Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ;Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '01142 229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Three-component coordination networks based on [Ru(phen)(CN)4]2- anions, near-infrared luminescent lanthanide(III) cations, and ancillary oligopyridine ligands: structures and photophysical properties ; _publ_contact_letter ; This CIF file contains details of the 10 new crystal structures in the paper 'Three component coordination networks based on...' by S. G. Baca et al, submitted to Dalton Trans. for publication. ; loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Svetlana G. Baca' 'Stephen Faulkner' 'Daniel Sykes' #======================================================== data_imw551m _database_code_depnum_ccdc_archive 'CCDC 636982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56.50 H52 Er K N16 O9.50 Ru2' _chemical_formula_weight 1515.64 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' K K 0.2009 0.2494 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.218(19) _cell_length_b 27.76(4) _cell_length_c 17.21(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.077(12) _cell_angle_gamma 90.00 _cell_volume 6643(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5286 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104774 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11691 _reflns_number_gt 9686 _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^)+(0.0960P)^2^+64.0891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11691 _refine_ls_number_parameters 789 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er -0.26793(2) 0.519990(11) 0.854985(18) 0.02447(12) Uani 1 1 d . . . Ru1 Ru 0.06529(4) 0.62124(2) 0.96205(4) 0.02658(16) Uani 1 1 d . . . Ru2 Ru -0.42861(5) 0.36788(2) 0.67877(4) 0.03864(18) Uani 1 1 d . . . N1 N 0.1753(4) 0.6726(2) 1.0002(4) 0.0321(14) Uani 1 1 d . . . N2 N 0.0062(4) 0.6834(2) 0.9004(5) 0.0405(17) Uani 1 1 d . . . N3 N 0.1328(6) 0.5944(4) 0.8029(5) 0.073(3) Uani 1 1 d . . . N4 N -0.1236(4) 0.5621(2) 0.9060(4) 0.0341(14) Uani 1 1 d . . . N5 N -0.0188(6) 0.6429(3) 1.1160(5) 0.061(2) Uani 1 1 d . . . N7 N -0.4833(6) 0.3109(3) 0.6010(5) 0.055(2) Uani 1 1 d . . . N8 N -0.3190(6) 0.3158(2) 0.7103(4) 0.0429(17) Uani 1 1 d . . . N9 N -0.5379(6) 0.3169(3) 0.8005(5) 0.0497(19) Uani 1 1 d . . . N10 N -0.3332(4) 0.4462(2) 0.8004(4) 0.0276(13) Uani 1 1 d . . . N11 N -0.3169(7) 0.4099(3) 0.5509(5) 0.055(2) Uani 1 1 d . . . N12 N -0.6051(8) 0.4369(5) 0.6200(6) 0.099(4) Uani 1 1 d . . . N13 N -0.3083(5) 0.5463(2) 0.9826(4) 0.0311(14) Uani 1 1 d . . . N14 N -0.4455(4) 0.5260(2) 0.8540(4) 0.0285(13) Uani 1 1 d . . . N15 N -0.3070(4) 0.6092(2) 0.8379(4) 0.0303(14) Uani 1 1 d . . . N16 N -0.3403(4) 0.5461(2) 0.7163(4) 0.0300(13) Uani 1 1 d . . . C1 C 0.2579(5) 0.6662(3) 1.0533(5) 0.0381(18) Uani 1 1 d . . . H1 H 0.2736 0.6351 1.0751 0.046 Uiso 1 1 calc R . . C2 C 0.3220(6) 0.7046(3) 1.0772(5) 0.045(2) Uani 1 1 d . . . H2 H 0.3802 0.6993 1.1149 0.054 Uiso 1 1 calc R . . C3 C 0.3009(7) 0.7492(4) 1.0467(6) 0.053(2) Uani 1 1 d . . . H3 H 0.3443 0.7750 1.0630 0.063 Uiso 1 1 calc R . . C4 C 0.2153(7) 0.7573(3) 0.9912(6) 0.051(2) Uani 1 1 d . . . C5 C 0.1873(9) 0.8023(4) 0.9541(8) 0.067(3) Uani 1 1 d . . . H5 H 0.2280 0.8295 0.9677 0.080 Uiso 1 1 calc R . . C6 C 0.1047(9) 0.8072(4) 0.9003(8) 0.071(3) Uani 1 1 d . . . H6 H 0.0890 0.8377 0.8761 0.085 Uiso 1 1 calc R . . C7 C 0.0389(7) 0.7675(3) 0.8780(8) 0.063(3) Uani 1 1 d . . . C8 C -0.0475(7) 0.7698(4) 0.8216(8) 0.074(4) Uani 1 1 d . . . H8 H -0.0662 0.7989 0.7937 0.089 Uiso 1 1 calc R . . C9 C -0.1039(7) 0.7308(4) 0.8069(8) 0.071(3) Uani 1 1 d . . . H9 H -0.1630 0.7324 0.7691 0.085 Uiso 1 1 calc R . . C10 C -0.0755(6) 0.6872(4) 0.8475(6) 0.055(3) Uani 1 1 d . . . H10 H -0.1163 0.6599 0.8365 0.066 Uiso 1 1 calc R . . C11 C 0.0646(6) 0.7227(3) 0.9154(6) 0.045(2) Uani 1 1 d . . . C12 C 0.1543(6) 0.7170(3) 0.9704(5) 0.0389(19) Uani 1 1 d . . . C13 C 0.1115(6) 0.6040(3) 0.8617(5) 0.0409(19) Uani 1 1 d . . . C14 C -0.0513(5) 0.5822(3) 0.9265(4) 0.0275(15) Uani 1 1 d . . . C15 C 0.0120(6) 0.6369(3) 1.0592(5) 0.0361(18) Uani 1 1 d . . . C17 C -0.5625(9) 0.3095(5) 0.5443(7) 0.075(4) Uani 1 1 d . . . H17 H -0.6025 0.3372 0.5349 0.090 Uiso 1 1 calc R . . C18 C -0.5887(12) 0.2682(6) 0.4980(7) 0.095(6) Uani 1 1 d . . . H18 H -0.6440 0.2689 0.4560 0.114 Uiso 1 1 calc R . . C19 C -0.5370(12) 0.2279(6) 0.5124(8) 0.091(5) Uani 1 1 d . . . H19 H -0.5557 0.1998 0.4816 0.110 Uiso 1 1 calc R . . C20 C -0.4561(10) 0.2278(4) 0.5724(8) 0.074(4) Uani 1 1 d . . . C21 C -0.3993(13) 0.1874(5) 0.5916(10) 0.094(6) Uani 1 1 d . . . H21 H -0.4191 0.1581 0.5645 0.113 Uiso 1 1 calc R . . C22 C -0.3171(13) 0.1877(4) 0.6471(10) 0.091(5) Uani 1 1 d . . . H22 H -0.2806 0.1589 0.6584 0.109 Uiso 1 1 calc R . . C23 C -0.2830(10) 0.2325(4) 0.6906(8) 0.071(4) Uani 1 1 d . . . C24 C -0.1973(10) 0.2377(4) 0.7438(9) 0.077(4) Uani 1 1 d . . . H24 H -0.1556 0.2108 0.7571 0.093 Uiso 1 1 calc R . . C25 C -0.1719(9) 0.2820(4) 0.7780(8) 0.069(3) Uani 1 1 d . . . H25 H -0.1118 0.2862 0.8137 0.083 Uiso 1 1 calc R . . C26 C -0.2354(7) 0.3204(3) 0.7595(6) 0.048(2) Uani 1 1 d . . . H26 H -0.2178 0.3509 0.7832 0.058 Uiso 1 1 calc R . . C27 C -0.3425(8) 0.2727(3) 0.6734(6) 0.054(3) Uani 1 1 d . . . C28 C -0.4300(8) 0.2706(4) 0.6142(6) 0.059(3) Uani 1 1 d . . . C29 C -0.4997(6) 0.3371(3) 0.7574(5) 0.041(2) Uani 1 1 d . . . C30 C -0.3685(5) 0.4163(3) 0.7568(4) 0.0269(15) Uani 1 1 d . . . C31 C -0.5393(8) 0.4122(4) 0.6428(6) 0.063(3) Uani 1 1 d . . . C32 C -0.3582(7) 0.3954(3) 0.5976(5) 0.044(2) Uani 1 1 d . . . C33 C -0.2412(6) 0.5562(3) 1.0462(5) 0.0391(19) Uani 1 1 d . . . H33 H -0.1762 0.5491 1.0448 0.047 Uiso 1 1 calc R . . C34 C -0.2608(7) 0.5764(3) 1.1151(5) 0.047(2) Uani 1 1 d . . . H34 H -0.2101 0.5836 1.1590 0.057 Uiso 1 1 calc R . . C35 C -0.3540(8) 0.5857(3) 1.1185(5) 0.048(2) Uani 1 1 d . . . H35 H -0.3686 0.5995 1.1650 0.057 Uiso 1 1 calc R . . C36 C -0.4283(6) 0.5749(3) 1.0535(5) 0.0385(19) Uani 1 1 d . . . C37 C -0.5279(7) 0.5809(3) 1.0544(6) 0.044(2) Uani 1 1 d . . . H37 H -0.5457 0.5937 1.1005 0.053 Uiso 1 1 calc R . . C38 C -0.5967(7) 0.5689(3) 0.9914(6) 0.046(2) Uani 1 1 d . . . H38 H -0.6625 0.5723 0.9941 0.055 Uiso 1 1 calc R . . C39 C -0.5723(6) 0.5510(3) 0.9208(5) 0.0367(19) Uani 1 1 d . . . C40 C -0.6417(6) 0.5386(3) 0.8540(6) 0.044(2) Uani 1 1 d . . . H40 H -0.7081 0.5428 0.8536 0.053 Uiso 1 1 calc R . . C41 C -0.6130(6) 0.5202(3) 0.7891(6) 0.043(2) Uani 1 1 d . . . H41 H -0.6595 0.5119 0.7429 0.052 Uiso 1 1 calc R . . C42 C -0.5151(6) 0.5137(3) 0.7904(5) 0.0355(18) Uani 1 1 d . . . H42 H -0.4967 0.5000 0.7452 0.043 Uiso 1 1 calc R . . C43 C -0.4736(5) 0.5440(2) 0.9178(5) 0.0301(16) Uani 1 1 d . . . C44 C -0.4023(6) 0.5557(2) 0.9849(5) 0.0322(17) Uani 1 1 d . . . C45 C -0.2811(6) 0.6421(3) 0.8935(5) 0.0368(18) Uani 1 1 d . . . H45 H -0.2405 0.6326 0.9422 0.044 Uiso 1 1 calc R . . C46 C -0.3105(7) 0.6907(3) 0.8844(6) 0.045(2) Uani 1 1 d . . . H46 H -0.2872 0.7135 0.9250 0.054 Uiso 1 1 calc R . . C47 C -0.3721(6) 0.7045(3) 0.8172(6) 0.046(2) Uani 1 1 d . . . H47 H -0.3950 0.7367 0.8111 0.055 Uiso 1 1 calc R . . C48 C -0.4017(6) 0.6708(3) 0.7570(6) 0.042(2) Uani 1 1 d . . . C49 C -0.4680(7) 0.6814(4) 0.6826(6) 0.056(3) Uani 1 1 d . . . H49 H -0.4972 0.7123 0.6755 0.068 Uiso 1 1 calc R . . C50 C -0.4888(8) 0.6498(4) 0.6249(7) 0.060(3) Uani 1 1 d . . . H50 H -0.5331 0.6579 0.5774 0.072 Uiso 1 1 calc R . . C51 C -0.4451(7) 0.6029(3) 0.6334(5) 0.047(2) Uani 1 1 d . . . C52 C -0.4549(7) 0.5696(4) 0.5693(5) 0.054(2) Uani 1 1 d . . . H52 H -0.4947 0.5771 0.5192 0.065 Uiso 1 1 calc R . . C53 C -0.4075(8) 0.5274(3) 0.5802(5) 0.050(2) Uani 1 1 d . . . H53 H -0.4122 0.5053 0.5374 0.060 Uiso 1 1 calc R . . C54 C -0.3516(6) 0.5163(3) 0.6540(5) 0.0394(19) Uani 1 1 d . . . H54 H -0.3198 0.4860 0.6606 0.047 Uiso 1 1 calc R . . C55 C -0.3852(5) 0.5897(3) 0.7046(5) 0.0326(17) Uani 1 1 d . . . C56 C -0.3655(5) 0.6237(3) 0.7688(5) 0.0305(16) Uani 1 1 d . . . O1 O -0.1559(4) 0.4977(2) 0.7795(4) 0.0450(14) Uani 1 1 d . . . H1B H -0.1522 0.4781 0.7422 0.054 Uiso 1 1 d R . . H1C H -0.1037 0.5009 0.8073 0.054 Uiso 1 1 d R . . K1A K -0.9084(2) 0.48658(12) 0.52002(17) 0.0269(6) Uani 0.50 1 d PU . . K1B K -0.9019(5) 0.4433(2) 0.5070(4) 0.0329(14) Uani 0.25 1 d PU . . K1C K -0.8754(6) 0.5091(3) 0.5878(4) 0.0436(17) Uani 0.25 1 d PU . . O4 O 0.0209(6) 0.4774(3) 0.8783(6) 0.087(3) Uani 1 1 d U . . O3 O -0.1903(6) 0.7018(4) 1.0763(6) 0.101(3) Uani 1 1 d U . . O2 O -0.2711(6) 0.7974(4) 0.7049(7) 0.119(4) Uani 1 1 d U . . O5 O -0.1432(9) 0.4375(5) 0.6610(8) 0.139(5) Uani 1 1 d U . . O6 O 0.0243(9) 0.3968(5) 0.7341(6) 0.121(4) Uani 1 1 d U . . O7 O -0.0924(14) 0.5838(7) 0.7140(12) 0.093(6) Uiso 0.50 1 d P . . O8 O -0.1112(16) 0.7865(8) 1.0594(13) 0.104(6) Uiso 0.50 1 d P . . O9 O -0.210(2) 0.6398(12) 0.6301(19) 0.164(11) Uiso 0.50 1 d P . . O10 O -0.2228(17) 0.8696(9) 0.8143(14) 0.116(7) Uiso 0.50 1 d P . . O100 O -0.8386(13) 0.6198(6) 0.6476(11) 0.083(5) Uiso 0.50 1 d P . . C100 C -0.7369(18) 0.6214(9) 0.6514(14) 0.071(6) Uiso 0.50 1 d P . . O21 O -0.8854(13) 0.4974(7) 0.7372(10) 0.079(5) Uiso 0.50 1 d P . . O20 O -0.7330(17) 0.5150(8) 0.5579(14) 0.112(7) Uiso 0.50 1 d P . . N6A N 0.1838(4) 0.5358(2) 1.0537(4) 0.0289(13) Uani 1 1 d . . . C16A C 0.1371(5) 0.5666(3) 1.0193(4) 0.0273(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.02049(18) 0.02356(19) 0.02806(19) 0.00106(12) 0.00209(13) 0.00000(12) Ru1 0.0184(3) 0.0257(3) 0.0353(3) 0.0044(2) 0.0049(2) 0.0015(2) Ru2 0.0435(4) 0.0373(4) 0.0353(4) -0.0147(3) 0.0088(3) -0.0063(3) N1 0.023(3) 0.033(3) 0.043(4) 0.002(3) 0.014(3) -0.002(3) N2 0.023(3) 0.036(4) 0.062(5) 0.015(3) 0.008(3) 0.002(3) N3 0.051(5) 0.127(9) 0.042(5) -0.011(5) 0.012(4) 0.009(5) N4 0.026(3) 0.032(3) 0.043(4) 0.003(3) 0.004(3) -0.001(3) N5 0.057(5) 0.065(6) 0.069(6) -0.016(4) 0.034(5) -0.008(4) N7 0.064(5) 0.060(5) 0.045(5) -0.028(4) 0.022(4) -0.025(4) N8 0.055(5) 0.030(4) 0.051(4) -0.013(3) 0.027(4) -0.009(3) N9 0.046(4) 0.045(4) 0.062(5) -0.013(4) 0.021(4) -0.006(4) N10 0.027(3) 0.027(3) 0.030(3) -0.002(3) 0.007(3) 0.001(3) N11 0.072(6) 0.055(5) 0.040(4) 0.003(4) 0.018(4) 0.018(4) N12 0.075(7) 0.139(11) 0.066(7) -0.038(7) -0.027(5) 0.050(7) N13 0.035(3) 0.026(3) 0.032(3) 0.002(3) 0.006(3) 0.005(3) N14 0.028(3) 0.025(3) 0.033(3) 0.004(3) 0.006(3) 0.002(2) N15 0.026(3) 0.029(3) 0.037(4) 0.002(3) 0.009(3) -0.003(3) N16 0.031(3) 0.026(3) 0.033(3) 0.002(3) 0.005(3) -0.003(3) C1 0.028(4) 0.041(5) 0.046(5) -0.009(4) 0.010(3) -0.008(3) C2 0.035(4) 0.053(6) 0.049(5) -0.009(4) 0.013(4) -0.020(4) C3 0.049(6) 0.048(6) 0.067(6) -0.017(5) 0.027(5) -0.023(4) C4 0.050(5) 0.034(5) 0.076(7) -0.001(4) 0.032(5) -0.008(4) C5 0.066(7) 0.033(5) 0.110(10) 0.002(5) 0.039(7) -0.012(5) C6 0.075(8) 0.034(5) 0.115(10) 0.023(6) 0.043(7) 0.010(5) C7 0.043(5) 0.036(5) 0.116(9) 0.028(6) 0.033(6) 0.010(4) C8 0.042(6) 0.060(7) 0.124(11) 0.053(7) 0.024(6) 0.016(5) C9 0.040(5) 0.067(7) 0.100(9) 0.041(7) 0.001(6) 0.008(5) C10 0.029(4) 0.054(6) 0.081(7) 0.033(5) 0.010(4) 0.005(4) C11 0.036(5) 0.034(4) 0.070(6) 0.014(4) 0.024(4) 0.004(4) C12 0.029(4) 0.033(4) 0.060(5) 0.005(4) 0.020(4) -0.005(3) C13 0.025(4) 0.057(5) 0.039(5) 0.006(4) 0.002(3) 0.004(4) C14 0.023(4) 0.029(4) 0.030(4) 0.002(3) 0.005(3) 0.004(3) C15 0.029(4) 0.029(4) 0.052(5) 0.000(4) 0.014(4) -0.002(3) C17 0.084(8) 0.088(9) 0.057(7) -0.036(6) 0.024(6) -0.043(7) C18 0.117(12) 0.120(12) 0.057(7) -0.050(8) 0.038(8) -0.083(11) C19 0.129(13) 0.090(10) 0.074(9) -0.061(8) 0.065(9) -0.074(10) C20 0.102(9) 0.049(6) 0.096(9) -0.047(6) 0.075(8) -0.040(6) C21 0.133(13) 0.065(9) 0.111(12) -0.055(8) 0.086(11) -0.051(9) C22 0.147(14) 0.026(5) 0.135(13) -0.017(7) 0.107(12) 0.000(7) C23 0.087(9) 0.034(5) 0.110(10) -0.020(6) 0.063(8) -0.012(5) C24 0.090(9) 0.039(6) 0.123(11) -0.001(6) 0.069(9) 0.012(6) C25 0.068(7) 0.049(6) 0.099(9) 0.002(6) 0.040(7) 0.012(5) C26 0.054(6) 0.036(5) 0.060(6) -0.004(4) 0.025(5) 0.000(4) C27 0.069(7) 0.034(5) 0.073(7) -0.020(5) 0.048(6) -0.012(4) C28 0.076(7) 0.059(6) 0.058(6) -0.030(5) 0.047(6) -0.034(6) C29 0.038(4) 0.036(4) 0.051(5) -0.023(4) 0.011(4) -0.006(4) C30 0.028(4) 0.029(4) 0.025(4) 0.001(3) 0.010(3) 0.002(3) C31 0.058(6) 0.086(8) 0.042(5) -0.024(5) 0.003(5) 0.005(6) C32 0.060(6) 0.039(5) 0.033(5) -0.006(4) 0.009(4) 0.011(4) C33 0.044(5) 0.037(4) 0.034(4) -0.003(3) 0.004(4) -0.003(4) C34 0.063(6) 0.041(5) 0.037(5) -0.004(4) 0.008(4) -0.002(4) C35 0.079(7) 0.034(5) 0.036(5) -0.001(4) 0.024(5) -0.001(4) C36 0.055(5) 0.016(4) 0.050(5) 0.001(3) 0.024(4) -0.001(3) C37 0.060(6) 0.020(4) 0.064(6) 0.006(4) 0.039(5) 0.008(4) C38 0.050(5) 0.024(4) 0.073(7) 0.009(4) 0.035(5) 0.007(4) C39 0.038(4) 0.017(3) 0.061(5) 0.009(3) 0.026(4) 0.001(3) C40 0.026(4) 0.036(4) 0.074(6) 0.007(4) 0.015(4) 0.004(3) C41 0.027(4) 0.034(4) 0.064(6) 0.015(4) 0.000(4) 0.001(3) C42 0.027(4) 0.029(4) 0.048(5) 0.005(3) 0.001(3) -0.001(3) C43 0.033(4) 0.017(3) 0.042(4) 0.006(3) 0.011(3) 0.000(3) C44 0.042(4) 0.017(3) 0.044(4) 0.008(3) 0.022(4) 0.005(3) C45 0.039(4) 0.033(4) 0.040(5) 0.000(3) 0.013(4) -0.005(3) C46 0.048(5) 0.029(4) 0.062(6) -0.010(4) 0.020(4) -0.006(4) C47 0.047(5) 0.030(4) 0.065(6) 0.006(4) 0.022(5) 0.008(4) C48 0.037(4) 0.032(4) 0.057(5) 0.011(4) 0.013(4) 0.004(3) C49 0.054(6) 0.046(6) 0.066(7) 0.023(5) 0.006(5) 0.013(5) C50 0.065(7) 0.041(5) 0.064(7) 0.021(5) -0.009(5) 0.007(5) C51 0.046(5) 0.045(5) 0.045(5) 0.014(4) -0.001(4) -0.003(4) C52 0.059(6) 0.059(6) 0.033(5) 0.015(4) -0.013(4) -0.003(5) C53 0.070(6) 0.044(5) 0.031(5) 0.004(4) -0.002(4) -0.009(5) C54 0.044(5) 0.038(5) 0.034(4) 0.004(4) 0.004(4) -0.007(4) C55 0.033(4) 0.030(4) 0.037(4) 0.010(3) 0.011(3) -0.003(3) C56 0.028(4) 0.028(4) 0.036(4) 0.007(3) 0.007(3) -0.002(3) O1 0.026(3) 0.061(4) 0.049(4) -0.008(3) 0.011(3) 0.004(3) K1A 0.0203(14) 0.0411(18) 0.0210(14) -0.0080(12) 0.0081(11) 0.0035(12) K1B 0.033(3) 0.038(3) 0.020(3) 0.017(2) -0.014(2) -0.016(3) K1C 0.051(4) 0.054(4) 0.029(3) 0.003(3) 0.016(3) 0.013(3) O4 0.056(5) 0.080(6) 0.119(8) -0.008(5) 0.002(5) 0.008(4) O3 0.060(5) 0.118(8) 0.120(8) 0.004(6) 0.005(5) 0.030(5) O2 0.057(5) 0.150(10) 0.155(10) 0.098(8) 0.033(6) 0.051(6) O5 0.105(8) 0.167(12) 0.139(10) -0.081(9) 0.014(7) 0.023(8) O6 0.118(9) 0.147(10) 0.091(7) 0.001(7) 0.008(6) -0.003(8) N6A 0.022(3) 0.028(3) 0.036(3) 0.002(3) 0.004(3) 0.002(3) C16A 0.018(3) 0.027(4) 0.037(4) -0.003(3) 0.006(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.339(6) . ? Er1 N6A 2.349(6) 3_567 ? Er1 N10 2.361(6) . ? Er1 N4 2.365(7) . ? Er1 N13 2.492(7) . ? Er1 N16 2.501(7) . ? Er1 N14 2.527(7) . ? Er1 N15 2.541(7) . ? Ru1 C14 1.968(8) . ? Ru1 C16A 1.974(8) . ? Ru1 C15 2.023(9) . ? Ru1 C13 2.029(9) . ? Ru1 N2 2.106(7) . ? Ru1 N1 2.116(7) . ? Ru2 C30 1.965(8) . ? Ru2 C31 1.991(12) . ? Ru2 C32 2.030(10) . ? Ru2 C29 2.039(10) . ? Ru2 N8 2.112(8) . ? Ru2 N7 2.113(7) . ? N1 C1 1.341(10) . ? N1 C12 1.345(10) . ? N2 C10 1.321(11) . ? N2 C11 1.364(11) . ? N3 C13 1.147(12) . ? N4 C14 1.158(10) . ? N5 C15 1.163(11) . ? N7 C17 1.327(15) . ? N7 C28 1.344(15) . ? N8 C26 1.312(12) . ? N8 C27 1.365(11) . ? N9 C29 1.153(12) . ? N10 C30 1.161(9) . ? N11 C32 1.163(12) . ? N12 C31 1.160(14) . ? N13 C33 1.322(10) . ? N13 C44 1.371(10) . ? N14 C43 1.341(10) . ? N14 C42 1.357(10) . ? N15 C45 1.319(10) . ? N15 C56 1.362(10) . ? N16 C54 1.336(10) . ? N16 C55 1.364(10) . ? C1 C2 1.407(11) . ? C1 H1 0.9500 . ? C2 C3 1.353(14) . ? C2 H2 0.9500 . ? C3 C4 1.399(15) . ? C3 H3 0.9500 . ? C4 C12 1.414(12) . ? C4 C5 1.422(15) . ? C5 C6 1.342(17) . ? C5 H5 0.9500 . ? C6 C7 1.445(16) . ? C6 H6 0.9500 . ? C7 C8 1.399(16) . ? C7 C11 1.413(12) . ? C8 C9 1.339(16) . ? C8 H8 0.9500 . ? C9 C10 1.413(13) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.429(13) . ? C17 C18 1.400(16) . ? C17 H17 0.9500 . ? C18 C19 1.33(2) . ? C18 H18 0.9500 . ? C19 C20 1.38(2) . ? C19 H19 0.9500 . ? C20 C21 1.38(2) . ? C20 C28 1.399(13) . ? C21 C22 1.35(2) . ? C21 H21 0.9500 . ? C22 C23 1.481(17) . ? C22 H22 0.9500 . ? C23 C24 1.370(19) . ? C23 C27 1.393(16) . ? C24 C25 1.379(17) . ? C24 H24 0.9500 . ? C25 C26 1.391(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.435(16) . ? C33 C34 1.393(12) . ? C33 H33 0.9500 . ? C34 C35 1.362(14) . ? C34 H34 0.9500 . ? C35 C36 1.401(13) . ? C35 H35 0.9500 . ? C36 C44 1.413(11) . ? C36 C37 1.430(12) . ? C37 C38 1.342(14) . ? C37 H37 0.9500 . ? C38 C39 1.421(12) . ? C38 H38 0.9500 . ? C39 C40 1.393(13) . ? C39 C43 1.429(11) . ? C40 C41 1.365(14) . ? C40 H40 0.9500 . ? C41 C42 1.398(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.405(11) . ? C45 C46 1.412(12) . ? C45 H45 0.9500 . ? C46 C47 1.353(13) . ? C46 H46 0.9500 . ? C47 C48 1.392(13) . ? C47 H47 0.9500 . ? C48 C56 1.405(11) . ? C48 C49 1.452(13) . ? C49 C50 1.311(15) . ? C49 H49 0.9500 . ? C50 C51 1.436(13) . ? C50 H50 0.9500 . ? C51 C55 1.388(12) . ? C51 C52 1.425(14) . ? C52 C53 1.344(14) . ? C52 H52 0.9500 . ? C53 C54 1.384(12) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.435(11) . ? O1 H1B 0.8507 . ? O1 H1C 0.8001 . ? K1A K1B 1.229(8) . ? K1A K1C 1.320(8) . ? K1A O20 2.57(2) . ? K1A K1A 2.657(7) 3_366 ? K1A K1C 3.243(9) 3_366 ? K1A K1B 3.279(8) 3_366 ? K1B K1C 2.278(11) . ? K1B O20 3.10(2) . ? K1B K1A 3.279(8) 3_366 ? K1B K1C 3.503(11) 3_366 ? K1B K1B 4.180(15) 3_366 ? K1C O20 2.20(3) . ? K1C O21 2.625(19) . ? K1C K1A 3.243(9) 3_366 ? K1C O100 3.25(2) . ? K1C K1B 3.503(11) 3_366 ? K1C K1C 4.178(17) 3_366 ? O100 C100 1.43(3) . ? N6A C16A 1.164(9) . ? N6A Er1 2.349(6) 3_567 ? 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 O1 Er1 N6A 83.5(2) . 3_567 ? O1 Er1 N10 78.8(2) . . ? N6A Er1 N10 78.3(2) 3_567 . ? O1 Er1 N4 72.5(2) . . ? N6A Er1 N4 78.3(2) 3_567 . ? N10 Er1 N4 144.6(2) . . ? O1 Er1 N13 151.1(2) . . ? N6A Er1 N13 77.5(2) 3_567 . ? N10 Er1 N13 117.5(2) . . ? N4 Er1 N13 82.5(2) . . ? O1 Er1 N16 74.8(2) . . ? N6A Er1 N16 151.6(2) 3_567 . ? N10 Er1 N16 79.8(2) . . ? N4 Er1 N16 111.3(2) . . ? N13 Er1 N16 129.2(2) . . ? O1 Er1 N14 144.0(2) . . ? N6A Er1 N14 114.6(2) 3_567 . ? N10 Er1 N14 75.3(2) . . ? N4 Er1 N14 139.2(2) . . ? N13 Er1 N14 64.7(2) . . ? N16 Er1 N14 76.3(2) . . ? O1 Er1 N15 110.6(2) . . ? N6A Er1 N15 142.1(2) 3_567 . ? N10 Er1 N15 137.8(2) . . ? N4 Er1 N15 73.3(2) . . ? N13 Er1 N15 74.4(2) . . ? N16 Er1 N15 64.6(2) . . ? N14 Er1 N15 74.94(19) . . ? C14 Ru1 C16A 92.6(3) . . ? C14 Ru1 C15 86.5(3) . . ? C16A Ru1 C15 89.9(3) . . ? C14 Ru1 C13 90.4(3) . . ? C16A Ru1 C13 91.0(3) . . ? C15 Ru1 C13 176.8(3) . . ? C14 Ru1 N2 94.2(3) . . ? C16A Ru1 N2 172.6(3) . . ? C15 Ru1 N2 93.5(3) . . ? C13 Ru1 N2 86.1(3) . . ? C14 Ru1 N1 170.8(3) . . ? C16A Ru1 N1 95.3(3) . . ? C15 Ru1 N1 88.8(3) . . ? C13 Ru1 N1 94.2(3) . . ? N2 Ru1 N1 78.2(3) . . ? C30 Ru2 C31 89.5(4) . . ? C30 Ru2 C32 90.4(3) . . ? C31 Ru2 C32 91.4(4) . . ? C30 Ru2 C29 92.2(3) . . ? C31 Ru2 C29 89.8(4) . . ? C32 Ru2 C29 177.2(3) . . ? C30 Ru2 N8 95.8(3) . . ? C31 Ru2 N8 174.6(4) . . ? C32 Ru2 N8 89.5(3) . . ? C29 Ru2 N8 89.1(3) . . ? C30 Ru2 N7 174.4(3) . . ? C31 Ru2 N7 96.0(4) . . ? C32 Ru2 N7 90.8(3) . . ? C29 Ru2 N7 86.5(3) . . ? N8 Ru2 N7 78.7(3) . . ? C1 N1 C12 118.2(7) . . ? C1 N1 Ru1 127.5(5) . . ? C12 N1 Ru1 114.1(5) . . ? C10 N2 C11 118.5(7) . . ? C10 N2 Ru1 127.9(6) . . ? C11 N2 Ru1 113.5(5) . . ? C14 N4 Er1 175.7(6) . . ? C17 N7 C28 117.5(9) . . ? C17 N7 Ru2 129.1(9) . . ? C28 N7 Ru2 113.4(7) . . ? C26 N8 C27 119.0(9) . . ? C26 N8 Ru2 128.3(6) . . ? C27 N8 Ru2 112.7(7) . . ? C30 N10 Er1 163.4(6) . . ? C33 N13 C44 118.4(7) . . ? C33 N13 Er1 122.1(5) . . ? C44 N13 Er1 119.1(5) . . ? C43 N14 C42 117.6(7) . . ? C43 N14 Er1 119.1(5) . . ? C42 N14 Er1 123.2(5) . . ? C45 N15 C56 117.1(7) . . ? C45 N15 Er1 124.8(5) . . ? C56 N15 Er1 117.9(5) . . ? C54 N16 C55 117.2(7) . . ? C54 N16 Er1 122.9(5) . . ? C55 N16 Er1 118.9(5) . . ? N1 C1 C2 121.4(8) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 120.1(9) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C12 116.4(9) . . ? C3 C4 C5 124.8(9) . . ? C12 C4 C5 118.8(10) . . ? C6 C5 C4 121.5(10) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 122.0(10) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C11 117.5(9) . . ? C8 C7 C6 125.1(9) . . ? C11 C7 C6 117.3(10) . . ? C9 C8 C7 119.9(9) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0(10) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N2 C10 C9 122.0(9) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? N2 C11 C7 122.0(9) . . ? N2 C11 C12 117.4(7) . . ? C7 C11 C12 120.7(8) . . ? N1 C12 C4 123.6(8) . . ? N1 C12 C11 116.8(7) . . ? C4 C12 C11 119.7(8) . . ? N3 C13 Ru1 176.5(8) . . ? N4 C14 Ru1 175.2(6) . . ? N5 C15 Ru1 175.7(8) . . ? N7 C17 C18 121.8(15) . . ? N7 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 120.7(15) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.0(11) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 122.6(12) . . ? C19 C20 C28 118.2(13) . . ? C21 C20 C28 119.2(14) . . ? C22 C21 C20 122.9(11) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C21 C22 C23 120.5(13) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C27 118.2(10) . . ? C24 C23 C22 125.2(12) . . ? C27 C23 C22 116.5(13) . . ? C23 C24 C25 119.7(11) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.1(12) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N8 C26 C25 122.0(10) . . ? N8 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? N8 C27 C23 121.7(11) . . ? N8 C27 C28 117.2(9) . . ? C23 C27 C28 121.0(10) . . ? N7 C28 C20 122.7(12) . . ? N7 C28 C27 117.5(8) . . ? C20 C28 C27 119.8(12) . . ? N9 C29 Ru2 175.7(7) . . ? N10 C30 Ru2 177.3(6) . . ? N12 C31 Ru2 177.7(10) . . ? N11 C32 Ru2 178.2(8) . . ? N13 C33 C34 123.4(8) . . ? N13 C33 H33 118.3 . . ? C34 C33 H33 118.3 . . ? C35 C34 C33 118.8(9) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.2(8) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C44 117.5(8) . . ? C35 C36 C37 123.3(8) . . ? C44 C36 C37 119.1(8) . . ? C38 C37 C36 121.2(8) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.7(8) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 122.4(8) . . ? C40 C39 C43 117.9(8) . . ? C38 C39 C43 119.7(8) . . ? C41 C40 C39 119.1(8) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 120.1(9) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? N14 C42 C41 122.4(8) . . ? N14 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? N14 C43 C44 118.2(7) . . ? N14 C43 C39 122.9(7) . . ? C44 C43 C39 118.9(7) . . ? N13 C44 C43 118.2(7) . . ? N13 C44 C36 121.5(8) . . ? C43 C44 C36 120.2(7) . . ? N15 C45 C46 123.4(8) . . ? N15 C45 H45 118.3 . . ? C46 C45 H45 118.3 . . ? C47 C46 C45 119.3(8) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 119.1(8) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C56 118.3(8) . . ? C47 C48 C49 124.0(8) . . ? C56 C48 C49 117.7(8) . . ? C50 C49 C48 122.4(9) . . ? C50 C49 H49 118.8 . . ? C48 C49 H49 118.8 . . ? C49 C50 C51 120.3(9) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C55 C51 C52 117.0(8) . . ? C55 C51 C50 120.2(9) . . ? C52 C51 C50 122.7(8) . . ? C53 C52 C51 119.5(8) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C52 C53 C54 119.9(9) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? N16 C54 C53 123.2(8) . . ? N16 C54 H54 118.4 . . ? C53 C54 H54 118.4 . . ? N16 C55 C51 123.2(8) . . ? N16 C55 C56 117.4(7) . . ? C51 C55 C56 119.3(7) . . ? N15 C56 C48 122.6(7) . . ? N15 C56 C55 117.6(7) . . ? C48 C56 C55 119.7(7) . . ? Er1 O1 H1B 138.2 . . ? Er1 O1 H1C 107.0 . . ? H1B O1 H1C 108.9 . . ? K1B K1A K1C 126.7(5) . . ? K1B K1A O20 103.9(6) . . ? K1C K1A O20 58.9(6) . . ? K1B K1A K1A 109.5(4) . 3_366 ? K1C K1A K1A 104.1(4) . 3_366 ? O20 K1A K1A 145.8(5) . 3_366 ? K1B K1A K1C 91.8(3) . 3_366 ? K1C K1A K1C 127.4(3) . 3_366 ? O20 K1A K1C 152.6(5) . 3_366 ? K1A K1A K1C 23.25(16) 3_366 3_366 ? K1B K1A K1B 130.2(3) . 3_366 ? K1C K1A K1B 88.5(4) . 3_366 ? O20 K1A K1B 125.5(5) . 3_366 ? K1A K1A K1B 20.68(14) 3_366 3_366 ? K1C K1A K1B 40.88(19) 3_366 3_366 ? K1A K1B K1C 27.7(3) . . ? K1A K1B O20 53.5(5) . . ? K1C K1B O20 45.1(5) . . ? K1A K1B K1A 49.8(3) . 3_366 ? K1C K1B K1A 68.7(3) . 3_366 ? O20 K1B K1A 103.0(5) . 3_366 ? K1A K1B K1C 67.7(3) . 3_366 ? K1C K1B K1C 90.0(3) . 3_366 ? O20 K1B K1C 117.4(5) . 3_366 ? K1A K1B K1C 22.13(14) 3_366 3_366 ? K1A K1B K1B 36.8(3) . 3_366 ? K1C K1B K1B 56.9(3) . 3_366 ? O20 K1B K1B 90.1(5) . 3_366 ? K1A K1B K1B 12.97(8) 3_366 3_366 ? K1C K1B K1B 33.03(16) 3_366 3_366 ? K1A K1C O20 90.2(7) . . ? K1A K1C K1B 25.6(3) . . ? O20 K1C K1B 87.7(7) . . ? K1A K1C O21 136.5(7) . . ? O20 K1C O21 118.7(8) . . ? K1B K1C O21 117.6(5) . . ? K1A K1C K1A 52.6(3) . 3_366 ? O20 K1C K1A 132.3(7) . 3_366 ? K1B K1C K1A 70.4(3) . 3_366 ? O21 K1C K1A 109.0(5) . 3_366 ? K1A K1C O100 137.0(6) . . ? O20 K1C O100 84.7(7) . . ? K1B K1C O100 161.2(5) . . ? O21 K1C O100 81.1(6) . . ? K1A K1C O100 102.5(4) 3_366 . ? K1A K1C K1B 69.4(4) . 3_366 ? O20 K1C K1B 130.6(7) . 3_366 ? K1B K1C K1B 90.0(3) . 3_366 ? O21 K1C K1B 105.9(5) . 3_366 ? K1A K1C K1B 20.53(13) 3_366 3_366 ? O100 K1C K1B 82.0(4) . 3_366 ? K1A K1C K1C 38.1(3) . 3_366 ? O20 K1C K1C 121.5(7) . 3_366 ? K1B K1C K1C 57.0(3) . 3_366 ? O21 K1C K1C 118.8(5) . 