4(5) . . ? N8 C8 Ru2 176.6(4) . . ? N7 C7 Ru2 178.0(4) . . ? N6 C6 Ru2 177.9(4) . . ? C5 N5 Yb1 151.8(4) . . ? C5 N5 K2 111.0(4) . 3_575 ? Yb1 N5 K2 94.49(13) . 3_575 ? N5 C5 Ru2 177.9(4) . . ? N4 C4 Ru1 175.1(4) . . ? N3 C3 Ru1 179.6(5) . . ? N2 C2 Ru1 178.0(4) . . ? C1 N1 Yb1 160.0(4) . . ? C1 N1 K2 105.3(4) . 3_575 ? Yb1 N1 K2 94.35(12) . 3_575 ? N1 C1 Ru1 178.0(4) . . ? N21 C26 C25 121.0(5) . . ? N21 C26 C27 115.0(4) . . ? C25 C26 C27 123.9(5) . . ? C26 C25 C24 120.1(5) . . ? C23 C24 C25 118.8(5) . . ? C24 C23 C22 118.8(5) . . ? N21 C22 C23 123.0(5) . . ? C22 N21 C26 118.3(4) . . ? C22 N21 Ru1 125.9(3) . . ? C26 N21 Ru1 115.8(3) . . ? C31 N32 C27 118.8(4) . . ? C31 N32 Ru1 125.5(3) . . ? C27 N32 Ru1 115.6(3) . . ? N32 C31 C30 122.9(5) . . ? C29 C30 C31 118.4(5) . . ? C28 C29 C30 118.9(5) . . ? C29 C28 C27 120.5(5) . . ? N32 C27 C28 120.5(5) . . ? N32 C27 C26 116.0(4) . . ? C28 C27 C26 123.5(4) . . ? C51 N52 C47 118.1(4) . . ? C51 N52 Ru2 126.2(3) . . ? C47 N52 Ru2 115.6(3) . . ? N52 C51 C50 123.4(5) . . ? C51 C50 C49 118.8(5) . . ? C50 C49 C48 119.5(5) . . ? C49 C48 C47 118.6(5) . . ? N52 C47 C48 121.6(4) . . ? N52 C47 C46 115.9(4) . . ? C48 C47 C46 122.5(4) . . ? N41 C46 C45 121.2(4) . . ? N41 C46 C47 115.3(4) . . ? C45 C46 C47 123.5(5) . . ? C44 C45 C46 119.9(5) . . ? C45 C44 C43 118.6(4) . . ? C42 C43 C44 119.1(5) . . ? N41 C42 C43 122.7(5) . . ? C42 N41 C46 118.6(4) . . ? C42 N41 Ru2 125.8(3) . . ? C46 N41 Ru2 115.6(3) . . ? C64 C65 C66 119.5(5) . . ? C65 C64 C63 119.5(5) . . ? C64 C63 C62 118.5(5) . . ? N61 C62 C63 122.3(5) . . ? C62 N61 C66 118.8(4) . . ? C62 N61 Ru3 124.9(3) . . ? C66 N61 Ru3 116.3(3) . . ? N61 C66 C65 121.3(4) . . ? N61 C66 C67 114.8(4) . . ? C65 C66 C67 123.9(4) . . ? N72 C67 C68 122.2(5) . . ? N72 C67 C66 115.5(4) . . ? C68 C67 C66 122.3(5) . . ? C67 C68 C69 118.9(5) . . ? C70 C69 C68 119.0(5) . . ? C69 C70 C71 119.3(5) . . ? N72 C71 C70 122.1(5) . . ? C67 N72 C71 118.5(4) . . ? C67 N72 Ru3 116.5(3) . . ? C71 N72 Ru3 125.0(3) . . ? N92 C91 C90 122.7(5) . . ? C91 C90 C89 118.9(5) . . ? C90 C89 C88 119.4(5) . . ? C89 C88 C87 119.0(5) . . ? N92 C87 C88 121.2(4) . . ? N92 C87 C86 116.0(4) . . ? C88 C87 C86 122.8(5) . . ? N81 C86 C85 121.9(4) . . ? N81 C86 C87 115.5(4) . . ? C85 C86 C87 122.6(4) . . ? C86 C85 C84 118.5(5) . . ? C83 C84 C85 118.9(5) . . ? C84 C83 C82 119.4(5) . . ? N81 C82 C83 122.3(5) . . ? C91 N92 C87 118.7(4) . . ? C91 N92 Ru4 126.0(3) . . ? C87 N92 Ru4 115.3(3) . . ? C82 N81 C86 118.9(4) . . ? C82 N81 Ru4 125.2(3) . . ? C86 N81 Ru4 116.0(3) . . ? O15 Yb1 O16 90.8(2) . . ? O15 Yb1 O12 86.72(12) . . ? O16 Yb1 O12 143.58(13) . . ? O15 Yb1 O11 144.92(12) . . ? O16 Yb1 O11 79.5(2) . . ? O12 Yb1 O11 81.88(14) . . ? O15 Yb1 O14 72.36(11) . . ? O16 Yb1 O14 71.26(14) . . ? O12 Yb1 O14 73.39(12) . . ? O11 Yb1 O14 72.60(12) . . ? O15 Yb1 O13 73.71(13) . . ? O16 Yb1 O13 143.03(16) . . ? O12 Yb1 O13 70.29(12) . . ? O11 Yb1 O13 131.30(14) . . ? O14 Yb1 O13 130.94(14) . . ? O15 Yb1 N1 83.11(13) . . ? O16 Yb1 N1 69.90(15) . . ? O12 Yb1 N1 145.25(13) . . ? O11 Yb1 N1 123.39(15) . . ? O14 Yb1 N1 133.24(13) . . ? O13 Yb1 N1 74.96(14) . . ? O15 Yb1 N5 145.12(12) . . ? O16 Yb1 N5 107.6(2) . . ? O12 Yb1 N5 94.48(14) . . ? O11 Yb1 N5 69.18(13) . . ? O14 Yb1 N5 141.17(12) . . ? O13 Yb1 N5 73.97(14) . . ? N1 Yb1 N5 76.19(15) . . ? O15 Yb1 K2 130.02(8) . 3_575 ? O16 Yb1 K2 56.65(16) . 3_575 ? O12 Yb1 K2 142.42(9) . 3_575 ? O11 Yb1 K2 71.27(11) . 3_575 ? O14 Yb1 K2 120.27(8) . 3_575 ? O13 Yb1 K2 108.63(11) . 3_575 ? N1 Yb1 K2 52.12(11) . 3_575 ? N5 Yb1 K2 51.88(11) . 