3_366 ? K1A K1C K1C 14.54(10) 3_366 3_366 ? O100 K1C K1C 113.5(4) . 3_366 ? K1B K1C K1C 33.05(17) 3_366 3_366 ? C100 O100 K1C 97.9(13) . . ? K1C O20 K1A 30.9(4) . . ? K1C O20 K1B 47.2(5) . . ? K1A O20 K1B 22.6(3) . . ? C16A N6A Er1 168.7(6) . 3_567 ? N6A C16A Ru1 176.4(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.974 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.181 #===END data_imw571m _database_code_depnum_ccdc_archive 'CCDC 636983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H100 K2 N32 Nd2 O18 Ru4' _chemical_formula_weight 2953.20 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' K K 0.2009 0.2494 '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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3600(9) _cell_length_b 27.9387(16) _cell_length_c 17.3122(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.949(3) _cell_angle_gamma 90.00 _cell_volume 6819.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8526 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.23 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2948 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_T_max 0.8913 _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 APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 188070 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11993 _reflns_number_gt 8993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1298P)^2^+11.3854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11993 _refine_ls_number_parameters 820 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.2083 _refine_ls_wR_factor_gt 0.1931 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Nd1 Nd -0.26430(2) 0.020482(13) -0.64734(2) 0.03129(15) Uani 1 1 d . . . Ru1 Ru 0.06816(4) 0.12388(2) -0.53562(4) 0.03577(19) Uani 1 1 d . . . Ru2 Ru -0.42950(5) -0.13238(2) -0.82386(4) 0.0433(2) Uani 1 1 d . . . K1A K -0.8683(3) 0.00839(15) -0.9141(2) 0.0384(9) Uani 0.40 1 d PU . 1 K1B K -0.9093(3) -0.00998(18) -0.9972(4) 0.0389(13) Uani 0.30 1 d PU . 2 K1C K -0.9876(4) 0.0100(2) -1.0742(4) 0.0476(14) Uani 0.30 1 d PU . 3 C1 C 0.2599(5) 0.1660(3) -0.4438(4) 0.0388(17) Uani 1 1 d . . . H1 H 0.2739 0.1348 -0.4231 0.047 Uiso 1 1 calc R . . C2 C 0.3244(6) 0.2024(3) -0.4198(5) 0.049(2) Uani 1 1 d . . . H2 H 0.3811 0.1958 -0.3832 0.059 Uiso 1 1 calc R . . C3 C 0.3070(6) 0.2473(3) -0.4482(5) 0.057(2) Uani 1 1 d . . . H3 H 0.3512 0.2722 -0.4312 0.068 Uiso 1 1 calc R . . C4 C 0.2239(6) 0.2572(3) -0.5026(6) 0.052(2) Uani 1 1 d . . . C5 C 0.1984(8) 0.3019(3) -0.5392(6) 0.066(3) Uani 1 1 d . . . H5 H 0.2409 0.3280 -0.5264 0.079 Uiso 1 1 calc R . . C6 C 0.1186(9) 0.3092(3) -0.5903(7) 0.073(3) Uani 1 1 d . . . H6 H 0.1054 0.3401 -0.6123 0.088 Uiso 1 1 calc R . . C7 C 0.0509(7) 0.2710(3) -0.6132(7) 0.068(3) Uani 1 1 d . . . C8 C -0.0327(8) 0.2747(4) -0.6692(8) 0.090(4) Uani 1 1 d . . . H8 H -0.0488 0.3041 -0.6962 0.108 Uiso 1 1 calc R . . C9 C -0.0908(7) 0.2362(4) -0.6849(7) 0.083(4) Uani 1 1 d . . . H9 H -0.1474 0.2383 -0.7234 0.100 Uiso 1 1 calc R . . C10 C -0.0670(6) 0.1933(3) -0.6441(6) 0.062(3) Uani 1 1 d . . . H10 H -0.1103 0.1673 -0.6532 0.074 Uiso 1 1 calc R . . C11 C 0.0736(6) 0.2259(3) -0.5777(5) 0.050(2) Uani 1 1 d . . . C12 C 0.1600(5) 0.2188(3) -0.5240(5) 0.0416(18) Uani 1 1 d . . . C13 C -0.0450(5) 0.0854(2) -0.5729(5) 0.0418(18) Uani 1 1 d . . . C14 C 0.0139(6) 0.1384(3) -0.4367(6) 0.051(2) Uani 1 1 d . . . C15 C 0.1172(6) 0.1072(3) -0.6357(6) 0.051(2) Uani 1 1 d . . . C16 C 0.1349(5) 0.0680(3) -0.4828(5) 0.0387(17) Uani 1 1 d . . . C17 C -0.2441(6) 0.0598(3) -0.4534(5) 0.0452(19) Uani 1 1 d . . . H17 H -0.1796 0.0530 -0.4550 0.054 Uiso 1 1 calc R . . C18 C -0.2652(7) 0.0800(3) -0.3852(5) 0.052(2) Uani 1 1 d . . . H18 H -0.2159 0.0878 -0.3423 0.062 Uiso 1 1 calc R . . C19 C -0.3553(7) 0.0882(3) -0.3810(5) 0.054(2) Uani 1 1 d . . . H19 H -0.3696 0.1023 -0.3347 0.065 Uiso 1 1 calc R . . C20 C -0.4298(6) 0.0765(2) -0.4430(4) 0.0407(18) Uani 1 1 d . . . C21 C -0.5277(6) 0.0817(3) -0.4426(5) 0.047(2) Uani 1 1 d . . . H21 H -0.5462 0.0947 -0.3971 0.057 Uiso 1 1 calc R . . C22 C -0.5948(6) 0.0692(3) -0.5025(5) 0.046(2) Uani 1 1 d . . . H22 H -0.6595 0.0723 -0.4983 0.055 Uiso 1 1 calc R . . C23 C -0.5708(5) 0.0510(2) -0.5740(5) 0.0353(16) Uani 1 1 d . . . C24 C -0.6404(5) 0.0388(3) -0.6394(5) 0.047(2) Uani 1 1 d . . . H24 H -0.7058 0.0429 -0.6383 0.057 Uiso 1 1 calc R . . C25 C -0.6120(5) 0.0205(2) -0.7056(5) 0.0415(18) Uani 1 1 d . . . H25 H -0.6573 0.0118 -0.7508 0.050 Uiso 1 1 calc R . . C26 C -0.5147(5) 0.0152(2) -0.7041(4) 0.0364(17) Uani 1 1 d . . . H26 H -0.4959 0.0019 -0.7493 0.044 Uiso 1 1 calc R . . C27 C -0.4750(5) 0.0452(2) -0.5791(4) 0.0325(16) Uani 1 1 d . . . C28 C -0.4026(5) 0.0571(2) -0.5127(4) 0.0339(16) Uani 1 1 d . . . C29 C -0.2801(5) 0.1454(2) -0.6127(5) 0.0420(18) Uani 1 1 d . . . H29 H -0.2383 0.1361 -0.5657 0.050 Uiso 1 1 calc R . . C30 C -0.3108(6) 0.1937(3) -0.6206(5) 0.048(2) Uani 1 1 d . . . H30 H -0.2878 0.2165 -0.5808 0.057 Uiso 1 1 calc R . . C31 C -0.3736(6) 0.2067(3) -0.6861(5) 0.047(2) Uani 1 1 d . . . H31 H -0.3971 0.2385 -0.6918 0.056 Uiso 1 1 calc R . . C32 C -0.4033(5) 0.1729(3) -0.7452(5) 0.0411(18) Uani 1 1 d . . . C33 C -0.4705(7) 0.1843(3) -0.8167(5) 0.058(2) Uani 1 1 d . . . H33 H -0.4991 0.2150 -0.8230 0.070 Uiso 1 1 calc R . . C34 C -0.4921(7) 0.1515(3) -0.8737(6) 0.064(3) Uani 1 1 d . . . H34 H -0.5372 0.1593 -0.9195 0.077 Uiso 1 1 calc R . . C35 C -0.4492(6) 0.1050(3) -0.8676(5) 0.051(2) Uani 1 1 d . . . C36 C -0.4623(8) 0.0712(4) -0.9307(5) 0.067(3) Uani 1 1 d . . . H36 H -0.5030 0.0785 -0.9792 0.081 Uiso 1 1 calc R . . C37 C -0.4161(8) 0.0286(3) -0.9208(5) 0.063(3) Uani 1 1 d . . . H37 H -0.4229 0.0061 -0.9626 0.076 Uiso 1 1 calc R . . C38 C -0.3588(6) 0.0185(3) -0.8490(5) 0.046(2) Uani 1 1 d . . . H38 H -0.3279 -0.0117 -0.8429 0.055 Uiso 1 1 calc R . . C39 C -0.3877(5) 0.0922(2) -0.7970(4) 0.0372(17) Uani 1 1 d . . . C40 C -0.3669(5) 0.1261(2) -0.7351(4) 0.0310(15) Uani 1 1 d . . . C41 C -0.2399(7) -0.1813(3) -0.7447(5) 0.051(2) Uani 1 1 d . . . H41 H -0.2216 -0.1513 -0.7206 0.061 Uiso 1 1 calc R . . C42 C -0.1792(8) -0.2203(3) -0.7274(6) 0.070(3) Uani 1 1 d . . . H42 H -0.1204 -0.2173 -0.6918 0.084 Uiso 1 1 calc R . . C43 C -0.2073(10) -0.2643(3) -0.7644(8) 0.082(4) Uani 1 1 d . . . H43 H -0.1672 -0.2914 -0.7527 0.098 Uiso 1 1 calc R . . C44 C -0.2900(9) -0.2688(3) -0.8160(7) 0.068(3) Uani 1 1 d . . . C45 C -0.3269(11) -0.3129(3) -0.8592(8) 0.087(4) Uani 1 1 d . . . H45 H -0.2915 -0.3417 -0.8491 0.105 Uiso 1 1 calc R . . C46 C -0.4072(11) -0.3135(4) -0.9111(8) 0.089(4) Uani 1 1 d . . . H46 H -0.4290 -0.3429 -0.9356 0.107 Uiso 1 1 calc R . . C47 C -0.4596(10) -0.2731(4) -0.9305(7) 0.081(4) Uani 1 1 d . . . C48 C -0.5410(11) -0.2706(5) -0.9901(7) 0.097(5) Uani 1 1 d . . . H48 H -0.5605 -0.2978 -1.0220 0.116 Uiso 1 1 calc R . . C49 C -0.5921(10) -0.2293(5) -1.0023(6) 0.090(4) Uani 1 1 d . . . H49 H -0.6482 -0.2282 -1.0414 0.109 Uiso 1 1 calc R . . C50 C -0.5628(8) -0.1887(4) -0.9579(6) 0.076(3) Uani 1 1 d . . . H50 H -0.5996 -0.1604 -0.9677 0.091 Uiso 1 1 calc R . . C51 C -0.4340(8) -0.2291(3) -0.8892(6) 0.063(3) Uani 1 1 d . . . C52 C -0.3459(8) -0.2283(3) -0.8302(6) 0.063(3) Uani 1 1 d . . . C53 C -0.3702(5) -0.0853(2) -0.7463(4) 0.0339(16) Uani 1 1 d . . . C54 C -0.3568(7) -0.1043(3) -0.9032(5) 0.051(2) Uani 1 1 d . . . C55 C -0.5345(8) -0.0871(4) -0.8590(5) 0.064(3) Uani 1 1 d . . . C56 C -0.5010(6) -0.1635(3) -0.7466(5) 0.0427(18) Uani 1 1 d . . . N1 N 0.1786(4) 0.1729(2) -0.4950(4) 0.0385(14) Uani 1 1 d . . . N2 N 0.0130(4) 0.1877(2) -0.5936(4) 0.0478(17) Uani 1 1 d . . . N3 N -0.1160(5) 0.0650(2) -0.5951(4) 0.0496(18) Uani 1 1 d . . . N4 N -0.0158(6) 0.1443(3) -0.3800(6) 0.079(3) Uani 1 1 d . . . N5 N 0.1408(6) 0.0978(4) -0.6928(5) 0.077(3) Uani 1 1 d . . . N6 N -0.3101(4) 0.0494(2) -0.5169(4) 0.0361(14) Uani 1 1 d . . . N7 N -0.4474(4) 0.02749(18) -0.6443(3) 0.0299(13) Uani 1 1 d . . . N8 N -0.3333(4) -0.0568(2) -0.7006(3) 0.0349(13) Uani 1 1 d . . . N9 N -0.3070(4) 0.1126(2) -0.6676(4) 0.0349(14) Uani 1 1 d . . . N10 N -0.3224(5) -0.1849(2) -0.7937(4) 0.0470(17) Uani 1 1 d . . . N11 N -0.4851(6) -0.1883(3) -0.9023(4) 0.058(2) Uani 1 1 d . . . N13 N -0.3127(6) -0.0879(3) -0.9479(4) 0.063(2) Uani 1 1 d . . . N14 N -0.5406(5) -0.1833(2) -0.7043(4) 0.0533(18) Uani 1 1 d . . . N16 N -0.3440(4) 0.0485(2) -0.7873(3) 0.0340(13) Uani 1 1 d . . . N17 N -0.5980(8) -0.0612(4) -0.8802(6) 0.097(3) Uani 1 1 d . . . O1 O -0.1503(5) -0.0013(2) -0.7291(4) 0.0729(19) Uani 1 1 d . . . H1B H -0.1876 -0.0189 -0.7570 0.087 Uiso 1 1 d R . . H1C H -0.1066 -0.0218 -0.7153 0.087 Uiso 1 1 d R . . O2 O -0.8636(11) 0.0566(6) -1.1503(10) 0.092(5) Uani 0.50 1 d P . . O3 O -0.8876(11) 0.0009(5) -0.7638(11) 0.100(5) Uani 0.50 1 d P . . O4 O -0.7152(14) 0.0178(6) -0.9380(11) 0.115(7) Uani 0.50 1 d P . . O5 O 0.2146(14) 0.6371(9) -0.3084(11) 0.138(8) Uani 0.50 1 d P . . O6 O 0.0250(7) 0.5236(3) -0.1216(7) 0.130(4) Uani 1 1 d . . . H6B H 0.0494 0.5166 -0.1611 0.156 Uiso 1 1 d R . . H6C H -0.0113 0.5007 -0.1145 0.156 Uiso 1 1 d R . . O7 O -0.2717(6) 0.2063(4) -0.2998(7) 0.161(6) Uani 1 1 d . . . H7B H -0.3314 0.2092 -0.3142 0.193 Uiso 1 1 d R . . H7C H -0.2717 0.1801 -0.2748 0.193 Uiso 1 1 d R . . O8 O -0.1917(6) 0.1991(3) -0.4303(5) 0.114(3) Uani 1 1 d . . . H8B H -0.1962 0.2050 -0.3830 0.137 Uiso 1 1 d R . . H8C H -0.1416 0.1819 -0.4172 0.137 Uiso 1 1 d R . . O9 O -0.1109(12) 0.2845(6) -0.4436(11) 0.101(4) Uani 0.50 1 d PU A 1 O9' O -0.0164(12) 0.2835(6) -0.4063(11) 0.104(4) Uani 0.50 1 d PU B 2 O10 O -0.0295(11) 0.3951(5) -0.7360(8) 0.201(6) Uani 1 1 d . . . H10B H -0.0738 0.3791 -0.7639 0.242 Uiso 1 1 d R . . H10C H 0.0074 0.4149 -0.7524 0.242 Uiso 1 1 d R . . O11 O -0.7276(15) 0.1236(7) -0.8422(9) 0.110(5) Uani 0.50 1 d PU C 1 O11' O -0.8305(15) 0.1181(7) -0.8453(9) 0.109(5) Uani 0.50 1 d PU D 2 N15 N 0.1789(4) 0.0363(2) -0.4496(4) 0.0439(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0272(2) 0.0220(2) 0.0440(3) 0.00199(15) 0.00512(17) 0.00139(13) Ru1 0.0240(3) 0.0256(3) 0.0573(4) 0.0080(3) 0.0068(3) 0.0017(2) Ru2 0.0616(4) 0.0293(3) 0.0407(4) -0.0119(3) 0.0137(3) -0.0027(3) K1A 0.040(2) 0.041(2) 0.033(2) 0.0052(17) 0.0050(17) -0.0049(17) K1B 0.012(2) 0.028(2) 0.079(4) -0.028(2) 0.015(2) -0.0018(18) K1C 0.023(3) 0.043(3) 0.079(4) 0.011(3) 0.015(3) -0.004(2) C1 0.032(4) 0.045(4) 0.040(4) -0.005(3) 0.010(3) 0.001(3) C2 0.041(5) 0.054(5) 0.055(5) -0.008(4) 0.017(4) -0.011(4) C3 0.057(6) 0.062(6) 0.055(5) -0.019(5) 0.021(4) -0.027(5) C4 0.053(5) 0.036(5) 0.075(6) -0.010(4) 0.030(5) -0.010(4) C5 0.080(7) 0.037(5) 0.089(8) -0.005(5) 0.036(6) -0.020(5) C6 0.093(8) 0.029(5) 0.108(9) 0.014(5) 0.046(7) -0.003(5) C7 0.060(6) 0.036(5) 0.114(8) 0.026(5) 0.028(6) 0.009(4) C8 0.060(7) 0.052(6) 0.159(12) 0.058(7) 0.020(7) 0.009(5) C9 0.050(6) 0.069(7) 0.123(10) 0.040(7) -0.006(6) 0.017(5) C10 0.033(4) 0.055(5) 0.095(7) 0.033(5) 0.005(4) 0.010(4) C11 0.050(5) 0.029(4) 0.076(6) 0.007(4) 0.025(4) 0.002(3) C12 0.037(4) 0.032(4) 0.060(5) 0.002(4) 0.022(4) -0.006(3) C13 0.035(4) 0.022(4) 0.066(5) 0.011(3) 0.006(4) 0.004(3) C14 0.038(5) 0.041(5) 0.077(6) 0.003(4) 0.018(4) -0.006(4) C15 0.034(4) 0.059(5) 0.058(6) 0.004(4) 0.001(4) 0.009(4) C16 0.023(4) 0.034(4) 0.059(5) -0.001(4) 0.007(3) -0.005(3) C17 0.045(5) 0.039(4) 0.047(5) -0.002(4) -0.002(4) -0.004(3) C18 0.064(6) 0.038(5) 0.048(5) -0.009(4) 0.000(4) -0.009(4) C19 0.096(8) 0.028(4) 0.039(5) -0.001(3) 0.014(5) -0.002(4) C20 0.068(5) 0.014(3) 0.044(4) 0.006(3) 0.021(4) 0.001(3) C21 0.073(6) 0.024(4) 0.053(5) 0.009(3) 0.034(5) 0.010(4) C22 0.053(5) 0.022(4) 0.070(6) 0.005(4) 0.031(5) 0.005(3) C23 0.041(4) 0.015(3) 0.054(5) 0.009(3) 0.020(4) -0.001(3) C24 0.032(4) 0.032(4) 0.081(6) 0.012(4) 0.019(4) 0.004(3) C25 0.032(4) 0.034(4) 0.056(5) 0.007(3) 0.002(4) -0.002(3) C26 0.037(4) 0.027(4) 0.045(4) 0.000(3) 0.006(3) 0.003(3) C27 0.044(4) 0.012(3) 0.045(4) 0.007(3) 0.016(3) 0.005(3) C28 0.045(4) 0.017(3) 0.042(4) 0.005(3) 0.015(3) 0.001(3) C29 0.041(4) 0.027(4) 0.055(5) -0.003(3) 0.000(4) 0.000(3) C30 0.048(5) 0.027(4) 0.070(6) -0.006(4) 0.016(4) -0.004(3) C31 0.049(5) 0.026(4) 0.068(6) 0.006(4) 0.018(4) 0.006(3) C32 0.042(4) 0.031(4) 0.050(5) 0.008(3) 0.008(4) 0.001(3) C33 0.066(6) 0.042(5) 0.065(6) 0.021(4) 0.007(5) 0.016(4) C34 0.082(7) 0.042(5) 0.059(6) 0.014(4) -0.012(5) 0.010(5) C35 0.065(6) 0.040(4) 0.045(5) 0.012(4) 0.005(4) 0.000(4) C36 0.089(7) 0.063(6) 0.043(5) 0.013(4) -0.006(5) -0.003(5) C37 0.109(8) 0.043(5) 0.037(5) -0.002(4) 0.011(5) -0.002(5) C38 0.070(6) 0.028(4) 0.045(5) 0.003(3) 0.021(4) -0.001(4) C39 0.039(4) 0.030(4) 0.045(4) 0.009(3) 0.014(3) -0.004(3) C40 0.025(3) 0.026(4) 0.043(4) 0.006(3) 0.009(3) 0.001(3) C41 0.073(6) 0.035(4) 0.052(5) 0.003(4) 0.031(5) 0.010(4) C42 0.079(7) 0.057(6) 0.082(7) 0.013(5) 0.037(6) 0.019(5) C43 0.108(10) 0.038(6) 0.121(10) 0.017(6) 0.076(9) 0.028(6) C44 0.094(8) 0.030(5) 0.096(8) 0.001(5) 0.059(7) 0.007(5) C45 0.139(12) 0.020(5) 0.129(11) -0.009(6) 0.093(10) 0.002(6) C46 0.138(12) 0.039(6) 0.115(10) -0.033(6) 0.082(9) -0.026(7) C47 0.123(10) 0.049(6) 0.095(8) -0.041(6) 0.079(8) -0.041(6) C48 0.162(13) 0.083(9) 0.060(7) -0.046(7) 0.060(8) -0.074(9) C49 0.134(11) 0.083(9) 0.057(7) -0.029(6) 0.025(7) -0.049(8) C50 0.100(9) 0.070(7) 0.057(6) -0.028(5) 0.015(6) -0.032(6) C51 0.094(8) 0.048(5) 0.062(6) -0.025(4) 0.052(6) -0.029(5) C52 0.096(8) 0.031(5) 0.079(7) -0.010(4) 0.061(6) -0.011(5) C53 0.039(4) 0.025(4) 0.042(4) 0.003(3) 0.018(3) 0.001(3) C54 0.083(6) 0.027(4) 0.044(5) -0.007(3) 0.016(5) 0.005(4) C55 0.078(7) 0.060(6) 0.049(5) -0.017(4) -0.002(5) 0.005(5) C56 0.045(4) 0.031(4) 0.054(5) -0.014(4) 0.013(4) -0.006(3) N1 0.035(3) 0.031(3) 0.053(4) -0.001(3) 0.020(3) 0.001(3) N2 0.031(3) 0.033(3) 0.079(5) 0.018(3) 0.010(3) 0.005(3) N3 0.034(4) 0.033(4) 0.077(5) 0.008(3) -0.001(3) 0.001(3) N4 0.057(5) 0.092(7) 0.100(7) -0.011(5) 0.043(5) -0.009(5) N5 0.061(5) 0.114(8) 0.056(5) -0.001(5) 0.011(4) 0.009(5) N6 0.034(3) 0.029(3) 0.044(4) 0.003(3) 0.005(3) 0.001(2) N7 0.033(3) 0.020(3) 0.037(3) 0.003(2) 0.008(3) 0.001(2) N8 0.045(4) 0.024(3) 0.037(3) -0.001(3) 0.011(3) 0.001(3) N9 0.029(3) 0.026(3) 0.049(4) 0.000(3) 0.008(3) -0.003(2) N10 0.074(5) 0.025(3) 0.051(4) -0.007(3) 0.036(4) 0.000(3) N11 0.085(6) 0.041(4) 0.053(5) -0.021(3) 0.027(4) -0.013(4) N13 0.103(6) 0.044(4) 0.049(4) 0.000(3) 0.030(4) 0.008(4) N14 0.055(4) 0.042(4) 0.066(5) -0.022(4) 0.019(4) -0.005(3) N16 0.042(3) 0.027(3) 0.036(3) 0.004(3) 0.014(3) 0.003(2) N17 0.107(8) 0.095(8) 0.077(6) -0.024(5) -0.013(6) 0.035(7) O1 0.055(4) 0.069(4) 0.106(5) 0.003(4) 0.043(4) 0.010(3) O2 0.087(11) 0.090(11) 0.108(12) -0.050(9) 0.040(9) 0.017(9) O3 0.084(11) 0.049(8) 0.172(17) 0.036(10) 0.035(11) -0.006(8) O4 0.147(16) 0.097(12) 0.133(15) 0.069(11) 0.108(13) 0.049(11) O5 0.114(15) 0.20(2) 0.085(12) 0.058(14) -0.017(11) -0.009(15) O6 0.100(7) 0.111(8) 0.170(10) 0.012(6) -0.001(7) -0.022(6) O7 0.075(6) 0.207(12) 0.215(12) -0.147(10) 0.063(7) -0.073(7) O8 0.076(6) 0.142(8) 0.118(7) 0.007(6) 0.004(5) 0.032(6) O9 0.085(8) 0.084(8) 0.130(11) 0.030(8) 0.012(7) 0.021(7) O9' 0.087(8) 0.088(8) 0.133(11) 0.028(8) 0.013(7) 0.021(7) O10 0.234(17) 0.211(15) 0.156(11) 0.032(11) 0.030(11) 0.004(13) O11 0.149(12) 0.125(11) 0.061(7) 0.008(6) 0.030(9) -0.014(10) O11' 0.147(12) 0.125(11) 0.059(7) 0.008(6) 0.030(9) -0.015(10) N15 0.031(3) 0.027(3) 0.069(5) 0.006(3) -0.002(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.436(6) . ? Nd1 N15 2.460(6) 3_554 ? Nd1 N8 2.479(6) . ? Nd1 N3 2.483(7) . ? Nd1 N16 2.596(6) . ? Nd1 N6 2.597(6) . ? Nd1 N7 2.647(6) . ? Nd1 N9 2.654(6) . ? Nd1 H1B 2.6125 . ? Ru1 C13 1.952(8) . ? Ru1 C16 1.965(8) . ? Ru1 C15 2.045(10) . ? Ru1 C14 2.051(10) . ? Ru1 N1 2.113(6) . ? Ru1 N2 2.123(6) . ? Ru2 C53 1.956(7) . ? Ru2 C55 1.975(11) . ? Ru2 C56 2.031(9) . ? Ru2 C54 2.034(9) . ? Ru2 N10 2.118(7) . ? Ru2 N11 2.123(7) . ? K1A O4 2.328(17) . ? K1A O3 2.678(19) . ? K1A K1A 4.371(8) 3_353 ? K1B K1B 2.649(9) 3_353 ? K1B O4 2.89(2) . ? K1B O2 3.402(19) . ? K1C K1C 2.716(13) 3_353 ? K1C O2 2.738(18) . ? K1C O3 3.04(2) 3_353 ? C1 N1 1.339(9) . ? C1 C2 1.385(10) . ? C1 H1 0.9500 . ? C2 C3 1.353(12) . ? C2 H2 0.9500 . ? C3 C4 1.400(13) . ? C3 H3 0.9500 . ? C4 C12 1.413(11) . ? C4 C5 1.417(13) . ? C5 C6 1.324(15) . ? C5 H5 0.9500 . ? C6 C7 1.447(14) . ? C6 H6 0.9500 . ? C7 C8 1.397(15) . ? C7 C11 1.412(11) . ? C8 C9 1.357(15) . ? C8 H8 0.9500 . ? C9 C10 1.400(12) . ? C9 H9 0.9500 . ? C10 N2 1.314(10) . ? C10 H10 0.9500 . ? C11 N2 1.373(10) . ? C11 C12 1.415(12) . ? C12 N1 1.385(9) . ? C13 N3 1.168(10) . ? C14 N4 1.155(11) . ? C15 N5 1.134(11) . ? C16 N15 1.173(9) . ? C17 N6 1.340(9) . ? C17 C18 1.393(12) . ? C17 H17 0.9500 . ? C18 C19 1.330(12) . ? C18 H18 0.9500 . ? C19 C20 1.401(12) . ? C19 H19 0.9500 . ? C20 C21 1.415(12) . ? C20 C28 1.444(10) . ? C21 C22 1.320(12) . ? C21 H21 0.9500 . ? C22 C23 1.440(11) . ? C22 H22 0.9500 . ? C23 C24 1.403(11) . ? C23 C27 1.404(10) . ? C24 C25 1.385(12) . ? C24 H24 0.9500 . ? C25 C26 1.400(10) . ? C25 H25 0.9500 . ? C26 N7 1.321(9) . ? C26 H26 0.9500 . ? C27 N7 1.359(9) . ? C27 C28 1.434(10) . ? C28 N6 1.362(9) . ? C29 N9 1.324(9) . ? C29 C30 1.417(10) . ? C29 H29 0.9500 . ? C30 C31 1.359(12) . ? C30 H30 0.9500 . ? C31 C32 1.398(11) . ? C31 H31 0.9500 . ? C32 C40 1.407(10) . ? C32 C33 1.452(11) . ? C33 C34 1.338(13) . ? C33 H33 0.9500 . ? C34 C35 1.433(12) . ? C34 H34 0.9500 . ? C35 C39 1.412(11) . ? C35 C36 1.428(12) . ? C36 C37 1.357(13) . ? C36 H36 0.9500 . ? C37 C38 1.384(12) . ? C37 H37 0.9500 . ? C38 N16 1.342(9) . ? C38 H38 0.9500 . ? C39 N16 1.367(9) . ? C39 C40 1.419(10) . ? C40 N9 1.365(9) . ? C41 N10 1.324(11) . ? C41 C42 1.391(12) . ? C41 H41 0.9500 . ? C42 C43 1.408(15) . ? C42 H42 0.9500 . ? C43 C44 1.350(16) . ? C43 H43 0.9500 . ? C44 C52 1.381(13) . ? C44 C45 1.486(15) . ? C45 C46 1.320(18) . ? C45 H45 0.9500 . ? C46 C47 1.364(18) . ? C46 H46 0.9500 . ? C47 C48 1.406(19) . ? C47 C51 1.434(12) . ? C48 C49 1.362(19) . ? C48 H48 0.9500 . ? C49 C50 1.388(14) . ? C49 H49 0.9500 . ? C50 N11 1.329(13) . ? C50 H50 0.9500 . ? C51 N11 1.352(13) . ? C51 C52 1.467(15) . ? C52 N10 1.379(10) . ? C53 N8 1.176(9) . ? C54 N13 1.182(11) . ? C55 N17 1.167(12) . ? C56 N14 1.151(10) . ? O1 H1B 0.8153 . ? O1 H1C 0.8498 . ? O3 K1C 3.04(2) 3_353 ? O6 H6B 0.8497 . ? O6 H6C 0.8500 . ? O7 H7B 0.8498 . ? O7 H7C 0.8499 . ? O8 H8B 0.8499 . ? O8 H8C 0.8596 . ? O10 H10B 0.8499 . ? O10 H10C 0.8500 . ? N15 Nd1 2.460(6) 3_554 ? 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 O1 Nd1 N15 86.1(2) . 3_554 ? O1 Nd1 N8 80.3(2) . . ? N15 Nd1 N8 78.74(19) 3_554 . ? O1 Nd1 N3 73.2(2) . . ? N15 Nd1 N3 78.0(2) 3_554 . ? N8 Nd1 N3 145.7(2) . . ? O1 Nd1 N16 76.0(2) . . ? N15 Nd1 N16 154.9(2) 3_554 . ? N8 Nd1 N16 80.90(18) . . ? N3 Nd1 N16 112.6(2) . . ? O1 Nd1 N6 153.1(2) . . ? N15 Nd1 N6 77.5(2) 3_554 . ? N8 Nd1 N6 116.39(19) . . ? N3 Nd1 N6 82.5(2) . . ? N16 Nd1 N6 125.32(18) . . ? O1 Nd1 N7 144.1(2) . . ? N15 Nd1 N7 113.75(19) 3_554 . ? N8 Nd1 N7 75.12(18) . . ? N3 Nd1 N7 137.9(2) . . ? N16 Nd1 N7 74.51(17) . . ? N6 Nd1 N7 62.84(18) . . ? O1 Nd1 N9 109.2(2) . . ? N15 Nd1 N9 142.0(2) 3_554 . ? N8 Nd1 N9 136.83(18) . . ? N3 Nd1 N9 73.93(19) . . ? N16 Nd1 N9 62.22(18) . . ? N6 Nd1 N9 73.94(18) . . ? N7 Nd1 N9 74.06(16) . . ? O1 Nd1 H1B 18.2 . . ? N15 Nd1 H1B 90.0 3_554 . ? N8 Nd1 H1B 63.7 . . ? N3 Nd1 H1B 91.4 . . ? N16 Nd1 H1B 67.7 . . ? N6 Nd1 H1B 166.9 . . ? N7 Nd1 H1B 127.1 . . ? N9 Nd1 H1B 115.6 . . ? C13 Ru1 C16 91.0(3) . . ? C13 Ru1 C15 89.7(3) . . ? C16 Ru1 C15 89.9(3) . . ? C13 Ru1 C14 87.7(3) . . ? C16 Ru1 C14 89.8(3) . . ? C15 Ru1 C14 177.4(3) . . ? C13 Ru1 N1 172.6(3) . . ? C16 Ru1 N1 95.3(3) . . ? C15 Ru1 N1 94.1(3) . . ? C14 Ru1 N1 88.5(3) . . ? C13 Ru1 N2 95.4(3) . . ? C16 Ru1 N2 172.9(3) . . ? C15 Ru1 N2 87.0(3) . . ? C14 Ru1 N2 93.6(3) . . ? N1 Ru1 N2 78.6(2) . . ? C53 Ru2 C55 89.3(3) . . ? C53 Ru2 C56 92.5(3) . . ? C55 Ru2 C56 91.5(4) . . ? C53 Ru2 C54 89.5(3) . . ? C55 Ru2 C54 90.3(4) . . ? C56 Ru2 C54 177.3(3) . . ? C53 Ru2 N10 95.5(3) . . ? C55 Ru2 N10 175.2(3) . . ? C56 Ru2 N10 88.6(3) . . ? C54 Ru2 N10 89.5(3) . . ? C53 Ru2 N11 174.7(3) . . ? C55 Ru2 N11 95.9(4) . . ? C56 Ru2 N11 86.0(3) . . ? C54 Ru2 N11 91.8(3) . . ? N10 Ru2 N11 79.3(3) . . ? O4 K1A O3 117.2(6) . . ? O4 K1A K1A 128.0(5) . 3_353 ? O3 K1A K1A 114.6(4) . 3_353 ? K1B K1B O4 146.4(4) 3_353 . ? K1B K1B O2 101.0(4) 3_353 . ? O4 K1B O2 79.3(4) . . ? K1C K1C O2 140.1(5) 3_353 . ? K1C K1C O3 133.7(4) 3_353 3_353 ? O2 K1C O3 85.8(5) . 3_353 ? N1 C1 C2 122.9(8) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 120.3(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C12 117.1(8) . . ? C3 C4 C5 126.1(8) . . ? C12 C4 C5 116.8(9) . . ? C6 C5 C4 123.5(9) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C7 121.4(9) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C11 117.8(9) . . ? C8 C7 C6 125.4(9) . . ? C11 C7 C6 116.8(9) . . ? C9 C8 C7 119.6(9) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.7(10) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.6(9) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N2 C11 C7 121.4(8) . . ? N2 C11 C12 117.8(7) . . ? C7 C11 C12 120.8(8) . . ? N1 C12 C4 122.4(7) . . ? N1 C12 C11 116.8(7) . . ? C4 C12 C11 120.7(7) . . ? N3 C13 Ru1 175.8(7) . . ? N4 C14 Ru1 176.8(8) . . ? N5 C15 Ru1 177.2(8) . . ? N15 C16 Ru1 176.2(6) . . ? N6 C17 C18 123.3(8) . . ? N6 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C19 C18 C17 119.2(8) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 121.8(8) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 126.0(8) . . ? C19 C20 C28 116.1(8) . . ? C21 C20 C28 117.9(7) . . ? C22 C21 C20 123.1(8) . . ? C22 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C21 C22 C23 120.7(8) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C27 118.5(7) . . ? C24 C23 C22 122.1(7) . . ? C27 C23 C22 119.5(7) . . ? C25 C24 C23 118.8(7) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 118.3(7) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? N7 C26 C25 124.5(7) . . ? N7 C26 H26 117.8 . . ? C25 C26 H26 117.8 . . ? N7 C27 C23 122.6(7) . . ? N7 C27 C28 117.9(6) . . ? C23 C27 C28 119.5(6) . . ? N6 C28 C27 119.1(6) . . ? N6 C28 C20 121.7(7) . . ? C27 C28 C20 119.2(7) . . ? N9 C29 C30 123.0(7) . . ? N9 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C31 C30 C29 118.8(8) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C32 119.4(7) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C32 C40 118.8(7) . . ? C31 C32 C33 122.4(7) . . ? C40 C32 C33 118.8(7) . . ? C34 C33 C32 120.1(8) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 122.0(8) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C39 C35 C36 117.6(8) . . ? C39 C35 C34 118.9(8) . . ? C36 C35 C34 123.4(8) . . ? C37 C36 C35 119.5(8) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 119.0(8) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N16 C38 C37 124.4(7) . . ? N16 C38 H38 117.8 . . ? C37 C38 H38 117.8 . . ? N16 C39 C35 122.0(7) . . ? N16 C39 C40 118.5(6) . . ? C35 C39 C40 119.4(7) . . ? N9 C40 C32 121.4(7) . . ? N9 C40 C39 118.0(6) . . ? C32 C40 C39 120.4(7) . . ? N10 C41 C42 121.7(9) . . ? N10 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C43 118.1(11) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C44 C43 C42 121.5(10) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C43 C44 C52 116.7(10) . . ? C43 C44 C45 126.6(10) . . ? C52 C44 C45 116.7(12) . . ? C46 C45 C44 122.3(11) . . ? C46 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C45 C46 C47 121.8(11) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C46 C47 C48 124.4(11) . . ? C46 C47 C51 120.6(13) . . ? C48 C47 C51 115.0(12) . . ? C49 C48 C47 120.2(10) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 C50 120.6(13) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? N11 C50 C49 122.2(12) . . ? N11 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? N11 C51 C47 124.0(11) . . ? N11 C51 C52 118.2(8) . . ? C47 C51 C52 117.8(11) . . ? N10 C52 C44 123.7(11) . . ? N10 C52 C51 115.8(8) . . ? C44 C52 C51 120.4(9) . . ? N8 C53 Ru2 178.7(6) . . ? N13 C54 Ru2 178.5(8) . . ? N17 C55 Ru2 178.4(10) . . ? N14 C56 Ru2 176.6(7) . . ? C1 N1 C12 117.2(6) . . ? C1 N1 Ru1 129.2(5) . . ? C12 N1 Ru1 113.6(5) . . ? C10 N2 C11 118.7(7) . . ? C10 N2 Ru1 128.0(6) . . ? C11 N2 Ru1 113.2(5) . . ? C13 N3 Nd1 177.6(7) . . ? C17 N6 C28 117.8(7) . . ? C17 N6 Nd1 121.6(5) . . ? C28 N6 Nd1 120.4(5) . . ? C26 N7 C27 117.4(6) . . ? C26 N7 Nd1 123.2(5) . . ? C27 N7 Nd1 119.4(4) . . ? C53 N8 Nd1 159.6(5) . . ? C29 N9 C40 118.4(6) . . ? C29 N9 Nd1 123.1(5) . . ? C40 N9 Nd1 118.2(4) . . ? C41 N10 C52 118.1(8) . . ? C41 N10 Ru2 128.7(5) . . ? C52 N10 Ru2 113.2(7) . . ? C50 N11 C51 117.9(8) . . ? C50 N11 Ru2 129.2(7) . . ? C51 N11 Ru2 112.8(7) . . ? C38 N16 C39 117.4(6) . . ? C38 N16 Nd1 121.9(5) . . ? C39 N16 Nd1 119.6(5) . . ? Nd1 O1 H1B 93.3 . . ? Nd1 O1 H1C 123.2 . . ? H1B O1 H1C 97.2 . . ? K1C O2 K1B 29.0(2) . . ? K1A O3 K1C 42.6(3) . 3_353 ? K1A O4 K1B 32.0(3) . . ? H6B O6 H6C 107.5 . . ? H7B O7 H7C 97.7 . . ? H8B O8 H8C 93.9 . . ? H10B O10 H10C 126.8 . . ? C16 N15 Nd1 166.7(6) . 3_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.504 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.230 #===END data_imw772r _database_code_depnum_ccdc_archive 'CCDC 636984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H110 K2 N32 O19 Pr2 Ru4' _chemical_formula_weight 3020.66 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' K K 0.2009 0.2494 '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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.400(3) _cell_length_b 28.050(6) _cell_length_c 17.400(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.91(3) _cell_angle_gamma 90.00 _cell_volume 6901(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6550 _exptl_absorpt_correction_T_max 0.8545 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94220 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12161 _reflns_number_gt 8941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+32.0723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12161 _refine_ls_number_parameters 849 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.2070 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.168 _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 Pr1 Pr 0.76314(3) 0.020493(14) 0.14790(3) 0.03405(15) Uani 1 1 d . . . Ru1 Ru 0.43099(4) 0.12448(2) 0.03460(4) 0.03752(19) Uani 1 1 d . . . Ru2 Ru 0.93047(5) -0.13196(2) 0.32482(4) 0.0442(2) Uani 1 1 d . . . K1A K 0.4870(4) 0.0097(3) 0.5726(5) 0.0565(13) Uani 0.30 1 d PU . 1 K1B K 0.4086(3) -0.01025(16) 0.5002(3) 0.0471(9) Uani 0.40 1 d PU . 2 K1C K 0.3675(4) 0.0087(2) 0.4135(4) 0.0394(11) Uani 0.30 1 d PU . 3 C1 C 0.2399(6) 0.1658(3) -0.0576(5) 0.0433(19) Uani 1 1 d . . . H1 H 0.2264 0.1345 -0.0776 0.052 Uiso 1 1 calc R . . C2 C 0.1749(6) 0.2020(3) -0.0826(5) 0.051(2) Uani 1 1 d . . . H2 H 0.1185 0.1953 -0.1191 0.062 Uiso 1 1 calc R . . C3 C 0.1928(7) 0.2471(4) -0.0543(6) 0.059(3) Uani 1 1 d . . . H3 H 0.1487 0.2719 -0.0712 0.071 Uiso 1 1 calc R . . C4 C 0.2750(6) 0.2570(3) -0.0008(6) 0.052(2) Uani 1 1 d . . . C5 C 0.2998(9) 0.3030(4) 0.0360(7) 0.069(3) Uani 1 1 d . . . H5 H 0.2576 0.3290 0.0227 0.083 Uiso 1 1 calc R . . C6 C 0.3792(9) 0.3100(3) 0.0875(8) 0.074(3) Uani 1 1 d . . . H6 H 0.3917 0.3406 0.1106 0.089 Uiso 1 1 calc R . . C7 C 0.4471(8) 0.2721(3) 0.1093(7) 0.067(3) Uani 1 1 d . . . C8 C 0.5294(9) 0.2767(4) 0.1642(9) 0.091(4) Uani 1 1 d . . . H8 H 0.5445 0.3062 0.1906 0.109 Uiso 1 1 calc R . . C9 C 0.5897(8) 0.2383(4) 0.1803(8) 0.082(4) Uani 1 1 d . . . H9 H 0.6477 0.2413 0.2166 0.099 Uiso 1 1 calc R . . C10 C 0.5649(6) 0.1950(4) 0.1431(7) 0.067(3) Uani 1 1 d . . . H10 H 0.6068 0.1687 0.1551 0.080 Uiso 1 1 calc R . . C11 C 0.4248(6) 0.2266(3) 0.0755(6) 0.049(2) Uani 1 1 d . . . C12 C 0.3380(6) 0.2189(3) 0.0210(6) 0.048(2) Uani 1 1 d . . . C13 C 0.5450(6) 0.0862(3) 0.0732(5) 0.0424(19) Uani 1 1 d . . . C14 C 0.3653(5) 0.0685(3) -0.0178(5) 0.0427(19) Uani 1 1 d . . . C15 C 0.4842(6) 0.1379(3) -0.0640(6) 0.053(2) Uani 1 1 d . . . C16 C 0.3817(6) 0.1088(3) 0.1345(6) 0.050(2) Uani 1 1 d . . . C17 C 0.7422(7) -0.1822(3) 0.2474(6) 0.054(2) Uani 1 1 d . . . H17 H 0.7237 -0.1525 0.2230 0.064 Uiso 1 1 calc R . . C18 C 0.6808(8) -0.2213(4) 0.2301(7) 0.072(3) Uani 1 1 d . . . H18 H 0.6223 -0.2181 0.1946 0.086 Uiso 1 1 calc R . . C19 C 0.7075(10) -0.2646(4) 0.2661(8) 0.079(4) Uani 1 1 d . . . H19 H 0.6675 -0.2917 0.2546 0.095 Uiso 1 1 calc R . . C20 C 0.7921(9) -0.2685(3) 0.3188(8) 0.069(3) Uani 1 1 d . . . C21 C 0.8281(12) -0.3131(4) 0.3610(9) 0.085(4) Uani 1 1 d . . . H21 H 0.7938 -0.3420 0.3498 0.102 Uiso 1 1 calc R . . C22 C 0.9081(12) -0.3128(4) 0.4144(9) 0.087(4) Uani 1 1 d . . . H22 H 0.9286 -0.3416 0.4409 0.104 Uiso 1 1 calc R . . C23 C 0.9628(9) -0.2718(4) 0.4327(7) 0.074(4) Uani 1 1 d . . . C24 C 1.0439(11) -0.2696(5) 0.4907(7) 0.086(4) Uani 1 1 d . . . H24 H 1.0637 -0.2969 0.5219 0.103 Uiso 1 1 calc R . . C25 C 1.0954(10) -0.2284(5) 0.5031(7) 0.084(4) Uani 1 1 d . . . H25 H 1.1512 -0.2271 0.5422 0.100 Uiso 1 1 calc R . . C26 C 1.0652(9) -0.1879(4) 0.4576(6) 0.074(3) Uani 1 1 d . . . H26 H 1.1021 -0.1597 0.4662 0.089 Uiso 1 1 calc R . . C27 C 0.9351(8) -0.2285(3) 0.3901(6) 0.062(3) Uani 1 1 d . . . C28 C 0.8481(8) -0.2278(3) 0.3327(6) 0.059(3) Uani 1 1 d . . . C29 C 0.8703(6) -0.0854(3) 0.2469(5) 0.0372(17) Uani 1 1 d . . . C30 C 0.8580(7) -0.1035(3) 0.4039(5) 0.051(2) Uani 1 1 d . . . C31 C 1.0023(6) -0.1630(3) 0.2473(5) 0.0442(19) Uani 1 1 d . . . C32 C 1.0367(8) -0.0864(4) 0.3587(6) 0.064(3) Uani 1 1 d . . . C33 C 0.8600(7) 0.0191(3) 0.3486(5) 0.048(2) Uani 1 1 d . . . H33 H 0.8296 -0.0111 0.3427 0.058 Uiso 1 1 calc R . . C34 C 0.9174(9) 0.0292(4) 0.4202(6) 0.068(3) Uani 1 1 d . . . H34 H 0.9244 0.0069 0.4619 0.082 Uiso 1 1 calc R . . C35 C 0.9635(8) 0.0719(4) 0.4293(6) 0.069(3) Uani 1 1 d . . . H35 H 1.0045 0.0792 0.4773 0.083 Uiso 1 1 calc R . . C36 C 0.9504(7) 0.1052(3) 0.3674(5) 0.052(2) Uani 1 1 d . . . C37 C 0.9941(8) 0.1517(4) 0.3726(6) 0.066(3) Uani 1 1 d . . . H37 H 1.0408 0.1592 0.4173 0.079 Uiso 1 1 calc R . . C38 C 0.9708(7) 0.1849(4) 0.3161(6) 0.061(3) Uani 1 1 d . . . H38 H 0.9981 0.2158 0.3228 0.073 Uiso 1 1 calc R . . C39 C 0.9039(6) 0.1733(3) 0.2449(5) 0.045(2) Uani 1 1 d . . . C40 C 0.8743(6) 0.2071(3) 0.1868(6) 0.050(2) Uani 1 1 d . . . H40 H 0.8982 0.2387 0.1923 0.060 Uiso 1 1 calc R . . C41 C 0.8102(6) 0.1940(3) 0.1217(6) 0.048(2) Uani 1 1 d . . . H41 H 0.7860 0.2169 0.0828 0.058 Uiso 1 1 calc R . . C42 C 0.7807(6) 0.1458(3) 0.1132(5) 0.0428(19) Uani 1 1 d . . . H42 H 0.7400 0.1365 0.0660 0.051 Uiso 1 1 calc R . . C43 C 0.8672(5) 0.1265(3) 0.2349(5) 0.0342(17) Uani 1 1 d . . . C44 C 0.8885(5) 0.0923(3) 0.2979(5) 0.0394(18) Uani 1 1 d . . . C45 C 1.0149(5) 0.0150(3) 0.2041(5) 0.0393(18) Uani 1 1 d . . . H45 H 0.9959 0.0020 0.2492 0.047 Uiso 1 1 calc R . . C46 C 1.1117(6) 0.0199(3) 0.2052(6) 0.047(2) Uani 1 1 d . . . H46 H 1.1568 0.0107 0.2499 0.056 Uiso 1 1 calc R . . C47 C 1.1405(6) 0.0384(3) 0.1399(6) 0.050(2) Uani 1 1 d . . . H47 H 1.2058 0.0424 0.1391 0.060 Uiso 1 1 calc R . . C48 C 1.0713(6) 0.0512(3) 0.0743(5) 0.0410(19) Uani 1 1 d . . . C49 C 1.0954(7) 0.0696(3) 0.0021(6) 0.050(2) Uani 1 1 d . . . H49 H 1.1600 0.0729 -0.0019 0.060 Uiso 1 1 calc R . . C50 C 1.0292(7) 0.0816(3) -0.0576(6) 0.048(2) Uani 1 1 d . . . H50 H 1.0475 0.0941 -0.1033 0.058 Uiso 1 1 calc R . . C51 C 0.9301(7) 0.0766(3) -0.0565(5) 0.044(2) Uani 1 1 d . . . C52 C 0.8568(8) 0.0884(3) -0.1185(5) 0.059(3) Uani 1 1 d . . . H52 H 0.8715 0.1026 -0.1644 0.071 Uiso 1 1 calc R . . C53 C 0.7652(8) 0.0801(3) -0.1145(6) 0.057(2) Uani 1 1 d . . . H53 H 0.7161 0.0876 -0.1574 0.068 Uiso 1 1 calc R . . C54 C 0.7441(6) 0.0602(3) -0.0457(5) 0.048(2) Uani 1 1 d . . . H54 H 0.6798 0.0541 -0.0433 0.058 Uiso 1 1 calc R . . C55 C 0.9025(6) 0.0575(2) 0.0130(5) 0.0366(17) Uani 1 1 d . . . C56 C 0.9760(5) 0.0455(2) 0.0789(5) 0.0352(17) Uani 1 1 d . . . C57 C 0.5100(14) 0.2154(9) 0.4004(14) 0.185(10) Uani 1 1 d . . . H57A H 0.5067 0.2279 0.3473 0.277 Uiso 1 1 calc R A 1 H57B H 0.4712 0.2353 0.4283 0.277 Uiso 1 1 calc R A 1 H57C H 0.4864 0.1826 0.3975 0.277 Uiso 1 1 calc R A 1 C58 C 0.2259(17) 0.1248(9) 0.3402(12) 0.169(10) Uani 1 1 d . . . H58A H 0.2174 0.1591 0.3464 0.253 Uiso 1 1 calc R B 1 H58B H 0.2035 0.1077 0.3823 0.253 Uiso 1 1 calc R B 1 H58C H 0.1896 0.1144 0.2895 0.253 Uiso 1 1 calc R B 1 N1 N 0.3202(4) 0.1732(2) -0.0069(4) 0.0393(15) Uani 1 1 d . . . N2 N 0.4852(5) 0.1888(3) 0.0915(5) 0.0519(19) Uani 1 1 d . . . N3 N 0.6147(5) 0.0658(3) 0.0951(5) 0.0513(19) Uani 1 1 d . . . N4 N 0.3211(5) 0.0365(2) -0.0491(5) 0.0485(18) Uani 1 1 d . . . N5 N 0.5145(7) 0.1430(4) -0.1211(6) 0.079(3) Uani 1 1 d . . . N6 N 0.3584(7) 0.1000(4) 0.1925(6) 0.078(3) Uani 1 1 d . . . N7 N 0.8241(6) -0.1848(2) 0.2959(4) 0.0464(18) Uani 1 1 d . . . N8 N 0.9867(6) -0.1875(3) 0.4028(5) 0.057(2) Uani 1 1 d . . . N9 N 0.8332(5) -0.0572(2) 0.2016(4) 0.0376(15) Uani 1 1 d . . . N10 N 0.8136(7) -0.0870(3) 0.4475(5) 0.061(2) Uani 1 1 d . . . N11 N 1.0426(5) -0.1834(3) 0.2054(5) 0.0534(19) Uani 1 1 d . . . N12 N 1.0998(8) -0.0606(4) 0.3796(6) 0.097(4) Uani 1 1 d . . . N13 N 0.8446(5) 0.0487(2) 0.2876(4) 0.0383(15) Uani 1 1 d . . . N14 N 0.8075(4) 0.1128(2) 0.1683(4) 0.0352(14) Uani 1 1 d . . . N15 N 0.9475(4) 0.0274(2) 0.1438(4) 0.0344(14) Uani 1 1 d . . . N16 N 0.8108(5) 0.0495(2) 0.0169(4) 0.0395(15) Uani 1 1 d . . . O1 O 0.6489(5) -0.0017(3) 0.2307(5) 0.080(2) Uani 1 1 d . . . H1B H 0.6598 -0.0296 0.2493 0.095 Uiso 1 1 d R . . H1C H 0.5972 -0.0079 0.1998 0.095 Uiso 1 1 d R . . O2 O 0.2196(16) 0.0170(7) 0.4420(13) 0.141(10) Uani 0.50 1 d P . . O3 O 0.3658(11) 0.0556(6) 0.6476(11) 0.088(5) Uani 0.50 1 d P . . O4 O 0.6156(13) 0.0001(6) 0.7385(13) 0.108(7) Uani 0.50 1 d P . . O5 O 0.260(2) -0.0876(13) 0.5185(15) 0.218(19) Uani 0.50 1 d P . . O6 O 0.7719(8) 0.2051(6) 0.8004(10) 0.093(7) Uani 0.50 1 d P . . O7 O 0.5285(13) 0.1039(5) 0.7322(9) 0.086(5) Uani 0.50 1 d P . . O8 O 0.6887(6) 0.1970(4) -0.0693(6) 0.108(3) Uani 1 1 d . . . H8B H 0.6888 0.2040 -0.1170 0.130 Uiso 1 1 d R . . H8C H 0.6635 0.2170 -0.0424 0.130 Uiso 1 1 d R . . O9 O 0.634(3) 0.1458(12) 0.5433(13) 0.24(2) Uani 0.50 1 d P C 1 O10 O 0.709(2) 0.157(2) 0.3493(19) 0.31(3) Uani 0.50 1 d P D 1 O11 O 0.5262(8) 0.0234(4) 0.8748(7) 0.127(4) Uani 1 1 d . E 1 O12 O 0.7196(15) 0.1302(12) 0.6889(12) 0.180(14) Uani 0.50 1 d P F 1 O13 O 0.6119(11) 0.2163(5) 0.4437(10) 0.180(6) Uani 1 1 d . G 1 H13 H 0.6403 0.1988 0.4156 0.216 Uiso 1 1 d R G 1 O14 O 0.3263(18) 0.1144(9) 0.3438(9) 0.267(12) Uani 1 1 d . H 1 H14 H 0.3477 0.0989 0.3845 0.321 Uiso 1 1 d R H 1 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 Pr1 0.0327(2) 0.0232(2) 0.0448(3) -0.00091(18) 0.00355(18) -0.00160(16) Ru1 0.0294(3) 0.0269(3) 0.0555(4) -0.0077(3) 0.0062(3) -0.0014(2) Ru2 0.0630(5) 0.0287(4) 0.0411(4) 0.0099(3) 0.0106(3) 0.0018(3) K1A 0.037(2) 0.052(3) 0.082(3) -0.001(3) 0.014(2) 0.004(2) K1B 0.0320(17) 0.0393(19) 0.072(2) 0.0131(18) 0.0145(17) 0.0021(15) K1C 0.033(2) 0.034(2) 0.052(3) 0.003(2) 0.011(2) 0.0053(19) C1 0.038(4) 0.047(5) 0.046(5) 0.007(4) 0.010(4) 0.003(4) C2 0.047(5) 0.057(6) 0.052(5) 0.008(5) 0.016(4) 0.013(4) C3 0.057(6) 0.062(6) 0.063(6) 0.018(5) 0.023(5) 0.028(5) C4 0.052(5) 0.040(5) 0.072(6) 0.010(5) 0.028(5) 0.011(4) C5 0.084(8) 0.039(5) 0.092(8) 0.003(5) 0.033(7) 0.019(5) C6 0.094(9) 0.028(5) 0.106(9) -0.014(6) 0.034(8) 0.003(5) C7 0.064(6) 0.037(5) 0.103(9) -0.019(5) 0.027(6) -0.008(5) C8 0.075(8) 0.059(7) 0.139(12) -0.054(8) 0.021(8) -0.019(6) C9 0.058(6) 0.056(7) 0.126(11) -0.042(7) 0.000(6) -0.009(5) C10 0.039(5) 0.054(6) 0.102(8) -0.033(6) -0.001(5) -0.003(4) C11 0.045(5) 0.034(4) 0.071(6) -0.011(4) 0.019(4) -0.003(4) C12 0.052(5) 0.033(4) 0.065(6) -0.001(4) 0.027(4) 0.001(4) C13 0.037(4) 0.023(4) 0.065(6) -0.007(4) 0.006(4) -0.002(3) C14 0.032(4) 0.035(4) 0.060(5) -0.001(4) 0.004(4) 0.004(3) C15 0.039(5) 0.041(5) 0.080(7) -0.003(5) 0.016(5) 0.003(4) C16 0.040(5) 0.051(5) 0.059(6) -0.003(5) 0.008(4) -0.003(4) C17 0.067(6) 0.042(5) 0.057(6) -0.001(4) 0.026(5) -0.006(4) C18 0.080(7) 0.054(6) 0.090(8) -0.012(6) 0.040(6) -0.023(5) C19 0.099(9) 0.041(6) 0.114(10) -0.015(6) 0.061(8) -0.022(6) C20 0.093(8) 0.029(5) 0.102(9) -0.001(5) 0.058(7) -0.005(5) C21 0.133(12) 0.026(5) 0.117(11) 0.010(6) 0.076(10) -0.008(6) C22 0.128(12) 0.042(6) 0.110(11) 0.026(7) 0.075(10) 0.019(7) C23 0.106(9) 0.043(6) 0.090(8) 0.033(6) 0.067(8) 0.030(6) C24 0.134(12) 0.074(9) 0.063(7) 0.041(7) 0.053(8) 0.057(8) C25 0.119(11) 0.074(8) 0.057(7) 0.017(6) 0.014(7) 0.043(8) C26 0.099(9) 0.068(7) 0.056(6) 0.023(6) 0.016(6) 0.029(6) C27 0.089(8) 0.049(6) 0.062(6) 0.025(5) 0.047(6) 0.030(5) C28 0.086(7) 0.033(5) 0.073(7) 0.006(5) 0.049(6) 0.003(5) C29 0.048(5) 0.026(4) 0.040(4) -0.001(4) 0.016(4) -0.002(3) C30 0.081(7) 0.033(5) 0.041(5) 0.004(4) 0.014(5) -0.007(4) C31 0.048(5) 0.033(4) 0.051(5) 0.011(4) 0.010(4) 0.005(4) C32 0.080(7) 0.053(6) 0.053(6) 0.012(5) -0.002(5) -0.007(5) C33 0.070(6) 0.034(5) 0.042(5) -0.005(4) 0.014(4) 0.001(4) C34 0.106(9) 0.050(6) 0.044(5) 0.003(5) 0.004(5) 0.001(6) C35 0.097(8) 0.063(7) 0.040(5) -0.007(5) -0.007(5) 0.002(6) C36 0.062(6) 0.040(5) 0.052(5) -0.010(4) 0.005(4) -0.003(4) C37 0.084(7) 0.045(6) 0.061(6) -0.013(5) -0.005(5) -0.015(5) C38 0.070(6) 0.045(5) 0.064(6) -0.020(5) 0.005(5) -0.011(5) C39 0.050(5) 0.033(4) 0.054(5) -0.013(4) 0.017(4) -0.005(4) C40 0.055(5) 0.030(4) 0.068(6) -0.004(4) 0.019(5) -0.004(4) C41 0.055(5) 0.027(4) 0.065(6) 0.002(4) 0.017(4) 0.003(4) C42 0.044(5) 0.029(4) 0.054(5) 0.002(4) 0.007(4) 0.001(3) C43 0.032(4) 0.027(4) 0.044(4) -0.004(3) 0.009(3) -0.001(3) C44 0.041(4) 0.034(4) 0.044(5) -0.011(4) 0.011(4) 0.004(3) C45 0.038(4) 0.034(4) 0.043(4) 0.000(4) 0.001(3) -0.003(3) C46 0.040(4) 0.033(4) 0.064(6) -0.003(4) 0.002(4) 0.002(3) C47 0.038(4) 0.028(4) 0.084(7) -0.013(4) 0.011(5) -0.007(3) C48 0.046(5) 0.019(4) 0.061(5) -0.009(4) 0.018(4) -0.003(3) C49 0.057(5) 0.023(4) 0.079(7) -0.004(4) 0.035(5) -0.003(4) C50 0.072(6) 0.023(4) 0.059(6) -0.007(4) 0.036(5) -0.009(4) C51 0.072(6) 0.016(4) 0.048(5) -0.007(3) 0.018(4) -0.006(4) C52 0.103(8) 0.032(5) 0.041(5) 0.006(4) 0.015(5) 0.002(5) C53 0.074(7) 0.040(5) 0.050(5) 0.010(4) -0.005(5) 0.008(5) C54 0.050(5) 0.043(5) 0.048(5) 0.006(4) -0.002(4) 0.006(4) C55 0.054(5) 0.014(3) 0.045(4) -0.005(3) 0.017(4) -0.005(3) C56 0.043(4) 0.018(3) 0.047(5) -0.005(3) 0.014(4) -0.001(3) C57 0.115(15) 0.21(3) 0.22(2) -0.01(2) 0.004(16) 0.078(16) C58 0.19(2) 0.18(2) 0.154(19) -0.055(16) 0.087(18) -0.004(18) N1 0.035(3) 0.035(4) 0.051(4) 0.001(3) 0.016(3) 0.001(3) N2 0.040(4) 0.037(4) 0.079(5) -0.019(4) 0.014(4) -0.005(3) N3 0.044(4) 0.036(4) 0.071(5) -0.009(4) 0.004(4) 0.002(3) N4 0.041(4) 0.032(4) 0.068(5) -0.005(4) 0.000(3) -0.002(3) N5 0.064(6) 0.093(7) 0.087(7) 0.013(6) 0.033(5) 0.011(5) N6 0.070(6) 0.097(8) 0.069(6) 0.001(6) 0.017(5) -0.006(5) N7 0.070(5) 0.026(3) 0.051(4) 0.004(3) 0.031(4) 0.003(3) N8 0.086(6) 0.038(4) 0.051(5) 0.019(4) 0.025(4) 0.011(4) N9 0.050(4) 0.025(3) 0.038(4) 0.000(3) 0.011(3) -0.001(3) N10 0.102(7) 0.037(4) 0.050(5) 0.001(4) 0.027(5) -0.005(4) N11 0.056(5) 0.046(4) 0.060(5) 0.022(4) 0.015(4) 0.007(4) N12 0.109(8) 0.083(7) 0.084(7) 0.020(6) -0.020(6) -0.034(7) N13 0.046(4) 0.027(3) 0.044(4) -0.004(3) 0.013(3) -0.001(3) N14 0.032(3) 0.031(3) 0.043(4) 0.000(3) 0.009(3) 0.001(3) N15 0.039(3) 0.023(3) 0.041(4) -0.003(3) 0.007(3) -0.001(3) N16 0.043(4) 0.029(3) 0.046(4) -0.001(3) 0.004(3) 0.000(3) O1 0.060(4) 0.080(5) 0.108(6) 0.000(5) 0.042(4) -0.010(4) O2 0.166(19) 0.125(16) 0.168(19) -0.115(15) 0.126(17) -0.087(15) O3 0.074(10) 0.077(11) 0.121(14) 0.050(10) 0.037(9) -0.003(8) O4 0.088(12) 0.067(11) 0.176(19) -0.049(12) 0.041(12) 0.012(9) O5 0.20(3) 0.29(4) 0.13(2) -0.06(2) -0.039(19) 0.19(3) O6 0.027(6) 0.118(12) 0.147(14) 0.124(11) 0.049(7) 0.052(7) O7 0.137(15) 0.060(9) 0.067(10) 0.010(8) 0.034(10) 0.009(10) O8 0.082(6) 0.118(8) 0.122(8) 0.000(6) 0.013(5) -0.013(6) O9 0.39(5) 0.25(3) 0.083(15) 0.074(19) 0.10(2) 0.25(4) O10 0.12(2) 0.63(9) 0.19(3) -0.13(4) 0.05(2) 0.17(4) O11 0.102(8) 0.108(8) 0.156(10) 0.016(7) -0.011(7) -0.021(6) O12 0.103(16) 0.33(4) 0.085(14) 0.101(19) -0.037(12) -0.06(2) O13 0.168(13) 0.137(12) 0.225(16) 0.037(11) 0.011(12) 0.011(10) O14 0.33(3) 0.37(3) 0.112(11) 0.081(15) 0.072(15) 0.15(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O1 2.463(7) . ? Pr1 N4 2.489(7) 3_655 ? Pr1 N9 2.506(6) . ? Pr1 N3 2.508(7) . ? Pr1 N13 2.614(7) . ? Pr1 N16 2.631(7) . ? Pr1 N14 2.675(6) . ? Pr1 N15 2.676(6) . ? Ru1 C14 1.966(8) . ? Ru1 C13 1.971(8) . ? Ru1 C15 2.042(11) . ? Ru1 C16 2.046(10) . ? Ru1 N1 2.121(6) . ? Ru1 N2 2.133(7) . ? Ru2 C29 1.963(8) . ? Ru2 C32 1.996(11) . ? Ru2 C30 2.041(10) . ? Ru2 C31 2.043(9) . ? Ru2 N7 2.122(8) . ? Ru2 N8 2.124(7) . ? K1A K1A 2.678(15) 3_656 ? K1A O3 2.696(18) . ? K1A O4 3.13(2) . ? K1B K1B 2.695(8) 3_656 ? K1B O2 2.82(3) . ? K1B O5 3.10(4) . ? K1B O3 3.31(2) . ? K1C O2 2.29(2) . ? K1C O4 2.71(2) 3_656 ? K1C K1C 4.417(11) 3_656 ? K1C H14 2.5849 . ? C1 N1 1.331(10) . ? C1 C2 1.394(12) . ? C1 H1 0.9500 . ? C2 C3 1.365(14) . ? C2 H2 0.9500 . ? C3 C4 1.388(14) . ? C3 H3 0.9500 . ? C4 C12 1.408(12) . ? C4 C5 1.455(14) . ? C5 C6 1.327(16) . ? C5 H5 0.9500 . ? C6 C7 1.446(15) . ? C6 H6 0.9500 . ? C7 C8 1.380(17) . ? C7 C11 1.419(12) . ? C8 C9 1.381(17) . ? C8 H8 0.9500 . ? C9 C10 1.391(13) . ? C9 H9 0.9500 . ? C10 N2 1.328(12) . ? C10 H10 0.9500 . ? C11 N2 1.366(11) . ? C11 C12 1.435(13) . ? C12 N1 1.377(10) . ? C13 N3 1.154(10) . ? C14 N4 1.173(10) . ? C15 N5 1.168(13) . ? C16 N6 1.150(12) . ? C17 N7 1.317(12) . ? C17 C18 1.405(13) . ? C17 H17 0.9500 . ? C18 C19 1.389(16) . ? C18 H18 0.9500 . ? C19 C20 1.384(17) . ? C19 H19 0.9500 . ? C20 C28 1.394(14) . ? C20 C21 1.492(16) . ? C21 C22 1.336(19) . ? C21 H21 0.9500 . ? C22 C23 1.395(18) . ? C22 H22 0.9500 . ? C23 C24 1.393(18) . ? C23 C27 1.439(13) . ? C24 C25 1.368(19) . ? C24 H24 0.9500 . ? C25 C26 1.405(15) . ? C25 H25 0.9500 . ? C26 N8 1.333(14) . ? C26 H26 0.9500 . ? C27 N8 1.365(14) . ? C27 C28 1.447(16) . ? C28 N7 1.377(11) . ? C29 N9 1.171(10) . ? C30 N10 1.175(12) . ? C31 N11 1.164(11) . ? C32 N12 1.164(13) . ? C33 N13 1.333(10) . ? C33 C34 1.386(13) . ? C33 H33 0.9500 . ? C34 C35 1.364(15) . ? C34 H34 0.9500 . ? C35 C36 1.411(14) . ? C35 H35 0.9500 . ? C36 C44 1.408(12) . ? C36 C37 1.443(13) . ? C37 C38 1.349(14) . ? C37 H37 0.9500 . ? C38 C39 1.455(13) . ? C38 H38 0.9500 . ? C39 C40 1.392(12) . ? C39 C43 1.415(10) . ? C40 C41 1.369(13) . ? C40 H40 0.9500 . ? C41 C42 1.417(11) . ? C41 H41 0.9500 . ? C42 N14 1.336(10) . ? C42 H42 0.9500 . ? C43 N14 1.361(10) . ? C43 C44 1.446(11) . ? C44 N13 1.372(10) . ? C45 N15 1.333(10) . ? C45 C46 1.397(11) . ? C45 H45 0.9500 . ? C46 C47 1.382(13) . ? C46 H46 0.9500 . ? C47 C48 1.412(13) . ? C47 H47 0.9500 . ? C48 C56 1.399(11) . ? C48 C49 1.460(12) . ? C49 C50 1.314(13) . ? C49 H49 0.9500 . ? C50 C51 1.437(13) . ? C50 H50 0.9500 . ? C51 C52 1.400(13) . ? C51 C55 1.447(11) . ? C52 C53 1.354(14) . ? C52 H52 0.9500 . ? C53 C54 1.406(13) . ? C53 H53 0.9500 . ? C54 N16 1.343(10) . ? C54 H54 0.9500 . ? C55 N16 1.354(10) . ? C55 C56 1.446(11) . ? C56 N15 1.369(10) . ? C57 O13 1.52(2) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 O14 1.46(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? N4 Pr1 2.489(7) 3_655 ? O1 H1B 0.8500 . ? O1 H1C 0.8497 . ? O4 K1C 2.71(2) 3_656 ? O8 H8B 0.8534 . ? O8 H8C 0.8534 . ? O13 H13 0.8494 . ? O14 H14 0.8400 . ? 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 O1 Pr1 N4 87.1(3) . 3_655 ? O1 Pr1 N9 80.1(2) . . ? N4 Pr1 N9 79.0(2) 3_655 . ? O1 Pr1 N3 74.1(3) . . ? N4 Pr1 N3 78.6(2) 3_655 . ? N9 Pr1 N3 146.4(2) . . ? O1 Pr1 N13 76.4(2) . . ? N4 Pr1 N13 155.7(2) 3_655 . ? N9 Pr1 N13 80.7(2) . . ? N3 Pr1 N13 112.9(2) . . ? O1 Pr1 N16 153.8(2) . . ? N4 Pr1 N16 76.9(2) 3_655 . ? N9 Pr1 N16 116.1(2) . . ? N3 Pr1 N16 82.5(2) . . ? N13 Pr1 N16 124.6(2) . . ? O1 Pr1 N14 109.6(2) . . ? N4 Pr1 N14 141.9(2) 3_655 . ? N9 Pr1 N14 136.3(2) . . ? N3 Pr1 N14 73.9(2) . . ? N13 Pr1 N14 61.93(19) . . ? N16 Pr1 N14 73.77(19) . . ? O1 Pr1 N15 144.0(2) . . ? N4 Pr1 N15 112.6(2) 3_655 . ? N9 Pr1 N15 75.0(2) . . ? N3 Pr1 N15 137.3(2) . . ? N13 Pr1 N15 74.34(19) . . ? N16 Pr1 N15 62.1(2) . . ? N14 Pr1 N15 73.77(18) . . ? C14 Ru1 C13 91.1(3) . . ? C14 Ru1 C15 89.0(4) . . ? C13 Ru1 C15 88.1(4) . . ? C14 Ru1 C16 90.5(4) . . ? C13 Ru1 C16 89.6(4) . . ? C15 Ru1 C16 177.6(4) . . ? C14 Ru1 N1 95.3(3) . . ? C13 Ru1 N1 172.7(3) . . ? C15 Ru1 N1 88.4(3) . . ? C16 Ru1 N1 93.9(3) . . ? C14 Ru1 N2 172.9(3) . . ? C13 Ru1 N2 95.4(3) . . ? C15 Ru1 N2 94.1(3) . . ? C16 Ru1 N2 86.7(3) . . ? N1 Ru1 N2 78.4(3) . . ? C29 Ru2 C32 89.5(4) . . ? C29 Ru2 C30 89.4(3) . . ? C32 Ru2 C30 90.7(4) . . ? C29 Ru2 C31 92.3(3) . . ? C32 Ru2 C31 90.7(4) . . ? C30 Ru2 C31 177.8(3) . . ? C29 Ru2 N7 95.5(3) . . ? C32 Ru2 N7 175.0(3) . . ? C30 Ru2 N7 89.7(3) . . ? C31 Ru2 N7 88.7(3) . . ? C29 Ru2 N8 174.4(3) . . ? C32 Ru2 N8 95.9(4) . . ? C30 Ru2 N8 92.2(3) . . ? C31 Ru2 N8 85.9(3) . . ? N7 Ru2 N8 79.0(3) . . ? K1A K1A O3 140.5(6) 3_656 . ? K1A K1A O4 133.5(5) 3_656 . ? O3 K1A O4 85.4(5) . . ? K1B K1B O2 144.8(5) 3_656 . ? K1B K1B O5 147.2(5) 3_656 . ? O2 K1B O5 65.9(6) . . ? K1B K1B O3 102.0(4) 3_656 . ? O2 K1B O3 79.6(4) . . ? O5 K1B O3 94.5(5) . . ? O2 K1C O4 118.6(8) . 3_656 ? O2 K1C K1C 125.7(7) . 3_656 ? O4 K1C K1C 115.4(4) 3_656 3_656 ? O2 K1C H14 82.5 . . ? O4 K1C H14 85.7 3_656 . ? K1C K1C H14 106.9 3_656 . ? N1 C1 C2 122.7(8) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.5(9) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.5(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 116.9(9) . . ? C3 C4 C5 125.5(9) . . ? C12 C4 C5 117.6(9) . . ? C6 C5 C4 122.5(9) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 121.5(10) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C11 117.9(10) . . ? C8 C7 C6 124.2(10) . . ? C11 C7 C6 117.7(10) . . ? C7 C8 C9 119.5(10) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 119.5(11) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 122.8(10) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 121.9(9) . . ? N2 C11 C12 117.4(7) . . ? C7 C11 C12 120.6(9) . . ? N1 C12 C4 123.0(9) . . ? N1 C12 C11 117.0(8) . . ? C4 C12 C11 120.0(8) . . ? N3 C13 Ru1 176.2(7) . . ? N4 C14 Ru1 175.9(7) . . ? N5 C15 Ru1 176.4(9) . . ? N6 C16 Ru1 176.7(8) . . ? N7 C17 C18 123.0(10) . . ? N7 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C19 C18 C17 118.5(12) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C20 C19 C18 120.1(10) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C28 117.3(10) . . ? C19 C20 C21 125.0(11) . . ? C28 C20 C21 117.8(12) . . ? C22 C21 C20 120.7(11) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 122.7(12) . . ? C21 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C24 C23 C22 124.2(11) . . ? C24 C23 C27 116.6(12) . . ? C22 C23 C27 119.2(13) . . ? C25 C24 C23 120.5(10) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.5(13) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N8 C26 C25 122.7(13) . . ? N8 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? N8 C27 C23 122.6(11) . . ? N8 C27 C28 118.2(8) . . ? C23 C27 C28 119.2(11) . . ? N7 C28 C20 123.4(11) . . ? N7 C28 C27 116.3(9) . . ? C20 C28 C27 120.3(10) . . ? N9 C29 Ru2 178.5(7) . . ? N10 C30 Ru2 177.8(9) . . ? N11 C31 Ru2 175.8(7) . . ? N12 C32 Ru2 178.4(10) . . ? N13 C33 C34 124.7(8) . . ? N13 C33 H33 117.7 . . ? C34 C33 H33 117.7 . . ? C35 C34 C33 118.6(9) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C34 C35 C36 120.1(9) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C44 C36 C35 117.1(8) . . ? C44 C36 C37 119.0(9) . . ? C35 C36 C37 123.9(9) . . ? C38 C37 C36 122.2(9) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 120.0(9) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C43 119.1(8) . . ? C40 C39 C38 121.9(8) . . ? C43 C39 C38 118.9(8) . . ? C41 C40 C39 119.0(8) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 118.9(8) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? N14 C42 C41 123.1(8) . . ? N14 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? N14 C43 C39 121.8(7) . . ? N14 C43 C44 117.9(6) . . ? C39 C43 C44 120.1(7) . . ? N13 C44 C36 122.9(8) . . ? N13 C44 C43 117.7(7) . . ? C36 C44 C43 119.3(7) . . ? N15 C45 C46 124.1(8) . . ? N15 C45 H45 118.0 . . ? C46 C45 H45 118.0 . . ? C47 C46 C45 118.7(8) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C46 C47 C48 119.0(8) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C56 C48 C47 118.3(8) . . ? C56 C48 C49 119.1(8) . . ? C47 C48 C49 122.6(8) . . ? C50 C49 C48 121.0(8) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 122.6(8) . . ? C49 C50 H50 118.7 . . ? C51 C50 H50 118.7 . . ? C52 C51 C50 124.9(9) . . ? C52 C51 C55 116.5(8) . . ? C50 C51 C55 118.6(8) . . ? C53 C52 C51 121.3(9) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 118.9(9) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? N16 C54 C53 122.8(9) . . ? N16 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? N16 C55 C51 121.9(8) . . ? N16 C55 C56 119.8(7) . . ? C51 C55 C56 118.3(7) . . ? N15 C56 C48 122.7(7) . . ? N15 C56 C55 116.8(7) . . ? C48 C56 C55 120.4(7) . . ? C1 N1 C12 117.4(7) . . ? C1 N1 Ru1 128.9(6) . . ? C12 N1 Ru1 113.7(6) . . ? C10 N2 C11 118.2(8) . . ? C10 N2 Ru1 128.2(6) . . ? C11 N2 Ru1 113.5(6) . . ? C13 N3 Pr1 177.4(8) . . ? C14 N4 Pr1 164.3(7) . 3_655 ? C17 N7 C28 117.6(8) . . ? C17 N7 Ru2 129.2(6) . . ? C28 N7 Ru2 113.2(7) . . ? C26 N8 C27 118.1(9) . . ? C26 N8 Ru2 129.2(7) . . ? C27 N8 Ru2 112.6(7) . . ? C29 N9 Pr1 159.7(6) . . ? C33 N13 C44 116.6(7) . . ? C33 N13 Pr1 122.0(5) . . ? C44 N13 Pr1 120.4(5) . . ? C42 N14 C43 117.8(7) . . ? C42 N14 Pr1 123.1(5) . . ? C43 N14 Pr1 118.8(5) . . ? C45 N15 C56 117.3(7) . . ? C45 N15 Pr1 122.6(5) . . ? C56 N15 Pr1 120.1(5) . . ? C54 N16 C55 118.5(7) . . ? C54 N16 Pr1 120.5(6) . . ? C55 N16 Pr1 120.7(5) . . ? Pr1 O1 H1B 111.1 . . ? Pr1 O1 H1C 106.5 . . ? H1B O1 H1C 97.4 . . ? K1C O2 K1B 34.6(4) . . ? K1A O3 K1B 29.1(3) . . ? K1C O4 K1A 41.9(4) 3_656 . ? H8B O8 H8C 117.3 . . ? C57 O13 H13 103.3 . . ? C58 O14 H14 109.