3_575 ? O15 Yb1 K2 40.99(8) . . ? O16 Yb1 K2 121.30(18) . . ? O12 Yb1 K2 45.79(9) . . ? O11 Yb1 K2 118.53(11) . . ? O14 Yb1 K2 64.33(8) . . ? O13 Yb1 K2 66.76(11) . . ? N1 Yb1 K2 118.03(11) . . ? N5 Yb1 K2 131.10(11) . . ? K2 Yb1 K2 170.063(15) 3_575 . ? Yb1 O12 K2 102.86(12) . . ? Yb1 O15 K2 108.82(11) . . ? O24 Yb2 O22 145.41(12) . . ? O24 Yb2 O26 88.31(12) . . ? O22 Yb2 O26 88.39(14) . . ? O24 Yb2 O25 71.13(12) . . ? O22 Yb2 O25 139.74(14) . . ? O26 Yb2 O25 73.32(12) . . ? O24 Yb2 O23 73.98(12) . . ? O22 Yb2 O23 72.04(12) . . ? O26 Yb2 O23 73.83(11) . . ? O25 Yb2 O23 132.07(13) . . ? O24 Yb2 N9 91.11(14) . . ? O22 Yb2 N9 109.41(15) . . ? O26 Yb2 N9 147.45(13) . . ? O25 Yb2 N9 75.73(14) . . ? O23 Yb2 N9 136.84(13) . . ? O24 Yb2 O21 83.26(13) . . ? O22 Yb2 O21 79.34(15) . . ? O26 Yb2 O21 143.82(12) . . ? O25 Yb2 O21 134.89(13) . . ? O23 Yb2 O21 70.01(12) . . ? N9 Yb2 O21 68.11(13) . . ? O24 Yb2 N13 142.73(12) . . ? O22 Yb2 N13 70.88(14) . . ? O26 Yb2 N13 83.90(14) . . ? O25 Yb2 N13 71.72(14) . . ? O23 Yb2 N13 136.89(13) . . ? N9 Yb2 N13 77.05(16) . . ? O21 Yb2 N13 122.53(15) . . ? O24 Yb2 K1 138.40(9) . . ? O22 Yb2 K1 60.21(10) . . ? O26 Yb2 K1 131.95(8) . . ? O25 Yb2 K1 106.58(11) . . ? O23 Yb2 K1 121.33(8) . . ? N9 Yb2 K1 50.18(12) . . ? O21 Yb2 K1 69.48(10) . . ? N13 Yb2 K1 53.12(11) . . ? O24 Yb2 K1 50.28(9) . 3_465 ? O22 Yb2 K1 117.39(10) . 3_465 ? O26 Yb2 K1 38.15(8) . 3_465 ? O25 Yb2 K1 67.76(10) . 3_465 ? O23 Yb2 K1 64.78(8) . 3_465 ? N9 Yb2 K1 133.16(11) . 3_465 ? O21 Yb2 K1 121.43(10) . 3_465 ? N13 Yb2 K1 115.84(11) . 3_465 ? K1 Yb2 K1 168.890(16) . 3_465 ? Yb2 O26 K1 112.77(12) . 3_465 ? O112 K1 O106 119.27(11) . . ? O112 K1 O110 71.08(11) . . ? O106 K1 O110 145.13(13) . . ? O112 K1 O111 120.84(11) . . ? O106 K1 O111 118.79(11) . . ? O110 K1 O111 68.38(11) . . ? O112 K1 O26 120.75(11) . 3_565 ? O106 K1 O26 77.69(11) . 3_565 ? O110 K1 O26 69.45(10) . 3_565 ? O111 K1 O26 81.82(10) . 3_565 ? O112 K1 N9 107.78(11) . . ? O106 K1 N9 88.34(12) . . ? O110 K1 N9 121.77(11) . . ? O111 K1 N9 63.72(11) . . ? O26 K1 N9 130.30(10) 3_565 . ? O112 K1 N13 61.52(10) . . ? O106 K1 N13 89.90(12) . . ? O110 K1 N13 121.48(11) . . ? O111 K1 N13 108.61(11) . . ? O26 K1 N13 166.75(10) 3_565 . ? N9 K1 N13 52.73(10) . . ? O112 K1 Yb2 75.10(8) . . ? O106 K1 Yb2 111.30(10) . . ? O110 K1 Yb2 103.52(8) . . ? O111 K1 Yb2 74.67(8) . . ? O26 K1 Yb2 156.33(7) 3_565 . ? N9 K1 Yb2 33.63(7) . . ? N13 K1 Yb2 34.40(7) . . ? O112 K1 Yb2 97.04(8) . 3_565 ? O106 K1 Yb2 73.36(10) . 3_565 ? O110 K1 Yb2 72.28(8) . 3_565 ? O111 K1 Yb2 109.17(8) . 3_565 ? O26 K1 Yb2 29.08(6) 3_565 3_565 ? N9 K1 Yb2 154.28(8) . 3_565 ? N13 K1 Yb2 142.19(8) . 3_565 ? Yb2 K1 Yb2 172.05(3) . 3_565 ? O113 K2 O103 112.07(11) . . ? O113 K2 O114 147.17(13) . . ? O103 K2 O114 68.83(11) . . ? O113 K2 O118 127.10(11) . . ? O103 K2 O118 118.88(11) . . ? O114 K2 O118 69.57(12) . . ? O113 K2 O15 78.68(12) . . ? O103 K2 O15 78.71(10) . . ? O114 K2 O15 69.21(11) . . ? O118 K2 O15 123.35(11) . . ? O113 K2 O12 73.09(11) . . ? O103 K2 O12 138.48(11) . . ? O114 K2 O12 85.43(10) . . ? O118 K2 O12 78.16(11) . . ? O15 K2 O12 61.50(8) . . ? O113 K2 N5 83.01(12) . 3_475 ? O103 K2 N5 62.12(10) . 3_475 ? O114 K2 N5 121.32(11) . 3_475 ? O118 K2 N5 108.30(12) . 3_475 ? O15 K2 N5 125.89(10) . 3_475 ? O12 K2 N5 153.22(10) . 3_475 ? O113 K2 N1 91.39(12) . 3_475 ? O103 K2 N1 105.00(11) . 3_475 ? O114 K2 N1 120.69(12) . 3_475 ? O118 K2 N1 63.30(11) . 3_475 ? O15 K2 N1 170.06(10) . 3_475 ? O12 K2 N1 116.22(9) . 3_475 ? N5 K2 N1 51.32(10) 3_475 3_475 ? O113 K2 Yb1 109.02(10) . 3_475 ? O103 K2 Yb1 71.99(8) . 3_475 ? O114 K2 Yb1 102.42(9) . 3_475 ? O118 K2 Yb1 75.63(9) . 3_475 ? O15 K2 Yb1 150.50(7) . 3_475 ? O12 K2 Yb1 147.78(7) . 3_475 ? N5 K2 Yb1 33.62(7) 3_475 3_475 ? N1 K2 Yb1 33.53(7) 3_475 3_475 ? O113 K2 Yb1 74.70(10) . . ? O103 K2 Yb1 107.95(8) . . ? O114 K2 Yb1 74.12(9) . . ? O118 K2 Yb1 101.27(9) . . ? O15 K2 Yb1 30.19(6) . . ? O12 K2 Yb1 31.35(6) . . ? N5 K2 Yb1 149.91(8) 3_475 . ? N1 K2 Yb1 147.00(7) 3_475 . ? Yb1 K2 Yb1 176.10(4) 3_475 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 70.17 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.733 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.104 #===END data_imw52m _database_code_depnum_ccdc_archive 'CCDC 235084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H74 N18 O25 Ru3 Yb2' _chemical_formula_sum 'C42 H74 N18 O25 Ru3 Yb2' _chemical_formula_weight 1880.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 14.442(2) _cell_length_b 15.449(2) _cell_length_c 16.392(2) _cell_angle_alpha 76.905(2) _cell_angle_beta 69.370(2) _cell_angle_gamma 79.148(2) _cell_volume 3309.