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.862 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.202 #===END data_imw419m _database_code_depnum_ccdc_archive 'CCDC 636985' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H80 Er2 N22 O20 Ru3' _chemical_formula_weight 2211.31 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 25.548(3) _cell_length_b 26.416(3) _cell_length_c 11.7932(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7958.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4376 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5981 _exptl_absorpt_correction_T_max 0.6395 _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 APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 130827 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7012 _reflns_number_gt 6638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+59.3828P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7012 _refine_ls_number_parameters 547 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Er1 Er 0.639793(9) 0.279301(9) 0.329089(19) 0.01285(10) Uani 1 1 d . . . Ru1 Ru 0.5000 0.13365(2) 0.2500 0.01253(14) Uani 1 2 d S . . Ru2 Ru 0.755488(16) 0.381519(15) 0.00726(3) 0.01198(11) Uani 1 1 d . . . C1 C 0.5422(2) 0.2858(2) 0.1261(5) 0.0195(11) Uani 1 1 d . . . H1 H 0.5433 0.2501 0.1343 0.023 Uiso 1 1 calc R . . C2 C 0.5125(2) 0.3064(2) 0.0377(5) 0.0238(12) Uani 1 1 d . . . H2 H 0.4935 0.2848 -0.0119 0.029 Uiso 1 1 calc R . . C3 C 0.5110(2) 0.3574(2) 0.0230(5) 0.0251(13) Uani 1 1 d . . . H3 H 0.4921 0.3716 -0.0386 0.030 Uiso 1 1 calc R . . C4 C 0.5376(2) 0.3891(2) 0.0996(5) 0.0213(12) Uani 1 1 d . . . C5 C 0.5357(2) 0.4430(2) 0.0935(5) 0.0261(13) Uani 1 1 d . . . H5 H 0.5195 0.4586 0.0300 0.031 Uiso 1 1 calc R . . C6 C 0.5562(2) 0.4723(2) 0.1754(5) 0.0270(14) Uani 1 1 d . . . H6 H 0.5538 0.5081 0.1703 0.032 Uiso 1 1 calc R . . C7 C 0.5820(2) 0.4492(2) 0.2710(5) 0.0222(12) Uani 1 1 d . . . C8 C 0.5999(2) 0.4776(2) 0.3639(5) 0.0257(13) Uani 1 1 d . . . H8 H 0.5951 0.5133 0.3659 0.031 Uiso 1 1 calc R . . C9 C 0.6242(2) 0.4533(2) 0.4513(5) 0.0254(13) Uani 1 1 d . . . H9 H 0.6355 0.4717 0.5161 0.030 Uiso 1 1 calc R . . C10 C 0.6323(2) 0.4010(2) 0.4445(5) 0.0224(12) Uani 1 1 d . . . H10 H 0.6513 0.3850 0.5038 0.027 Uiso 1 1 calc R . . C11 C 0.5887(2) 0.3964(2) 0.2754(5) 0.0175(11) Uani 1 1 d . . . C12 C 0.5650(2) 0.3652(2) 0.1884(5) 0.0187(11) Uani 1 1 d . . . C13 C 0.7114(2) 0.4641(2) 0.1728(4) 0.0178(11) Uani 1 1 d . . . H13 H 0.6964 0.4370 0.2149 0.021 Uiso 1 1 calc R . . C14 C 0.7045(2) 0.5135(2) 0.2113(5) 0.0190(11) Uani 1 1 d . . . H14 H 0.6852 0.5196 0.2788 0.023 Uiso 1 1 calc R . . C15 C 0.7254(2) 0.5533(2) 0.1526(5) 0.0204(12) Uani 1 1 d . . . H15 H 0.7206 0.5870 0.1788 0.024 Uiso 1 1 calc R . . C16 C 0.7542(2) 0.5439(2) 0.0530(4) 0.0163(11) Uani 1 1 d . . . C17 C 0.7796(2) 0.5827(2) -0.0119(5) 0.0220(12) Uani 1 1 d . . . H17 H 0.7767 0.6170 0.0114 0.026 Uiso 1 1 calc R . . C18 C 0.8075(2) 0.5712(2) -0.1055(5) 0.0212(12) Uani 1 1 d . . . H18 H 0.8236 0.5977 -0.1476 0.025 Uiso 1 1 calc R . . C19 C 0.8133(2) 0.5198(2) -0.1424(4) 0.0164(11) Uani 1 1 d . . . C20 C 0.8431(2) 0.5059(2) -0.2376(4) 0.0182(11) Uani 1 1 d . . . H20 H 0.8592 0.5311 -0.2833 0.022 Uiso 1 1 calc R . . C21 C 0.8487(2) 0.4557(2) -0.2638(4) 0.0178(11) Uani 1 1 d . . . H21 H 0.8687 0.4458 -0.3280 0.021 Uiso 1 1 calc R . . C22 C 0.8247(2) 0.4191(2) -0.1952(4) 0.0158(11) Uani 1 1 d . . . H22 H 0.8298 0.3844 -0.2133 0.019 Uiso 1 1 calc R . . C23 C 0.7899(2) 0.4806(2) -0.0797(4) 0.0142(10) Uani 1 1 d . . . C24 C 0.75958(19) 0.4929(2) 0.0198(4) 0.0139(10) Uani 1 1 d . . . C25 C 0.6867(2) 0.3838(2) -0.0827(5) 0.0237(13) Uani 1 1 d . . . C26 C 0.8226(2) 0.37602(19) 0.0991(4) 0.0166(11) Uani 1 1 d . . . C27 C 0.7819(2) 0.3205(2) -0.0722(4) 0.0157(11) Uani 1 1 d . . . C28 C 0.7157(2) 0.34325(19) 0.1224(4) 0.0156(11) Uani 1 1 d . . . C29 C 0.5626(2) 0.0724(2) 0.4318(4) 0.0173(11) Uani 1 1 d . . . H29 H 0.5738 0.1041 0.4611 0.021 Uiso 1 1 calc R . . C30 C 0.5776(2) 0.0279(2) 0.4874(5) 0.0211(12) Uani 1 1 d . . . H30 H 0.5984 0.0300 0.5540 0.025 Uiso 1 1 calc R . . C31 C 0.5628(2) -0.0185(2) 0.4472(5) 0.0212(12) Uani 1 1 d . . . H31 H 0.5732 -0.0486 0.4853 0.025 Uiso 1 1 calc R . . C32 C 0.5318(2) -0.0211(2) 0.3483(5) 0.0185(11) Uani 1 1 d . . . C33 C 0.5152(2) -0.0678(2) 0.2969(5) 0.0235(12) Uani 1 1 d . . . H33A H 0.5258 -0.0991 0.3294 0.028 Uiso 1 1 calc R . . C34 C 0.5169(2) 0.02503(19) 0.2981(5) 0.0144(10) Uani 1 1 d . . . C35 C 0.5430(2) 0.1865(2) 0.3228(4) 0.0136(11) Uani 1 1 d . . . C36 C 0.5559(2) 0.13623(19) 0.1264(5) 0.0173(11) Uani 1 1 d . . . N1 N 0.56889(18) 0.31421(17) 0.1992(4) 0.0181(10) Uani 1 1 d . . . N2 N 0.61499(18) 0.37243(18) 0.3599(4) 0.0185(10) Uani 1 1 d . . . N3 N 0.73846(17) 0.45334(17) 0.0783(4) 0.0147(9) Uani 1 1 d . . . N4 N 0.79509(17) 0.43066(16) -0.1062(4) 0.0145(9) Uani 1 1 d . . . N5 N 0.86149(19) 0.37104(19) 0.1498(4) 0.0203(10) Uani 1 1 d . . . N6 N 0.6460(2) 0.3835(2) -0.1257(6) 0.0446(17) Uani 1 1 d . . . N8 N 0.69040(18) 0.32313(18) 0.1906(4) 0.0173(10) Uani 1 1 d . . . N9 N 0.53270(17) 0.07133(17) 0.3379(3) 0.0143(9) Uani 1 1 d . . . N10 N 0.57201(19) 0.21828(17) 0.3519(4) 0.0192(10) Uani 1 1 d . . . N11 N 0.80378(19) 0.28852(18) -0.1206(4) 0.0201(10) Uani 1 1 d . . . N12 N 0.58796(19) 0.14149(18) 0.0572(4) 0.0216(10) Uani 1 1 d . . . O1W O 0.61531(17) 0.28134(15) 0.5206(3) 0.0244(9) Uani 1 1 d . . . H1B H 0.6077 0.3125 0.5281 0.029 Uiso 1 1 d R . . H1C H 0.6011 0.2573 0.5573 0.029 Uiso 1 1 d R . . O2W O 0.71293(14) 0.31438(14) 0.4246(3) 0.0175(8) Uani 1 1 d . . . H2B H 0.7395 0.3114 0.3818 0.021 Uiso 1 1 d R . . H2C H 0.7229 0.3009 0.4864 0.021 Uiso 1 1 d R . . O3W O 0.64671(15) 0.22845(15) 0.1580(3) 0.0176(8) Uani 1 1 d . . . H3B H 0.6307 0.2002 0.1592 0.021 Uiso 1 1 d R . . H3C H 0.6451 0.2510 0.1068 0.021 Uiso 1 1 d R . . O4W O 0.56227(15) 0.20641(15) 0.6439(3) 0.0214(8) Uani 1 1 d . . . H4B H 0.5801 0.1807 0.6246 0.026 Uiso 1 1 d R . . H4C H 0.5567 0.2081 0.7149 0.026 Uiso 1 1 d R . . O5W O 0.5678(7) 0.3645(5) 0.7018(13) 0.086(4) Uani 0.50 1 d PU A 1 O5W' O 0.5462(6) 0.4060(5) 0.7435(12) 0.082(4) Uani 0.50 1 d PU B 2 O6W O 0.45213(16) 0.20708(16) 0.6195(4) 0.0270(9) Uani 1 1 d . . . H6B H 0.4852 0.2107 0.6229 0.032 Uiso 1 1 d R . . H6C H 0.4415 0.1822 0.5799 0.032 Uiso 1 1 d R . . O7W O 0.36507(15) 0.26804(16) 0.5596(3) 0.0225(9) Uani 1 1 d . . . H7B H 0.3593 0.2993 0.5673 0.027 Uiso 1 1 d R . . H7C H 0.3930 0.2547 0.5852 0.027 Uiso 1 1 d R . . O8W O 0.69826(16) 0.20681(16) 0.7989(4) 0.0260(9) Uani 1 1 d . . . H8B H 0.6811 0.1857 0.7591 0.031 Uiso 1 1 d R . . H8C H 0.6760 0.2249 0.8337 0.031 Uiso 1 1 d R . . O9W O 0.7397(3) 0.2774(2) 0.6374(5) 0.0567(16) Uani 1 1 d . . . H9C H 0.7707 0.2891 0.6391 0.068 Uiso 1 1 d R . . H9BB H 0.7024 0.2966 0.6666 0.068 Uiso 1 1 d R . . O10W O 0.6588(3) 0.3357(3) 0.6722(5) 0.0661(18) Uani 1 1 d . . . H10B H 0.6868 0.3528 0.6652 0.079 Uiso 1 1 d R . . H10C H 0.6492 0.3493 0.7341 0.079 Uiso 1 1 d 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 Er1 0.01452(15) 0.01591(15) 0.00812(14) 0.00137(8) 0.00037(8) -0.00131(9) Ru1 0.0137(3) 0.0161(3) 0.0078(3) 0.000 -0.0006(2) 0.000 Ru2 0.0145(2) 0.0145(2) 0.0069(2) 0.00008(15) 0.00110(15) -0.00058(16) C1 0.018(3) 0.024(3) 0.016(3) 0.001(2) 0.001(2) -0.005(2) C2 0.018(3) 0.039(3) 0.014(3) -0.001(2) 0.000(2) 0.000(2) C3 0.019(3) 0.039(4) 0.018(3) 0.004(3) -0.001(2) 0.002(3) C4 0.016(3) 0.030(3) 0.018(3) 0.006(2) 0.005(2) 0.002(2) C5 0.023(3) 0.034(3) 0.021(3) 0.009(3) 0.002(2) 0.010(3) C6 0.027(3) 0.024(3) 0.030(3) 0.009(2) 0.010(3) 0.009(3) C7 0.018(3) 0.030(3) 0.019(3) 0.003(2) 0.008(2) 0.002(2) C8 0.024(3) 0.022(3) 0.031(3) -0.002(3) 0.009(3) 0.004(2) C9 0.022(3) 0.029(3) 0.026(3) -0.007(3) 0.001(2) 0.000(2) C10 0.025(3) 0.022(3) 0.021(3) -0.002(2) 0.000(2) 0.001(2) C11 0.014(2) 0.022(3) 0.017(3) 0.005(2) 0.003(2) 0.002(2) C12 0.017(3) 0.025(3) 0.014(3) 0.002(2) 0.006(2) -0.001(2) C13 0.017(3) 0.028(3) 0.008(2) 0.001(2) 0.002(2) 0.000(2) C14 0.019(3) 0.025(3) 0.013(3) -0.005(2) 0.002(2) 0.004(2) C15 0.020(3) 0.020(3) 0.021(3) -0.007(2) -0.005(2) 0.006(2) C16 0.021(3) 0.017(3) 0.011(2) 0.002(2) -0.002(2) 0.007(2) C17 0.028(3) 0.017(3) 0.021(3) -0.002(2) -0.002(2) 0.006(2) C18 0.030(3) 0.019(3) 0.015(3) 0.007(2) -0.001(2) -0.003(2) C19 0.021(3) 0.019(3) 0.009(2) 0.004(2) -0.003(2) -0.001(2) C20 0.022(3) 0.024(3) 0.008(2) 0.006(2) -0.001(2) -0.004(2) C21 0.017(3) 0.026(3) 0.010(2) 0.002(2) 0.001(2) 0.000(2) C22 0.017(3) 0.019(3) 0.011(2) -0.001(2) 0.000(2) 0.000(2) C23 0.015(2) 0.019(3) 0.009(2) 0.0018(19) -0.002(2) -0.001(2) C24 0.014(2) 0.019(3) 0.009(2) 0.001(2) -0.0023(19) 0.004(2) C25 0.030(3) 0.020(3) 0.021(3) 0.007(2) -0.001(3) -0.007(2) C26 0.024(3) 0.016(3) 0.010(2) -0.001(2) 0.007(2) -0.002(2) C27 0.020(3) 0.018(3) 0.010(2) 0.004(2) 0.000(2) -0.006(2) C28 0.018(3) 0.015(3) 0.013(3) -0.003(2) -0.005(2) 0.003(2) C29 0.017(3) 0.023(3) 0.012(2) -0.001(2) 0.001(2) -0.001(2) C30 0.019(3) 0.032(3) 0.012(3) 0.007(2) -0.002(2) 0.001(2) C31 0.021(3) 0.026(3) 0.016(3) 0.009(2) 0.003(2) 0.003(2) C32 0.015(3) 0.022(3) 0.018(3) 0.002(2) 0.004(2) 0.001(2) C33 0.026(3) 0.020(3) 0.025(3) 0.004(2) 0.005(2) 0.001(2) C34 0.014(2) 0.013(2) 0.016(3) 0.000(2) 0.004(2) 0.001(2) C35 0.014(2) 0.017(3) 0.010(2) 0.0022(19) 0.0009(19) 0.001(2) C36 0.022(3) 0.013(3) 0.016(3) -0.001(2) -0.007(2) 0.002(2) N1 0.017(2) 0.024(2) 0.014(2) 0.0043(19) 0.0012(18) -0.0033(19) N2 0.018(2) 0.025(2) 0.013(2) 0.0008(19) 0.0010(19) 0.0008(19) N3 0.016(2) 0.019(2) 0.010(2) -0.0017(17) -0.0003(17) -0.0008(18) N4 0.016(2) 0.018(2) 0.009(2) 0.0000(17) -0.0035(17) -0.0004(18) N5 0.025(3) 0.022(3) 0.014(2) -0.0015(19) -0.001(2) -0.0004(19) N6 0.036(3) 0.047(4) 0.050(4) 0.022(3) -0.026(3) -0.017(3) N8 0.018(2) 0.023(2) 0.010(2) 0.0013(18) 0.0015(18) -0.0004(19) N9 0.015(2) 0.018(2) 0.010(2) 0.0018(16) -0.0005(17) 0.0021(18) N10 0.025(3) 0.025(3) 0.009(2) 0.0038(18) 0.0009(19) 0.004(2) N11 0.023(2) 0.023(2) 0.015(2) 0.0002(19) 0.0026(19) -0.003(2) N12 0.024(3) 0.024(2) 0.017(2) -0.0015(19) 0.005(2) 0.001(2) O1W 0.032(2) 0.023(2) 0.018(2) 0.0028(16) 0.0087(18) -0.0009(17) O2W 0.0168(18) 0.023(2) 0.0123(18) 0.0029(15) 0.0017(15) -0.0006(15) O3W 0.023(2) 0.0153(19) 0.015(2) 0.0024(15) 0.0001(15) -0.0048(15) O4W 0.023(2) 0.023(2) 0.0174(19) 0.0026(16) 0.0043(16) 0.0050(17) O5W 0.117(9) 0.066(6) 0.075(7) 0.023(6) -0.058(7) -0.022(6) O5W' 0.114(9) 0.057(6) 0.073(7) 0.028(6) -0.058(7) -0.025(6) O6W 0.023(2) 0.034(2) 0.023(2) -0.0029(18) -0.0016(17) 0.0005(18) O7W 0.026(2) 0.025(2) 0.016(2) 0.0000(17) 0.0003(16) 0.0037(17) O8W 0.024(2) 0.028(2) 0.026(2) -0.0082(18) 0.0023(18) 0.0013(18) O9W 0.062(4) 0.072(4) 0.036(3) 0.010(3) -0.014(3) -0.013(3) O10W 0.077(5) 0.060(4) 0.061(4) -0.011(3) 0.005(3) -0.014(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 Er1 O1W 2.344(4) . ? Er1 O2W 2.370(4) . ? Er1 N11 2.375(5) 2_655 ? Er1 N10 2.381(5) . ? Er1 N8 2.383(4) . ? Er1 O3W 2.430(4) . ? Er1 N1 2.545(5) . ? Er1 N2 2.566(5) . ? Ru1 C35 1.974(5) . ? Ru1 C35 1.974(5) 3_655 ? Ru1 C36 2.041(6) 3_655 ? Ru1 C36 2.041(6) . ? Ru1 N9 2.117(4) 3_655 ? Ru1 N9 2.117(4) . ? Ru2 C28 1.974(5) . ? Ru2 C27 1.982(5) . ? Ru2 C26 2.034(6) . ? Ru2 C25 2.053(6) . ? Ru2 N3 2.119(4) . ? Ru2 N4 2.121(4) . ? C1 N1 1.331(7) . ? C1 C2 1.399(8) . ? C1 H1 0.9500 . ? C2 C3 1.360(9) . ? C2 H2 0.9500 . ? C3 C4 1.406(9) . ? C3 H3 0.9500 . ? C4 C12 1.409(8) . ? C4 C5 1.428(8) . ? C5 C6 1.344(9) . ? C5 H5 0.9500 . ? C6 C7 1.441(8) . ? C6 H6 0.9500 . ? C7 C8 1.404(9) . ? C7 C11 1.406(8) . ? C8 C9 1.364(9) . ? C8 H8 0.9500 . ? C9 C10 1.401(8) . ? C9 H9 0.9500 . ? C10 N2 1.327(8) . ? C10 H10 0.9500 . ? C11 N2 1.358(7) . ? C11 C12 1.450(8) . ? C12 N1 1.355(7) . ? C13 N3 1.342(7) . ? C13 C14 1.395(8) . ? C13 H13 0.9500 . ? C14 C15 1.366(8) . ? C14 H14 0.9500 . ? C15 C16 1.408(8) . ? C15 H15 0.9500 . ? C16 C24 1.409(7) . ? C16 C17 1.434(8) . ? C17 C18 1.349(8) . ? C17 H17 0.9500 . ? C18 C19 1.434(8) . ? C18 H18 0.9500 . ? C19 C20 1.405(8) . ? C19 C23 1.406(7) . ? C20 C21 1.368(8) . ? C20 H20 0.9500 . ? C21 C22 1.403(8) . ? C21 H21 0.9500 . ? C22 N4 1.330(7) . ? C22 H22 0.9500 . ? C23 N4 1.363(7) . ? C23 C24 1.442(7) . ? C24 N3 1.363(7) . ? C25 N6 1.159(8) . ? C26 N5 1.166(7) . ? C27 N11 1.164(7) . ? C28 N8 1.162(7) . ? C29 N9 1.345(7) . ? C29 C30 1.399(8) . ? C29 H29 0.9500 . ? C30 C31 1.369(8) . ? C30 H30 0.9500 . ? C31 C32 1.411(8) . ? C31 H31 0.9500 . ? C32 C34 1.407(7) . ? C32 C33 1.440(8) . ? C33 C33 1.352(12) 3_655 ? C33 H33A 0.9500 . ? C34 N9 1.371(7) . ? C34 C34 1.426(11) 3_655 ? C35 N10 1.170(7) . ? C36 N12 1.165(7) . ? N11 Er1 2.375(5) 2_654 ? O1W H1B 0.8500 . ? O1W H1C 0.8501 . ? O2W H2B 0.8501 . ? O2W H2C 0.8501 . ? O3W H3B 0.8500 . ? O3W H3C 0.8502 . ? O4W H4B 0.8501 . ? O4W H4C 0.8500 . ? O6W H6B 0.8499 . ? O6W H6C 0.8500 . ? O7W H7B 0.8447 . ? O7W H7C 0.8506 . ? O8W H8B 0.8500 . ? O8W H8C 0.8500 . ? O9W H9C 0.8499 . ? O9W H9BB 1.1324 . ? O10W H10B 0.8498 . ? O10W H10C 0.8500 . ? 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 O1W Er1 O2W 75.13(14) . . ? O1W Er1 N11 86.48(15) . 2_655 ? O2W Er1 N11 72.40(14) . 2_655 ? O1W Er1 N10 73.31(15) . . ? O2W Er1 N10 141.66(14) . . ? N11 Er1 N10 84.41(16) 2_655 . ? O1W Er1 N8 142.55(15) . . ? O2W Er1 N8 73.03(14) . . ? N11 Er1 N8 102.03(16) 2_655 . ? N10 Er1 N8 143.20(15) . . ? O1W Er1 O3W 146.30(14) . . ? O2W Er1 O3W 123.59(13) . . ? N11 Er1 O3W 75.30(15) 2_655 . ? N10 Er1 O3W 76.84(14) . . ? N8 Er1 O3W 70.13(14) . . ? O1W Er1 N1 112.43(15) . . ? O2W Er1 N1 134.86(14) . . ? N11 Er1 N1 148.84(15) 2_655 . ? N10 Er1 N1 78.21(15) . . ? N8 Er1 N1 78.32(15) . . ? O3W Er1 N1 75.67(14) . . ? O1W Er1 N2 77.04(14) . . ? O2W Er1 N2 75.68(14) . . ? N11 Er1 N2 146.90(15) 2_655 . ? N10 Er1 N2 116.97(15) . . ? N8 Er1 N2 76.41(15) . . ? O3W Er1 N2 131.70(14) . . ? N1 Er1 N2 64.02(15) . . ? C35 Ru1 C35 89.9(3) . 3_655 ? C35 Ru1 C36 93.2(2) . 3_655 ? C35 Ru1 C36 84.1(2) 3_655 3_655 ? C35 Ru1 C36 84.1(2) . . ? C35 Ru1 C36 93.2(2) 3_655 . ? C36 Ru1 C36 176.2(3) 3_655 . ? C35 Ru1 N9 169.38(19) . 3_655 ? C35 Ru1 N9 96.75(19) 3_655 3_655 ? C36 Ru1 N9 95.73(18) 3_655 3_655 ? C36 Ru1 N9 87.26(18) . 3_655 ? C35 Ru1 N9 96.75(19) . . ? C35 Ru1 N9 169.38(19) 3_655 . ? C36 Ru1 N9 87.26(18) 3_655 . ? C36 Ru1 N9 95.73(18) . . ? N9 Ru1 N9 77.9(2) 3_655 . ? C28 Ru2 C27 94.8(2) . . ? C28 Ru2 C26 91.8(2) . . ? C27 Ru2 C26 84.7(2) . . ? C28 Ru2 C25 86.0(2) . . ? C27 Ru2 C25 94.0(2) . . ? C26 Ru2 C25 177.3(2) . . ? C28 Ru2 N3 94.66(19) . . ? C27 Ru2 N3 169.88(19) . . ? C26 Ru2 N3 91.52(18) . . ? C25 Ru2 N3 90.1(2) . . ? C28 Ru2 N4 173.07(19) . . ? C27 Ru2 N4 92.11(19) . . ? C26 Ru2 N4 88.70(18) . . ? C25 Ru2 N4 93.67(19) . . ? N3 Ru2 N4 78.41(16) . . ? N1 C1 C2 122.8(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.6(6) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C12 116.8(5) . . ? C3 C4 C5 123.0(5) . . ? C12 C4 C5 120.1(5) . . ? C6 C5 C4 121.6(5) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C11 117.5(5) . . ? C8 C7 C6 122.2(6) . . ? C11 C7 C6 120.3(5) . . ? C9 C8 C7 119.1(6) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 119.3(6) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 123.7(6) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N2 C11 C7 123.4(5) . . ? N2 C11 C12 117.3(5) . . ? C7 C11 C12 119.2(5) . . ? N1 C12 C4 123.5(5) . . ? N1 C12 C11 118.0(5) . . ? C4 C12 C11 118.5(5) . . ? N3 C13 C14 122.2(5) . . ? N3 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 120.4(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.4(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C24 116.8(5) . . ? C15 C16 C17 123.7(5) . . ? C24 C16 C17 119.4(5) . . ? C18 C17 C16 121.1(5) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C23 117.3(5) . . ? C20 C19 C18 123.2(5) . . ? C23 C19 C18 119.5(5) . . ? C21 C20 C19 119.4(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 119.5(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? N4 C22 C21 123.1(5) . . ? N4 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? N4 C23 C19 123.4(5) . . ? N4 C23 C24 117.1(5) . . ? C19 C23 C24 119.5(5) . . ? N3 C24 C16 123.6(5) . . ? N3 C24 C23 116.9(5) . . ? C16 C24 C23 119.5(5) . . ? N6 C25 Ru2 174.4(6) . . ? N5 C26 Ru2 177.3(5) . . ? N11 C27 Ru2 170.5(5) . . ? N8 C28 Ru2 176.0(5) . . ? N9 C29 C30 121.6(5) . . ? N9 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C31 C30 C29 121.0(5) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.0(5) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C34 C32 C31 117.3(5) . . ? C34 C32 C33 119.1(5) . . ? C31 C32 C33 123.7(5) . . ? C33 C33 C32 120.9(3) 3_655 . ? C33 C33 H33A 119.5 3_655 . ? C32 C33 H33A 119.5 . . ? N9 C34 C32 123.3(5) . . ? N9 C34 C34 116.8(3) . 3_655 ? C32 C34 C34 119.9(3) . 3_655 ? N10 C35 Ru1 170.8(4) . . ? N12 C36 Ru1 175.0(5) . . ? C1 N1 C12 117.5(5) . . ? C1 N1 Er1 123.4(4) . . ? C12 N1 Er1 117.9(4) . . ? C10 N2 C11 116.8(5) . . ? C10 N2 Er1 124.7(4) . . ? C11 N2 Er1 117.8(4) . . ? C13 N3 C24 117.6(5) . . ? C13 N3 Ru2 128.5(4) . . ? C24 N3 Ru2 113.9(3) . . ? C22 N4 C23 117.3(4) . . ? C22 N4 Ru2 129.0(4) . . ? C23 N4 Ru2 113.7(3) . . ? C28 N8 Er1 178.1(4) . . ? C29 N9 C34 117.9(5) . . ? C29 N9 Ru1 127.6(4) . . ? C34 N9 Ru1 114.2(3) . . ? C35 N10 Er1 155.8(4) . . ? C27 N11 Er1 164.3(4) . 2_654 ? Er1 O1W H1B 100.6 . . ? Er1 O1W H1C 125.9 . . ? H1B O1W H1C 125.0 . . ? Er1 O2W H2B 108.1 . . ? Er1 O2W H2C 118.6 . . ? H2B O2W H2C 103.4 . . ? Er1 O3W H3B 115.9 . . ? Er1 O3W H3C 101.4 . . ? H3B O3W H3C 127.2 . . ? H4B O4W H4C 113.3 . . ? H6B O6W H6C 115.5 . . ? H7B O7W H7C 120.9 . . ? H8B O8W H8C 106.8 . . ? H9C O9W H9BB 127.8 . . ? H10B O10W H10C 95.9 . . ? 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 O1W H1B N2 0.85 2.55 3.063(6) 120.3 . O1W H1C O4W 0.85 1.96 2.805(6) 174.2 . O2W H2B O8W 0.85 1.93 2.768(6) 169.5 2_654 O2W H2C O9W 0.85 1.93 2.778(7) 171.9 . O3W H3B N12 0.85 2.25 2.991(6) 146.1 . O3W H3C O7W 0.85 2.03 2.788(5) 148.1 3_655 O4W H4B N5 0.85 2.04 2.826(6) 152.5 2_655 O4W H4C O6W 0.85 1.97 2.815(6) 175.2 3_656 O6W H6B O4W 0.85 1.99 2.829(6) 169.4 . O6W H6C N12 0.85 2.08 2.896(6) 160.2 3_655 O7W H7B N6 0.84 2.33 3.161(7) 167.2 3_655 O7W H7C O6W 0.85 2.01 2.835(6) 164.2 . O8W H8B N5 0.85 2.26 3.106(6) 177.7 2_655 O8W H8C O7W 0.85 1.99 2.832(6) 168.1 3_656 O9W H9C O3W 0.85 2.17 2.916(8) 146.1 2_655 O10W H10B O9W 0.85 2.43 2.610(10) 92.7 . O10W H10C N6 0.85 1.89 2.717(10) 165.5 1_556 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.730 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.157 #===END data_imw513m _database_code_depnum_ccdc_archive 'CCDC 636986' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H80 N22 Nd2 O20 Ru3' _chemical_formula_weight 2165.27 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 25.497(3) _cell_length_b 26.744(2) _cell_length_c 11.8709(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8094.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7025 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.54 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4312 _exptl_absorpt_coefficient_mu 1.892 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6195 _exptl_absorpt_correction_T_max 0.8482 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50490 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6852 _reflns_number_gt 5912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+37.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6852 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.639335(11) 0.277782(9) 1.33343(2) 0.01734(9) Uani 1 1 d . . . Ru2 Ru 0.5000 0.131274(18) 1.2500 0.01333(13) Uani 1 2 d S . . Ru3 Ru 0.754350(16) 0.383092(13) 1.00703(3) 0.01465(11) Uani 1 1 d . . . C1 C 0.71097(19) 0.46455(18) 1.1711(4) 0.0190(11) Uani 1 1 d . . . H1A H 0.6963 0.4379 1.2136 0.023 Uiso 1 1 calc R . . C2 C 0.7037(2) 0.51377(18) 1.2089(4) 0.0220(11) Uani 1 1 d . . . H2 H 0.6843 0.5199 1.2758 0.026 Uiso 1 1 calc R . . C3 C 0.7243(2) 0.55295(18) 1.1500(4) 0.0235(12) Uani 1 1 d . . . H3A H 0.7194 0.5863 1.1755 0.028 Uiso 1 1 calc R . . C4 C 0.7526(2) 0.54340(17) 1.0516(4) 0.0180(11) Uani 1 1 d . . . C5 C 0.7774(2) 0.58151(18) 0.9858(4) 0.0254(12) Uani 1 1 d . . . H5 H 0.7740 0.6155 1.0082 0.030 Uiso 1 1 calc R . . C6 C 0.8054(2) 0.57042(17) 0.8928(4) 0.0235(12) Uani 1 1 d . . . H6A H 0.8210 0.5965 0.8501 0.028 Uiso 1 1 calc R . . C7 C 0.8118(2) 0.51950(17) 0.8577(4) 0.0174(11) Uani 1 1 d . . . C8 C 0.8413(2) 0.50558(17) 0.7621(4) 0.0198(11) Uani 1 1 d . . . H8A H 0.8569 0.5304 0.7157 0.024 Uiso 1 1 calc R . . C9 C 0.8470(2) 0.45609(17) 0.7371(4) 0.0185(11) Uani 1 1 d . . . H9A H 0.8674 0.4462 0.6739 0.022 Uiso 1 1 calc R . . C10 C 0.82284(19) 0.41995(17) 0.8044(4) 0.0168(11) Uani 1 1 d . . . H10A H 0.8274 0.3857 0.7857 0.020 Uiso 1 1 calc R . . C11 C 0.78845(19) 0.48114(16) 0.9204(4) 0.0149(10) Uani 1 1 d . . . C12 C 0.75870(19) 0.49313(16) 1.0186(4) 0.0147(10) Uani 1 1 d . . . C13 C 0.7159(2) 0.34461(17) 1.1226(4) 0.0183(11) Uani 1 1 d . . . C14 C 0.6847(2) 0.38589(17) 0.9201(4) 0.0228(12) Uani 1 1 d . . . C15 C 0.8218(2) 0.37722(16) 1.0972(4) 0.0173(11) Uani 1 1 d . . . C16 C 0.7781(2) 0.32307(17) 0.9257(4) 0.0197(11) Uani 1 1 d . . . C17 C 0.6297(2) 0.40146(19) 1.4448(5) 0.0269(12) Uani 1 1 d . . . H17A H 0.6477 0.3858 1.5053 0.032 Uiso 1 1 calc R . . C18 C 0.6226(2) 0.4535(2) 1.4487(5) 0.0302(13) Uani 1 1 d . . . H18A H 0.6344 0.4722 1.5120 0.036 Uiso 1 1 calc R . . C19 C 0.5987(2) 0.4770(2) 1.3609(5) 0.0290(13) Uani 1 1 d . . . H19A H 0.5941 0.5122 1.3619 0.035 Uiso 1 1 calc R . . C20 C 0.5811(2) 0.44892(19) 1.2694(4) 0.0251(12) Uani 1 1 d . . . C21 C 0.5561(2) 0.4711(2) 1.1734(5) 0.0328(14) Uani 1 1 d . . . H21A H 0.5539 0.5065 1.1673 0.039 Uiso 1 1 calc R . . C22 C 0.5356(2) 0.4421(2) 1.0916(5) 0.0322(14) Uani 1 1 d . . . H22A H 0.5199 0.4575 1.0278 0.039 Uiso 1 1 calc R . . C23 C 0.5369(2) 0.3889(2) 1.0984(4) 0.0266(12) Uani 1 1 d . . . C24 C 0.5106(2) 0.3580(2) 1.0223(4) 0.0327(14) Uani 1 1 d . . . H24A H 0.4922 0.3721 0.9604 0.039 Uiso 1 1 calc R . . C25 C 0.5114(2) 0.3078(2) 1.0375(4) 0.0330(14) Uani 1 1 d . . . H25A H 0.4924 0.2866 0.9880 0.040 Uiso 1 1 calc R . . C26 C 0.5404(2) 0.2874(2) 1.1268(4) 0.0287(13) Uani 1 1 d . . . H26A H 0.5414 0.2520 1.1349 0.034 Uiso 1 1 calc R . . C27 C 0.5637(2) 0.36603(19) 1.1883(4) 0.0231(12) Uani 1 1 d . . . C28 C 0.5870(2) 0.39635(18) 1.2746(4) 0.0218(11) Uani 1 1 d . . . C29 C 0.56219(19) 0.07038(17) 1.4302(4) 0.0180(11) Uani 1 1 d . . . H29A H 0.5732 0.1017 1.4594 0.022 Uiso 1 1 calc R . . C30 C 0.5776(2) 0.02683(19) 1.4861(4) 0.0241(12) Uani 1 1 d . . . H30A H 0.5983 0.0290 1.5524 0.029 Uiso 1 1 calc R . . C31 C 0.5631(2) -0.01899(18) 1.4455(4) 0.0225(12) Uani 1 1 d . . . H31A H 0.5736 -0.0487 1.4831 0.027 Uiso 1 1 calc R . . C32 C 0.5323(2) -0.02152(17) 1.3476(4) 0.0185(11) Uani 1 1 d . . . C33 C 0.5153(2) -0.06747(16) 1.2967(4) 0.0236(12) Uani 1 1 d . . . H33 H 0.5256 -0.0984 1.3291 0.028 Uiso 1 1 calc R . . C34 C 0.51704(19) 0.02420(15) 1.2980(4) 0.0136(10) Uani 1 1 d . . . C35 C 0.5417(2) 0.18364(17) 1.3261(4) 0.0171(11) Uani 1 1 d . . . C36 C 0.5569(2) 0.13451(16) 1.1296(4) 0.0191(11) Uani 1 1 d . . . N1 N 0.73765(15) 0.45391(14) 1.0781(3) 0.0145(8) Uani 1 1 d . . . N2 N 0.79377(16) 0.43149(13) 0.8935(3) 0.0146(9) Uani 1 1 d . . . N3 N 0.69127(18) 0.32405(15) 1.1902(3) 0.0226(10) Uani 1 1 d . . . N4 N 0.6441(2) 0.38534(17) 0.8775(4) 0.0354(12) Uani 1 1 d . . . N5 N 0.86058(19) 0.37139(15) 1.1467(4) 0.0236(10) Uani 1 1 d . . . N6 N 0.79797(19) 0.29060(15) 0.8759(4) 0.0281(11) Uani 1 1 d . . . N7 N 0.61254(17) 0.37314(15) 1.3609(3) 0.0221(10) Uani 1 1 d . . . N8 N 0.56662(17) 0.31539(15) 1.2006(3) 0.0236(10) Uani 1 1 d . . . N9 N 0.56921(17) 0.21475(14) 1.3603(3) 0.0194(9) Uani 1 1 d . . . N10 N 0.53277(16) 0.06981(13) 1.3382(3) 0.0139(8) Uani 1 1 d . . . N11 N 0.58866(18) 0.14043(14) 1.0609(3) 0.0223(10) Uani 1 1 d . . . O1W O 0.61526(16) 0.27934(13) 1.5324(3) 0.0339(10) Uani 1 1 d . . . H1B H 0.6266 0.3008 1.5794 0.041 Uiso 1 1 d R . . H1C H 0.5925 0.2582 1.5544 0.041 Uiso 1 1 d R . . O2W O 0.71578(14) 0.31391(12) 1.4304(3) 0.0241(8) Uani 1 1 d . . . H2B H 0.7274 0.2948 1.4819 0.029 Uiso 1 1 d R . . H2C H 0.7415 0.3133 1.3848 0.029 Uiso 1 1 d R . . O3W O 0.64545(15) 0.22734(13) 1.1538(3) 0.0286(9) Uani 1 1 d . . . H3B H 0.6329 0.1985 1.1404 0.034 Uiso 1 1 d R . . H3C H 0.6488 0.2451 1.0948 0.034 Uiso 1 1 d R . . O4W O 0.56272(15) 0.20420(13) 1.6502(3) 0.0299(9) Uani 1 1 d . . . H4B H 0.5797 0.1769 1.6478 0.036 Uiso 1 1 d R . . H4C H 0.5555 0.2017 1.7199 0.036 Uiso 1 1 d R . . O6W O 0.45366(17) 0.20588(14) 1.6145(3) 0.0367(10) Uani 1 1 d . . . H6B H 0.4403 0.1855 1.5676 0.044 Uiso 1 1 d R . . H6C H 0.4868 0.2077 1.6210 0.044 Uiso 1 1 d R . . O7W O 0.7399(2) 0.27625(17) 0.6378(4) 0.0577(14) Uani 1 1 d . . . H7B H 0.7732 0.2754 0.6429 0.069 Uiso 1 1 d R . . H7C H 0.7308 0.2483 0.6654 0.069 Uiso 1 1 d R . . O8W O 0.30333(18) 0.20595(16) 1.7033(4) 0.0467(11) Uani 1 1 d . . . H8B H 0.3240 0.2221 1.6606 0.056 Uiso 1 1 d R . . H8C H 0.3179 0.1815 1.7367 0.056 Uiso 1 1 d R . . O9W O 0.6630(2) 0.3373(2) 0.6732(4) 0.0728(16) Uani 1 1 d . . . H9C H 0.6789 0.3100 0.7116 0.087 Uiso 1 1 d R . . H9B H 0.6566 0.3475 0.7486 0.087 Uiso 1 1 d R . . O10W O 0.36574(16) 0.26829(14) 1.5631(3) 0.0361(10) Uani 1 1 d . . . H10B