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8048 _cell_measurement_theta_min 4.812 _cell_measurement_theta_max 54.825 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 3.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2695 _exptl_absorpt_correction_T_max 0.2803 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _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 35749 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.56 _reflns_number_total 14538 _reflns_number_gt 11590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+34.1551P] 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 14538 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.78519(5) 0.74765(5) 0.53325(4) 0.03303(17) Uani 1 1 d . . . Ru2 Ru 0.93028(5) 0.27373(4) 0.16989(4) 0.02651(15) Uani 1 1 d . . . Ru3 Ru 0.49925(5) -0.24345(4) 0.25229(4) 0.02713(15) Uani 1 1 d . . . Yb1 Yb 1.14132(3) -0.04131(2) 0.25821(3) 0.03348(11) Uani 1 1 d . . . Yb2 Yb 0.63108(3) 0.06823(3) 0.23555(3) 0.04535(13) Uani 1 1 d . . . N1 N 0.9138(10) 0.8897(7) 0.5328(7) 0.078(4) Uani 1 1 d . . . N2 N 0.6596(8) 0.7462(7) 0.7364(6) 0.063(3) Uani 1 1 d . . . N3 N 0.6270(10) 0.9028(7) 0.4894(9) 0.080(4) Uani 1 1 d . . . N4 N 0.9103(11) 0.7563(10) 0.3289(7) 0.098(5) Uani 1 1 d . . . N5 N 0.8787(5) 0.6349(5) 0.5687(5) 0.0340(16) Uani 1 1 d . . . N6 N 0.7136(5) 0.6413(4) 0.5320(4) 0.0260(13) Uani 1 1 d . . . N7 N 0.7595(6) 0.1589(5) 0.2014(6) 0.0405(17) Uani 1 1 d . . . N8 N 0.8432(6) 0.2862(7) 0.3759(6) 0.051(2) Uani 1 1 d . . . N9 N 1.0365(7) 0.2360(6) -0.0264(6) 0.050(2) Uani 1 1 d . . . N10 N 1.0616(6) 0.1004(5) 0.2252(6) 0.049(2) Uani 1 1 d . . . N11 N 0.8546(5) 0.3979(4) 0.1269(4) 0.0264(13) Uani 1 1 d . . . N12 N 1.0292(5) 0.3661(5) 0.1534(5) 0.0326(15) Uani 1 1 d . . . N13 N 0.5978(7) -0.0762(6) 0.2456(7) 0.056(2) Uani 1 1 d . . . N14 N 0.2987(6) -0.1251(5) 0.2488(5) 0.0431(18) Uani 1 1 d . . . N15 N 0.4136(6) -0.2570(6) 0.4618(5) 0.0441(19) Uani 1 1 d . . . N16 N 0.5937(7) -0.2255(7) 0.0431(6) 0.057(2) Uani 1 1 d . . . N17 N 0.6190(5) -0.3404(5) 0.2677(5) 0.0295(14) Uani 1 1 d . . . N18 N 0.4484(5) -0.3635(4) 0.2537(4) 0.0280(14) Uani 1 1 d . . . O1 O 0.5589(15) 0.0511(7) 0.3804(7) 0.189(10) Uani 1 1 d . . . H1A H 0.4960 0.0520 0.4031 0.227 Uiso 1 1 d R . . H1B H 0.5947 0.0437 0.4135 0.227 Uiso 1 1 d R . . O2 O 0.4625(12) 0.0788(11) 0.2427(11) 0.141(5) Uiso 1 1 d . . . H2A H 0.4443 0.1074 0.1990 0.169 Uiso 1 1 d R . . H2B H 0.4203 0.0540 0.2889 0.169 Uiso 1 1 d R . . O3 O 0.6003(15) 0.1506(13) 0.1018(13) 0.170(7) Uiso 1 1 d . . . H3A H 0.5425 0.1588 0.0969 0.204 Uiso 1 1 d R . . H3B H 0.6485 0.1725 0.0595 0.204 Uiso 1 1 d R . . O4 O 0.5522(5) 0.2101(5) 0.2646(5) 0.0464(16) Uani 1 1 d . . . H4A H 0.5822 0.2534 0.2625 0.19(11) Uiso 1 1 d R . . H4B H 0.4906 0.2229 0.2919 0.10(6) Uiso 1 1 d R . . O5 O 0.7470(6) 0.0245(6) 0.1094(5) 0.058(2) Uani 1 1 d . . . H5A H 0.7279 0.0136 0.0696 0.070 Uiso 1 1 d R . . H5B H 0.8088 0.0193 0.1025 0.070 Uiso 1 1 d R . . O6 O 0.7520(7) -0.0209(7) 0.2899(7) 0.089(4) Uani 1 1 d . . . H6A H 0.7365 -0.0678 0.3279 0.107 Uiso 1 1 d R . . H6B H 0.8106 -0.0065 0.2733 0.107 Uiso 1 1 d R . . O7 O 0.9675(14) -0.0459(13) 0.3107(12) 0.169(7) Uiso 1 1 d . . . H7A H 0.9269 -0.0098 0.3427 0.203 Uiso 1 1 d R . . H7B H 0.9458 -0.0836 0.2936 0.203 Uiso 1 1 d R . . O8 O 1.0942(9) -0.0458(6) 0.4079(6) 0.087(3) Uani 1 1 d . . . H8A H 1.0989 -0.0884 0.4499 0.104 Uiso 1 1 d R . . H8B H 1.0841 0.0030 0.4272 0.104 Uiso 1 1 d R . . O9 O 1.2340(6) 0.0506(6) 0.2892(6) 0.072(3) Uani 1 1 d . . . H9A H 1.2039 0.0905 0.3208 0.087 Uiso 1 1 d R . . H9B H 1.2973 0.0438 0.2690 0.087 Uiso 1 1 d R . . O10 O 1.2511(6) 0.0144(6) 0.1222(5) 0.071(3) Uani 1 1 d . . . H10A H 1.2914 0.0495 0.1192 0.086 Uiso 1 1 d R . . H10B H 1.2508 -0.0002 0.0754 0.086 Uiso 1 1 d R . . O11 O 1.1297(13) -0.0938(12) 0.1452(12) 0.158(6) Uiso 1 1 d . . . H11A H 1.0890 -0.0647 0.1190 0.190 Uiso 1 1 d R . . H11B H 1.1288 -0.1492 0.1476 0.190 Uiso 1 1 d R . . O12 O 1.1099(5) -0.1883(4) 0.3239(4) 0.0438(15) Uani 1 1 d . . . H12A H 1.1330 -0.2155 0.3651 0.053 Uiso 1 1 d R . . H12B H 1.0754 -0.2146 0.3065 0.053 Uiso 1 1 d R . . O13 O 0.4516(19) 0.0228(17) 0.0843(17) 0.222(10) Uiso 1 1 d . . . O14 O 0.9524(9) 0.0383(8) 0.0763(8) 0.091(3) Uiso 1 1 d . . . O15 O 0.8187(8) 0.0734(8) 0.3935(7) 0.088(3) Uiso 1 1 d . . . O16 O 0.6281(5) 0.2853(4) 0.3541(4) 0.0370(13) Uiso 1 1 d . . . O17 O 0.7708(5) 0.8725(4) 0.0310(4) 0.0422(15) Uiso 1 1 d . . . O18 O 0.336(3) 0.837(2) 0.049(2) 0.297(15) Uiso 1 1 d . . . O19 O 0.2025(5) 0.7311(4) 0.4407(4) 0.0400(14) Uiso 1 1 d . . . O20 O 0.3320(8) 0.9491(7) 0.4181(7) 0.079(3) Uiso 1 1 d . . . O21 O 0.4177(16) 0.5800(15) 0.9922(14) 0.104(8) Uiso 0.58(2) 1 d P A 1 O21' O 0.3934(15) 0.6911(14) 0.9226(13) 0.061(7) Uiso 0.42(2) 1 d P A 2 O23 O 0.5518(11) 0.7065(10) 0.9185(10) 0.124(5) Uiso 1 1 d . . . O24 O 0.6449(15) 0.8295(14) 0.8593(13) 0.174(7) Uiso 1 1 d . . . O25 O 0.8615(18) 0.3084(17) 0.7924(16) 0.214(10) Uiso 1 1 d . . . O26 O 0.9680(16) 0.2362(15) 0.8418(14) 0.183(8) Uiso 1 1 d . . . C1 C 0.8639(9) 0.8380(7) 0.5341(6) 0.052(3) Uani 1 1 d . . . C2 C 0.7086(8) 0.7465(6) 0.6633(6) 0.041(2) Uani 1 1 d . . . C3 C 0.6874(9) 0.8448(7) 0.5048(7) 0.054(3) Uani 1 1 d . . . C4 C 0.8630(9) 0.7521(8) 0.4022(7) 0.053(3) Uani 1 1 d . . . C5 C 0.9604(7) 0.6362(9) 0.5907(7) 0.050(3) Uani 1 1 d . . . H5C H 0.9818 0.6922 0.5860 0.060 Uiso 1 1 calc R . . C6 C 1.0134(8) 0.5587(11) 0.6195(8) 0.067(4) Uani 1 1 d . . . H6C H 1.0700 0.5620 0.6351 0.080 Uiso 1 1 calc R . . C7 C 0.9853(7) 0.4773(9) 0.6259(7) 0.055(3) Uani 1 1 d . . . H7C H 1.0221 0.4236 0.6451 0.065 Uiso 1 1 calc R . . C8 C 0.9015(6) 0.4746(7) 0.6038(6) 0.0373(19) Uani 1 1 d . . . H8A' H 0.8795 0.4190 0.6084 0.045 Uiso 1 1 calc R . . C9 C 0.8507(6) 0.5542(6) 0.5750(5) 0.0316(17) Uani 1 1 d . . . C10 C 0.7604(6) 0.5582(5) 0.5498(5) 0.0277(16) Uani 1 1 d . . . C11 C 0.7259(6) 0.4816(5) 0.5454(5) 0.0298(16) Uani 1 1 d . . . H11A' H 0.7614 0.4242 0.5563 0.036 Uiso 1 1 calc R . . C12 C 0.6390(7) 0.4904(6) 0.5249(6) 0.038(2) Uani 1 1 d . . . H12A' H 0.6134 0.4394 0.5215 0.046 Uiso 1 1 calc R . . C13 C 0.5901(7) 0.5763(7) 0.5092(6) 0.038(2) Uani 1 1 d . . . H13A H 0.5300 0.5845 0.4956 0.046 Uiso 1 1 calc R . . C14 C 0.6290(6) 0.6485(6) 0.5136(6) 0.0315(17) Uani 1 1 d . . . H14A H 0.5944 0.7065 0.5030 0.038 Uiso 1 1 calc R . . C15 C 0.8251(6) 0.1996(5) 0.1880(6) 0.0301(17) Uani 1 1 d . . . C16 C 0.8725(6) 0.2850(6) 0.3009(6) 0.0330(18) Uani 1 1 d . . . C17 C 0.9953(6) 0.2532(5) 0.0436(6) 0.0337(18) Uani 1 1 d . . . C18 C 1.0117(6) 0.1651(6) 0.2061(6) 0.038(2) Uani 1 1 d . . . C19 C 0.7675(6) 0.4083(6) 0.1112(6) 0.0339(18) Uani 1 1 d . . . H19A H 0.7351 0.3568 0.1217 0.041 Uiso 1 1 calc R . . C20 C 0.7228(7) 0.4907(6) 0.0804(6) 0.041(2) Uani 1 1 d . . . H20A H 0.6614 0.4955 0.0696 0.049 Uiso 1 1 calc R . . C21 C 0.7693(8) 0.5654(6) 0.0657(6) 0.047(2) Uani 1 1 d . . . H21A H 0.7406 0.6228 0.0444 0.056 Uiso 1 1 calc R . . C22 C 0.8584(8) 0.5558(6) 0.0824(6) 0.042(2) Uani 1 1 d . . . H22A H 0.8906 0.6069 0.0740 0.051 Uiso 1 1 calc R . . C23 C 0.9011(7) 0.4706(5) 0.1119(5) 0.0331(18) Uani 1 1 d . . . C24 C 0.9956(7) 0.4543(6) 0.1298(5) 0.0328(18) Uani 1 1 d . . . C25 C 1.0515(8) 0.5221(7) 0.1234(6) 0.046(2) Uani 1 1 d . . . H25A H 1.0279 0.5831 0.1078 0.055 Uiso 1 1 calc R . . C26 C 1.1405(9) 0.4994(8) 0.1401(7) 0.056(3) Uani 1 1 d . . . H26A H 1.1793 0.5448 0.1352 0.068 Uiso 1 1 calc R . . C27 C 1.1737(8) 0.4107(8) 0.1639(7) 0.050(3) Uani 1 1 d . . . H27A H 1.2351 0.3940 0.1757 0.060 Uiso 1 1 calc R . . C28 C 1.1157(7) 0.3472(7) 0.1700(6) 0.042(2) Uani 1 1 d . . . H28A H 1.1382 0.2862 0.1872 0.050 Uiso 1 1 calc R . . C29 C 0.5619(7) -0.1384(6) 0.2473(6) 0.039(2) Uani 1 1 d . . . C30 C 0.3746(7) -0.1662(6) 0.2467(6) 0.0345(18) Uani 1 1 d . . . C31 C 0.4445(6) -0.2536(5) 0.3865(6) 0.0297(16) Uani 1 1 d . . . C32 C 0.5584(7) -0.2315(6) 0.1184(6) 0.0361(19) Uani 1 1 d . . . C33 C 0.7037(6) -0.3243(6) 0.2766(6) 0.0359(19) Uani 1 1 d . . . H33A H 0.7143 -0.2641 0.2707 0.043 Uiso 1 1 calc R . . C34 C 0.7744(7) -0.3913(7) 0.2939(7) 0.045(2) Uani 1 1 d . . . H34A H 0.8345 -0.3778 0.2968 0.053 Uiso 1 1 calc R . . C35 C 0.7565(7) -0.4799(7) 0.3071(7) 0.044(2) Uani 1 1 d . . . H35A H 0.8031 -0.5276 0.3219 0.053 Uiso 1 1 calc R . . C36 C 0.6704(6) -0.4976(6) 0.2983(6) 0.0353(18) Uani 1 1 d . . . H36A H 