H 0.3981 0.2605 1.5644 0.043 Uiso 1 1 d R . . H10C H 0.3668 0.3000 1.5614 0.043 Uiso 1 1 d R . . O5W' O 0.5492(6) 0.5879(5) 1.2431(13) 0.100(5) Uani 0.50 1 d P A 1 O5W O 0.5555(8) 0.6263(6) 1.2346(15) 0.144(8) Uani 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01496(18) 0.02163(14) 0.01543(14) 0.00327(10) 0.00000(11) -0.00697(11) Ru2 0.0113(3) 0.0139(2) 0.0148(3) 0.000 -0.0019(2) 0.000 Ru3 0.0124(3) 0.01784(19) 0.01374(19) 0.00052(14) 0.00285(16) -0.00312(15) C1 0.008(3) 0.033(3) 0.016(2) -0.001(2) 0.001(2) 0.001(2) C2 0.016(3) 0.033(3) 0.016(2) -0.004(2) 0.000(2) 0.004(2) C3 0.021(3) 0.026(3) 0.023(3) -0.004(2) -0.003(2) 0.010(2) C4 0.018(3) 0.021(2) 0.016(2) 0.0017(19) -0.004(2) 0.008(2) C5 0.032(4) 0.018(2) 0.026(3) 0.002(2) 0.001(2) 0.008(2) C6 0.028(4) 0.021(2) 0.022(3) 0.008(2) 0.002(2) 0.000(2) C7 0.013(3) 0.023(2) 0.016(2) 0.0062(19) 0.000(2) 0.000(2) C8 0.016(3) 0.027(3) 0.017(2) 0.008(2) 0.001(2) -0.002(2) C9 0.011(3) 0.031(3) 0.014(2) 0.003(2) 0.000(2) -0.002(2) C10 0.011(3) 0.022(2) 0.017(2) -0.0030(19) 0.001(2) 0.0006(19) C11 0.009(3) 0.022(2) 0.014(2) 0.0020(18) -0.003(2) 0.0026(19) C12 0.011(3) 0.019(2) 0.014(2) 0.0031(18) -0.003(2) 0.0029(19) C13 0.014(3) 0.019(2) 0.022(2) -0.001(2) 0.000(2) -0.002(2) C14 0.023(4) 0.024(2) 0.022(3) 0.001(2) 0.004(2) -0.003(2) C15 0.020(3) 0.016(2) 0.016(2) 0.0000(18) 0.005(2) -0.001(2) C16 0.017(3) 0.019(2) 0.024(3) 0.006(2) 0.000(2) -0.008(2) C17 0.017(3) 0.036(3) 0.028(3) -0.002(2) -0.001(2) 0.001(2) C18 0.020(4) 0.035(3) 0.035(3) -0.008(2) 0.001(3) 0.000(2) C19 0.018(4) 0.030(3) 0.039(3) -0.001(2) 0.009(3) 0.005(2) C20 0.009(3) 0.035(3) 0.032(3) 0.005(2) 0.007(2) 0.003(2) C21 0.024(4) 0.036(3) 0.038(3) 0.010(3) 0.012(3) 0.010(2) C22 0.021(4) 0.045(3) 0.030(3) 0.013(3) 0.007(3) 0.011(3) C23 0.012(3) 0.046(3) 0.021(3) 0.006(2) 0.005(2) 0.003(2) C24 0.020(4) 0.056(4) 0.022(3) 0.011(3) -0.002(2) 0.002(3) C25 0.022(4) 0.054(4) 0.023(3) 0.000(3) -0.004(2) -0.003(3) C26 0.020(4) 0.039(3) 0.027(3) 0.007(2) -0.001(2) -0.010(2) C27 0.011(3) 0.036(3) 0.022(3) 0.007(2) 0.005(2) -0.002(2) C28 0.007(3) 0.036(3) 0.023(3) 0.006(2) 0.008(2) 0.001(2) C29 0.011(3) 0.024(2) 0.019(2) 0.000(2) -0.002(2) 0.000(2) C30 0.018(3) 0.037(3) 0.017(2) 0.006(2) -0.001(2) 0.001(2) C31 0.015(3) 0.027(3) 0.025(3) 0.012(2) 0.003(2) 0.005(2) C32 0.008(3) 0.024(2) 0.024(3) 0.006(2) 0.003(2) 0.000(2) C33 0.021(3) 0.013(2) 0.036(3) 0.008(2) 0.006(2) 0.003(2) C34 0.009(3) 0.016(2) 0.015(2) 0.0014(18) 0.0034(19) 0.0011(18) C35 0.016(3) 0.020(2) 0.016(2) 0.0032(19) 0.002(2) 0.003(2) C36 0.023(4) 0.013(2) 0.021(3) -0.0031(19) -0.007(2) 0.005(2) N1 0.006(2) 0.023(2) 0.0148(19) 0.0016(16) -0.0007(16) -0.0009(16) N2 0.013(2) 0.0180(19) 0.0128(19) 0.0016(15) -0.0008(17) -0.0004(16) N3 0.021(3) 0.025(2) 0.021(2) 0.0020(18) 0.0031(19) -0.0087(19) N4 0.031(4) 0.037(3) 0.038(3) 0.001(2) -0.009(3) -0.006(2) N5 0.025(3) 0.023(2) 0.023(2) -0.0013(17) 0.002(2) -0.0020(19) N6 0.033(3) 0.023(2) 0.029(2) -0.0009(19) 0.008(2) -0.004(2) N7 0.012(3) 0.031(2) 0.024(2) 0.0036(18) 0.0015(19) -0.0019(18) N8 0.016(3) 0.035(2) 0.019(2) 0.0038(18) -0.0006(19) -0.0094(19) N9 0.017(3) 0.023(2) 0.017(2) -0.0007(17) -0.0011(18) -0.0026(18) N10 0.008(2) 0.0199(19) 0.0136(19) -0.0003(15) -0.0010(16) 0.0019(16) N11 0.022(3) 0.022(2) 0.023(2) -0.0015(17) 0.004(2) -0.0018(18) O1W 0.039(3) 0.040(2) 0.0232(19) -0.0021(16) 0.0085(18) -0.0178(18) O2W 0.018(2) 0.0270(18) 0.0275(19) 0.0022(15) -0.0026(16) -0.0047(15) O3W 0.027(3) 0.036(2) 0.0228(19) 0.0000(15) 0.0016(16) -0.0145(17) O4W 0.033(3) 0.0317(19) 0.0253(19) 0.0037(16) 0.0051(17) 0.0054(17) O6W 0.034(3) 0.047(2) 0.030(2) -0.0024(18) -0.0044(19) 0.0007(19) O7W 0.063(4) 0.065(3) 0.046(3) 0.011(2) -0.023(3) -0.006(3) O8W 0.038(3) 0.052(3) 0.051(3) 0.022(2) -0.001(2) 0.001(2) O9W 0.105(5) 0.070(3) 0.043(3) -0.006(3) -0.002(3) -0.018(3) O10W 0.036(3) 0.039(2) 0.033(2) 0.0060(17) 0.0078(19) 0.0090(18) O5W' 0.106(12) 0.080(9) 0.113(11) -0.042(9) -0.047(9) 0.015(9) O5W 0.175(18) 0.114(12) 0.145(15) -0.052(12) -0.130(14) 0.046(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 Nd1 O1W 2.441(4) . ? Nd1 O2W 2.461(3) . ? Nd1 N9 2.478(4) . ? Nd1 N6 2.481(5) 2_655 ? Nd1 N3 2.485(4) . ? Nd1 O3W 2.528(3) . ? Nd1 N8 2.633(4) . ? Nd1 N7 2.660(4) . ? Ru2 C35 1.976(5) . ? Ru2 C35 1.976(5) 3_657 ? Ru2 C36 2.039(6) . ? Ru2 C36 2.039(6) 3_657 ? Ru2 N10 2.121(4) 3_657 ? Ru2 N10 2.121(4) . ? Ru3 C16 1.969(5) . ? Ru3 C13 1.976(5) . ? Ru3 C15 2.032(6) . ? Ru3 C14 2.054(6) . ? Ru3 N1 2.117(4) . ? Ru3 N2 2.121(4) . ? C1 N1 1.327(6) . ? C1 C2 1.403(7) . ? C1 H1A 0.9500 . ? C2 C3 1.365(7) . ? C2 H2 0.9500 . ? C3 C4 1.397(7) . ? C3 H3A 0.9500 . ? C4 C12 1.409(6) . ? C4 C5 1.431(7) . ? C5 C6 1.348(7) . ? C5 H5 0.9500 . ? C6 C7 1.433(7) . ? C6 H6A 0.9500 . ? C7 C11 1.400(6) . ? C7 C8 1.411(7) . ? C8 C9 1.364(7) . ? C8 H8A 0.9500 . ? C9 C10 1.398(6) . ? C9 H9A 0.9500 . ? C10 N2 1.328(6) . ? C10 H10A 0.9500 . ? C11 N2 1.372(6) . ? C11 C12 1.427(6) . ? C12 N1 1.374(6) . ? C13 N3 1.157(6) . ? C14 N4 1.154(7) . ? C15 N5 1.161(6) . ? C16 N6 1.166(6) . ? C17 N7 1.325(7) . ? C17 C18 1.406(7) . ? C17 H17A 0.9500 . ? C18 C19 1.361(8) . ? C18 H18A 0.9500 . ? C19 C20 1.394(8) . ? C19 H19A 0.9500 . ? C20 C28 1.415(7) . ? C20 C21 1.435(7) . ? C21 C22 1.348(8) . ? C21 H21A 0.9500 . ? C22 C23 1.426(7) . ? C22 H22A 0.9500 . ? C23 C24 1.396(8) . ? C23 C27 1.406(7) . ? C24 C25 1.354(8) . ? C24 H24A 0.9500 . ? C25 C26 1.404(8) . ? C25 H25A 0.9500 . ? C26 N8 1.333(7) . ? C26 H26A 0.9500 . ? C27 N8 1.364(6) . ? C27 C28 1.436(7) . ? C28 N7 1.363(6) . ? C29 N10 1.325(6) . ? C29 C30 1.397(7) . ? C29 H29A 0.9500 . ? C30 C31 1.368(7) . ? C30 H30A 0.9500 . ? C31 C32 1.404(7) . ? C31 H31A 0.9500 . ? C32 C34 1.412(6) . ? C32 C33 1.436(7) . ? C33 C33 1.355(10) 3_657 ? C33 H33 0.9500 . ? C34 N10 1.370(6) . ? C34 C34 1.434(9) 3_657 ? C35 N9 1.162(6) . ? C36 N11 1.159(6) . ? N6 Nd1 2.481(5) 2_654 ? O1W H1B 0.8500 . ? O1W H1C 0.8501 . ? O2W H2B 0.8498 . ? O2W H2C 0.8501 . ? O3W H3B 0.8498 . ? O3W H3C 0.8504 . ? O4W H4B 0.8499 . ? O4W H4C 0.8501 . ? O6W H6B 0.8501 . ? O6W H6C 0.8493 . ? O7W H7B 0.8509 . ? O7W H7C 0.8497 . ? O8W H8B 0.8494 . ? O8W H8C 0.8500 . ? O9W H9C 0.9499 . ? O9W H9B 0.9500 . ? O10W H10B 0.8500 . ? O10W H10C 0.8501 . ? 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 O1W Nd1 O2W 74.92(12) . . ? O1W Nd1 N9 72.88(13) . . ? O2W Nd1 N9 141.10(12) . . ? O1W Nd1 N6 88.74(14) . 2_655 ? O2W Nd1 N6 71.58(12) . 2_655 ? N9 Nd1 N6 86.40(14) . 2_655 ? O1W Nd1 N3 141.95(13) . . ? O2W Nd1 N3 72.69(13) . . ? N9 Nd1 N3 144.23(13) . . ? N6 Nd1 N3 99.36(15) 2_655 . ? O1W Nd1 O3W 147.24(12) . . ? O2W Nd1 O3W 123.73(12) . . ? N9 Nd1 O3W 77.88(12) . . ? N6 Nd1 O3W 74.84(13) 2_655 . ? N3 Nd1 O3W 69.87(12) . . ? O1W Nd1 N8 113.31(14) . . ? O2W Nd1 N8 133.44(12) . . ? N9 Nd1 N8 80.14(13) . . ? N6 Nd1 N8 148.97(14) 2_655 . ? N3 Nd1 N8 77.03(14) . . ? O3W Nd1 N8 75.06(13) . . ? O1W Nd1 N7 78.49(12) . . ? O2W Nd1 N7 76.68(12) . . ? N9 Nd1 N7 116.82(13) . . ? N6 Nd1 N7 147.92(14) 2_655 . ? N3 Nd1 N7 75.12(13) . . ? O3W Nd1 N7 129.10(12) . . ? N8 Nd1 N7 61.73(13) . . ? C35 Ru2 C35 89.8(3) . 3_657 ? C35 Ru2 C36 84.69(19) . . ? C35 Ru2 C36 91.85(19) 3_657 . ? C35 Ru2 C36 91.85(19) . 3_657 ? C35 Ru2 C36 84.69(19) 3_657 3_657 ? C36 Ru2 C36 175.1(2) . 3_657 ? C35 Ru2 N10 170.67(18) . 3_657 ? C35 Ru2 N10 96.42(16) 3_657 3_657 ? C36 Ru2 N10 88.12(16) . 3_657 ? C36 Ru2 N10 95.66(16) 3_657 3_657 ? C35 Ru2 N10 96.42(16) . . ? C35 Ru2 N10 170.67(18) 3_657 . ? C36 Ru2 N10 95.66(16) . . ? C36 Ru2 N10 88.12(16) 3_657 . ? N10 Ru2 N10 78.4(2) 3_657 . ? C16 Ru3 C13 93.93(19) . . ? C16 Ru3 C15 86.26(19) . . ? C13 Ru3 C15 90.82(19) . . ? C16 Ru3 C14 92.8(2) . . ? C13 Ru3 C14 86.5(2) . . ? C15 Ru3 C14 177.10(18) . . ? C16 Ru3 N1 170.74(17) . . ? C13 Ru3 N1 95.13(17) . . ? C15 Ru3 N1 91.69(16) . . ? C14 Ru3 N1 89.65(17) . . ? C16 Ru3 N2 92.32(17) . . ? C13 Ru3 N2 173.72(16) . . ? C15 Ru3 N2 88.89(17) . . ? C14 Ru3 N2 93.90(17) . . ? N1 Ru3 N2 78.61(14) . . ? N1 C1 C2 122.3(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C12 117.6(4) . . ? C3 C4 C5 123.7(4) . . ? C12 C4 C5 118.6(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C11 C7 C8 117.4(4) . . ? C11 C7 C6 119.6(4) . . ? C8 C7 C6 123.0(4) . . ? C9 C8 C7 119.2(4) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? N2 C10 C9 122.8(4) . . ? N2 C10 H10A 118.6 . . ? C9 C10 H10A 118.6 . . ? N2 C11 C7 122.9(4) . . ? N2 C11 C12 117.4(4) . . ? C7 C11 C12 119.7(4) . . ? N1 C12 C4 122.9(4) . . ? N1 C12 C11 117.1(4) . . ? C4 C12 C11 120.0(4) . . ? N3 C13 Ru3 176.3(5) . . ? N4 C14 Ru3 175.0(5) . . ? N5 C15 Ru3 176.5(4) . . ? N6 C16 Ru3 171.6(4) . . ? N7 C17 C18 123.3(5) . . ? N7 C17 H17A 118.4 . . ? C18 C17 H17A 118.4 . . ? C19 C18 C17 119.3(5) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 119.5(5) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C19 C20 C28 117.8(5) . . ? C19 C20 C21 122.7(5) . . ? C28 C20 C21 119.5(5) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C21 C22 C23 121.6(5) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C24 C23 C27 117.8(5) . . ? C24 C23 C22 122.9(5) . . ? C27 C23 C22 119.2(5) . . ? C25 C24 C23 119.6(5) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 119.7(5) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? N8 C26 C25 122.8(5) . . ? N8 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? N8 C27 C23 122.6(5) . . ? N8 C27 C28 117.5(4) . . ? C23 C27 C28 119.8(5) . . ? N7 C28 C20 122.4(5) . . ? N7 C28 C27 118.5(4) . . ? C20 C28 C27 119.0(5) . . ? N10 C29 C30 122.8(4) . . ? N10 C29 H29A 118.6 . . ? C30 C29 H29A 118.6 . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C30 C31 C32 119.1(4) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C31 C32 C34 117.2(4) . . ? C31 C32 C33 123.9(4) . . ? C34 C32 C33 118.8(4) . . ? C33 C33 C32 121.2(3) 3_657 . ? C33 C33 H33 119.4 3_657 . ? C32 C33 H33 119.4 . . ? N10 C34 C32 123.1(4) . . ? N10 C34 C34 117.0(2) . 3_657 ? C32 C34 C34 119.9(3) . 3_657 ? N9 C35 Ru2 172.7(4) . . ? N11 C36 Ru2 174.5(4) . . ? C1 N1 C12 117.7(4) . . ? C1 N1 Ru3 128.8(3) . . ? C12 N1 Ru3 113.5(3) . . ? C10 N2 C11 117.7(4) . . ? C10 N2 Ru3 128.9(3) . . ? C11 N2 Ru3 113.3(3) . . ? C13 N3 Nd1 178.5(4) . . ? C16 N6 Nd1 158.7(4) . 2_654 ? C17 N7 C28 117.5(4) . . ? C17 N7 Nd1 123.7(3) . . ? C28 N7 Nd1 117.9(3) . . ? C26 N8 C27 117.4(4) . . ? C26 N8 Nd1 122.1(4) . . ? C27 N8 Nd1 118.8(3) . . ? C35 N9 Nd1 151.4(4) . . ? C29 N10 C34 117.6(4) . . ? C29 N10 Ru2 128.4(3) . . ? C34 N10 Ru2 113.8(3) . . ? Nd1 O1W H1B 124.2 . . ? Nd1 O1W H1C 117.2 . . ? H1B O1W H1C 118.4 . . ? Nd1 O2W H2B 112.0 . . ? Nd1 O2W H2C 107.8 . . ? H2B O2W H2C 100.4 . . ? Nd1 O3W H3B 128.1 . . ? Nd1 O3W H3C 113.7 . . ? H3B O3W H3C 113.1 . . ? H4B O4W H4C 94.3 . . ? H6B O6W H6C 119.6 . . ? H7B O7W H7C 103.0 . . ? H8B O8W H8C 113.6 . . ? H9C O9W H9B 80.9 . . ? H10B O10W H10C 102.3 . . ? 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 O1W H1B O9W 0.85 1.75 2.584(6) 167.1 1_556 O1W H1C O4W 0.85 1.99 2.791(5) 156.7 . O2W H2B O7W 0.85 1.94 2.730(5) 153.7 1_556 O2W H2C O8W 0.85 1.96 2.790(6) 164.6 4_558 O3W H3B N11 0.85 2.14 2.952(5) 160.0 . O3W H3C O10W 0.85 2.01 2.812(5) 157.2 3_657 O4W H4B N5 0.85 2.00 2.813(6) 160.9 2_655 O4W H4C O6W 0.85 1.98 2.824(5) 170.4 3_658 O6W H6B N11 0.85 2.08 2.927(6) 173.7 3_657 O6W H6C O4W 0.85 1.97 2.813(6) 172.2 . O7W H7B O3W 0.85 2.08 2.930(7) 179.3 2_654 O7W H7C O8W 0.85 2.11 2.883(7) 150.4 3_657 O8W H8B O10W 0.85 2.00 2.843(6) 172.0 . O8W H8C N5 0.85 2.26 3.095(6) 168.0 4_458 O9W H9C O7W 0.95 2.00 2.587(8) 117.9 . O9W H9B N4 0.95 1.86 2.787(7) 163.8 . O10W H10B O6W 0.85 2.12 2.861(6) 145.2 . O10W H10C N4 0.85 2.41 3.219(6) 159.1 3_657 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.513 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.114 #===END data_imw634r _database_code_depnum_ccdc_archive 'CCDC 636987' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H80 N22 O20 Ru3 Yb2' _chemical_formula_weight 2222.87 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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 25.8453(14) _cell_length_b 25.9396(15) _cell_length_c 11.8135(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7920.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7158 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4392 _exptl_absorpt_coefficient_mu 2.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5469 _exptl_absorpt_correction_T_max 0.7160 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59590 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6964 _reflns_number_gt 6227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+99.0369P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6964 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.141180(12) 0.781770(14) 0.82807(2) 0.01847(11) Uani 1 1 d . . . Ru1 Ru 0.25773(2) 0.88180(2) 0.50765(4) 0.01626(14) Uani 1 1 d . . . Ru2 Ru 0.0000 0.63645(4) 0.7500 0.0191(2) Uani 1 2 d S . . C1 C 0.2145(3) 0.9661(3) 0.6714(6) 0.0220(17) Uani 1 1 d . . . H1 H 0.1994 0.9388 0.7137 0.026 Uiso 1 1 calc R . . C2 C 0.2084(3) 1.0171(3) 0.7088(6) 0.0246(18) Uani 1 1 d . . . H2 H 0.1892 1.0237 0.7758 0.030 Uiso 1 1 calc R . . C3 C 0.2296(3) 1.0572(3) 0.6508(6) 0.0277(19) Uani 1 1 d . . . H3 H 0.2251 1.0916 0.6765 0.033 Uiso 1 1 calc R . . C4 C 0.2582(3) 1.0468(3) 0.5521(6) 0.0229(17) Uani 1 1 d . . . C5 C 0.2839(4) 1.0855(3) 0.4873(6) 0.032(2) Uani 1 1 d . . . H5 H 0.2817 1.1205 0.5106 0.038 Uiso 1 1 calc R . . C6 C 0.3112(4) 1.0735(3) 0.3938(6) 0.031(2) Uani 1 1 d . . . H6 H 0.3271 1.1003 0.3514 0.037 Uiso 1 1 calc R . . C7 C 0.3165(3) 1.0216(3) 0.3575(5) 0.0217(17) Uani 1 1 d . . . C8 C 0.3457(3) 1.0060(3) 0.2618(6) 0.0251(18) Uani 1 1 d . . . H8 H 0.3619 1.0311 0.2151 0.030 Uiso 1 1 calc R . . C9 C 0.3505(3) 0.9553(3) 0.2372(6) 0.0235(17) Uani 1 1 d . . . H9 H 0.3703 0.9448 0.1735 0.028 Uiso 1 1 calc R . . C10 C 0.3263(3) 0.9182(3) 0.3051(5) 0.0197(16) Uani 1 1 d . . . H10 H 0.3306 0.8828 0.2871 0.024 Uiso 1 1 calc R . . C11 C 0.2930(3) 0.9822(3) 0.4206(6) 0.0191(16) Uani 1 1 d . . . C12 C 0.2629(3) 0.9955(3) 0.5199(5) 0.0193(16) Uani 1 1 d . . . C13 C 0.2168(3) 0.8437(3) 0.6215(6) 0.0193(16) Uani 1 1 d . . . C14 C 0.1912(3) 0.8844(3) 0.4143(6) 0.0216(17) Uani 1 1 d . . . C15 C 0.3234(3) 0.8754(3) 0.6008(5) 0.0208(17) Uani 1 1 d . . . C16 C 0.2839(3) 0.8199(3) 0.4294(6) 0.0187(16) Uani 1 1 d . . . C17 C 0.0435(3) 0.7887(4) 0.6304(6) 0.0261(19) Uani 1 1 d . . . H17 H 0.0455 0.7523 0.6377 0.031 Uiso 1 1 calc R . . C18 C 0.0117(3) 0.8094(4) 0.5444(6) 0.031(2) Uani 1 1 d . . . H18 H -0.0081 0.7874 0.4970 0.037 Uiso 1 1 calc R . . C19 C 0.0100(3) 0.8615(4) 0.5307(7) 0.032(2) Uani 1 1 d . . . H19 H -0.0098 0.8763 0.4711 0.039 Uiso 1 1 calc R . . C20 C 0.0375(3) 0.8931(4) 0.6050(6) 0.029(2) Uani 1 1 d . . . C21 C 0.0362(3) 0.9478(4) 0.6003(7) 0.036(2) Uani 1 1 d . . . H21 H 0.0190 0.9640 0.5387 0.043 Uiso 1 1 calc R . . C22 C 0.0584(3) 0.9775(4) 0.6800(7) 0.035(2) Uani 1 1 d . . . H22 H 0.0564 1.0140 0.6745 0.042 Uiso 1 1 calc R . . C23 C 0.0849(3) 0.9543(4) 0.7725(6) 0.029(2) Uani 1 1 d . . . C24 C 0.1046(3) 0.9829(4) 0.8635(7) 0.034(2) Uani 1 1 d . . . H24 H 0.1002 1.0192 0.8659 0.041 Uiso 1 1 calc R . . C25 C 0.1303(3) 0.9580(4) 0.9488(7) 0.033(2) Uani 1 1 d . . . H25 H 0.1431 0.9767 1.0121 0.040 Uiso 1 1 calc R . . C26 C 0.1375(3) 0.9045(3) 0.9414(6) 0.029(2) Uani 1 1 d . . . H26 H 0.1571 0.8881 0.9991 0.035 Uiso 1 1 calc R . . C27 C 0.0914(3) 0.9004(3) 0.7758(6) 0.0245(18) Uani 1 1 d . . . C28 C 0.0668(3) 0.8697(3) 0.6911(6) 0.0243(18) Uani 1 1 d . . . C29 C 0.0440(3) 0.6899(3) 0.8214(5) 0.0180(16) Uani 1 1 d . . . C30 C 0.0622(3) 0.5739(3) 0.9305(6) 0.0243(18) Uani 1 1 d . . . H30 H 0.0734 0.6062 0.9598 0.029 Uiso 1 1 calc R . . C31 C 0.0771(3) 0.5289(3) 0.9867(6) 0.0259(18) Uani 1 1 d . . . H31 H 0.0976 0.5311 1.0533 0.031 Uiso 1 1 calc R . . C32 C 0.0625(3) 0.4823(4) 0.9472(6) 0.029(2) Uani 1 1 d . . . H32 H 0.0729 0.4518 0.9854 0.035 Uiso 1 1 calc R . . C33 C 0.0316(3) 0.4793(3) 0.8479(6) 0.0239(18) Uani 1 1 d . . . C34 C 0.0148(3) 0.4314(3) 0.7974(7) 0.0291(19) Uani 1 1 d . . . H34 H 0.0245 0.3996 0.8310 0.035 Uiso 1 1 calc R . . C35 C 0.0173(3) 0.5260(3) 0.7992(6) 0.0222(17) Uani 1 1 d . . . C36 C 0.0543(3) 0.6395(3) 0.6236(6) 0.0255(18) Uani 1 1 d . . . N1 N 0.2412(2) 0.9551(3) 0.5773(5) 0.0195(14) Uani 1 1 d . . . N2 N 0.2973(2) 0.9311(2) 0.3944(4) 0.0183(14) Uani 1 1 d . . . N3 N 0.1908(2) 0.8247(3) 0.6894(5) 0.0212(14) Uani 1 1 d . . . N4 N 0.1518(3) 0.8840(3) 0.3660(6) 0.0367(18) Uani 1 1 d . . . N5 N 0.3620(2) 0.8689(3) 0.6510(5) 0.0264(16) Uani 1 1 d . . . N6 N 0.3063(3) 0.7876(3) 0.3814(5) 0.0247(15) Uani 1 1 d . . . N7 N 0.0706(2) 0.8172(3) 0.7009(5) 0.0237(15) Uani 1 1 d . . . N8 N 0.1186(2) 0.8755(3) 0.8586(5) 0.0226(15) Uani 1 1 d . . . N9 N 0.0733(2) 0.7210(3) 0.8493(5) 0.0209(14) Uani 1 1 d . . . N10 N 0.0330(2) 0.5735(2) 0.8372(5) 0.0187(13) Uani 1 1 d . . . N11 N 0.0842(3) 0.6449(3) 0.5521(5) 0.0353(18) Uani 1 1 d . . . O1W O 0.1162(2) 0.7862(2) 1.0175(4) 0.0278(13) Uani 1 1 d . . . H1B H 0.0983 0.7625 1.0480 0.033 Uiso 1 1 d R . . H1C H 0.1168 0.8120 1.0619 0.033 Uiso 1 1 d R . . O2W O 0.1468(2) 0.7300(2) 0.6570(4) 0.0239(12) Uani 1 1 d . . . H2B H 0.1771 0.7225 0.6821 0.029 Uiso 1 1 d R . . H2C H 0.1298 0.7020 0.6447 0.029 Uiso 1 1 d R . . O3W O 0.21343(19) 0.8160(2) 0.9203(4) 0.0221(12) Uani 1 1 d . . . H3B H 0.2376 0.8150 0.8716 0.026 Uiso 1 1 d R . . H3C H 0.2260 0.8080 0.9845 0.026 Uiso 1 1 d R . . O4W O 0.1365(2) 0.7705(2) 0.4423(4) 0.0286(13) Uani 1 1 d . . . H4B H 0.1061 0.7804 0.4259 0.034 Uiso 1 1 d R . . H4C H 0.1538 0.7974 0.4259 0.034 Uiso 1 1 d R . . O5W O 0.0536(12) 0.8979(15) 0.232(2) 0.108(17) Uani 0.35(2) 1 d P A 1 O5W' O 0.0886(4) 0.8653(4) 0.1745(7) 0.030(3) Uani 0.65(2) 1 d P A 2 O6W O 0.4348(2) 0.7917(2) 0.6454(4) 0.0289(13) Uani 1 1 d . . . H6B H 0.4133 0.8163 0.6396 0.035 Uiso 1 1 d R . . H6C H 0.4571 0.7909 0.5925 0.035 Uiso 1 1 d R . . O7W O 0.0459(2) 0.7123(3) 0.3778(5) 0.0457(18) Uani 1 1 d . . . O8W O 0.2403(3) 0.7898(4) 0.1375(5) 0.063(2) Uani 1 1 d . . . O9W O 0.1992(2) 0.7118(2) 0.2952(5) 0.0357(15) Uani 1 1 d . . . H9B H 0.1803 0.7293 0.3398 0.043 Uiso 1 1 d R . . H9C H 0.1764 0.6974 0.2540 0.043 Uiso 1 1 d R . . O10W O 0.1603(9) 0.8337(9) 0.1691(14) 0.105(8) Uani 0.50 1 d P . . H10B H 0.1635 0.8016 0.1881 0.126 Uiso 0.50 1 d PR . . H10C H 0.1573 0.8525 0.2038 0.126 Uiso 0.50 1 d PR . . O11W O 0.0000 0.8075(5) 0.2500 0.073(3) Uani 1 2 d S . . H11B H 0.0336 0.7983 0.2468 0.088 Uiso 0.50 1 d PR . . H11C H -0.0159 0.8339 0.2553 0.088 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01673(17) 0.0292(2) 0.00952(15) 0.00448(13) 0.00090(11) 0.00128(15) Ru1 0.0183(3) 0.0228(3) 0.0077(2) 0.0003(2) 0.0026(2) 0.0011(3) Ru2 0.0172(4) 0.0311(5) 0.0090(4) 0.000 -0.0017(3) 0.000 C1 0.022(4) 0.030(5) 0.015(3) -0.001(3) -0.001(3) 0.003(3) C2 0.025(4) 0.036(5) 0.013(3) -0.003(3) 0.001(3) 0.005(4) C3 0.030(4) 0.035(5) 0.019(4) -0.003(3) -0.002(3) 0.009(4) C4 0.032(4) 0.023(5) 0.013(3) -0.001(3) -0.008(3) 0.019(4) C5 0.054(6) 0.022(5) 0.020(4) 0.001(3) -0.002(4) 0.013(4) C6 0.050(5) 0.025(5) 0.017(4) 0.007(3) 0.002(4) 0.004(4) C7 0.026(4) 0.032(5) 0.006(3) 0.003(3) -0.004(3) 0.000(4) C8 0.035(4) 0.030(5) 0.011(3) 0.006(3) 0.002(3) -0.002(4) C9 0.021(4) 0.038(5) 0.012(3) -0.001(3) 0.003(3) 0.003(4) C10 0.019(4) 0.028(5) 0.012(3) -0.002(3) 0.002(3) 0.005(3) C11 0.023(4) 0.022(4) 0.012(3) 0.000(3) -0.002(3) 0.007(3) C12 0.021(4) 0.029(5) 0.007(3) 0.003(3) 0.000(3) 0.005(3) C13 0.020(4) 0.028(5) 0.010(3) 0.000(3) -0.004(3) 0.003(3) C14 0.032(4) 0.017(4) 0.015(3) 0.000(3) 0.005(3) -0.001(3) C15 0.032(4) 0.022(4) 0.009(3) 0.002(3) 0.010(3) 0.000(3) C16 0.016(4) 0.028(5) 0.011(3) -0.002(3) 0.001(3) -0.001(3) C17 0.017(4) 0.043(6) 0.018(4) 0.009(3) 0.003(3) -0.001(4) C18 0.020(4) 0.058(6) 0.014(4) 0.007(4) 0.000(3) -0.002(4) C19 0.023(4) 0.050(6) 0.024(4) 0.018(4) -0.001(3) 0.000(4) C20 0.021(4) 0.049(6) 0.017(4) 0.006(4) 0.004(3) 0.001(4) C21 0.032(5) 0.047(6) 0.030(4) 0.022(4) 0.003(4) 0.013(4) C22 0.030(5) 0.048(6) 0.026(4) 0.010(4) 0.004(4) 0.011(4) C23 0.025(4) 0.042(6) 0.021(4) 0.012(4) 0.009(3) 0.009(4) C24 0.034(5) 0.041(6) 0.029(4) 0.003(4) 0.011(4) 0.013(4) C25 0.039(5) 0.038(6) 0.022(4) -0.006(4) 0.006(3) 0.017(4) C26 0.032(5) 0.041(6) 0.014(4) 0.001(3) 0.004(3) 0.013(4) C27 0.015(4) 0.044(6) 0.014(3) 0.006(3) 0.006(3) 0.006(4) C28 0.018(4) 0.041(5) 0.013(3) 0.013(3) 0.007(3) 0.004(4) C29 0.019(4) 0.027(5) 0.008(3) 0.003(3) 0.000(3) 0.002(4) C30 0.020(4) 0.041(5) 0.011(3) -0.003(3) 0.001(3) 0.000(4) C31 0.022(4) 0.040(5) 0.016(4) 0.003(3) -0.006(3) 0.002(4) C32 0.020(4) 0.047(6) 0.019(4) 0.011(4) 0.001(3) 0.004(4) C33 0.022(4) 0.031(5) 0.020(4) 0.001(3) 0.003(3) 0.006(4) C34 0.032(5) 0.027(5) 0.029(4) 0.005(4) 0.002(3) -0.001(4) C35 0.018(4) 0.035(5) 0.013(3) 0.000(3) -0.003(3) -0.001(4) C36 0.034(5) 0.024(5) 0.018(4) -0.007(3) -0.008(3) -0.002(4) N1 0.016(3) 0.031(4) 0.011(3) -0.002(3) -0.001(2) 0.002(3) N2 0.021(3) 0.025(4) 0.009(3) 0.001(2) -0.003(2) 0.000(3) N3 0.023(3) 0.031(4) 0.010(3) 0.001(3) -0.001(2) -0.004(3) N4 0.039(4) 0.042(5) 0.029(4) 0.007(3) -0.013(3) -0.011(4) N5 0.024(4) 0.045(5) 0.011(3) -0.001(3) 0.000(3) 0.005(3) N6 0.027(4) 0.029(4) 0.018(3) 0.003(3) 0.003(3) -0.003(3) N7 0.016(3) 0.045(5) 0.010(3) 0.007(3) 0.002(2) -0.001(3) N8 0.018(3) 0.036(4) 0.014(3) 0.007(3) 0.006(2) 0.008(3) N9 0.021(3) 0.034(4) 0.007(3) 0.003(3) -0.001(2) 0.003(3) N10 0.019(3) 0.026(4) 0.011(3) 0.001(3) -0.001(2) -0.002(3) N11 0.038(4) 0.049(5) 0.019(3) -0.010(3) 0.010(3) -0.014(4) O1W 0.028(3) 0.039(4) 0.017(3) 0.006(2) 0.005(2) -0.002(3) O2W 0.020(3) 0.031(3) 0.020(3) 0.000(2) -0.004(2) -0.007(2) O3W 0.017(3) 0.037(3) 0.012(2) 0.004(2) -0.0002(19) 0.001(2) O4W 0.025(3) 0.038(4) 0.023(3) 0.005(2) 0.003(2) 0.001(3) O5W 0.09(2) 0.18(4) 0.058(18) 0.05(2) -0.048(17) -0.06(2) O5W' 0.031(6) 0.043(6) 0.015(4) -0.005(4) -0.004(4) 0.004(4) O6W 0.030(3) 0.037(4) 0.019(3) -0.006(2) 0.001(2) 0.008(3) O7W 0.038(4) 0.079(5) 0.020(3) -0.008(3) -0.003(3) 0.003(4) O8W 0.041(4) 0.124(7) 0.024(3) 0.016(4) -0.007(3) -0.001(4) O9W 0.024(3) 0.056(4) 0.027(3) -0.011(3) -0.002(2) 0.004(3) O10W 0.136(19) 0.130(19) 0.049(10) -0.003(11) -0.009(11) -0.043(16) O11W 0.064(7) 0.099(10) 0.056(7) 0.000 0.002(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1W 2.333(5) . ? Yb1 O3W 2.337(5) . ? Yb1 N6 2.341(7) 2_565 ? Yb1 N3 2.359(6) . ? Yb1 N9 2.370(7) . ? Yb1 O2W 2.431(5) . ? Yb1 N8 2.527(7) . ? Yb1 N7 2.536(6) . ? Yb1 H2B 2.4903 . ? Yb1 H3B 2.6867 . ? Ru1 C16 1.972(8) . ? Ru1 C13 1.975(7) . ? Ru1 C15 2.030(8) . ? Ru1 C14 2.045(8) . ? Ru1 N2 2.114(6) . ? Ru1 N1 2.116(6) . ? Ru2 C29 1.981(8) . ? Ru2 C29 1.981(8) 3_556 ? Ru2 C36 2.050(8) . ? Ru2 C36 2.050(8) 3_556 ? Ru2 N10 2.111(6) 3_556 ? Ru2 N10 2.111(6) . ? C1 N1 1.339(9) . ? C1 C2 1.403(11) . ? C1 H1 0.9500 . ? C2 C3 1.361(12) . ? C2 H2 0.9500 . ? C3 C4 1.405(10) . ? C3 H3 0.9500 . ? C4 C12 1.390(11) . ? C4 C5 1.427(12) . ? C5 C6 1.347(11) . ? C5 H5 0.9500 . ? C6 C7 1.420(12) . ? C6 H6 0.9500 . ? C7 C11 1.404(11) . ? C7 C8 1.417(10) . ? C8 C9 1.353(11) . ? C8 H8 0.9500 . ? C9 C10 1.400(11) . ? C9 H9 0.9500 . ? C10 N2 1.337(9) . ? C10 H10 0.9500 . ? C11 N2 1.367(10) . ? C11 C12 1.449(9) . ? C12 N1 1.368(10) . ? C13 N3 1.158(9) . ? C14 N4 1.166(10) . ? C15 N5 1.172(10) . ? C16 N6 1.166(10) . ? C17 N7 1.314(10) . ? C17 C18 1.414(11) . ? C17 H17 0.9500 . ? C18 C19 1.363(13) . ? C18 H18 0.9500 . ? C19 C20 1.395(12) . ? C19 H19 0.9500 . ? C20 C28 1.407(11) . ? C20 C21 1.421(13) . ? C21 C22 1.345(13) . ? C21 H21 0.9500 . ? C22 C23 1.424(11) . ? C22 H22 0.9500 . ? C23 C24 1.401(12) . ? C23 C27 1.407(12) . ? C24 C25 1.369(12) . ? C24 H24 0.9500 . ? C25 C26 1.402(12) . ? C25 H25 0.9500 . ? C26 N8 1.327(10) . ? C26 H26 0.9500 . ? C27 N8 1.368(9) . ? C27 C28 1.429(11) . ? C28 N7 1.369(11) . ? C29 N9 1.156(10) . ? C30 N10 1.338(9) . ? C30 C31 1.396(11) . ? C30 H30 0.9500 . ? C31 C32 1.350(12) . ? C31 H31 0.9500 . ? C32 C33 1.422(11) . ? C32 H32 0.9500 . ? C33 C35 1.392(11) . ? C33 C34 1.445(12) . ? C34 C34 1.354(16) 3_556 ? C34 H34 0.9500 . ? C35 N10 1.372(10) . ? C35 C35 1.467(14) 3_556 ? C36 N11 1.154(10) . ? N6 Yb1 2.341(7) 2_564 ? O1W H1B 0.8498 . ? O1W H1C 0.8501 . ? O2W H2B 0.8602 . ? O2W H2C 0.8599 . ? O3W H3B 0.8502 . ? O3W H3C 0.8500 . ? O4W H4B 0.8499 . ? O4W H4C 0.8498 . ? O6W H6B 0.8499 . ? O6W H6C 0.8499 . ? O9W H9B 0.8494 . ? O9W H9C 0.8499 . ? O10W H10B 0.8666 . ? O10W H10C 0.6424 . ? O11W H11B 0.9001 . ? O11W H11C 0.8000 . ? 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 O1W Yb1 O3W 75.83(18) . . ? O1W Yb1 N6 86.6(2) . 2_565 ? O3W Yb1 N6 72.7(2) . 