0.6573 -0.5576 0.3066 0.042 Uiso 1 1 calc R . . C37 C 0.6041(6) -0.4270(5) 0.2774(5) 0.0288(16) Uani 1 1 d . . . C38 C 0.5126(6) -0.4399(5) 0.2626(5) 0.0286(16) Uani 1 1 d . . . C39 C 0.4922(7) -0.5221(6) 0.2574(6) 0.0357(18) Uani 1 1 d . . . H39A H 0.5365 -0.5746 0.2661 0.043 Uiso 1 1 calc R . . C40 C 0.4075(8) -0.5272(7) 0.2395(7) 0.044(2) Uani 1 1 d . . . H40A H 0.3937 -0.5828 0.2337 0.053 Uiso 1 1 calc R . . C41 C 0.3425(7) -0.4500(7) 0.2301(6) 0.043(2) Uani 1 1 d . . . H41A H 0.2832 -0.4524 0.2185 0.052 Uiso 1 1 calc R . . C42 C 0.3647(6) -0.3696(6) 0.2377(6) 0.0353(19) Uani 1 1 d . . . H42A H 0.3196 -0.3171 0.2314 0.042 Uiso 1 1 calc R . . 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 0.0362(4) 0.0333(4) 0.0289(3) -0.0102(3) 0.0001(3) -0.0174(3) Ru2 0.0227(3) 0.0191(3) 0.0345(3) -0.0027(2) -0.0057(2) -0.0038(2) Ru3 0.0266(3) 0.0271(3) 0.0294(3) -0.0018(2) -0.0098(3) -0.0095(2) Yb1 0.0394(2) 0.02305(18) 0.0358(2) 0.00514(14) -0.01544(16) -0.00454(14) Yb2 0.0388(2) 0.0429(2) 0.0570(3) -0.0188(2) -0.00464(19) -0.02020(18) N1 0.125(10) 0.065(7) 0.060(6) -0.012(5) -0.024(6) -0.060(7) N2 0.073(7) 0.051(5) 0.042(5) -0.013(4) 0.012(5) -0.008(5) N3 0.088(8) 0.040(5) 0.090(9) 0.000(5) -0.022(7) 0.013(5) N4 0.115(10) 0.142(12) 0.042(6) -0.027(7) 0.013(6) -0.094(10) N5 0.020(3) 0.056(5) 0.031(4) -0.023(3) -0.002(3) -0.009(3) N6 0.026(3) 0.030(3) 0.021(3) -0.005(3) -0.005(2) -0.008(3) N7 0.037(4) 0.033(4) 0.052(5) -0.007(3) -0.012(4) -0.009(3) N8 0.035(4) 0.068(6) 0.048(5) -0.014(4) -0.009(4) -0.008(4) N9 0.052(5) 0.041(5) 0.051(5) -0.024(4) -0.001(4) -0.001(4) N10 0.031(4) 0.026(4) 0.072(6) 0.011(4) -0.009(4) -0.001(3) N11 0.028(3) 0.020(3) 0.027(3) -0.005(2) -0.005(3) 0.002(2) N12 0.032(4) 0.031(4) 0.035(4) -0.005(3) -0.007(3) -0.013(3) N13 0.045(5) 0.053(5) 0.067(6) -0.025(5) 0.004(4) -0.021(4) N14 0.046(5) 0.035(4) 0.045(5) 0.004(3) -0.020(4) 0.000(3) N15 0.035(4) 0.059(5) 0.041(5) -0.010(4) -0.015(3) -0.007(4) N16 0.057(6) 0.070(6) 0.039(5) -0.003(4) -0.011(4) -0.010(5) N17 0.022(3) 0.037(4) 0.032(3) -0.010(3) -0.008(3) -0.006(3) N18 0.032(3) 0.031(3) 0.025(3) -0.001(3) -0.012(3) -0.011(3) O1 0.32(2) 0.058(6) 0.051(6) 0.027(5) 0.048(9) 0.065(10) O4 0.044(4) 0.036(3) 0.058(4) -0.001(3) -0.017(3) -0.008(3) O5 0.058(5) 0.069(5) 0.054(4) -0.023(4) -0.009(4) -0.024(4) O6 0.084(7) 0.082(7) 0.117(8) 0.044(6) -0.071(6) -0.049(5) O8 0.140(9) 0.043(5) 0.059(5) -0.017(4) 0.008(6) -0.036(5) O9 0.041(4) 0.080(6) 0.097(7) -0.047(5) 0.000(4) -0.015(4) O10 0.055(5) 0.086(6) 0.044(4) 0.016(4) -0.012(4) 0.019(4) O12 0.060(4) 0.029(3) 0.041(4) 0.003(3) -0.018(3) -0.010(3) C1 0.068(7) 0.057(6) 0.034(5) -0.019(5) 0.002(5) -0.039(5) C2 0.053(6) 0.028(4) 0.034(5) -0.011(4) 0.001(4) -0.006(4) C3 0.075(8) 0.035(5) 0.042(6) -0.002(4) -0.004(5) -0.019(5) C4 0.066(7) 0.062(7) 0.036(5) -0.015(5) 0.002(5) -0.047(6) C5 0.031(5) 0.085(8) 0.048(6) -0.032(6) -0.013(4) -0.015(5) C6 0.031(5) 0.131(12) 0.052(7) -0.033(7) -0.018(5) -0.014(6) C7 0.032(5) 0.089(9) 0.049(6) -0.016(6) -0.024(4) 0.005(5) C8 0.030(4) 0.051(5) 0.032(4) -0.011(4) -0.012(3) 0.002(4) C9 0.024(4) 0.047(5) 0.027(4) -0.019(4) -0.004(3) -0.006(3) C10 0.022(4) 0.033(4) 0.028(4) -0.007(3) -0.007(3) -0.005(3) C11 0.029(4) 0.030(4) 0.034(4) -0.007(3) -0.013(3) -0.005(3) C12 0.043(5) 0.038(5) 0.042(5) -0.002(4) -0.018(4) -0.024(4) C13 0.030(4) 0.052(5) 0.039(5) 0.002(4) -0.019(4) -0.017(4) C14 0.024(4) 0.033(4) 0.036(4) 0.002(3) -0.013(3) -0.005(3) C15 0.031(4) 0.015(3) 0.039(4) -0.004(3) -0.007(3) -0.002(3) C16 0.021(4) 0.035(4) 0.039(5) -0.006(4) -0.005(3) -0.005(3) C17 0.025(4) 0.020(4) 0.052(5) -0.008(4) -0.006(4) -0.004(3) C18 0.024(4) 0.034(4) 0.045(5) 0.003(4) -0.005(4) -0.007(3) C19 0.030(4) 0.033(4) 0.034(4) -0.007(3) -0.006(3) 0.000(3) C20 0.034(5) 0.040(5) 0.036(5) -0.003(4) -0.004(4) 0.008(4) C21 0.055(6) 0.028(4) 0.038(5) 0.003(4) -0.006(4) 0.010(4) C22 0.053(6) 0.022(4) 0.037(5) -0.006(3) 0.005(4) -0.005(4) C23 0.040(5) 0.027(4) 0.026(4) -0.009(3) 0.003(3) -0.010(3) C24 0.043(5) 0.028(4) 0.027(4) -0.005(3) -0.007(3) -0.012(3) C25 0.069(7) 0.039(5) 0.035(5) -0.006(4) -0.013(5) -0.031(5) C26 0.075(8) 0.067(7) 