2_565 ? O1W Yb1 N3 142.5(2) . . ? O3W Yb1 N3 73.17(18) . . ? N6 Yb1 N3 103.6(2) 2_565 . ? O1W Yb1 N9 74.10(19) . . ? O3W Yb1 N9 142.55(18) . . ? N6 Yb1 N9 83.7(2) 2_565 . ? N3 Yb1 N9 142.10(19) . . ? O1W Yb1 O2W 147.28(19) . . ? O3W Yb1 O2W 123.34(17) . . ? N6 Yb1 O2W 76.36(19) 2_565 . ? N3 Yb1 O2W 69.59(19) . . ? N9 Yb1 O2W 76.41(18) . . ? O1W Yb1 N8 75.63(19) . . ? O3W Yb1 N8 75.68(19) . . ? N6 Yb1 N8 146.7(2) 2_565 . ? N3 Yb1 N8 76.7(2) . . ? N9 Yb1 N8 117.0(2) . . ? O2W Yb1 N8 131.64(18) . . ? O1W Yb1 N7 110.58(19) . . ? O3W Yb1 N7 135.5(2) . . ? N6 Yb1 N7 148.8(2) 2_565 . ? N3 Yb1 N7 79.0(2) . . ? N9 Yb1 N7 76.8(2) . . ? O2W Yb1 N7 75.57(19) . . ? N8 Yb1 N7 64.5(2) . . ? O1W Yb1 H2B 143.0 . . ? O3W Yb1 H2B 105.0 . . ? N6 Yb1 H2B 59.7 2_565 . ? N3 Yb1 H2B 66.9 . . ? N9 Yb1 H2B 86.5 . . ? O2W Yb1 H2B 20.1 . . ? N8 Yb1 H2B 141.2 . . ? N7 Yb1 H2B 94.7 . . ? O1W Yb1 H3B 93.3 . . ? O3W Yb1 H3B 17.8 . . ? N6 Yb1 H3B 69.9 2_565 . ? N3 Yb1 H3B 58.5 . . ? N9 Yb1 H3B 151.5 . . ? O2W Yb1 H3B 106.3 . . ? N8 Yb1 H3B 83.0 . . ? N7 Yb1 H3B 131.7 . . ? H2B Yb1 H3B 89.1 . . ? C16 Ru1 C13 95.4(3) . . ? C16 Ru1 C15 84.3(3) . . ? C13 Ru1 C15 92.2(3) . . ? C16 Ru1 C14 93.6(3) . . ? C13 Ru1 C14 86.2(3) . . ? C15 Ru1 C14 177.2(3) . . ? C16 Ru1 N2 91.7(3) . . ? C13 Ru1 N2 172.8(3) . . ? C15 Ru1 N2 89.3(3) . . ? C14 Ru1 N2 92.6(3) . . ? C16 Ru1 N1 169.5(3) . . ? C13 Ru1 N1 94.4(3) . . ? C15 Ru1 N1 91.8(3) . . ? C14 Ru1 N1 90.6(3) . . ? N2 Ru1 N1 78.5(2) . . ? C29 Ru2 C29 91.2(4) . 3_556 ? C29 Ru2 C36 83.7(3) . . ? C29 Ru2 C36 93.2(3) 3_556 . ? C29 Ru2 C36 93.2(3) . 3_556 ? C29 Ru2 C36 83.7(3) 3_556 3_556 ? C36 Ru2 C36 175.5(5) . 3_556 ? C29 Ru2 N10 168.7(3) . 3_556 ? C29 Ru2 N10 95.9(3) 3_556 3_556 ? C36 Ru2 N10 87.2(3) . 3_556 ? C36 Ru2 N10 96.3(3) 3_556 3_556 ? C29 Ru2 N10 95.9(3) . . ? C29 Ru2 N10 168.7(3) 3_556 . ? C36 Ru2 N10 96.3(3) . . ? C36 Ru2 N10 87.2(3) 3_556 . ? N10 Ru2 N10 78.6(3) 3_556 . ? N1 C1 C2 121.2(7) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C3 C2 C1 121.2(7) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 118.8(8) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C12 C4 C3 117.2(7) . . ? C12 C4 C5 119.1(7) . . ? C3 C4 C5 123.7(7) . . ? C6 C5 C4 121.4(8) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.2(8) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C11 C7 C8 116.5(7) . . ? C11 C7 C6 119.1(7) . . ? C8 C7 C6 124.3(7) . . ? C9 C8 C7 119.9(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 122.1(7) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? N2 C11 C7 123.4(7) . . ? N2 C11 C12 117.3(7) . . ? C7 C11 C12 119.3(7) . . ? N1 C12 C4 124.2(6) . . ? N1 C12 C11 116.1(7) . . ? C4 C12 C11 119.8(7) . . ? N3 C13 Ru1 175.0(7) . . ? N4 C14 Ru1 175.8(7) . . ? N5 C15 Ru1 175.8(7) . . ? N6 C16 Ru1 169.5(7) . . ? N7 C17 C18 123.4(8) . . ? N7 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C19 C18 C17 118.8(8) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 119.4(8) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C28 118.4(8) . . ? C19 C20 C21 123.3(8) . . ? C28 C20 C21 118.3(8) . . ? C22 C21 C20 122.3(8) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 120.0(9) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C27 117.5(7) . . ? C24 C23 C22 122.6(9) . . ? C27 C23 C22 119.8(8) . . ? C25 C24 C23 119.4(9) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 119.0(8) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N8 C26 C25 123.9(7) . . ? N8 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? N8 C27 C23 123.3(7) . . ? N8 C27 C28 117.7(8) . . ? C23 C27 C28 118.9(7) . . ? N7 C28 C20 122.0(8) . . ? N7 C28 C27 117.7(7) . . ? C20 C28 C27 120.3(8) . . ? N9 C29 Ru2 170.7(6) . . ? N10 C30 C31 122.7(8) . . ? N10 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C32 C31 C30 120.5(7) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.5(8) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C35 C33 C32 116.2(8) . . ? C35 C33 C34 119.9(7) . . ? C32 C33 C34 123.9(8) . . ? C34 C34 C33 120.7(4) 3_556 . ? C34 C34 H34 119.6 3_556 . ? C33 C34 H34 119.6 . . ? N10 C35 C33 124.7(6) . . ? N10 C35 C35 116.0(4) . 3_556 ? C33 C35 C35 119.3(4) . 3_556 ? N11 C36 Ru2 175.2(8) . . ? C1 N1 C12 117.4(7) . . ? C1 N1 Ru1 128.2(5) . . ? C12 N1 Ru1 114.4(5) . . ? C10 N2 C11 117.9(6) . . ? C10 N2 Ru1 128.3(5) . . ? C11 N2 Ru1 113.8(5) . . ? C13 N3 Yb1 176.6(6) . . ? C16 N6 Yb1 166.3(6) . 2_564 ? C17 N7 C28 117.9(7) . . ? C17 N7 Yb1 123.6(6) . . ? C28 N7 Yb1 117.5(5) . . ? C26 N8 C27 116.7(7) . . ? C26 N8 Yb1 124.5(5) . . ? C27 N8 Yb1 118.1(5) . . ? C29 N9 Yb1 156.8(5) . . ? C30 N10 C35 116.4(7) . . ? C30 N10 Ru2 128.6(6) . . ? C35 N10 Ru2 114.6(4) . . ? Yb1 O1W H1B 121.5 . . ? Yb1 O1W H1C 128.7 . . ? H1B O1W H1C 108.6 . . ? Yb1 O2W H2B 83.9 . . ? Yb1 O2W H2C 125.2 . . ? H2B O2W H2C 109.6 . . ? Yb1 O3W H3B 105.1 . . ? Yb1 O3W H3C 128.9 . . ? H3B O3W H3C 108.4 . . ? H4B O4W H4C 100.7 . . ? H6B O6W H6C 113.6 . . ? H9B O9W H9C 101.2 . . ? H10B O10W H10C 125.1 . . ? H11B O11W H11C 136.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.852 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.155 #===END data_imw516m _database_code_depnum_ccdc_archive 'CCDC 636988' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H77 N24 Nd2 O15.50 Ru3' _chemical_formula_weight 2190.33 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8466(6) _cell_length_b 27.2848(15) _cell_length_c 31.3415(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9275.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8314 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.19 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4356 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6463 _exptl_absorpt_correction_T_max 0.8794 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 127611 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16304 _reflns_number_gt 13217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+54.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.474(18) _refine_ls_number_reflns 16304 _refine_ls_number_parameters 1163 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 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 Nd1 Nd 0.35571(5) 0.82971(2) 0.508475(19) 0.03472(15) Uani 1 1 d . . . Nd2 Nd 0.40330(5) 0.83076(2) 0.00131(2) 0.04450(18) Uani 1 1 d . . . Ru1 Ru 0.37075(8) 0.63858(3) 0.46937(3) 0.0357(2) Uani 1 1 d . . . Ru2 Ru 0.41783(7) 0.63252(3) 0.02602(3) 0.0318(2) Uani 1 1 d . . . Ru3 Ru 0.69278(12) 0.76909(5) 0.24973(4) 0.0734(4) Uani 1 1 d . . . C1 C 0.3711(11) 0.7083(5) 0.3906(4) 0.048(3) Uani 1 1 d . . . H1 H 0.3813 0.7341 0.4106 0.058 Uiso 1 1 calc R . . C2 C 0.3710(15) 0.7207(6) 0.3474(5) 0.078(5) Uani 1 1 d . . . H2 H 0.3899 0.7533 0.3388 0.094 Uiso 1 1 calc R . . C3 C 0.3435(19) 0.6857(8) 0.3174(6) 0.101(6) Uani 1 1 d . . . H3 H 0.3350 0.6937 0.2881 0.121 Uiso 1 1 calc R . . C4 C 0.3278(14) 0.6358(8) 0.3330(5) 0.091(6) Uani 1 1 d . . . C5 C 0.304(3) 0.5962(9) 0.3053(6) 0.156(12) Uani 1 1 d . . . H5 H 0.2972 0.6019 0.2755 0.187 Uiso 1 1 calc R . . C6 C 0.2902(18) 0.5485(8) 0.3210(6) 0.111(8) Uani 1 1 d . . . H6 H 0.2756 0.5225 0.3015 0.133 Uiso 1 1 calc R . . C7 C 0.2978(16) 0.5372(7) 0.3673(6) 0.090(6) Uani 1 1 d . . . C8 C 0.2860(15) 0.4919(6) 0.3848(7) 0.087(6) Uani 1 1 d . . . H8 H 0.2720 0.4640 0.3673 0.105 Uiso 1 1 calc R . . C9 C 0.2945(14) 0.4876(6) 0.4275(6) 0.081(5) Uani 1 1 d . . . H9 H 0.2861 0.4564 0.4406 0.097 Uiso 1 1 calc R . . C10 C 0.3148(11) 0.5276(5) 0.4516(5) 0.062(4) Uani 1 1 d . . . H10 H 0.3188 0.5233 0.4816 0.075 Uiso 1 1 calc R . . C11 C 0.3233(12) 0.5778(5) 0.3936(4) 0.058(4) Uani 1 1 d . . . C12 C 0.3369(11) 0.6257(5) 0.3764(4) 0.055(3) Uani 1 1 d . . . C13 C 0.4093(9) 0.7029(4) 0.4917(3) 0.035(2) Uani 1 1 d . . . C14 C 0.1881(12) 0.6510(4) 0.4782(3) 0.039(3) Uani 1 1 d . . . C15 C 0.5524(11) 0.6296(4) 0.4651(4) 0.039(3) Uani 1 1 d . . . C16 C 0.3841(9) 0.6115(4) 0.5291(4) 0.034(2) Uani 1 1 d . . . C17 C 0.4329(14) 0.7755(7) 0.6039(5) 0.072(4) Uani 1 1 d . . . H17 H 0.4090 0.7477 0.5876 0.086 Uiso 1 1 calc R . . C18 C 0.4806(15) 0.7695(8) 0.6455(6) 0.092(6) Uani 1 1 d . . . H18 H 0.4876 0.7379 0.6580 0.111 Uiso 1 1 calc R . . C19 C 0.517(3) 0.8115(14) 0.6677(9) 0.171(16) Uani 1 1 d . . . H19 H 0.5498 0.8086 0.6957 0.205 Uiso 1 1 calc R . . C20 C 0.506(3) 0.8556(11) 0.6496(9) 0.141(11) Uani 1 1 d . . . H20 H 0.5320 0.8841 0.6646 0.169 Uiso 1 1 calc R . . C21 C 0.4592(13) 0.8596(7) 0.6111(5) 0.078(5) Uani 1 1 d . . . C22 C 0.4442(14) 0.9082(7) 0.5906(7) 0.084(6) Uani 1 1 d . . . C23 C 0.4653(17) 0.9516(9) 0.6155(7) 0.112(8) Uani 1 1 d . . . H23 H 0.4869 0.9483 0.6447 0.134 Uiso 1 1 calc R . . C24 C 0.455(2) 0.9969(8) 0.5986(9) 0.117(9) Uani 1 1 d . . . H24 H 0.4719 1.0258 0.6144 0.140 Uiso 1 1 calc R . . C25 C 0.4174(18) 0.9978(7) 0.5550(9) 0.119(9) Uani 1 1 d . . . H25 H 0.4075 1.0283 0.5407 0.142 Uiso 1 1 calc R . . C26 C 0.3958(15) 0.9555(5) 0.5342(7) 0.078(5) Uani 1 1 d . . . C27 C 0.3518(14) 0.9567(4) 0.4895(8) 0.088(6) Uani 1 1 d . . . C28 C 0.3312(18) 1.0003(6) 0.4666(9) 0.117(10) Uani 1 1 d . . . H28 H 0.3446 1.0309 0.4803 0.141 Uiso 1 1 calc R . . C29 C 0.292(2) 0.9996(9) 0.4254(10) 0.129(12) Uani 1 1 d . . . H29 H 0.2816 1.0291 0.4098 0.155 Uiso 1 1 calc R . . C30 C 0.2700(19) 0.9558(7) 0.4071(7) 0.099(7) Uani 1 1 d . . . H30 H 0.2415 0.9548 0.3784 0.119 Uiso 1 1 calc R . . C31 C 0.2866(15) 0.9138(6) 0.4282(6) 0.078(5) Uani 1 1 d . . . H31 H 0.2670 0.8836 0.4147 0.094 Uiso 1 1 calc R . . C32 C 0.3904(11) 0.6825(4) 0.1141(4) 0.052(3) Uani 1 1 d . . . H32 H 0.3939 0.7125 0.0987 0.062 Uiso 1 1 calc R . . C33 C 0.3803(14) 0.6849(7) 0.1584(5) 0.074(4) Uani 1 1 d . . . H33 H 0.3763 0.7158 0.1722 0.089 Uiso 1 1 calc R . . C34 C 0.3763(15) 0.6430(7) 0.1817(5) 0.087(5) Uani 1 1 d . . . H34 H 0.3710 0.6444 0.2119 0.104 Uiso 1 1 calc R . . C35 C 0.3802(13) 0.5948(6) 0.1594(4) 0.064(4) Uani 1 1 d . . . C36 C 0.3696(15) 0.5512(7) 0.1800(5) 0.086(5) Uani 1 1 d . . . H36 H 0.3606 0.5506 0.2101 0.103 Uiso 1 1 calc R . . C37 C 0.3719(14) 0.5068(7) 0.1570(5) 0.074(4) Uani 1 1 d . . . H37 H 0.3684 0.4763 0.1716 0.089 Uiso 1 1 calc R . . C38 C 0.3795(11) 0.5081(5) 0.1112(4) 0.057(3) Uani 1 1 d . . . C39 C 0.3714(12) 0.4671(5) 0.0859(5) 0.054(3) Uani 1 1 d . . . H39 H 0.3641 0.4357 0.0987 0.065 Uiso 1 1 calc R . . C40 C 0.3739(11) 0.4710(4) 0.0436(5) 0.058(4) Uani 1 1 d . . . H40 H 0.3716 0.4425 0.0262 0.070 Uiso 1 1 calc R . . C41 C 0.3803(10) 0.5199(4) 0.0242(4) 0.047(3) Uani 1 1 d . . . H41 H 0.3797 0.5232 -0.0059 0.057 Uiso 1 1 calc R . . C42 C 0.3824(9) 0.5554(4) 0.0914(4) 0.039(3) Uani 1 1 d . . . C43 C 0.3832(11) 0.5989(5) 0.1143(4) 0.047(3) Uani 1 1 d . . . C44 C 0.4504(9) 0.7009(4) 0.0150(4) 0.037(3) Uani 1 1 d . . . C45 C 0.2385(10) 0.6476(4) 0.0140(3) 0.036(3) Uani 1 1 d . . . C46 C 0.6045(9) 0.6251(3) 0.0318(3) 0.025(2) Uani 1 1 d . . . C47 C 0.4414(11) 0.6177(4) -0.0356(4) 0.043(3) Uani 1 1 d . . . C48 C 0.3956(14) 0.9272(5) 0.0752(5) 0.073(5) Uani 1 1 d . . . H48 H 0.3921 0.8996 0.0937 0.087 Uiso 1 1 calc R . . C49 C 0.3767(15) 0.9724(5) 0.0931(5) 0.074(4) Uani 1 1 d . . . H49 H 0.3536 0.9760 0.1221 0.089 Uiso 1 1 calc R . . C50 C 0.3926(13) 1.0122(5) 0.0670(6) 0.069(4) Uani 1 1 d . . . H50 H 0.3876 1.0445 0.0781 0.082 Uiso 1 1 calc R . . C51 C 0.4159(12) 1.0044(4) 0.0244(5) 0.054(3) Uani 1 1 d . . . H51 H 0.4189 1.0318 0.0057 0.065 Uiso 1 1 calc R . . C52 C 0.4354(10) 0.9574(4) 0.0076(4) 0.047(3) Uani 1 1 d . . . C53 C 0.4737(10) 0.9477(4) -0.0359(4) 0.043(3) Uani 1 1 d . . . C54 C 0.5181(13) 0.9861(5) -0.0629(5) 0.059(4) Uani 1 1 d . . . H54 H 0.5211 1.0189 -0.0528 0.071 Uiso 1 1 calc R . . C55 C 0.5557(13) 0.9750(5) -0.1029(5) 0.061(4) Uani 1 1 d . . . H55 H 0.5839 1.0007 -0.1209 0.073 Uiso 1 1 calc R . . C56 C 0.5545(13) 0.9271(6) -0.1187(5) 0.071(4) Uani 1 1 d . . . H56 H 0.5824 0.9190 -0.1466 0.085 Uiso 1 1 calc R . . C57 C 0.5083(11) 0.8913(4) -0.0898(5) 0.049(3) Uani 1 1 d . . . C58 C 0.5074(12) 0.8396(6) -0.1039(5) 0.061(4) Uani 1 1 d . . . C59 C 0.5513(19) 0.8265(7) -0.1438(6) 0.097(6) Uani 1 1 d . . . H59 H 0.5869 0.8504 -0.1621 0.116 Uiso 1 1 calc R . . C60 C 0.543(2) 0.7806(11) -0.1561(7) 0.127(9) Uani 1 1 d . . . H60 H 0.5685 0.7718 -0.1841 0.153 Uiso 1 1 calc R . . C61 C 0.501(2) 0.7474(8) -0.1310(9) 0.125(10) Uani 1 1 d . . . H61 H 0.5002 0.7141 -0.1399 0.150 Uiso 1 1 calc R . . C62 C 0.4565(15) 0.7604(6) -0.0896(6) 0.086(6) Uani 1 1 d . . . H62 H 0.4253 0.7357 -0.0712 0.103 Uiso 1 1 calc R . . C63 C 0.6963(14) 0.7199(7) 0.1604(4) 0.079(5) Uani 1 1 d . . . H63 H 0.7001 0.7521 0.1489 0.094 Uiso 1 1 calc R . . C64 C 0.6951(15) 0.6798(11) 0.1327(5) 0.109(9) Uani 1 1 d . . . H64 H 0.6996 0.6854 0.1029 0.131 Uiso 1 1 calc R . . C65 C 0.6879(17) 0.6351(10) 0.1468(6) 0.089(6) Uani 1 1 d . . . H65 H 0.6849 0.6068 0.1292 0.107 Uiso 1 1 calc R . . C66 C 0.685(4) 0.6342(14) 0.197(2) 0.27(3) Uani 1 1 d . . . C67 C 0.6754(16) 0.5998(19) 0.2028(10) 0.24(3) Uani 1 1 d . . . H67 H 0.6708 0.5784 0.1789 0.293 Uiso 1 1 calc R . . C68 C 0.666(2) 0.5746(7) 0.2489(10) 0.143(10) Uani 1 1 d . . . H68 H 0.6606 0.5405 0.2545 0.172 Uiso 1 1 calc R . . C69 C 0.6692(18) 0.6160(9) 0.2824(6) 0.108(7) Uani 1 1 d . . . C70 C 0.6618(15) 0.6132(9) 0.3293(7) 0.105(7) Uani 1 1 d . . . H70 H 0.6553 0.5827 0.3437 0.126 Uiso 1 1 calc R . . C71 C 0.6646(14) 0.6566(8) 0.3511(6) 0.088(6) Uani 1 1 d . . . H71 H 0.6584 0.6562 0.3813 0.105 Uiso 1 1 calc R . . C72 C 0.6763(13) 0.7010(7) 0.3304(4) 0.078(5) Uani 1 1 d . . . H72 H 0.6813 0.7302 0.3468 0.094 Uiso 1 1 calc R . . C73 C 0.6748(14) 0.6626(8) 0.2638(5) 0.083(5) Uani 1 1 d . . . C74 C 0.6821(15) 0.6714(9) 0.2181(6) 0.077(5) Uani 1 1 d . . . C75 C 0.8808(15) 0.7696(8) 0.2520(5) 0.092(6) Uani 1 1 d . . . C76 C 0.6927(15) 0.8148(8) 0.2985(5) 0.098(7) Uani 1 1 d . . . C77 C 0.7027(18) 0.8222(8) 0.2093(4) 0.096(7) Uani 1 1 d . . . C78 C 0.5025(18) 0.7737(7) 0.2463(5) 0.084(5) Uani 1 1 d . . . N1 N 0.3581(9) 0.6631(4) 0.4058(3) 0.049(2) Uani 1 1 d . . . N2 N 0.3294(8) 0.5718(4) 0.4368(3) 0.046(3) Uani 1 1 d . . . N3 N 0.4354(8) 0.7424(3) 0.5049(3) 0.036(2) Uani 1 1 d . . . N4 N 0.0858(8) 0.6568(3) 0.4856(3) 0.037(2) Uani 1 1 d . . . N5 N 0.6599(10) 0.6295(3) 0.4640(3) 0.049(3) Uani 1 1 d . . . N6 N 0.3919(10) 0.6003(4) 0.5638(4) 0.053(3) Uani 1 1 d . . . N7 N 0.4214(9) 0.8213(5) 0.5873(3) 0.061(3) Uani 1 1 d . . . N8 N 0.4058(9) 0.9115(5) 0.5498(4) 0.062(3) Uani 1 1 d . . . N9 N 0.3306(12) 0.9136(4) 0.4682(5) 0.070(4) Uani 1 1 d . . . N10 N 0.3952(8) 0.6416(4) 0.0922(3) 0.045(2) Uani 1 1 d . . . N11 N 0.3867(7) 0.5587(3) 0.0480(3) 0.035(2) Uani 1 1 d . . . N12 N 0.4753(8) 0.7430(3) 0.0086(4) 0.053(3) Uani 1 1 d . . . N13 N 0.7106(7) 0.6270(3) 0.0307(3) 0.031(2) Uani 1 1 d . . . N14 N 0.1353(8) 0.6583(3) 0.0045(3) 0.042(2) Uani 1 1 d . . . N15 N 0.4532(12) 0.6118(4) -0.0710(4) 0.064(3) Uani 1 1 d . . . N16 N 0.4191(10) 0.9185(4) 0.0330(4) 0.055(3) Uani 1 1 d . . . N17 N 0.4671(9) 0.9017(3) -0.0509(3) 0.044(2) Uani 1 1 d . . . N18 N 0.4581(10) 0.8076(4) -0.0765(4) 0.056(3) Uani 1 1 d . . . N19 N 0.6921(11) 0.7138(6) 0.2034(4) 0.067(3) Uani 1 1 d . . . N20 N 0.6806(11) 0.7041(5) 0.2872(4) 0.075(4) Uani 1 1 d . . . N21 N 0.9878(13) 0.7730(8) 0.2512(4) 0.119(7) Uani 1 1 d . . . N22 N 0.6920(16) 0.8401(7) 0.3292(4) 0.110(6) Uani 1 1 d . . . N23 N 0.7091(18) 0.8570(8) 0.1859(5) 0.125(7) Uani 1 1 d . . . N24 N 0.4004(16) 0.7729(7) 0.2435(5) 0.109(6) Uani 1 1 d . . . O1 O 0.2037(7) 0.7711(3) 0.5450(3) 0.048(2) Uani 1 1 d . . . H1B H 0.2050 0.7431 0.5569 0.058 Uiso 1 1 d R . . H1C H 0.1350 0.7678 0.5322 0.058 Uiso 1 1 d R . . O2 O 0.2014(8) 0.7979(3) 0.4560(3) 0.060(2) Uani 1 1 d . . . H2B H 0.1728 0.8098 0.4329 0.071 Uiso 1 1 d R . . H2C H 0.1336 0.7876 0.4662 0.071 Uiso 1 1 d R . . O3 O 0.4549(8) 0.8225(3) 0.4367(2) 0.049(2) Uani 1 1 d . . . H3B H 0.4535 0.8343 0.4116 0.059 Uiso 1 1 d R . . H3C H 0.5314 0.8215 0.4308 0.059 Uiso 1 1 d R . . O4 O 0.4943(8) 0.8204(3) 0.0733(3) 0.061(3) Uani 1 1 d . . . H4B H 0.5672 0.8268 0.0814 0.073 Uiso 1 1 d R . . H4C H 0.4483 0.8177 0.0951 0.073 Uiso 1 1 d R . . O5 O 0.2339(9) 0.8311(6) 0.0575(4) 0.116(5) Uani 1 1 d . . . H5B H 0.2641 0.8254 0.0820 0.139 Uiso 1 1 d R . . H5C H 0.1564 0.8270 0.0558 0.139 Uiso 1 1 d R . . O6 O 0.2394(7) 0.7689(3) -0.0210(5) 0.113(5) Uani 1 1 d . . . H6B H 0.2127 0.7405 -0.0145 0.135 Uiso 1 1 d R . . H6C H 0.1616 0.7720 -0.0228 0.135 Uiso 1 1 d R . . O7 O 0.7211(11) 0.8412(7) 0.0990(4) 0.151(8) Uani 1 1 d . . . O8 O 0.7076(8) 0.8191(3) 0.4171(3) 0.054(2) Uani 1 1 d . . . H8B H 0.7025 0.8258 0.3907 0.065 Uiso 1 1 d R . . H8C H 0.7590 0.8417 0.4226 0.065 Uiso 1 1 d R . . O9 O 0.4525(14) 0.8588(7) 0.3569(4) 0.164(8) Uani 1 1 d . . . H9B H 0.3779 0.8508 0.3614 0.197 Uiso 1 1 d R . . H9C H 0.4468 0.8806 0.3377 0.197 Uiso 1 1 d R . . O10 O 0.884(2) 0.9846(9) 0.2749(6) 0.091(7) Uani 0.50 1 d P . . O11 O 0.887(2) 0.9067(8) 0.3461(5) 0.107(10) Uani 0.50 1 d P . . O12 O 0.343(3) 0.8112(8) 0.1455(7) 0.117(11) Uani 0.50 1 d P . . O13 O 0.1067(17) 0.5899(11) 0.2223(6) 0.093(6) Uani 0.50 1 d PU A 1 O14 O 0.211(2) 0.8129(8) 0.2829(10) 0.107(9) Uani 0.50 1 d P B 1 O13' O -0.0046(18) 0.5995(11) 0.2354(6) 0.099(6) Uani 0.50 1 d PU C 2 O14' O 0.061(3) 0.8529(8) 0.3087(7) 0.102(8) Uani 0.50 1 d P D 2 O16 O 0.167(2) 0.8271(8) 0.3738(7) 0.092(5) Uani 0.50 1 d PU E 1 O17 O 0.041(4) 0.9794(8) 0.2004(8) 0.140(13) Uani 0.50 1 d P F 1 O15' O 0.9558(16) 0.8962(5) 0.1579(4) 0.046(4) Uani 0.50 1 d P G 2 O16' O 0.069(2) 0.8343(8) 0.3957(7) 0.086(5) Uani 0.50 1 d PU H 2 O17' O 0.265(2) 0.9577(12) 0.1942(7) 0.125(12) Uani 0.50 1 d P I 2 O18' O 0.349(4) 0.4449(8) 0.2591(11) 0.172(17) Uani 0.50 1 d P J 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0274(3) 0.0199(3) 0.0569(3) -0.0050(3) -0.0020(2) -0.0013(2) Nd2 0.0200(3) 0.0197(3) 0.0939(5) 0.0115(3) -0.0026(3) -0.0018(2) Ru1 0.0259(4) 0.0235(5) 0.0578(5) -0.0091(4) 0.0004(4) -0.0014(4) Ru2 0.0192(4) 0.0198(4) 0.0564(5) -0.0017(4) -0.0020(4) 0.0008(4) Ru3 0.0643(9) 0.1173(11) 0.0386(5) -0.0112(7) 0.0067(5) -0.0322(8) C1 0.044(7) 0.062(9) 0.037(6) -0.003(6) 0.005(5) -0.003(7) C2 0.086(11) 0.077(11) 0.072(10) -0.006(8) 0.013(9) -0.017(9) C3 0.118(16) 0.118(17) 0.067(10) -0.008(10) 0.010(10) -0.040(14) C4 0.054(9) 0.152(19) 0.067(10) -0.057(11) 0.019(7) -0.021(11) C5 0.25(3) 0.16(2) 0.064(11) -0.058(13) 0.036(14) -0.14(2) C6 0.107(15) 0.123(18) 0.103(14) -0.085(13) 0.034(12) -0.045(13) C7 0.087(12) 0.087(14) 0.096(13) -0.051(11) 0.038(10) -0.036(10) C8 0.077(11) 0.063(12) 0.122(15) -0.052(11) 0.033(11) -0.040(9) C9 0.057(9) 0.058(10) 0.128(15) -0.034(10) 0.038(10) -0.024(8) C10 0.043(7) 0.036(8) 0.108(11) -0.033(8) 0.026(7) -0.023(6) C11 0.055(9) 0.053(9) 0.066(9) -0.029(7) 0.010(7) -0.013(7) C12 0.039(7) 0.073(10) 0.053(8) -0.022(7) 0.006(6) -0.006(7) C13 0.023(5) 0.035(6) 0.046(6) 0.006(5) -0.014(5) 0.003(5) C14 0.054(8) 0.021(6) 0.043(6) -0.012(5) -0.012(5) 0.008(5) C15 0.041(7) 0.026(6) 0.051(7) -0.003(5) 0.003(5) 0.011(5) C16 0.028(6) 0.022(5) 0.052(7) -0.011(5) -0.001(5) 0.001(4) C17 0.056(9) 0.089(12) 0.072(10) 0.018(9) 0.001(8) 0.006(9) C18 0.064(11) 0.137(18) 0.076(11) 0.016(11) -0.003(9) 0.031(11) C19 0.12(2) 0.27(4) 0.12(2) -0.12(3) -0.056(17) 0.05(3) C20 0.16(2) 0.14(2) 0.12(2) -0.062(19) -0.054(17) 0.04(2) C21 0.046(8) 0.111(15) 0.077(10) -0.049(11) -0.007(7) -0.023(9) C22 0.048(9) 0.073(12) 0.132(16) -0.045(12) 0.022(10) -0.021(9) C23 0.092(14) 0.138(19) 0.105(14) -0.063(14) 0.036(11) -0.070(14) C24 0.126(19) 0.062(13) 0.16(2) -0.030(14) 0.060(17) -0.028(13) C25 0.083(13) 0.058(11) 0.21(2) -0.047(14) 0.087(16) -0.053(10) C26 0.071(10) 0.012(7) 0.150(16) -0.031(8) 0.036(11) -0.015(7) C27 0.059(9) 0.008(6) 0.197(19) 0.007(9) 0.057(12) 0.003(6) C28 0.078(14) 0.033(10) 0.24(3) 0.015(14) 0.098(18) -0.004(9) C29 0.075(14) 0.086(17) 0.23(3) 0.08(2) 0.076(19) 0.022(12) C30 0.110(15) 0.064(12) 0.124(16) 0.034(12) 0.039(12) 0.018(11) C31 0.082(11) 0.045(10) 0.107(14) 0.028(9) 0.005(10) 0.000(8) C32 0.042(7) 0.037(7) 0.077(9) -0.013(6) -0.002(6) 0.007(6) C33 0.070(10) 0.088(13) 0.066(9) -0.017(8) 0.010(8) 0.002(9) C34 0.078(11) 0.123(16) 0.058(9) -0.023(10) 0.012(8) -0.008(11) C35 0.053(9) 0.080(11) 0.061(8) 0.001(8) -0.005(7) -0.008(8) C36 0.065(10) 0.115(15) 0.077(10) 0.035(11) 0.025(9) -0.004(11) C37 0.066(10) 0.087(12) 0.069(10) 0.035(9) 0.006(8) 0.001(9) C38 0.035(7) 0.062(9) 0.074(9) 0.019(7) -0.002(6) 0.001(6) C39 0.048(8) 0.031(7) 0.085(10) 0.011(7) 0.001(7) -0.005(6) C40 0.041(7) 0.029(7) 0.105(11) 0.013(7) -0.017(7) -0.007(6) C41 0.028(6) 0.032(7) 0.081(9) 0.005(6) -0.004(6) -0.006(5) C42 0.020(5) 0.045(7) 0.051(7) 0.010(5) -0.002(5) -0.009(5) C43 0.036(7) 0.052(8) 0.054(7) 0.000(6) -0.001(5) 0.006(6) C44 0.014(5) 0.035(7) 0.063(7) 0.000(5) 0.002(5) 0.011(4) C45 0.030(6) 0.027(6) 0.052(7) -0.002(5) 0.008(5) -0.008(5) C46 0.020(5) 0.011(5) 0.045(6) -0.001(4) 0.005(4) 0.005(4) C47 0.036(7) 0.032(7) 0.062(8) 0.004(6) -0.009(6) 0.004(5) C48 0.073(10) 0.044(8) 0.100(11) 0.025(8) 0.041(9) 0.030(8) C49 0.084(11) 0.045(9) 0.093(11) -0.010(8) 0.015(9) 0.024(8) C50 0.050(9) 0.034(8) 0.121(14) 0.004(8) -0.012(9) 0.014(7) C51 0.064(8) 0.017(6) 0.081(9) 0.012(6) -0.012(8) -0.013(6) C52 0.038(6) 0.025(6) 0.077(8) 0.006(6) -0.006(6) -0.001(5) C53 0.034(6) 0.017(6) 0.077(9) 0.009(6) -0.017(6) -0.006(5) C54 0.061(9) 0.040(8) 0.075(9) 0.013(7) 0.002(7) -0.012(7) C55 0.056(8) 0.038(8) 0.089(11) 0.031(7) -0.004(8) -0.008(7) C56 0.049(8) 0.070(11) 0.093(11) 0.012(9) -0.011(8) -0.015(8) C57 0.037(7) 0.031(7) 0.078(9) 0.010(6) -0.011(6) -0.014(6) C58 0.041(7) 0.068(11) 0.073(9) -0.013(8) -0.009(6) -0.009(7) C59 0.130(16) 0.061(11) 0.100(13) -0.038(11) 0.016(11) -0.020(12) C60 0.13(2) 0.16(3) 0.089(15) -0.001(17) 0.011(14) -0.01(2) C61 0.13(2) 0.092(17) 0.16(2) -0.079(16) -0.078(18) 0.031(14) C62 0.068(11) 0.070(11) 0.119(14) -0.004(10) -0.065(11) -0.006(9) C63 0.069(10) 0.118(14) 0.049(8) -0.037(9) 0.011(7) -0.027(10) C64 0.049(9) 0.23(3) 0.047(9) -0.030(14) 0.009(7) -0.039(14) C65 0.068(11) 0.124(18) 0.074(12) -0.025(12) 0.006(9) -0.015(13) C66 0.23(5) 0.13(3) 0.44(8) 0.18(4) 0.09(5) 0.06(3) C67 0.030(10) 0.55(7) 0.15(2) -0.25(3) -0.030(12) 0.03(2) C68 0.11(2) 0.072(13) 0.24(3) -0.059(18) -0.03(2) -0.004(13) C69 0.080(13) 0.16(2) 0.088(13) 0.035(14) -0.016(10) -0.005(14) C70 0.043(10) 0.14(2) 0.134(18) 0.002(15) -0.011(10) -0.023(11) C71 0.052(10) 0.14(2) 0.069(10) 0.011(12) 0.000(8) -0.018(11) C72 0.058(10) 0.128(16) 0.048(8) -0.004(9) 0.009(7) -0.028(10) C73 0.056(10) 0.118(16) 0.076(11) -0.023(11) 0.007(8) -0.034(10) C74 0.062(10) 0.090(15) 0.080(11) -0.030(12) -0.014(8) 0.002(11) C75 0.057(12) 0.179(19) 0.040(7) -0.021(10) 0.007(7) -0.011(12) C76 0.060(10) 0.17(2) 0.060(10) 0.013(11) 0.009(8) -0.044(12) C77 0.104(13) 0.148(19) 0.037(8) 0.010(10) 0.001(8) -0.055(14) C78 0.062(12) 0.126(15) 0.064(10) -0.005(10) 0.005(8) -0.028(11) N1 0.031(5) 0.058(7) 0.059(6) -0.006(5) 0.004(4) -0.011(5) N2 0.024(5) 0.033(6) 0.081(7) -0.017(5) 0.006(5) -0.007(4) N3 0.032(5) 0.020(5) 0.055(5) -0.004(4) 0.003(4) 0.005(4) N4 0.021(5) 0.031(5) 0.059(6) 0.000(4) -0.003(4) 0.014(4) N5 0.045(7) 0.020(5) 0.082(7) -0.003(5) 0.007(5) 0.005(5) N6 0.059(7) 0.029(6) 0.070(7) -0.006(5) -0.004(6) 0.015(5) N7 0.028(5) 0.086(9) 0.068(7) -0.010(7) 0.002(5) -0.001(6) N8 0.032(6) 0.066(9) 0.088(9) -0.041(7) 0.010(6) -0.013(6) N9 0.075(9) 0.029(6) 0.106(10) 0.004(6) 0.034(8) 0.001(6) N10 0.031(5) 0.044(6) 0.059(6) -0.010(5) -0.003(4) 0.002(5) N11 0.014(4) 0.027(5) 0.063(6) 0.003(4) -0.004(4) -0.006(4) N12 0.034(5) 0.024(5) 0.100(8) 0.010(5) -0.015(6) 0.003(4) N13 0.021(5) 0.014(4) 0.059(6) -0.003(4) 0.006(4) -0.002(3) N14 0.025(5) 0.030(5) 0.071(6) 0.004(4) 0.000(5) -0.006(4) N15 0.087(9) 0.037(7) 0.067(8) 0.001(5) -0.004(7) 0.032(6) N16 0.043(6) 0.036(6) 0.086(8) 0.010(5) 0.005(6) 0.005(5) N17 0.035(5) 0.029(6) 0.068(7) 0.008(5) -0.008(5) -0.005(4) N18 0.049(7) 0.025(6) 0.094(8) -0.009(6) -0.019(6) -0.003(5) N19 0.056(7) 0.094(11) 0.053(7) -0.023(7) 0.005(6) -0.019(7) N20 0.052(7) 0.099(11) 0.075(9) -0.013(7) 0.016(6) -0.014(7) N21 0.037(8) 0.26(2) 0.061(8) -0.059(11) 0.010(6) -0.027(11) N22 0.130(13) 0.152(16) 0.047(7) -0.042(9) 0.001(8) -0.028(12) N23 0.128(14) 0.159(18) 0.089(11) -0.011(12) 0.023(10) -0.061(14) N24 0.073(11) 0.167(17) 0.088(11) -0.043(11) 0.019(8) -0.028(11) O1 0.031(4) 0.042(5) 0.072(5) 0.017(4) -0.004(4) -0.002(4) O2 0.044(5) 0.076(7) 0.058(5) 0.005(5) -0.006(4) -0.023(5) O3 0.052(5) 0.046(5) 0.049(4) -0.006(4) -0.002(4) -0.007(4) O4 0.037(5) 0.062(7) 0.083(6) 0.014(5) -0.018(4) -0.003(4) O5 0.042(6) 0.196(15) 0.108(8) 0.071(10) -0.019(5) -0.031(8) O6 0.016(4) 0.030(5) 0.292(18) -0.006(8) -0.011(7) -0.006(4) O7 0.078(8) 0.29(2) 0.087(8) 0.066(11) -0.027(6) -0.106(11) O8 0.062(5) 0.045(5) 0.056(5) -0.003(4) -0.003(4) 0.002(4) O9 0.122(12) 0.28(2) 0.090(9) 0.034(12) 0.025(9) 0.073(14) O10 0.071(14) 0.14(2) 0.066(12) -0.040(13) -0.003(11) 0.018(14) O11 0.19(2) 0.092(15) 0.037(9) -0.042(9) 0.069(12) -0.124(17) O12 0.19(3) 0.077(16) 0.088(15) -0.010(12) 0.100(18) -0.023(17) O13 0.040(8) 0.187(17) 0.051(9) 0.028(10) -0.009(7) -0.020(11) O14 0.060(14) 0.047(14) 0.21(3) -0.009(15) 0.020(16) -0.001(11) O13' 0.050(8) 0.189(17) 0.058(9) 0.022(10) -0.006(7) -0.020(11) O14' 0.15(2) 0.073(15) 0.083(14) -0.035(12) 0.013(15) -0.023(16) O16 0.114(14) 0.071(10) 0.090(12) 0.000(9) -0.007(9) 0.033(11) O17 0.27(4) 0.034(13) 0.12(2) -0.029(13) 0.01(2) -0.015(19) O15' 0.072(12) 0.031(9) 0.035(8) -0.003(7) -0.009(8) -0.022(8) O16' 0.108(14) 0.067(10) 0.083(11) -0.004(9) -0.007(9) 0.039(11) O17' 0.085(17) 0.21(3) 0.079(15) -0.055(18) 0.017(13) -0.087(19) O18' 0.29(5) 0.030(12) 0.19(3) -0.013(15) 0.11(3) 0.012(19) _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 Nd1 O3 2.501(8) . ? Nd1 O2 2.502(8) . ? Nd1 N4 2.530(9) 4_566 ? Nd1 N3 2.536(8) . ? Nd1 N5 2.548(11) 4_466 ? Nd1 O1 2.567(7) . ? Nd1 N7 2.581(11) . ? Nd1 N9 2.628(12) . ? Nd1 N8 2.636(11) . ? Nd2 O4 2.478(8) . ? Nd2 N12 2.528(9) . ? Nd2 N14 2.540(9) 4_565 ? Nd2 O5 2.545(11) . ? Nd2 O6 2.549(8) . ? Nd2 N18 2.587(12) . ? Nd2 N13 2.589(8) 4_465 ? Nd2 N16 2.597(10) . ? Nd2 N17 2.627(10) . ? Ru1 C13 1.935(11) . ? Ru1 C15 1.990(12) . ? Ru1 C16 2.019(12) . ? Ru1 C14 2.029(13) . ? Ru1 N1 2.106(10) . ? Ru1 N2 2.138(9) . ? Ru2 C44 1.930(11) . ? Ru2 C47 1.989(14) . ? Ru2 C45 2.024(11) . ? Ru2 C46 2.043(10) . ? Ru2 N10 2.104(9) . ? Ru2 N11 2.156(8) . ? Ru3 C77 1.928(19) . ? Ru3 C76 1.97(2) . ? Ru3 C75 2.041(17) . ? Ru3 C78 2.070(19) . ? Ru3 N19 2.093(12) . ? Ru3 N20 2.132(14) . ? C1 N1 1.330(15) . ? C1 C2 1.396(18) . ? C1 H1 0.9500 . ? C2 C3 1.37(2) . ? C2 H2 0.9500 . ? C3 C4 1.46(3) . ? C3 H3 0.9500 . ? C4 C12 1.39(2) . ? C4 C5 1.41(2) . ? C5 C6 1.40(3) . ? C5 H5 0.9500 . ? C6 C7 1.49(3) . ? C6 H6 0.9500 . ? C7 C8 1.36(2) . ? C7 C11 1.407(19) . ? C8 C9 1.35(2) . ? C8 H8 0.9500 . ? C9 C10 1.345(19) . ? C9 H9 0.9500 . ? C10 N2 1.301(16) . ? C10 H10 0.9500 . ? C11 N2 1.365(17) . ? C11 C12 1.422(19) . ? C12 N1 1.392(15) . ? C13 N3 1.190(13) . ? C14 N4 1.144(14) . ? C15 N5 1.167(14) . ? C16 N6 1.132(14) . ? C17 N7 1.361(19) . ? C17 C18 1.41(2) . ? C17 H17 0.9500 . ? C18 C19 1.40(3) . ? C18 H18 0.9500 . ? C19 C20 1.34(4) . ? C19 H19 0.9500 . ? C20 C21 1.32(3) . ? C20 H20 0.9500 . ? C21 N7 1.346(18) . ? C21 C22 1.48(3) . ? C22 N8 1.35(2) . ? C22 C23 1.44(2) . ? C23 C24 1.35(3) . ? C23 H23 0.9500 . ? C24 C25 1.43(3) . ? C24 H24 0.9500 . ? C25 C26 1.35(2) . ? C25 H25 0.9500 . ? C26 N8 1.30(2) . ? C26 C27 1.48(3) . ? C27 N9 1.37(2) . ? C27 C28 1.41(3) . ? C28 C29 1.36(3) . ? C28 H28 0.9500 . ? C29 C30 1.35(3) . ? C29 H29 0.9500 . ? C30 C31 1.34(2) . ? C30 H30 0.9500 . ? C31 N9 1.34(2) . ? C31 H31 0.9500 . ? C32 N10 1.311(14) . ? C32 C33 1.395(19) . ? C32 H32 0.9500 . ? C33 C34 1.36(2) . ? C33 H33 0.9500 . ? C34 C35 1.49(2) . ? C34 H34 0.9500 . ? C35 C36 1.36(2) . ? C35 C43 1.418(17) . ? C36 C37 1.41(2) . ? C36 H36 0.9500 . ? C37 C38 1.437(19) . ? C37 H37 0.9500 . ? C38 C39 1.374(18) . ? C38 C42 1.432(17) . ? C39 C40 1.330(18) . ? C39 H39 0.9500 . ? C40 C41 1.469(16) . ? C40 H40 0.9500 . ? C41 N11 1.294(14) . ? C41 H41 0.9500 . ? C42 N11 1.367(14) . ? C42 C43 1.387(16) . ? C43 N10 1.361(15) . ? C44 N12 1.198(13) . ? C45 N14 1.195(13) . ? C46 N13 1.152(12) . ? C47 N15 1.129(15) . ? C48 N16 1.368(17) . ? C48 C49 1.370(19) . ? C48 H48 0.9500 . ? C49 C50 1.37(2) . ? C49 H49 0.9500 . ? C50 C51 1.376(19) . ? C50 H50 0.9500 . ? C51 C52 1.401(16) . ? C51 H51 0.9500 . ? C52 N16 1.340(15) . ? C52 C53 1.451(18) . ? C53 N17 1.342(14) . ? C53 C54 1.430(16) . ? C54 C55 1.35(2) . ? C54 H54 0.9500 . ? C55 C56 1.40(2) . ? C55 H55 0.9500 . ? C56 C57 1.422(18) . ? C56 H56 0.9500 . ? C57 N17 1.330(16) . ? C57 C58 1.479(18) . ? C58 N18 1.337(17) . ? C58 C59 1.39(2) . ? C59 C60 1.31(3) . ? C59 H59 0.9500 . ? C60 C61 1.28(3) . ? C60 H60 0.9500 . ? C61 C62 1.43(3) . ? C61 H61 0.9500 . ? C62 N18 1.352(18) . ? C62 H62 0.9500 . ? C63 N19 1.361(18) . ? C63 C64 1.40(3) . ? C63 H63 0.9500 . ? C64 C65 1.30(3) . ? C64 H64 0.9500 . ? C65 C66 1.56(6) . ? C65 H65 0.9500 . ? C66 C67 0.96(6) . ? C66 C74 1.22(6) . ? C67 C68 1.60(5) . ? C67 H67 0.9500 . ? C68 C69 1.54(3) . ? C68 H68 0.9500 . ? C69 C73 1.40(3) . ? C69 C70 1.47(3) . ? C70 C71 1.37(3) . ? C70 H70 0.9500 . ? C71 C72 1.38(2) . ? C71 H71 0.9500 . ? C72 N20 1.356(17) . ? C72 H72 0.9500 . ? C73 N20 1.35(2) . ? C73 C74 1.46(3) . ? C74 N19 1.25(2) . ? C75 N21 1.164(18) . ? C76 N22 1.18(2) . ? C77 N23 1.20(2) . ? C78 N24 1.11(2) . ? N4 Nd1 2.530(9) 4_466 ? N5 Nd1 2.548(10) 4_566 ? N13 Nd2 2.589(8) 4_565 ? N14 Nd2 2.540(9) 4_465 ? O1 H1B 0.8501 . ? O1 H1C 0.8502 . ? O2 H2B 0.8502 . ? O2 H2C 0.8500 . ? O3 H3B 0.8497 . ? O3 H3C 0.8500 . ? O4 H4B 0.8498 . ? O4 H4C 0.8499 . ? O5 H5B 0.8497 . ? O5 H5C 0.8500 . ? O6 H6B 0.8503 . ? O6 H6C 0.8500 . ? O8 H8B 0.8498 . ? O8 H8C 0.8500 . ? O9 H9B 0.8493 . ? O9 H9C 0.8503 . ? 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 O3 Nd1 O2 70.7(3) . . ? O3 Nd1 N4 69.7(3) . 4_566 ? O2 Nd1 N4 139.3(3) . 4_566 ? O3 Nd1 N3 74.9(3) . . ? O2 Nd1 N3 82.7(3) . . ? N4 Nd1 N3 78.6(3) 4_566 . ? O3 Nd1 N5 134.2(3) . 4_466 ? O2 Nd1 N5 79.5(3) . 4_466 ? N4 Nd1 N5 137.2(3) 4_566 4_466 ? N3 Nd1 N5 135.2(3) . 4_466 ? O3 Nd1 O1 129.0(3) . . ? O2 Nd1 O1 69.4(3) . . ? N4 Nd1 O1 133.8(3) 4_566 . ? N3 Nd1 O1 69.7(3) . . ? N5 Nd1 O1 65.5(3) 4_466 . ? O3 Nd1 N7 137.3(3) . . ? O2 Nd1 N7 141.6(3) . . ? N4 Nd1 N7 70.8(3) 4_566 . ? N3 Nd1 N7 82.2(3) . . ? N5 Nd1 N7 86.8(3) 4_466 . ? O1 Nd1 N7 72.2(3) . . ? O3 Nd1 N9 71.4(3) . . ? O2 Nd1 N9 85.2(4) . . ? N4 Nd1 N9 90.6(3) 4_566 . ? N3 Nd1 N9 146.3(3) . . ? N5 Nd1 N9 72.3(3) 4_466 . ? O1 Nd1 N9 133.7(3) . . ? N7 Nd1 N9 124.4(4) . . ? O3 Nd1 N8 114.8(3) . . ? O2 Nd1 N8 139.0(4) . . ? N4 Nd1 N8 68.8(3) 4_566 . ? N3 Nd1 N8 138.2(4) . . ? N5 Nd1 N8 68.6(3) 4_466 . ? O1 Nd1 N8 116.1(3) . . ? N7 Nd1 N8 63.1(4) . . ? N9 Nd1 N8 61.3(4) . . ? O4 Nd2 N12 71.7(3) . . ? O4 Nd2 N14 71.6(3) . 4_565 ? N12 Nd2 N14 79.1(3) . 4_565 ? O4 Nd2 O5 70.0(3) . . ? N12 Nd2 O5 99.4(4) . . ? N14 Nd2 O5 139.8(3) 4_565 . ? O4 Nd2 O6 116.8(4) . . ? N12 Nd2 O6 67.2(3) . . ? N14 Nd2 O6 138.5(3) 4_565 . ? O5 Nd2 O6 71.9(4) . . ? O4 Nd2 N18 137.6(3) . . ? N12 Nd2 N18 77.5(4) . . ? N14 Nd2 N18 74.6(3) 4_565 . ? O5 Nd2 N18 145.0(4) . . ? O6 Nd2 N18 74.9(4) . . ? O4 Nd2 N13 136.5(3) . 4_465 ? N12 Nd2 N13 134.9(3) . 4_465 ? N14 Nd2 N13 136.1(3) 4_565 4_465 ? O5 Nd2 N13 71.6(3) . 4_465 ? O6 Nd2 N13 68.0(3) . 4_465 ? N18 Nd2 N13 85.9(3) . 4_465 ? O4 Nd2 N16 74.4(3) . . ? N12 Nd2 N16 144.8(3) . . ? N14 Nd2 N16 81.6(3) 4_565 . ? O5 Nd2 N16 77.2(4) . . ? O6 Nd2 N16 139.6(3) . . ? N18 Nd2 N16 124.8(3) . . ? N13 Nd2 N16 78.0(3) 4_465 . ? O4 Nd2 N17 123.1(3) . . ? N12 Nd2 N17 132.3(3) . . ? N14 Nd2 N17 66.9(3) 4_565 . ? O5 Nd2 N17 128.2(4) . . ? O6 Nd2 N17 120.1(4) . . ? N18 Nd2 N17 62.2(3) . . ? N13 Nd2 N17 69.1(3) 4_465 . ? N16 Nd2 N17 62.7(3) . . ? C13 Ru1 C15 85.5(4) . . ? C13 Ru1 C16 88.9(4) . . ? C15 Ru1 C16 86.9(4) . . ? C13 Ru1 C14 90.6(4) . . ? C15 Ru1 C14 175.2(4) . . ? C16 Ru1 C14 90.3(4) . . ? C13 Ru1 N1 93.9(4) . . ? C15 Ru1 N1 92.3(4) . . ? C16 Ru1 N1 177.0(4) . . ? C14 Ru1 N1 90.7(4) . . ? C13 Ru1 N2 172.6(4) . . ? C15 Ru1 N2 94.1(4) . . ? C16 Ru1 N2 98.4(4) . . ? C14 Ru1 N2 90.1(4) . . ? N1 Ru1 N2 78.7(4) . . ? C44 Ru2 C47 90.0(5) . . ? C44 Ru2 C45 86.9(4) . . ? C47 Ru2 C45 89.1(5) . . ? C44 Ru2 C46 86.0(4) . . ? C47 Ru2 C46 86.5(4) . . ? C45 Ru2 C46 171.6(4) . . ? C44 Ru2 N10 94.8(4) . . ? C47 Ru2 N10 174.9(4) . . ? C45 Ru2 N10 92.8(4) . . ? C46 Ru2 N10 92.2(4) . . ? C44 Ru2 N11 171.7(4) . . ? C47 Ru2 N11 98.0(4) . . ? C45 Ru2 N11 95.7(4) . . ? C46 Ru2 N11 92.0(3) . . ? N10 Ru2 N11 77.1(4) . . ? C77 Ru3 C76 92.0(7) . . ? C77 Ru3 C75 87.8(8) . . ? C76 Ru3 C75 88.2(6) . . ? C77 Ru3 C78 88.6(8) . . ? C76 Ru3 C78 90.1(7) . . ? C75 Ru3 C78 175.9(8) . . ? C77 Ru3 N19 94.9(7) . . ? C76 Ru3 N19 173.1(7) . . ? C75 Ru3 N19 91.9(6) . . ? C78 Ru3 N19 90.3(6) . . ? C77 Ru3 N20 172.3(6) . . ? C76 Ru3 N20 95.6(6) . . ? C75 Ru3 N20 92.8(7) . . ? C78 Ru3 N20 91.1(6) . . ? N19 Ru3 N20 77.4(5) . . ? N1 C1 C2 124.9(13) . . ? N1 C1 H1 117.5 . . ? C2 C1 H1 117.5 . . ? C3 C2 C1 119.7(16) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 116.6(16) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? C12 C4 C5 118(2) . . ? C12 C4 C3 120.2(15) . . ? C5 C4 C3 122.2(18) . . ? C6 C5 C4 121.1(19) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 122.1(15) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C11 119.9(17) . . ? C8 C7 C6 125.3(16) . . ? C11 C7 C6 114.8(17) . . ? C9 C8 C7 118.3(15) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C10 C9 C8 119.9(17) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 124.7(16) . . ? N2 C10 H10 117.6 . . ? C9 C10 H10 117.6 . . ? N2 C11 C7 119.7(14) . . ? N2 C11 C12 118.7(11) . . ? C7 C11 C12 121.6(14) . . ? N1 C12 C4 120.9(14) . . ? N1 C12 C11 116.2(11) . . ? C4 C12 C11 122.9(14) . . ? N3 C13 Ru1 178.6(10) . . ? N4 C14 Ru1 175.9(10) . . ? N5 C15 Ru1 172.7(10) . . ? N6 C16 Ru1 174.2(9) . . ? N7 C17 C18 119.6(17) . . ? N7 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 118(2) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C20 C19 C18 120(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 N7 124(2) . . ? C20 C21 C22 121(2) . . ? N7 C21 C22 114.9(15) . . ? N8 C22 C23 121(2) . . ? N8 C22 C21 120.2(14) . . ? C23 C22 C21 119(2) . . ? C24 C23 C22 122(2) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 115(2) . . ? C23 C24 H24 122.7 . . ? C25 C24 H24 122.7 . . ? C26 C25 C24 120(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? N8 C26 C25 126(2) . . ? N8 C26 C27 113.9(12) . . ? C25 C26 C27 119.7(19) . . ? N9 C27 C28 117(2) . . ? N9 C27 C26 119.7(13) . . ? C28 C27 C26 123.7(18) . . ? C29 C28 C27 122(2) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C30 C29 C28 118(2) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? C31 C30 C29 122(2) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 N9 120.9(18) . . ? C30 C31 H31 119.5 . . ? N9 C31 H31 119.5 . . ? N10 C32 C33 124.2(13) . . ? N10 C32 H32 117.9 . . ? C33 C32 H32 117.9 . . ? C34 C33 C32 120.0(15) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.3(14) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C43 123.0(15) . . ? C36 C35 C34 123.2(15) . . ? C43 C35 C34 113.5(14) . . ? C35 C36 C37 120.5(15) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.4(14) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C42 119.0(12) . . ? C39 C38 C37 123.6(13) . . ? C42 C38 C37 117.0(13) . . ? C40 C39 C38 120.6(12) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.1(13) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? N11 C41 C40 120.5(13) . . ? N11 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? N11 C42 C43 117.3(10) . . ? N11 C42 C38 119.4(11) . . ? C43 C42 C38 123.3(11) . . ? N10 C43 C42 118.1(10) . . ? N10 C43 C35 125.2(12) . . ? C42 C43 C35 116.5(12) . . ? N12 C44 Ru2 177.4(9) . . ? N14 C45 Ru2 175.5(9) . . ? N13 C46 Ru2 169.3(9) . . ? N15 C47 Ru2 176.3(11) . . ? N16 C48 C49 125.4(13) . . ? N16 C48 H48 117.3 . . ? C49 C48 H48 117.3 . . ? C50 C49 C48 116.8(15) . . ? C50 C49 H49 121.6 . . ? C48 C49 H49 121.6 . . ? C49 C50 C51 118.7(13) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C50 C51 C52 122.2(12) . . ? C50 C51 H51 118.9 . . ? C52 C51 H51 118.9 . . ? N16 C52 C51 118.9(12) . . ? N16 C52 C53 116.8(10) . . ? C51 C52 C53 124.3(11) . . ? N17 C53 C54 119.8(12) . . ? N17 C53 C52 119.0(10) . . ? C54 C53 C52 121.2(11) . . ? C55 C54 C53 119.0(13) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C54 C55 C56 122.3(13) . . ? C54 C55 H55 118.8 . . ? C56 C55 H55 118.8 . . ? C55 C56 C57 114.7(14) . . ? C55 C56 H56 122.6 . . ? C57 C56 H56 122.6 . . ? N17 C57 C56 123.9(12) . . ? N17 C57 C58 118.3(11) . . ? C56 C57 C58 117.8(14) . . ? N18 C58 C59 123.3(15) . . ? N18 C58 C57 115.7(12) . . ? C59 C58 C57 120.9(15) . . ? C60 C59 C58 119(2) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C61 C60 C59 121(2) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C60 C61 C62 120(2) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? N18 C62 C61 120.5(18) . . ? N18 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? N19 C63 C64 121.3(19) . . ? N19 C63 H63 119.4 . . ? C64 C63 H63 119.4 . . ? C65 C64 C63 121.7(18) . . ? C65 C64 H64 119.1 . . ? C63 C64 H64 119.1 . . ? C64 C65 C66 111(2) . . ? C64 C65 H65 124.5 . . ? C66 C65 H65 124.6 . . ? C67 C66 C74 134(7) . . ? C67 C66 C65 103(6) . . ? C74 C66 C65 123(3) . . ? C66 C67 C68 127(5) . . ? C66 C67 H67 116.5 . . ? C68 C67 H67 116.4 . . ? C69 C68 C67 107(2) . . ? C69 C68 H68 126.2 . . ? C67 C68 H68 126.3 . . ? C73 C69 C70 118(2) . . ? C73 C69 C68 112.4(18) . . ? C70 C69 C68 130(2) . . ? C71 C70 C69 117(2) . . ? C71 C70 H70 121.6 . . ? C69 C70 H70 121.6 . . ? C70 C71 C72 121.8(18) . . ? C70 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? N20 C72 C71 121.8(17) . . ? N20 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? N20 C73 C69 122.5(17) . . ? N20 C73 C74 113.2(19) . . ? C69 C73 C74 124.2(18) . . ? C66 C74 N19 125(3) . . ? C66 C74 C73 114(3) . . ? N19 C74 C73 121.3(17) . . ? N21 C75 Ru3 175(2) . . ? N22 C76 Ru3 176.5(18) . . ? N23 C77 Ru3 176.5(17) . . ? N24 C78 Ru3 175.1(19) . . ? C1 N1 C12 117.4(11) . . ? C1 N1 Ru1 128.8(8) . . ? C12 N1 Ru1 113.8(9) . . ? C10 N2 C11 117.4(11) . . ? C10 N2 Ru1 130.1(10) . . ? C11 N2 Ru1 112.5(8) . . ? C13 N3 Nd1 141.7(7) . . ? C14 N4 Nd1 172.5(9) . 4_466 ? C15 N5 Nd1 145.3(9) . 4_566 ? C21 N7 C17 118.2(15) . . ? C21 N7 Nd1 123.0(12) . . ? C17 N7 Nd1 118.2(10) . . ? C26 N8 C22 116.3(14) . . ? C26 N8 Nd1 125.3(11) . . ? C22 N8 Nd1 118.3(11) . . ? C31 N9 C27 120.8(15) . . ? C31 N9 Nd1 119.2(9) . . ? C27 N9 Nd1 119.7(12) . . ? C32 N10 C43 117.4(11) . . ? C32 N10 Ru2 128.3(9) . . ? C43 N10 Ru2 114.3(8) . . ? C41 N11 C42 121.2(10) . . ? C41 N11 Ru2 126.0(8) . . ? C42 N11 Ru2 112.6(7) . . ? C44 N12 Nd2 148.7(8) . . ? C46 N13 Nd2 147.0(8) . 4_565 ? C45 N14 Nd2 167.1(8) . 4_465 ? C52 N16 C48 117.4(11) . . ? C52 N16 Nd2 120.9(9) . . ? C48 N16 Nd2 121.2(8) . . ? C57 N17 C53 120.1(10) . . ? C57 N17 Nd2 120.2(7) . . ? C53 N17 Nd2 119.0(8) . . ? C58 N18 C62 115.5(14) . . ? C58 N18 Nd2 122.6(8) . . ? C62 N18 Nd2 121.1(11) . . ? C74 N19 C63 118.8(15) . . ? C74 N19 Ru3 114.4(11) . . ? C63 N19 Ru3 126.8(13) . . ? C73 N20 C72 119.2(16) . . ? C73 N20 Ru3 113.7(11) . . ? C72 N20 Ru3 127.1(12) . . ? Nd1 O1 H1B 138.1 . . ? Nd1 O1 H1C 114.8 . . ? H1B O1 H1C 97.2 . . ? Nd1 O2 H2B 132.2 . . ? Nd1 O2 H2C 116.5 . . ? H2B O2 H2C 97.4 . . ? Nd1 O3 H3B 142.6 . . ? Nd1 O3 H3C 128.2 . . ? H3B O3 H3C 80.1 . . ? Nd2 O4 H4B 128.4 . . ? Nd2 O4 H4C 120.6 . . ? H4B O4 H4C 108.8 . . ? Nd2 O5 H5B 110.3 . . ? Nd2 O5 H5C 132.0 . . ? H5B O5 H5C 114.5 . . ? Nd2 O6 H6B 140.8 . . ? Nd2 O6 H6C 130.1 . . ? H6B O6 H6C 76.7 . . ? H8B O8 H8C 94.7 . . ? H9B O9 H9C 103.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.335 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.137 #===END data_imw624m _database_code_depnum_ccdc_archive 'CCDC 636989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H196 N48 Nd4 O52 Ru6' _chemical_formula_weight 4758.99 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 21.4922(12) _cell_length_b 26.3727(15) _cell_length_c 17.1830(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9739.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4776 _exptl_absorpt_coefficient_mu 1.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3057 _exptl_absorpt_correction_T_max 0.8837 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCDarea detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73071 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8790 _reflns_number_gt 7783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+100.6003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8790 _refine_ls_number_parameters 655 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd -0.287625(15) 0.426143(14) 0.746807(19) 0.01370(13) Uani 1 1 d . . . Ru1 Ru -0.04403(2) 0.47269(2) 0.74596(3) 0.01379(16) Uani 1 1 d . . . Ru2 Ru -0.21173(3) 0.7500 0.57609(5) 0.0185(2) Uani 1 2 d S . . N1 N -0.0217(2) 0.5347(2) 0.8202(3) 0.0194(12) Uani 1 1 d . . . N2 N -0.0264(2) 0.5323(2) 0.6655(3) 0.0183(12) Uani 1 1 d . . . N3 N -0.0686(3) 0.3938(3) 0.8794(4) 0.0304(15) Uani 1 1 d . . . N4 N -0.0669(3) 0.3862(2) 0.6242(4) 0.0282(14) Uani 1 1 d . . . N5 N -0.1921(2) 0.4827(2) 0.7375(3) 0.0152(11) Uani 1 1 d . . . N7 N -0.3033(3) 0.4548(3) 0.6025(4) 0.0337(16) Uani 1 1 d . . . N8 N -0.3207(3) 0.5206(2) 0.7233(4) 0.0261(14) Uani 1 1 d . . . N9 N -0.3083(3) 0.4811(2) 0.8698(3) 0.0255(14) Uani 1 1 d . . . N10 N -0.1796(3) 0.6997(2) 0.6626(3) 0.0231(13) Uani 1 1 d . . . N11 N -0.0775(5) 0.7500 0.4932(7) 0.052(3) Uani 1 2 d S . . N12 N -0.3455(4) 0.7500 0.6580(5) 0.029(2) Uani 1 2 d S . . N13 N -0.2581(3) 0.6635(3) 0.4648(4) 0.047(2) Uani 1 1 d . . . C1 C -0.0189(3) 0.5356(3) 0.8979(4) 0.0277(16) Uani 1 1 d . . . H1 H -0.0289 0.5055 0.9258 0.033 Uiso 1 1 calc R . . C2 C -0.0018(4) 0.5787(3) 0.9399(5) 0.0361(19) Uani 1 1 d . . . H2 H -0.0001 0.5775 0.9951 0.043 Uiso 1 1 calc R . . C3 C 0.0123(4) 0.6225(3) 0.9018(5) 0.0338(18) Uani 1 1 d . . . H3 H 0.0241 0.6519 0.9300 0.041 Uiso 1 1 calc R . . C4 C 0.0092(3) 0.6236(3) 0.8197(5) 0.0279(16) Uani 1 1 d . . . C5 C 0.0214(4) 0.6683(3) 0.7741(6) 0.038(2) Uani 1 1 d . . . H5 H 0.0333 0.6988 0.7995 0.046 Uiso 1 1 calc R . . C6 C 0.0161(4) 0.6676(3) 0.6962(5) 0.0342(18) Uani 1 1 d . . . H6 H 0.0234 0.6978 0.6675 0.041 Uiso 1 1 calc R . . C7 C -0.0006(3) 0.6220(3) 0.6554(5) 0.0276(17) Uani 1 1 d . . . C8 C -0.0072(4) 0.6196(3) 0.5747(5) 0.0350(19) Uani 1 1 d . . . H8 H -0.0005 0.6488 0.5434 0.042 Uiso 1 1 calc R . . C9 C -0.0237(4) 0.5739(3) 0.5413(5) 0.0328(18) Uani 1 1 d . . . H9 H -0.0295 0.5717 0.4866 0.039 Uiso 1 1 calc R . . C10 C -0.0318(3) 0.5309(3) 0.5877(4) 0.0238(15) Uani 1 1 d . . . H10 H -0.0416 0.4996 0.5634 0.029 Uiso 1 1 calc R . . C11 C -0.0115(3) 0.5773(3) 0.6984(4) 0.0223(15) Uani 1 1 d . . . C12 C -0.0079(3) 0.5786(3) 0.7816(4) 0.0238(15) Uani 1 1 d . . . C13 C -0.0596(3) 0.4229(3) 0.8296(4) 0.0209(15) Uani 1 1 d . . . C14 C 0.0474(3) 0.4509(3) 0.7487(3) 0.0203(16) Uani 1 1 d . . . C15 C -0.0585(3) 0.4182(3) 0.6687(4) 0.0206(14) Uani 1 1 d . . . C16 C -0.1381(3) 0.4848(2) 0.7411(3) 0.0147(13) Uani 1 1 d . . . C17 C -0.2975(4) 0.4220(4) 0.5441(5) 0.049(3) Uani 1 1 d . . . H17 H -0.2844 0.3885 0.5564 0.059 Uiso 1 1 calc R . . C18 C -0.3093(5) 0.4330(6) 0.4672(6) 0.063(3) Uani 1 1 d . . . H18 H -0.3026 0.4087 0.4271 0.075 Uiso 1 1 calc R . . C19 C -0.3313(4) 0.4808(6) 0.4512(5) 0.064(4) Uani 1 1 d . . . H19 H -0.3421 0.4893 0.3993 0.077 Uiso 1 1 calc R . . C20 C -0.3380(4) 0.5166(5) 0.5090(5) 0.051(3) Uani 1 1 d . . . H20 H -0.3527 0.5498 0.4977 0.061 Uiso 1 1 calc R . . C21 C -0.3224(3) 0.5024(4) 0.5851(5) 0.036(2) Uani 1 1 d . . . C22 C -0.3244(3) 0.5392(3) 0.6500(5) 0.035(2) Uani 1 1 d . . . C23 C -0.3291(4) 0.5915(4) 0.6353(7) 0.049(3) Uani 1 1 d . . . H23 H -0.3307 0.6043 0.5837 0.059 Uiso 1 1 calc R . . C24 C -0.3316(4) 0.6238(3) 0.6994(8) 0.056(3) Uani 1 1 d . . . H24 H -0.3337 0.6594 0.6913 0.068 Uiso 1 1 calc R . . C25 C -0.3309(4) 0.6052(3) 0.7733(7) 0.047(2) Uani 1 1 d . . . H25 H -0.3336 0.6274 0.8167 0.056 Uiso 1 1 calc R . . C26 C -0.3260(3) 0.5526(3) 0.7841(6) 0.0337(19) Uani 1 1 d . . . C27 C -0.3268(3) 0.5303(3) 0.8630(5) 0.0313(18) Uani 1 1 d . . . C28 C -0.3464(4) 0.5581(4) 0.9269(6) 0.053(3) Uani 1 1 d . . . H28 H -0.3610 0.5918 0.9210 0.064 Uiso 1 1 calc R . . C29 C -0.3441(4) 0.5353(4) 0.9999(6) 0.054(3) Uani 1 1 d . . . H29 H -0.3563 0.5542 1.0444 0.065 Uiso 1 1 calc R . . C30 C -0.3248(4) 0.4866(5) 1.0086(5) 0.049(3) Uani 1 1 d . . . H30 H -0.3234 0.4708 1.0583 0.059 Uiso 1 1 calc R . . C31 C -0.3073(4) 0.4609(4) 0.9417(5) 0.038(2) Uani 1 1 d . . . H31 H -0.2938 0.4267 0.9469 0.045 Uiso 1 1 calc R . . C32 C -0.1796(3) 0.6489(3) 0.6614(5) 0.0308(18) Uani 1 1 d . . . H32 H -0.1931 0.6320 0.6155 0.037 Uiso 1 1 calc R . . C33 C -0.1607(4) 0.6198(3) 0.7247(6) 0.041(2) Uani 1 1 d . . . H33 H -0.1617 0.5839 0.7217 0.049 Uiso 1 1 calc R . . C34 C -0.1410(4) 0.6426(4) 0.7900(6) 0.045(2) Uani 1 1 d . . . H34 H -0.1280 0.6228 0.8333 0.054 Uiso 1 1 calc R . . C35 C -0.1396(3) 0.6961(3) 0.7945(5) 0.0334(18) Uani 1 1 d . . . C36 C -0.1593(3) 0.7232(3) 0.7288(4) 0.0261(16) Uani 1 1 d . . . C37 C -0.1190(4) 0.7240(4) 0.8616(5) 0.044(2) Uani 1 1 d . . . H37 H -0.1052 0.7062 0.9065 0.053 Uiso 1 1 calc R . . C38 C -0.1265(5) 0.7500 0.5243(7) 0.032(2) Uani 1 2 d S . . C39 C -0.2976(4) 0.7500 0.6271(6) 0.020(2) Uani 1 2 d S . . C40 C -0.2410(3) 0.6963(3) 0.5052(4) 0.0300(17) Uani 1 1 d . . . O1 O -0.2087(2) 0.3963(2) 0.8422(3) 0.0336(13) Uani 1 1 d . . . H1B H -0.2176 0.3784 0.8843 0.040 Uiso 1 1 d R . . H1C H -0.1710 0.3949 0.8418 0.040 Uiso 1 1 d R . . O2 O -0.2069(2) 0.3774(2) 0.6723(3) 0.0327(13) Uani 1 1 d . . . H2B H -0.1673 0.3874 0.6673 0.039 Uiso 1 1 d R . . H2C H -0.2008 0.3505 0.6753 0.039 Uiso 1 1 d R . . O3 O -0.3306(2) 0.3629(2) 0.8403(3) 0.0409(15) Uani 1 1 d . . . H3B H -0.3682 0.3579 0.8535 0.049 Uiso 1 1 d R . . H3C H -0.3136 0.3578 0.8843 0.049 Uiso 1 1 d R . . O4 O -0.3327(2) 0.3502(2) 0.6767(3) 0.0366(14) Uani 1 1 d . . . H4B H -0.3076 0.3428 0.6477 0.044 Uiso 1 1 d R . . H4C H -0.3725 0.3524 0.6592 0.044 Uiso 1 1 d R . . O5 O 0.0576(4) 0.2500 0.9603(5) 0.042(2) Uani 1 2 d S . . O6 O -0.0522(4) 0.2500 1.0484(5) 0.040(2) Uani 1 2 d S . . O8 O 0.0493(4) 0.7500 0.5274(9) 0.081(4) Uani 1 2 d S . . O10 O -0.2626(6) 0.6811(5) 0.9301(7) 0.126(4) Uani 1 1 d . . . O9 O -0.3005(9) 0.7500 0.8226(8) 0.125(6) Uani 1 2 d S . . O12 O -0.1875(6) 0.7292(5) 1.0455(8) 0.063(4) Uani 0.50 1 d P . . H10B H -0.2383 0.6942 0.9677 0.076 Uiso 1 1 d R . . H10C H -0.2490 0.6868 0.8863 0.076 Uiso 1 1 d R . . O11 O -0.0002(10) 0.2500 0.7459(8) 0.118(6) Uani 1 2 d S . . O13 O 0.0540(4) 0.3309(3) 0.6230(6) 0.093(3) Uani 1 1 d . . . O14 O -0.0884(8) 0.2784(6) 0.6337(12) 0.089(6) Uani 0.50 1 d P . . O15 O 0.0621(5) 0.3468(5) 0.9010(9) 0.054(3) Uani 0.50 1 d PU A 1 O15' O 0.0407(5) 0.3260(6) 0.8450(9) 0.054(3) Uani 0.50 1 d PU B 2 O16 O -0.0974(7) 0.2876(6) 0.8398(10) 0.070(3) Uani 0.50 1 d PU C 1 O16' O -0.1137(6) 0.2979(5) 0.9291(10) 0.068(3) Uani 0.50 1 d PU D 2 O17 O -0.3144(12) 0.7195(6) 1.2270(19) 0.162(14) Uani 0.50 1 d P . . O19 O -0.1226(6) 0.3309(4) 0.4977(8) 0.047(2) Uani 0.50 1 d PU E 1 O19' O -0.1471(6) 0.3131(5) 0.4291(9) 0.054(3) Uani 0.50 1 d PU F 2 N6 N 0.0972(3) 0.4373(2) 0.7514(3) 0.0221(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0091(2) 0.0164(2) 0.0156(2) 0.00242(13) 0.00026(12) -0.00177(13) Ru1 0.0080(3) 0.0149(3) 0.0185(3) 0.0011(2) -0.00089(18) -0.0012(2) Ru2 0.0185(4) 0.0179(4) 0.0191(4) 0.000 -0.0003(3) 0.000 N1 0.012(3) 0.024(3) 0.022(3) 0.001(2) 0.000(2) 0.002(2) N2 0.011(3) 0.021(3) 0.023(3) 0.000(2) 0.001(2) 0.000(2) N3 0.022(3) 0.034(4) 0.035(4) 0.013(3) -0.004(3) -0.005(3) N4 0.023(3) 0.028(3) 0.034(4) -0.006(3) -0.004(3) 0.001(3) N5 0.006(3) 0.012(3) 0.028(3) 0.002(2) -0.003(2) -0.001(2) N7 0.021(3) 0.058(5) 0.022(3) 0.009(3) -0.003(3) -0.004(3) N8 0.013(3) 0.019(3) 0.046(4) 0.007(3) 0.003(3) 0.001(2) N9 0.017(3) 0.037(4) 0.023(3) -0.010(3) -0.001(2) 0.002(3) N10 0.022(3) 0.020(3) 0.028(3) 0.001(3) 0.000(2) 0.001(2) N11 0.033(6) 0.056(7) 0.066(8) 0.000 0.010(6) 0.000 N12 0.025(5) 0.027(5) 0.036(5) 0.000 0.009(4) 0.000 N13 0.035(4) 0.060(5) 0.046(4) -0.029(4) -0.005(3) 0.009(4) C1 0.022(4) 0.036(4) 0.025(4) -0.004(3) -0.003(3) 0.005(3) C2 0.040(5) 0.041(5) 0.028(4) -0.006(4) -0.010(3) 0.005(4) C3 0.034(4) 0.026(4) 0.042(5) -0.011(4) -0.008(4) 0.002(3) C4 0.023(4) 0.022(4) 0.038(4) -0.007(3) -0.007(3) 0.000(3) C5 0.034(4) 0.020(4) 0.060(6) -0.005(4) -0.009(4) 0.002(3) C6 0.032(4) 0.019(4) 0.052(5) 0.003(4) 0.004(4) 0.000(3) C7 0.018(3) 0.019(4) 0.046(5) 0.006(3) 0.008(3) 0.002(3) C8 0.044(5) 0.027(4) 0.034(4) 0.015(4) 0.014(4) 0.008(4) C9 0.037(4) 0.033(4) 0.029(4) 0.006(3) 0.010(3) 0.003(3) C10 0.021(3) 0.025(4) 0.025(4) 0.003(3) 0.003(3) 0.004(3) C11 0.013(3) 0.023(4) 0.031(4) 0.002(3) 0.002(3) -0.001(3) C12 0.016(3) 0.022(4) 0.034(4) -0.005(3) 0.000(3) 0.004(3) C13 0.010(3) 0.027(4) 0.026(4) 0.001(3) -0.003(3) 0.001(3) C14 0.011(4) 0.034(4) 0.016(3) -0.002(3) -0.001(2) -0.015(3) C15 0.013(3) 0.023(4) 0.026(4) 0.003(3) 0.000(3) -0.002(3) C16 0.022(4) 0.007(3) 0.015(3) 0.004(2) -0.002(2) 0.000(3) C17 0.046(5) 0.080(7) 0.021(4) -0.010(5) -0.001(4) -0.014(5) C18 0.034(5) 0.121(11) 0.032(5) -0.007(6) -0.006(4) -0.021(6) C19 0.029(5) 0.137(12) 0.026(5) 0.021(6) -0.008(4) -0.021(6) C20 0.020(4) 0.096(8) 0.038(5) 0.033(6) -0.007(4) -0.011(5) C21 0.013(3) 0.063(6) 0.032(4) 0.025(4) -0.004(3) -0.005(4) C22 0.013(3) 0.038(5) 0.054(5) 0.031(4) -0.005(3) 0.000(3) C23 0.028(4) 0.042(5) 0.078(7) 0.031(5) 0.001(4) 0.003(4) C24 0.027(5) 0.024(5) 0.118(10) 0.022(6) -0.009(5) 0.002(4) C25 0.023(4) 0.029(5) 0.089(7) -0.001(5) -0.006(5) 0.002(4) C26 0.011(3) 0.024(4) 0.066(6) -0.011(4) -0.006(4) 0.002(3) C27 0.014(3) 0.036(4) 0.044(5) -0.022(4) 0.001(3) 0.005(3) C28 0.028(4) 0.062(6) 0.070(7) -0.036(6) 0.008(4) 0.001(4) C29 0.033(5) 0.079(8) 0.051(6) -0.028(6) 0.013(4) -0.007(5) C30 0.026(4) 0.094(8) 0.027(4) -0.014(5) 0.006(3) -0.006(5) C31 0.024(4) 0.061(6) 0.027(4) 0.000(4) 0.001(3) 0.000(4) C32 0.028(4) 0.014(3) 0.051(5) 0.004(3) 0.004(3) 0.004(3) C33 0.032(5) 0.019(4) 0.072(6) 0.013(4) 0.003(4) 0.005(3) C34 0.023(4) 0.052(6) 0.059(6) 0.036(5) 0.000(4) 0.007(4) C35 0.018(4) 0.050(5) 0.033(4) 0.014(4) -0.002(3) 0.003(3) C36 0.019(4) 0.030(4) 0.029(4) 0.010(3) -0.003(3) -0.001(3) C37 0.027(4) 0.079(6) 0.026(4) 0.008(4) -0.005(3) 0.007(4) C38 0.028(6) 0.025(6) 0.042(7) 0.000 0.006(5) 0.000 C39 0.023(5) 0.015(5) 0.021(5) 0.000 -0.007(4) 0.000 C40 0.028(4) 0.036(4) 0.025(4) -0.010(3) -0.007(3) 0.004(3) O1 0.017(3) 0.049(3) 0.035(3) 0.026(3) -0.001(2) 0.001(2) O2 0.025(3) 0.027(3) 0.047(3) -0.011(3) 0.006(2) 0.001(2) O3 0.023(3) 0.052(4) 0.048(4) 0.027(3) -0.002(2) -0.010(3) O4 0.017(3) 0.038(3) 0.055(4) -0.020(3) 0.009(2) -0.007(2) O5 0.031(4) 0.047(5) 0.049(5) 0.000 -0.004(4) 0.000 O6 0.036(4) 0.040(5) 0.044(5) 0.000 0.007(4) 0.000 O8 0.035(5) 0.028(5) 0.179(14) 0.000 0.020(7) 0.000 O10 0.131(10) 0.120(9) 0.128(10) -0.011(8) 0.002(8) 0.015(8) O9 0.206(19) 0.116(13) 0.054(8) 0.000 -0.038(10) 0.000 O12 0.038(7) 0.081(11) 0.070(9) -0.028(7) -0.005(6) -0.008(6) O11 0.139(17) 0.131(15) 0.083(11) 0.000 -0.010(9) 0.000 O13 0.044(4) 0.075(6) 0.160(9) -0.067(6) -0.031(5) 0.014(4) O14 0.065(10) 0.059(10) 0.144(17) 0.001(11) 0.009(11) -0.008(8) O15 0.023(5) 0.060(7) 0.078(8) 0.024(6) 0.006(5) 0.005(4) O15' 0.023(5) 0.060(7) 0.079(8) 0.024(6) 0.005(5) 0.004(4) O16 0.051(6) 0.052(6) 0.106(9) 0.020(7) -0.011(6) -0.003(5) O16' 0.049(6) 0.050(6) 0.104(9) 0.022(7) -0.011(6) -0.002(5) O17 0.136(19) 0.018(8) 0.33(4) -0.009(13) 0.15(2) -0.015(10) O19 0.042(5) 0.030(5) 0.070(7) -0.022(5) -0.012(5) 0.004(4) O19' 0.050(5) 0.035(5) 0.076(7) -0.017(5) -0.010(5) 0.004(4) N6 0.005(3) 0.028(3) 0.033(4) -0.003(3) 0.001(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.487(5) . ? Nd1 O3 2.494(5) . ? Nd1 N6 2.494(6) 6_557 ? Nd1 O2 2.510(5) . ? Nd1 O4 2.531(5) . ? Nd1 N5 2.544(5) . ? Nd1 N9 2.601(6) . ? Nd1 N7 2.615(6) . ? Nd1 N8 2.622(6) . ? Ru1 C13 1.974(7) . ? Ru1 C15 1.981(7) . ? Ru1 C14 2.048(7) . ? Ru1 C16 2.049(7) . ? Ru1 N2 2.127(6) . ? Ru1 N1 2.130(6) . ? Ru2 C40 1.970(7) . ? Ru2 C40 1.970(7) 7_575 ? Ru2 C38 2.036(11) . ? Ru2 C39 2.044(10) . ? Ru2 N10 2.109(6) 7_575 ? Ru2 N10 2.109(6) . ? N1 C1 1.337(9) . ? N1 C12 1.368(9) . ? N2 C10 1.342(9) . ? N2 C11 1.354(9) . ? N3 C13 1.166(9) . ? N4 C15 1.154(9) . ? N5 C16 1.162(9) . ? N7 C17 1.332(12) . ? N7 C21 1.352(11) . ? N8 C26 1.347(11) . ? N8 C22 1.355(10) . ? N9 C31 1.345(10) . ? N9 C27 1.363(10) . ? N10 C32 1.341(9) . ? N10 C36 1.366(10) . ? N11 C38 1.183(15) . ? N12 C39 1.158(13) . ? N13 C40 1.168(10) . ? C1 C2 1.396(11) . ? C1 H1 0.9500 . ? C2 C3 1.362(12) . ? C2 H2 0.9500 . ? C3 C4 1.412(11) . ? C3 H3 0.9500 . ? C4 C12 1.405(10) . ? C4 C5 1.439(11) . ? C5 C6 1.345(13) . ? C5 H5 0.9500 . ? C6 C7 1.438(11) . ? C6 H6 0.9500 . ? C7 C8 1.395(11) . ? C7 C11 1.410(10) . ? C8 C9 1.380(12) . ? C8 H8 0.9500 . ? C9 C10 1.398(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.431(11) . ? C14 N6 1.128(10) . ? C17 C18 1.376(13) . ? C17 H17 0.9500 . ? C18 C19 1.374(17) . ? C18 H18 0.9500 . ? C19 C20 1.378(16) . ? C19 H19 0.9500 . ? C20 C21 1.401(11) . ? C20 H20 0.9500 . ? C21 C22 1.480(13) . ? C22 C23 1.405(12) . ? C23 C24 1.393(16) . ? C23 H23 0.9500 . ? C24 C25 1.362(16) . ? C24 H24 0.9500 . ? C25 C26 1.403(12) . ? C25 H25 0.9500 . ? C26 C27 1.478(13) . ? C27 C28 1.385(11) . ? C28 C29 1.391(15) . ? C28 H28 0.9500 . ? C29 C30 1.359(15) . ? C29 H29 0.9500 . ? C30 C31 1.387(12) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.391(12) . ? C32 H32 0.9500 . ? C33 C34 1.342(14) . ? C33 H33 0.9500 . ? C34 C35 1.412(13) . ? C34 H34 0.9500 . ? C35 C36 1.402(10) . ? C35 C37 1.438(12) . ? C36 C36 1.416(15) 7_575 ? C37 C37 1.37(2) 7_575 ? C37 H37 0.9500 . ? O1 H1B 0.8835 . ? O1 H1C 0.8117 . ? O2 H2B 0.8951 . ? O2 H2C 0.7239 . ? O3 H3B 0.8499 . ? O3 H3C 0.8502 . ? O4 H4B 0.7601 . ? O4 H4C 0.9083 . ? O10 H10B 0.8988 . ? O10 H10C 0.8206 . ? O12 O12 1.10(3) 7_575 ? O14 O14 1.50(3) 7_565 ? O17 O17 1.61(3) 7_575 ? N6 Nd1 2.494(6) 6_657 ? 