0.041(5) -0.006(5) -0.017(5) -0.053(6) C27 0.053(6) 0.065(7) 0.042(5) 0.008(5) -0.025(5) -0.033(5) C28 0.038(5) 0.047(5) 0.035(5) 0.003(4) -0.008(4) -0.015(4) C29 0.035(5) 0.034(4) 0.049(5) -0.011(4) -0.007(4) -0.017(4) C30 0.041(5) 0.030(4) 0.030(4) 0.006(3) -0.013(4) -0.009(4) C31 0.025(4) 0.031(4) 0.034(4) -0.001(3) -0.011(3) -0.007(3) C32 0.035(4) 0.033(4) 0.038(5) 0.002(4) -0.010(4) -0.011(3) C33 0.026(4) 0.042(5) 0.046(5) -0.020(4) -0.009(4) -0.009(3) C34 0.025(4) 0.067(7) 0.052(6) -0.029(5) -0.014(4) -0.004(4) C35 0.036(5) 0.052(6) 0.054(6) -0.028(5) -0.022(4) 0.010(4) C36 0.033(4) 0.036(4) 0.037(5) -0.013(4) -0.012(4) 0.003(3) C37 0.032(4) 0.033(4) 0.024(4) -0.007(3) -0.008(3) -0.009(3) C38 0.030(4) 0.033(4) 0.023(4) -0.003(3) -0.009(3) -0.010(3) C39 0.040(5) 0.034(4) 0.034(4) -0.003(4) -0.011(4) -0.013(4) C40 0.056(6) 0.043(5) 0.043(5) -0.006(4) -0.016(5) -0.030(5) C41 0.042(5) 0.057(6) 0.044(5) 0.003(4) -0.023(4) -0.029(5) C42 0.032(4) 0.045(5) 0.032(4) 0.004(4) -0.015(4) -0.016(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 Ru1 C3 1.953(13) . ? Ru1 C1 1.964(9) . ? Ru1 C2 2.024(9) . ? Ru1 C4 2.035(10) . ? Ru1 N5 2.099(8) . ? Ru1 N6 2.106(6) . ? Ru2 C18 1.962(9) . ? Ru2 C15 1.973(8) . ? Ru2 C17 2.021(9) . ? Ru2 C16 2.047(9) . ? Ru2 N12 2.114(7) . ? Ru2 N11 2.124(6) . ? Ru3 C29 1.976(8) . ? Ru3 C30 1.983(9) . ? Ru3 C32 2.033(9) . ? Ru3 C31 2.038(8) . ? Ru3 N18 2.111(7) . ? Ru3 N17 2.112(7) . ? Yb1 O11 2.252(18) . ? Yb1 O8 2.293(9) . ? Yb1 N10 2.316(7) . ? Yb1 O10 2.319(8) . ? Yb1 O12 2.336(6) . ? Yb1 O7 2.358(19) . ? Yb1 O9 2.364(8) . ? Yb1 N14 2.366(8) 1_655 ? Yb1 H11A 2.7572 . ? Yb2 O1 2.206(10) . ? Yb2 O5 2.303(8) . ? Yb2 O6 2.318(9) . ? Yb2 N13 2.328(9) . ? Yb2 O4 2.341(7) . ? Yb2 N7 2.368(8) . ? Yb2 O2 2.372(16) . ? Yb2 O3 2.415(19) . ? Yb2 H1A 2.7397 . ? Yb2 H1B 2.7248 . ? N1 C1 1.165(13) . ? N2 C2 1.157(12) . ? N3 C3 1.176(16) . ? N4 C4 1.148(14) . ? N5 C5 1.354(11) . ? N5 C9 1.354(11) . ? N6 C14 1.339(10) . ? N6 C10 1.354(10) . ? N7 C15 1.165(11) . ? N8 C16 1.154(12) . ? N9 C17 1.157(12) . ? N10 C18 1.167(12) . ? N11 C19 1.343(11) . ? N11 C23 1.348(10) . ? N12 C28 1.337(12) . ? N12 C24 1.373(11) . ? N13 C29 1.164(12) . ? N14 C30 1.152(12) . ? N14 Yb1 2.366(8) 1_455 ? N15 C31 1.147(11) . ? N16 C32 1.146(13) . ? N17 C33 1.355(10) . ? N17 C37 1.359(10) . ? N18 C42 1.349(10) . ? N18 C38 1.371(11) . ? O1 H1A 0.8500 . ? O1 H1B 0.8502 . ? O2 H2A 0.8501 . ? O2 H2B 0.8500 . ? O3 H3A 0.8500 . ? O3 H3B 0.8501 . ? O4 H4A 0.8501 . ? O4 H4B 0.8500 . ? O5 H5A 0.8501 . ? O5 H5B 0.8500 . ? O6 H6A 0.8500 . ? O6 H6B 0.8500 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? O8 H8A 0.8501 . ? O8 H8B 0.8499 . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? O10 H10A 0.8499 . ? O10 H10B 0.8500 . ? O11 H11A 0.8499 . ? O11 H11B 0.8499 . ? O12 H12A 0.8502 . ? O12 H12B 0.8499 . ? C5 C6 1.377(19) . ? C5 H5C 0.9500 . ? C6 C7 1.365(19) . ? C6 H6C 0.9500 . ? C7 C8 1.389(13) . ? C7 H7C 0.9500 . ? C8 C9 1.384(13) . ? C8 H8A 0.9500 . ? C9 C10 1.487(11) . ? C10 C11 1.392(11) . ? C11 C12 1.387(12) . ? C11 H11A 0.9500 . ? C12 C13 1.394(14) . ? C12 H12A 0.9500 . ? C13 C14 1.366(12) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C19 C20 1.387(12) . ? C19 H19A 0.9500 . ? C20 C21 1.376(15) . ? C20 H20A 0.9500 . ? C21 C22 1.382(15) . ? C21 H21A 0.9500 . ? C22 C23 1.401(13) . ? C22 H22A 0.9500 . ? C23 C24 1.460(13) . ? C24 C25 1.403(12) . ? C25 C26 1.373(16) . ? C25 H25A 0.9500 . ? C26 C27 1.379(17) . ? C26 H26A 0.9500 . ? C27 C28 1.370(13) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C33 C34 1.366(14) . ? C33 H33A 0.9500 . ? C34 C35 1.394(15) . ? C34 H34A 0.9500 . ? C35 C36 1.384(13) . ? C35 H35A 0.9500 . ? C36 C37 1.377(12) . ? C36 H36A 0.9500 . ? C37 C38 1.479(11) . ? C38 C39 1.384(12) . ? C39 C40 1.374(13) . ? C39 H39A 0.9500 . ? C40 C41 1.388(15) . ? C40 H40A 0.9500 . ? C41 C42 1.381(13) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ru1 C1 88.6(5) . . ? C3 Ru1 C2 88.8(4) . . ? C1 Ru1 C2 90.4(4) . . ? C3 Ru1 C4 90.5(5) . . ? C1 Ru1 C4 88.3(4) . . ? C2 Ru1 C4 178.5(4) . . ? C3 Ru1 N5 174.2(4) . . ? C1 Ru1 N5 96.8(4) . . ? C2 Ru1 N5 89.0(3) . . ? C4 Ru1 N5 91.8(4) . . ? C3 Ru1 N6 97.0(4) . . ? C1 Ru1 N6 174.2(4) . . ? C2 Ru1 N6 91.1(3) . . ? C4 Ru1 N6 90.2(3) . . ? N5 Ru1 N6 77.7(3) . . ? C18 Ru2 C15 88.9(3) . . ? C18 Ru2 C17 88.2(4) . . ? C15 Ru2 C17 91.0(3) . . ? C18 Ru2 C16 86.8(4) . . ? C15 Ru2 C16 89.2(3) . . ? C17 Ru2 C16 175.0(3) . . ? C18 Ru2 N12 97.3(3) . . ? C15 Ru2 N12 173.1(3) . . ? C17 Ru2 N12 92.2(3) . . ? C16 Ru2 N12 88.1(3) . . ? C18 Ru2 N11 174.4(3) . . ? C15 Ru2 N11 96.6(3) . . ? C17 Ru2 N11 90.7(3) . . ? C16 Ru2 N11 94.2(3) . . ? N12 Ru2 N11 77.2(3) . . ? C29 Ru3 C30 91.0(4) . . ? C29 Ru3 C32 89.9(4) . . ? C30 Ru3 C32 93.1(4) . . ? C29 Ru3 C31 88.3(4) . . ? C30 Ru3 C31 88.0(3) . . ? C32 Ru3 C31 177.9(3) . . ? C29 Ru3 N18 173.6(3) . . ? C30 Ru3 N18 95.1(3) . . ? C32 Ru3 N18 88.0(3) . . ? C31 Ru3 N18 93.7(3) . . ? C29 Ru3 N17 96.4(3) . . ? C30 Ru3 N17 171.8(3) . . ? C32 Ru3 N17 90.5(3) . . ? C31 Ru3 N17 88.6(3) . . ? N18 Ru3 N17 77.7(3) . . ? O11 Yb1 O8 148.4(5) . . ? O11 Yb1 N10 95.6(5) . . ? O8 Yb1 N10 96.5(4) . . ? O11 Yb1 O10 67.0(5) . . ? O8 Yb1 O10 144.4(4) . . ? N10 Yb1 O10 77.9(3) . . ? O11 Yb1 O12 78.5(5) . . ? O8 Yb1 O12 74.0(3) . . ? N10 Yb1 O12 142.0(3) . . ? O10 Yb1 O12 130.4(3) . . ? O11 Yb1 O7 82.1(6) . . ? O8 Yb1 O7 74.6(5) . . ? N10 Yb1 O7 70.6(5) . . ? O10 Yb1 O7 133.0(5) . . ? O12 Yb1 O7 71.4(5) . . ? O11 Yb1 O9 141.4(5) . . ? O8 Yb1 O9 70.0(3) . . ? N10 Yb1 O9 77.9(3) . . ? O10 Yb1 O9 74.5(4) . . ? O12 Yb1 O9 128.9(3) . . ? O7 Yb1 O9 128.7(5) . . ? O11 Yb1 N14 92.7(5) . 1_655 ? O8 Yb1 N14 94.4(4) . 1_655 ? N10 Yb1 N14 144.1(3) . 1_655 ? O10 Yb1 N14 73.4(3) . 1_655 ? O12 Yb1 N14 73.9(3) . 1_655 ? O7 Yb1 N14 145.3(5) . 1_655 ? O9 Yb1 N14 74.0(3) . 1_655 ? O11 Yb1 H11A 15.8 . . ? O8 Yb1 H11A 146.6 . . ? N10 Yb1 H11A 80.4 . . ? O10 Yb1 H11A 67.9 . . ? O12 Yb1 H11A 88.0 . . ? O7 Yb1 H11A 73.1 . . ? O9 Yb1 H11A 139.6 . . ? N14 Yb1 H11A 107.6 1_655 . ? O1 Yb2 O5 152.5(4) . . ? O1 Yb2 O6 76.6(5) . . ? O5 Yb2 O6 77.9(4) . . ? O1 Yb2 N13 86.9(5) . . ? O5 Yb2 N13 77.2(3) . . ? O6 Yb2 N13 77.0(4) . . ? O1 Yb2 O4 74.4(3) . . ? O5 Yb2 O4 130.9(3) . . ? O6 Yb2 O4 127.9(3) . . ? N13 Yb2 O4 141.9(3) . . ? O1 Yb2 N7 106.2(6) . . ? O5 Yb2 N7 76.5(3) . . ? O6 Yb2 N7 74.3(3) . . ? N13 Yb2 N7 144.3(3) . . ? O4 Yb2 N7 73.6(3) . . ? O1 Yb2 O2 80.5(7) . . ? O5 Yb2 O2 115.1(4) . . ? O6 Yb2 O2 142.9(5) . . ? N13 Yb2 O2 72.9(5) . . ? O4 Yb2 O2 71.4(4) . . ? N7 Yb2 O2 141.0(4) . . ? O1 Yb2 O3 139.6(6) . . ? O5 Yb2 O3 67.2(5) . . ? O6 Yb2 O3 143.4(5) . . ? N13 Yb2 O3 104.6(5) . . ? O4 Yb2 O3 73.0(5) . . ? N7 Yb2 O3 86.9(5) . . ? O2 Yb2 O3 66.9(6) . . ? O1 Yb2 H1A 15.5 . . ? O5 Yb2 H1A 158.5 . . ? O6 Yb2 H1A 90.2 . . ? N13 Yb2 H1A 82.7 . . ? O4 Yb2 H1A 70.5 . . ? N7 Yb2 H1A 117.8 . . ? O2 Yb2 H1A 65.0 . . ? O3 Yb2 H1A 126.4 . . ? O1 Yb2 H1B 15.8 . . ? O5 Yb2 H1B 141.0 . . ? O6 Yb2 H1B 63.1 . . ? N13 Yb2 H1B 91.6 . . ? O4 Yb2 H1B 79.4 . . ? N7 Yb2 H1B 93.8 . . ? O2 Yb2 H1B 96.3 . . ? O3 Yb2 H1B 151.1 . . ? H1A Yb2 H1B 31.3 . . ? C5 N5 C9 117.7(9) . . ? C5 N5 Ru1 125.8(7) . . ? C9 N5 Ru1 116.4(5) . . ? C14 N6 C10 117.9(7) . . ? C14 N6 Ru1 126.4(6) . . ? C10 N6 Ru1 115.6(5) . . ? C15 N7 Yb2 175.8(7) . . ? C18 N10 Yb1 169.8(8) . . ? C19 N11 C23 118.8(7) . . ? C19 N11 Ru2 125.4(6) . . ? C23 N11 Ru2 115.8(6) . . ? C28 N12 C24 118.3(7) . . ? C28 N12 Ru2 126.4(6) . . ? C24 N12 Ru2 115.2(6) . . ? C29 N13 Yb2 164.8(9) . . ? C30 N14 Yb1 178.2(8) . 1_455 ? C33 N17 C37 118.1(7) . . ? C33 N17 Ru3 125.9(6) . . ? C37 N17 Ru3 115.7(5) . . ? C42 N18 C38 118.3(7) . . ? C42 N18 Ru3 125.7(6) . . ? C38 N18 Ru3 115.7(5) . . ? Yb2 O1 H1A 120.7 . . ? Yb2 O1 H1B 119.3 . . ? H1A O1 H1B 120.0 . . ? Yb2 O2 H2A 119.9 . . ? Yb2 O2 H2B 120.1 . . ? H2A O2 H2B 120.0 . . ? Yb2 O3 H3A 121.4 . . ? Yb2 O3 H3B 118.6 . . ? H3A O3 H3B 120.0 . . ? Yb2 O4 H4A 124.7 . . ? Yb2 O4 H4B 125.7 . . ? H4A O4 H4B 107.7 . . ? Yb2 O5 H5A 119.9 . . ? Yb2 O5 H5B 120.1 . . ? H5A O5 H5B 120.0 . . ? Yb2 O6 H6A 119.0 . . ? Yb2 O6 H6B 120.9 . . ? H6A O6 H6B 120.0 . . ? Yb1 O7 H7A 122.8 . . ? Yb1 O7 H7B 117.1 . . ? H7A O7 H7B 120.0 . . ? Yb1 O8 H8A 131.3 . . ? Yb1 O8 H8B 118.8 . . ? H8A O8 H8B 107.7 . . ? Yb1 O9 H9A 119.8 . . ? Yb1 O9 H9B 120.2 . . ? H9A O9 H9B 120.0 . . ? Yb1 O10 H10A 120.1 . . ? Yb1 O10 H10B 119.9 . . ? H10A O10 H10B 120.0 . . ? Yb1 O11 H11A 118.2 . . ? Yb1 O11 H11B 121.9 . . ? H11A O11 H11B 107.7 . . ? Yb1 O12 H12A 120.0 . . ? Yb1 O12 H12B 120.0 . . ? H12A O12 H12B 120.0 . . ? N1 C1 Ru1 177.4(12) . . ? N2 C2 Ru1 175.9(10) . . ? N3 C3 Ru1 178.6(11) . . ? N4 C4 Ru1 176.8(9) . . ? N5 C5 C6 121.9(11) . . ? N5 C5 H5C 119.0 . . ? C6 C5 H5C 119.0 . . ? C7 C6 C5 120.4(9) . . ? C7 C6 H6C 119.8 . . ? C5 C6 H6C 119.8 . . ? C6 C7 C8 118.5(11) . . ? C6 C7 H7C 120.8 . . ? C8 C7 H7C 120.8 . . ? C9 C8 C7 119.0(10) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? N5 C9 C8 122.4(8) . . ? N5 C9 C10 114.7(8) . . ? C8 C9 C10 123.0(8) . . ? N6 C10 C11 122.3(7) . . ? N6 C10 C9 115.4(7) . . ? C11 C10 C9 122.3(7) . . ? C12 C11 C10 118.9(8) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 118.1(7) . . ? C11 C12 H12A 121.0 . . ? C13 C12 H12A 121.0 . . ? C14 C13 C12 119.8(8) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? N6 C14 C13 122.9(8) . . ? N6 C14 H14A 118.5 . . ? C13 C14 H14A 118.5 . . ? N7 C15 Ru2 176.4(8) . . ? N8 C16 Ru2 175.7(8) . . ? N9 C17 Ru2 175.0(8) . . ? N10 C18 Ru2 178.1(9) . . ? N11 C19 C20 123.0(8) . . ? N11 C19 H19A 118.5 . . ? C20 C19 H19A 118.5 . . ? C21 C20 C19 118.5(9) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C20 C21 C22 119.1(8) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C21 C22 C23 119.9(9) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? N11 C23 C22 120.6(9) . . ? N11 C23 C24 115.9(7) . . ? C22 C23 C24 123.5(8) . . ? N12 C24 C25 120.2(9) . . ? N12 C24 C23 115.7(7) . . ? C25 C24 C23 124.1(8) . . ? C26 C25 C24 119.5(10) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 119.9(8) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 118.2(10) . . ? C28 C27 H27A 120.9 . . ? C26 C27 H27A 120.9 . . ? N12 C28 C27 123.9(10) . . ? N12 C28 H28A 118.0 . . ? C27 C28 H28A 118.0 . . ? N13 C29 Ru3 179.0(9) . . ? N14 C30 Ru3 175.2(8) . . ? N15 C31 Ru3 178.3(8) . . ? N16 C32 Ru3 178.5(9) . . ? N17 C33 C34 122.6(8) . . ? N17 C33 H33A 118.7 . . ? C34 C33 H33A 118.7 . . ? C33 C34 C35 118.7(8) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C36 C35 C34 119.4(9) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? C37 C36 C35 118.8(9) . . ? C37 C36 H36A 120.6 . . ? C35 C36 H36A 120.6 . . ? N17 C37 C36 122.2(7) . . ? N17 C37 C38 115.4(7) . . ? C36 C37 C38 122.4(8) . . ? N18 C38 C39 121.6(7) . . ? N18 C38 C37 114.9(7) . . ? C39 C38 C37 123.4(8) . . ? C40 C39 C38 119.5(9) . . ? C40 C39 H39A 120.3 . . ? C38 C39 H39A 120.3 . . ? C39 C40 C41 119.1(8) . . ? C39 C40 H40A 120.5 . . ? C41 C40 H40A 120.5 . . ? C42 C41 C40 119.6(8) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? N18 C42 C41 121.9(9) . . ? N18 C42 H42A 119.0 . . ? C41 C42 H42A 119.0 . . ? 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 O1 H1A N3 0.85 2.15 2.865(18) 141.1 2_666 O1 H1B N3 0.85 2.30 2.818(16) 119.3 1_545 O2 H2A O24 0.85 1.87 2.67(3) 156.6 2_666 O2 H2B O20 0.85 2.46 3.29(2) 165.2 1_545 O3 H3A O23 0.85 2.28 2.86(2) 125.6 2_666 O3 H3A O24 0.85 2.53 3.34(3) 159.8 2_666 O4 H4A O16 0.85 2.02 2.662(10) 131.2 . O4 H4B N2 0.85 2.32 3.011(14) 139.0 2_666 O5 H5A O17 0.85 2.32 2.834(10) 119.4 1_545 O5 H5B O14 0.85 2.03 2.862(14) 166.6 . O6 H6A N3 0.85 2.55 3.199(16) 134.4 1_545 O6 H6B O7 0.85 2.48 3.19(2) 141.4 . O6 H6B O15 0.85 2.59 2.956(15) 106.9 . O7 H7B N4 0.85 2.52 3.24(2) 143.1 1_545 O8 H8B N1 0.85 1.92 2.765(13) 169.8 2_766 O9 H9A N1 0.85 2.45 3.164(15) 142.0 2_766 O9 H9B O2 0.85 2.41 3.206(18) 155.3 1_655 O10 H10A O13 0.85 2.16 2.76(3) 127.6 1_655 O10 H10A O24 0.85 2.38 3.19(2) 161.1 2_766 O10 H10B O17 0.85 2.37 2.797(10) 111.5 2_765 O10 H10B O18 0.85 2.64 3.10(4) 115.7 1_645 O11 H11A O14 0.85 2.49 3.32(2) 165.5 . O11 H11B O26 0.85 2.05 2.76(3) 139.9 2_756 O11 H11B O25 0.85 2.43 3.23(3) 157.6 2_756 O12 H12A O19 0.85 1.82 2.665(9) 170.5 1_645 O12 H12B O25 0.85 2.25 2.83(3) 124.9 2_756 O12 H12B N4 0.85 2.40 3.128(14) 144.7 1_545 O3 H3B O18 0.85 1.75 2.29(4) 119.5 2_665 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 5.359 _refine_diff_density_min -4.023 _refine_diff_density_rms 0.216 #===END