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 O1 Nd1 O3 67.38(17) . . ? O1 Nd1 N6 134.91(17) . 6_557 ? O3 Nd1 N6 72.75(19) . 6_557 ? O1 Nd1 O2 72.74(19) . . ? O3 Nd1 O2 104.01(19) . . ? N6 Nd1 O2 138.85(18) 6_557 . ? O1 Nd1 O4 108.9(2) . . ? O3 Nd1 O4 68.6(2) . . ? N6 Nd1 O4 73.70(19) 6_557 . ? O2 Nd1 O4 67.45(16) . . ? O1 Nd1 N5 71.14(17) . . ? O3 Nd1 N5 137.04(18) . . ? N6 Nd1 N5 137.16(19) 6_557 . ? O2 Nd1 N5 73.16(17) . . ? O4 Nd1 N5 138.06(17) . . ? O1 Nd1 N9 75.94(19) . . ? O3 Nd1 N9 77.6(2) . . ? N6 Nd1 N9 75.78(18) 6_557 . ? O2 Nd1 N9 144.88(18) . . ? O4 Nd1 N9 139.67(18) . . ? N5 Nd1 N9 82.08(18) . . ? O1 Nd1 N7 143.60(18) . . ? O3 Nd1 N7 139.2(2) . . ? N6 Nd1 N7 81.37(19) 6_557 . ? O2 Nd1 N7 75.7(2) . . ? O4 Nd1 N7 74.3(2) . . ? N5 Nd1 N7 82.79(19) . . ? N9 Nd1 N7 126.0(2) . . ? O1 Nd1 N8 126.0(2) . . ? O3 Nd1 N8 129.4(2) . . ? N6 Nd1 N8 67.71(19) 6_557 . ? O2 Nd1 N8 126.52(19) . . ? O4 Nd1 N8 125.1(2) . . ? N5 Nd1 N8 69.62(17) . . ? N9 Nd1 N8 63.2(2) . . ? N7 Nd1 N8 62.9(2) . . ? C13 Ru1 C15 88.8(3) . . ? C13 Ru1 C14 87.7(3) . . ? C15 Ru1 C14 87.8(3) . . ? C13 Ru1 C16 88.0(3) . . ? C15 Ru1 C16 86.0(3) . . ? C14 Ru1 C16 172.5(3) . . ? C13 Ru1 N2 173.8(3) . . ? C15 Ru1 N2 97.4(2) . . ? C14 Ru1 N2 92.9(2) . . ? C16 Ru1 N2 92.0(2) . . ? C13 Ru1 N1 96.5(3) . . ? C15 Ru1 N1 173.8(2) . . ? C14 Ru1 N1 89.2(2) . . ? C16 Ru1 N1 97.3(2) . . ? N2 Ru1 N1 77.4(2) . . ? C40 Ru2 C40 91.9(5) . 7_575 ? C40 Ru2 C38 91.0(3) . . ? C40 Ru2 C38 91.0(3) 7_575 . ? C40 Ru2 C39 88.7(3) . . ? C40 Ru2 C39 88.7(3) 7_575 . ? C38 Ru2 C39 179.5(4) . . ? C40 Ru2 N10 172.8(3) . 7_575 ? C40 Ru2 N10 95.1(3) 7_575 7_575 ? C38 Ru2 N10 90.8(3) . 7_575 ? C39 Ru2 N10 89.6(3) . 7_575 ? C40 Ru2 N10 95.1(3) . . ? C40 Ru2 N10 172.8(3) 7_575 . ? C38 Ru2 N10 90.8(3) . . ? C39 Ru2 N10 89.6(3) . . ? N10 Ru2 N10 77.9(3) 7_575 . ? C1 N1 C12 117.5(6) . . ? C1 N1 Ru1 128.4(5) . . ? C12 N1 Ru1 114.1(5) . . ? C10 N2 C11 117.3(6) . . ? C10 N2 Ru1 127.7(5) . . ? C11 N2 Ru1 114.8(5) . . ? C16 N5 Nd1 146.0(5) . . ? C17 N7 C21 117.7(8) . . ? C17 N7 Nd1 121.0(6) . . ? C21 N7 Nd1 121.1(5) . . ? C26 N8 C22 119.2(7) . . ? C26 N8 Nd1 119.9(5) . . ? C22 N8 Nd1 120.2(5) . . ? C31 N9 C27 117.5(7) . . ? C31 N9 Nd1 121.5(6) . . ? C27 N9 Nd1 120.7(5) . . ? C32 N10 C36 117.8(7) . . ? C32 N10 Ru2 128.1(5) . . ? C36 N10 Ru2 114.0(5) . . ? N1 C1 C2 122.8(8) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 120.1(8) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.2(7) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C12 C4 C3 117.4(7) . . ? C12 C4 C5 119.1(7) . . ? C3 C4 C5 123.5(7) . . ? C6 C5 C4 121.0(7) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 121.2(7) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C11 117.8(7) . . ? C8 C7 C6 123.2(7) . . ? C11 C7 C6 119.0(7) . . ? C9 C8 C7 118.6(7) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C10 120.2(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 122.4(7) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? N2 C11 C7 123.6(7) . . ? N2 C11 C12 116.7(6) . . ? C7 C11 C12 119.7(7) . . ? N1 C12 C4 123.1(7) . . ? N1 C12 C11 117.0(6) . . ? C4 C12 C11 120.0(7) . . ? N3 C13 Ru1 179.5(7) . . ? N6 C14 Ru1 177.6(7) . . ? N4 C15 Ru1 179.4(7) . . ? N5 C16 Ru1 168.4(6) . . ? N7 C17 C18 124.7(11) . . ? N7 C17 H17 117.6 . . ? C18 C17 H17 117.6 . . ? C19 C18 C17 116.6(11) . . ? C19 C18 H18 121.7 . . ? C17 C18 H18 121.7 . . ? C18 C19 C20 121.4(9) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 117.6(10) . . ? C19 C20 H20 121.2 . . ? C21 C20 H20 121.2 . . ? N7 C21 C20 121.8(9) . . ? N7 C21 C22 116.9(7) . . ? C20 C21 C22 121.3(9) . . ? N8 C22 C23 121.8(9) . . ? N8 C22 C21 117.4(7) . . ? C23 C22 C21 120.8(8) . . ? C24 C23 C22 117.5(9) . . ? C24 C23 H23 121.3 . . ? C22 C23 H23 121.3 . . ? C25 C24 C23 121.0(8) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 118.7(10) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N8 C26 C25 121.6(9) . . ? N8 C26 C27 117.6(7) . . ? C25 C26 C27 120.9(8) . . ? N9 C27 C28 121.6(9) . . ? N9 C27 C26 117.0(6) . . ? C28 C27 C26 121.3(8) . . ? C27 C28 C29 118.4(10) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C30 C29 C28 121.2(9) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 117.0(9) . . ? C29 C30 H30 121.5 . . ? C31 C30 H30 121.5 . . ? N9 C31 C30 124.3(9) . . ? N9 C31 H31 117.9 . . ? C30 C31 H31 117.9 . . ? N10 C32 C33 122.5(8) . . ? N10 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C34 C33 C32 120.0(8) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0(8) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 117.3(8) . . ? C36 C35 C37 118.6(8) . . ? C34 C35 C37 124.2(8) . . ? N10 C36 C35 122.4(7) . . ? N10 C36 C36 116.9(4) . 7_575 ? C35 C36 C36 120.6(5) . 7_575 ? C37 C37 C35 120.8(5) 7_575 . ? C37 C37 H37 119.6 7_575 . ? C35 C37 H37 119.6 . . ? N11 C38 Ru2 179.1(11) . . ? N12 C39 Ru2 178.1(9) . . ? N13 C40 Ru2 178.2(8) . . ? Nd1 O1 H1B 124.1 . . ? Nd1 O1 H1C 133.5 . . ? H1B O1 H1C 101.5 . . ? Nd1 O2 H2B 123.7 . . ? Nd1 O2 H2C 126.2 . . ? H2B O2 H2C 97.0 . . ? Nd1 O3 H3B 128.8 . . ? Nd1 O3 H3C 121.3 . . ? H3B O3 H3C 98.4 . . ? Nd1 O4 H4B 104.0 . . ? Nd1 O4 H4C 117.8 . . ? H4B O4 H4C 117.9 . . ? H10B O10 H10C 112.5 . . ? C14 N6 Nd1 168.2(6) . 6_657 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.509 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.190 #===END data_imw639h _database_code_depnum_ccdc_archive 'CCDC 636990' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H69 Er2 N22 O19.50 Ru3' _chemical_formula_weight 2000.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 15.550(3) _cell_length_b 15.800(3) _cell_length_c 17.720(4) _cell_angle_alpha 111.07(3) _cell_angle_beta 95.38(3) _cell_angle_gamma 95.64(3) _cell_volume 4003.6(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1966 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5080 _exptl_absorpt_correction_T_max 0.8334 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCDarea detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58489 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14089 _reflns_number_gt 10473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+128.8941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14089 _refine_ls_number_parameters 969 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 Er1 Er -0.04380(4) 0.48619(4) 0.30672(4) 0.03178(18) Uani 1 1 d . . . Er2 Er 0.06847(4) 0.00122(4) 0.18657(4) 0.02900(17) Uani 1 1 d . . . Ru1 Ru -0.22561(7) 0.15946(7) 0.21427(7) 0.0302(3) Uani 1 1 d . . . Ru2 Ru 0.24943(7) 0.33655(7) 0.31354(8) 0.0330(3) Uani 1 1 d . . . Ru3 Ru 0.27441(11) -0.27521(10) 0.13209(9) 0.0553(4) Uani 1 1 d . . . C1 C -0.3090(11) -0.0193(10) 0.2302(10) 0.048(4) Uani 1 1 d . . . H1 H -0.2521 -0.0364 0.2320 0.058 Uiso 1 1 calc R . . C2 C -0.3832(15) -0.0773(12) 0.2398(12) 0.068(6) Uani 1 1 d . . . H2 H -0.3743 -0.1306 0.2508 0.082 Uiso 1 1 calc R . . C3 C -0.4635(12) -0.0551(13) 0.2331(12) 0.064(6) Uani 1 1 d . . . H3 H -0.5108 -0.0944 0.2385 0.077 Uiso 1 1 calc R . . C4 C -0.4809(12) 0.0217(11) 0.2187(12) 0.060(5) Uani 1 1 d . . . C5 C -0.5640(11) 0.0464(15) 0.2097(13) 0.074(7) Uani 1 1 d . . . H5 H -0.6137 0.0090 0.2138 0.089 Uiso 1 1 calc R . . C6 C -0.5739(11) 0.1231(14) 0.1950(12) 0.069(6) Uani 1 1 d . . . H6 H -0.6312 0.1373 0.1869 0.082 Uiso 1 1 calc R . . C7 C -0.5003(10) 0.1853(11) 0.1912(10) 0.052(5) Uani 1 1 d . . . C8 C -0.5063(10) 0.2674(12) 0.1822(11) 0.056(5) Uani 1 1 d . . . H8 H -0.5614 0.2879 0.1785 0.067 Uiso 1 1 calc R . . C9 C -0.4312(11) 0.3198(12) 0.1785(11) 0.056(5) Uani 1 1 d . . . H9 H -0.4343 0.3768 0.1726 0.067 Uiso 1 1 calc R . . C10 C -0.3518(10) 0.2888(10) 0.1837(11) 0.048(4) Uani 1 1 d . . . H10 H -0.3014 0.3246 0.1788 0.058 Uiso 1 1 calc R . . C11 C -0.4150(9) 0.1600(9) 0.1989(9) 0.038(4) Uani 1 1 d . . . C12 C -0.4045(10) 0.0766(10) 0.2126(10) 0.044(4) Uani 1 1 d . . . C13 C -0.1516(8) 0.2689(10) 0.2164(9) 0.031(3) Uani 1 1 d . . . C14 C -0.1209(9) 0.1013(9) 0.2298(9) 0.034(3) Uani 1 1 d . . . C15 C -0.2246(8) 0.0911(9) 0.0919(10) 0.032(3) Uani 1 1 d . . . C16 C -0.2257(9) 0.2288(10) 0.3341(10) 0.039(4) Uani 1 1 d . . . C17 C 0.3221(11) 0.5310(10) 0.3173(10) 0.045(4) Uani 1 1 d . . . H17 H 0.2641 0.5335 0.2967 0.054 Uiso 1 1 calc R . . C18 C 0.3847(12) 0.6075(11) 0.3329(12) 0.058(5) Uani 1 1 d . . . H18 H 0.3699 0.6600 0.3233 0.070 Uiso 1 1 calc R . . C19 C 0.4678(12) 0.6034(12) 0.3624(12) 0.062(5) Uani 1 1 d . . . H19 H 0.5119 0.6540 0.3732 0.075 Uiso 1 1 calc R . . C20 C 0.4897(9) 0.5261(11) 0.3772(11) 0.046(4) Uani 1 1 d . . . C21 C 0.5743(12) 0.5182(15) 0.4085(13) 0.071(6) Uani 1 1 d . . . H21 H 0.6210 0.5666 0.4207 0.085 Uiso 1 1 calc R . . C22 C 0.5875(11) 0.4421(15) 0.4207(12) 0.064(5) Uani 1 1 d . . . H22 H 0.6448 0.4388 0.4422 0.077 Uiso 1 1 calc R . . C23 C 0.5231(10) 0.3652(12) 0.4045(10) 0.050(4) Uani 1 1 d . . . C24 C 0.5369(11) 0.2861(13) 0.4207(11) 0.055(5) Uani 1 1 d . . . H24 H 0.5931 0.2789 0.4416 0.066 Uiso 1 1 calc R . . C25 C 0.4666(11) 0.2199(13) 0.4053(12) 0.059(5) Uani 1 1 d . . . H25 H 0.4737 0.1659 0.4159 0.071 Uiso 1 1 calc R . . C26 C 0.3845(10) 0.2314(11) 0.3742(10) 0.046(4) Uani 1 1 d . . . H26 H 0.3365 0.1854 0.3658 0.055 Uiso 1 1 calc R . . C27 C 0.4385(9) 0.3731(11) 0.3729(10) 0.042(4) Uani 1 1 d . . . C28 C 0.4213(9) 0.4522(10) 0.3581(10) 0.040(4) Uani 1 1 d . . . C29 C 0.1759(10) 0.2188(10) 0.2979(9) 0.037(4) Uani 1 1 d . . . C30 C 0.1448(9) 0.3832(9) 0.2836(9) 0.035(4) Uani 1 1 d . . . C31 C 0.2289(8) 0.3911(9) 0.4302(10) 0.037(4) Uani 1 1 d . . . C32 C 0.2594(8) 0.2761(10) 0.1909(11) 0.036(4) Uani 1 1 d . . . C33 C 0.3614(13) -0.1473(14) 0.0525(11) 0.064(5) Uani 1 1 d . . . H33 H 0.3096 -0.1197 0.0569 0.076 Uiso 1 1 calc R . . C34 C 0.4301(15) -0.1141(17) 0.0191(12) 0.080(7) Uani 1 1 d . . . H34 H 0.4235 -0.0663 -0.0007 0.096 Uiso 1 1 calc R . . C36 C 0.5072(17) -0.152(2) 0.0155(15) 0.097(8) Uani 1 1 d . . . H36 H 0.5553 -0.1273 -0.0034 0.116 Uiso 1 1 calc R . . C37 C 0.5127(15) -0.223(2) 0.0393(14) 0.091(8) Uani 1 1 d . . . C38 C 0.588(2) -0.266(3) 0.0356(18) 0.128(13) Uani 1 1 d . . . H38 H 0.6383 -0.2438 0.0180 0.154 Uiso 1 1 calc R . . C39 C 0.589(3) -0.338(3) 0.0567(18) 0.16(2) Uani 1 1 d . . . H39 H 0.6407 -0.3663 0.0510 0.194 Uiso 1 1 calc R . . C40 C 0.521(3) -0.377(2) 0.0869(15) 0.128(14) Uani 1 1 d . . . C41 C 0.517(3) -0.453(3) 0.107(2) 0.150(18) Uani 1 1 d . . . H41 H 0.5675 -0.4819 0.1081 0.180 Uiso 1 1 calc R . . C42 C 0.441(3) -0.488(2) 0.1262(16) 0.133(15) Uani 1 1 d . . . H42 H 0.4395 -0.5435 0.1359 0.159 Uiso 1 1 calc R . . C43 C 0.366(2) -0.4433(16) 0.1317(13) 0.110(11) Uani 1 1 d . . . H43 H 0.3142 -0.4670 0.1462 0.132 Uiso 1 1 calc R . . C44 C 0.4461(18) -0.3332(19) 0.0918(11) 0.091(9) Uani 1 1 d . . . C45 C 0.4417(15) -0.2569(15) 0.0690(11) 0.068(6) Uani 1 1 d . . . C46 C 0.1953(11) -0.1783(11) 0.1508(10) 0.045(4) Uani 1 1 d . . . C47 C 0.3392(13) -0.2033(13) 0.2452(13) 0.054(5) Uani 1 1 d . . . C48 C 0.2041(19) -0.3452(17) 0.0215(16) 0.092(8) Uani 1 1 d . . . C49 C 0.1960(17) -0.3411(13) 0.1792(12) 0.074(7) Uani 1 1 d . . . C50 C -0.0051(8) 0.3140(9) 0.3790(9) 0.031(3) Uani 1 1 d . . . H50 H -0.0125 0.2794 0.3220 0.037 Uiso 1 1 calc R . . C51 C 0.0083(9) 0.2705(9) 0.4317(10) 0.038(4) Uani 1 1 d . . . H51 H 0.0106 0.2065 0.4120 0.046 Uiso 1 1 calc R . . C52 C 0.0020(8) 0.4494(8) 0.4852(9) 0.027(3) Uani 1 1 d . . . C53 C -0.0042(9) 0.2308(9) 0.0824(9) 0.033(3) Uani 1 1 d . . . H53 H -0.0042 0.2952 0.1055 0.039 Uiso 1 1 calc R . . C54 C 0.0198(8) 0.1826(8) 0.1288(9) 0.027(3) Uani 1 1 d . . . H54 H 0.0362 0.2147 0.1859 0.033 Uiso 1 1 calc R . . C55 C -0.0028(8) 0.0500(8) 0.0171(8) 0.026(3) Uani 1 1 d . . . N1 N -0.3217(8) 0.0565(8) 0.2190(8) 0.038(3) Uani 1 1 d . . . N2 N -0.3419(7) 0.2116(8) 0.1951(7) 0.037(3) Uani 1 1 d . . . N3 N -0.1137(7) 0.3384(8) 0.2247(7) 0.033(3) Uani 1 1 d . . . N4 N -0.0596(7) 0.0665(8) 0.2346(8) 0.036(3) Uani 1 1 d . . . N5 N -0.2227(9) 0.0485(8) 0.0236(8) 0.043(3) Uani 1 1 d . . . N6 N -0.2248(9) 0.2742(11) 0.4033(9) 0.062(4) Uani 1 1 d . . . N7 N 0.3380(8) 0.4545(8) 0.3292(8) 0.040(3) Uani 1 1 d . . . N8 N 0.3705(8) 0.3041(8) 0.3559(8) 0.041(3) Uani 1 1 d . . . N9 N 0.1350(7) 0.1481(8) 0.2788(7) 0.034(3) Uani 1 1 d . . . N10 N 0.0812(7) 0.4143(8) 0.2706(7) 0.035(3) Uani 1 1 d . . . N11 N 0.2137(8) 0.4234(9) 0.4967(9) 0.049(4) Uani 1 1 d . . . N12 N 0.2575(8) 0.2389(9) 0.1218(9) 0.047(3) Uani 1 1 d . . . N13 N 0.3677(10) -0.2164(11) 0.0780(8) 0.059(4) Uani 1 1 d . . . N14 N 0.3707(15) -0.3645(12) 0.1152(10) 0.083(6) Uani 1 1 d . . . N15 N 0.1530(8) -0.1208(8) 0.1641(8) 0.043(3) Uani 1 1 d . . . N16 N 0.3752(12) -0.1665(12) 0.3101(11) 0.066(5) Uani 1 1 d . . . N17 N 0.163(2) -0.3902(15) -0.0431(14) 0.131(10) Uani 1 1 d . . . N18 N 0.1461(16) -0.3859(13) 0.2009(12) 0.098(7) Uani 1 1 d . . . N19 N -0.0083(7) 0.4051(7) 0.4054(7) 0.027(2) Uani 1 1 d . . . N21 N 0.0215(7) 0.0915(7) 0.0981(7) 0.025(2) Uani 1 1 d . . . N22 N -0.0281(7) 0.0889(7) -0.0345(7) 0.029(3) Uani 1 1 d . . . C56 C -0.0285(9) 0.1817(9) 0.0002(9) 0.036(4) Uani 1 1 d . . . H56 H -0.0463 0.2133 -0.0338 0.043 Uiso 1 1 calc R . . C35 C 0.0185(9) 0.3209(9) 0.5146(10) 0.040(4) Uani 1 1 d . . . N20 N 0.0147(7) 0.4126(7) 0.5398(7) 0.031(3) Uani 1 1 d . . . H35 H 0.0209 0.4466 0.5922 0.037 Uiso 1 1 calc R . . O1 O 0.0654(7) 0.6088(7) 0.3308(7) 0.052(3) Uani 1 1 d . . . H1B H 0.1049 0.6059 0.3660 0.062 Uiso 1 1 d R . . H1C H 0.0915 0.6309 0.3005 0.062 Uiso 1 1 d R . . O2 O -0.1277(8) 0.6033(8) 0.3123(8) 0.065(4) Uani 1 1 d . . . H2B H -0.1663 0.5881 0.2707 0.078 Uiso 1 1 d R . . H2C H -0.0900 0.6173 0.2895 0.078 Uiso 1 1 d R . . O3 O -0.0445(8) 0.4871(8) 0.1760(7) 0.060(3) Uani 1 1 d . . . H3B H -0.0749 0.4486 0.1327 0.072 Uiso 1 1 d R . . H3C H -0.0578 0.5391 0.1796 0.072 Uiso 1 1 d R . . O4 O -0.1766(6) 0.4598(7) 0.3577(7) 0.046(3) Uani 1 1 d . . . H4B H -0.1621 0.4896 0.4082 0.055 Uiso 1 1 d R . . H4C H -0.1809 0.4018 0.3427 0.055 Uiso 1 1 d R . . O5 O 0.1932(6) 0.0436(6) 0.1335(6) 0.031(2) Uani 1 1 d . . . H5B H 0.2135 0.0141 0.0902 0.037 Uiso 1 1 d R . . H5C H 0.2121 0.0964 0.1343 0.037 Uiso 1 1 d R . . O6 O 0.0919(9) -0.0151(8) 0.3112(7) 0.065(4) Uani 1 1 d . . . H6B H 0.1096 -0.0684 0.2965 0.078 Uiso 1 1 d R . . H6C H 0.0756 0.0039 0.3582 0.078 Uiso 1 1 d R . . O7 O -0.0431(7) -0.1236(6) 0.1633(7) 0.050(3) Uani 1 1 d . . . H7B H -0.0254 -0.1412 0.2013 0.060 Uiso 1 1 d R . . H7C H -0.0880 -0.1078 0.1858 0.060 Uiso 1 1 d R . . O8 O 0.946(2) 0.742(2) 0.287(2) 0.098(10) Uiso 0.50 1 d P . . O9 O 0.181(2) 0.403(2) 0.0944(19) 0.086(9) Uiso 0.50 1 d P . . O10 O 0.543(2) 0.845(2) 0.402(2) 0.097(10) Uiso 0.50 1 d P . . O11 O 0.385(2) 0.026(2) 0.419(3) 0.112(9) Uani 0.50 1 d PU A 1 O11' O 0.299(2) 0.020(2) 0.376(3) 0.111(9) Uani 0.50 1 d PU B 2 O12 O 0.6608(19) 0.733(2) 0.3420(18) 0.079(8) Uiso 0.50 1 d P . . O13 O 0.204(2) 0.191(2) -0.128(2) 0.104(11) Uiso 0.50 1 d P . . O14 O 0.7867(18) 0.7493(19) 0.4632(17) 0.072(7) Uiso 0.50 1 d P . . O15 O 0.898(3) 0.035(3) 0.441(4) 0.200(18) Uani 0.50 1 d PU C 1 O15' O 0.820(3) -0.027(3) 0.428(4) 0.201(18) Uani 0.50 1 d PU D 2 O16 O 0.7736(17) 0.1478(18) 0.4949(16) 0.069(7) Uiso 0.50 1 d P E 2 O17 O 0.9810(15) 0.6942(14) 0.1296(17) 0.157(9) Uani 1 1 d . F 2 O18 O 1.1417(15) 0.8287(15) 0.3426(14) 0.052(6) Uiso 0.50 1 d P G 2 O19 O 0.0833(17) 0.0924(14) 0.4668(11) 0.145(9) Uani 1 1 d . H 2 O20 O 0.1805(12) 0.1240(13) -0.0493(12) 0.031(5) Uani 0.50 1 d P I 2 O20' O 0.273(5) 0.129(2) -0.028(2) 0.19(3) Uani 0.50 1 d P I 2 O21 O 0.8085(9) 0.4013(9) 0.5574(9) 0.077(4) Uani 1 1 d . J 2 O22 O 0.697(2) 0.556(4) 0.258(3) 0.17(2) Uani 0.50 1 d P K 1 O22' O 0.722(3) 0.508(3) 0.117(4) 0.22(3) Uani 0.50 1 d P L 2 O23 O 0.180(3) 0.386(3) -0.058(3) 0.163(19) Uani 0.50 1 d P . . O24 O 0.872(2) 0.888(3) 0.300(2) 0.119(11) Uani 0.50 1 d PU M 1 O24' O 0.781(2) 0.821(3) 0.278(2) 0.120(11) Uani 0.50 1 d PU N 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0264(3) 0.0195(3) 0.0472(4) 0.0088(3) 0.0087(3) 0.0036(2) Er2 0.0286(3) 0.0191(3) 0.0376(4) 0.0068(3) 0.0127(3) 0.0027(2) Ru1 0.0238(6) 0.0220(6) 0.0424(7) 0.0055(5) 0.0174(5) 0.0050(4) Ru2 0.0191(5) 0.0212(6) 0.0513(8) 0.0022(5) 0.0147(5) 0.0032(4) Ru3 0.0904(12) 0.0437(8) 0.0440(8) 0.0216(7) 0.0203(8) 0.0353(8) C1 0.058(10) 0.028(8) 0.059(11) 0.012(8) 0.028(9) -0.002(7) C2 0.105(17) 0.028(9) 0.062(13) 0.008(9) 0.028(12) -0.019(10) C3 0.045(11) 0.052(12) 0.083(15) 0.010(10) 0.031(10) -0.020(9) C4 0.061(12) 0.031(9) 0.067(13) -0.007(8) 0.028(10) -0.010(8) C5 0.032(10) 0.063(13) 0.091(16) -0.009(12) 0.019(10) -0.024(9) C6 0.032(9) 0.057(12) 0.084(15) -0.012(11) 0.021(9) -0.007(8) C7 0.042(9) 0.045(10) 0.043(10) -0.017(8) 0.016(8) 0.002(8) C8 0.032(9) 0.051(11) 0.068(12) -0.004(9) 0.017(8) 0.017(8) C9 0.045(10) 0.046(10) 0.071(13) 0.013(9) 0.009(9) 0.018(8) C10 0.031(8) 0.034(9) 0.078(13) 0.018(8) 0.007(8) 0.009(7) C11 0.025(7) 0.027(8) 0.050(10) 0.001(7) 0.012(7) -0.001(6) C12 0.041(9) 0.032(8) 0.043(10) -0.009(7) 0.018(7) -0.002(7) C13 0.016(6) 0.034(8) 0.043(9) 0.011(7) 0.017(6) 0.006(6) C14 0.036(8) 0.027(7) 0.038(9) 0.012(7) 0.017(7) -0.010(6) C15 0.020(7) 0.020(7) 0.062(11) 0.019(7) 0.011(7) 0.006(5) C16 0.033(8) 0.039(9) 0.039(10) 0.008(7) 0.012(7) -0.001(7) C17 0.042(9) 0.032(8) 0.060(11) 0.014(8) 0.012(8) 0.004(7) C18 0.061(12) 0.032(9) 0.076(14) 0.016(9) 0.008(10) -0.010(8) C19 0.055(12) 0.043(10) 0.074(14) 0.012(10) 0.009(10) -0.028(9) C20 0.017(7) 0.045(10) 0.065(11) 0.013(8) 0.005(7) -0.010(6) C21 0.048(11) 0.075(15) 0.076(15) 0.017(12) 0.011(10) -0.019(10) C22 0.027(9) 0.083(15) 0.066(13) 0.014(11) -0.010(8) -0.003(9) C23 0.026(8) 0.059(11) 0.054(11) 0.008(9) 0.005(7) 0.012(8) C24 0.035(9) 0.069(12) 0.052(11) 0.011(9) 0.010(8) 0.010(9) C25 0.038(10) 0.064(12) 0.072(13) 0.018(10) 0.018(9) 0.013(9) C26 0.040(9) 0.036(9) 0.060(11) 0.014(8) 0.017(8) 0.009(7) C27 0.026(8) 0.042(9) 0.052(10) 0.009(8) 0.007(7) 0.000(7) C28 0.028(8) 0.036(8) 0.048(10) 0.005(7) 0.009(7) 0.004(6) C29 0.038(8) 0.034(9) 0.039(9) 0.005(7) 0.017(7) 0.020(7) C30 0.026(8) 0.029(7) 0.038(9) -0.005(6) 0.024(6) -0.002(6) C31 0.020(7) 0.022(7) 0.055(10) -0.008(7) 0.020(7) 0.007(6) C32 0.011(6) 0.033(8) 0.066(12) 0.019(8) 0.011(7) 0.005(6) C33 0.071(13) 0.078(14) 0.061(12) 0.039(11) 0.019(10) 0.038(11) C34 0.077(15) 0.109(19) 0.054(13) 0.029(13) 0.020(11) 0.008(14) C36 0.080(17) 0.15(3) 0.071(17) 0.045(17) 0.020(13) 0.024(17) C37 0.068(15) 0.16(3) 0.058(14) 0.038(16) 0.030(12) 0.053(16) C38 0.11(3) 0.21(4) 0.07(2) 0.06(2) 0.016(17) 0.04(3) C39 0.16(3) 0.27(6) 0.049(19) 0.01(2) 0.03(2) 0.12(4) C40 0.20(4) 0.15(3) 0.048(14) 0.021(15) 0.027(18) 0.15(3) C41 0.17(4) 0.22(4) 0.09(2) 0.05(2) 0.04(2) 0.15(4) C42 0.24(4) 0.09(2) 0.070(18) 0.019(15) 0.00(2) 0.13(3) C43 0.22(3) 0.080(16) 0.050(14) 0.025(12) 0.018(16) 0.09(2) C44 0.11(2) 0.14(2) 0.026(10) 0.022(12) 0.019(11) 0.082(18) C45 0.094(16) 0.077(14) 0.038(11) 0.019(10) 0.015(10) 0.044(12) C46 0.048(10) 0.049(10) 0.047(10) 0.024(8) 0.015(8) 0.013(8) C47 0.067(12) 0.051(11) 0.070(14) 0.038(11) 0.039(11) 0.036(10) C48 0.15(2) 0.073(16) 0.071(16) 0.034(13) 0.013(16) 0.055(16) C49 0.122(19) 0.045(11) 0.050(12) 0.010(10) -0.005(12) 0.033(12) C50 0.015(6) 0.028(7) 0.044(9) 0.006(7) 0.011(6) 0.004(5) C51 0.038(8) 0.019(7) 0.052(10) 0.006(7) 0.012(7) 0.001(6) C52 0.019(6) 0.021(7) 0.038(8) 0.009(6) 0.004(6) -0.006(5) C53 0.032(8) 0.014(6) 0.047(9) 0.003(6) 0.019(7) 0.004(6) C54 0.023(7) 0.023(7) 0.038(8) 0.010(6) 0.016(6) 0.004(5) C55 0.014(6) 0.024(7) 0.033(8) 0.005(6) 0.006(5) -0.002(5) N1 0.034(7) 0.029(7) 0.050(8) 0.010(6) 0.019(6) 0.000(5) N2 0.028(6) 0.031(7) 0.043(8) 0.003(6) 0.008(5) 0.005(5) N3 0.021(6) 0.033(7) 0.043(7) 0.009(6) 0.014(5) 0.005(5) N4 0.024(6) 0.035(7) 0.059(9) 0.024(6) 0.020(6) 0.014(5) N5 0.054(8) 0.029(7) 0.040(8) 0.001(6) 0.021(7) 0.010(6) N6 0.045(9) 0.068(10) 0.053(10) -0.004(8) 0.021(7) 0.004(7) N7 0.033(7) 0.022(6) 0.053(8) 0.001(6) 0.011(6) -0.003(5) N8 0.034(7) 0.027(7) 0.057(9) 0.009(6) 0.011(6) 0.001(5) N9 0.030(6) 0.024(6) 0.039(7) -0.002(5) 0.017(5) 0.001(5) N10 0.024(6) 0.033(7) 0.046(8) 0.012(6) 0.005(5) -0.001(5) N11 0.029(7) 0.041(8) 0.063(10) 0.004(7) 0.001(7) 0.006(6) N12 0.042(8) 0.045(8) 0.056(10) 0.015(7) 0.027(7) 0.013(6) N13 0.072(10) 0.080(11) 0.041(9) 0.032(8) 0.019(7) 0.038(9) N14 0.153(19) 0.063(11) 0.050(10) 0.024(9) 0.025(11) 0.069(12) N15 0.042(8) 0.031(7) 0.059(9) 0.019(6) 0.016(7) 0.013(6) N16 0.078(12) 0.070(11) 0.071(12) 0.036(10) 0.045(10) 0.031(9) N17 0.23(3) 0.074(15) 0.074(16) 0.024(12) -0.026(18) 0.011(17) N18 0.16(2) 0.060(12) 0.077(14) 0.041(11) 0.024(13) -0.015(13) N19 0.023(6) 0.018(5) 0.035(7) 0.005(5) 0.005(5) 0.000(4) N21 0.023(5) 0.017(5) 0.036(7) 0.011(5) 0.009(5) 0.001(4) N22 0.030(6) 0.019(6) 0.038(7) 0.008(5) 0.007(5) 0.011(5) C56 0.036(8) 0.020(7) 0.051(10) 0.006(7) 0.018(7) 0.012(6) C35 0.035(8) 0.025(7) 0.057(11) 0.007(7) 0.018(7) 0.007(6) N20 0.029(6) 0.015(5) 0.042(7) 0.002(5) 0.012(5) 0.000(5) O1 0.048(7) 0.040(6) 0.073(8) 0.033(6) 0.004(6) -0.005(5) O2 0.054(7) 0.055(8) 0.079(9) 0.016(7) -0.002(7) 0.025(6) O3 0.078(9) 0.053(7) 0.058(8) 0.034(6) 0.006(6) 0.001(6) O4 0.033(6) 0.038(6) 0.050(7) -0.004(5) 0.014(5) 0.008(5) O5 0.031(5) 0.020(5) 0.037(6) 0.004(4) 0.016(4) 0.001(4) O6 0.111(11) 0.044(7) 0.035(7) 0.009(6) 0.004(7) 0.015(7) O7 0.057(7) 0.027(5) 0.064(8) 0.009(5) 0.041(6) -0.001(5) O11 0.071(14) 0.066(13) 0.22(3) 0.083(17) 0.022(17) 0.000(12) O11' 0.070(14) 0.065(13) 0.22(3) 0.084(17) 0.021(17) 0.000(12) O15 0.16(3) 0.13(3) 0.35(5) 0.09(3) 0.20(3) 0.06(2) O15' 0.16(3) 0.13(3) 0.35(5) 0.09(3) 0.20(3) 0.06(2) O17 0.139(18) 0.101(15) 0.25(3) 0.091(18) 0.031(18) 0.004(13) O19 0.25(3) 0.117(15) 0.094(14) 0.048(12) 0.043(15) 0.103(17) O20 0.023(9) 0.030(11) 0.038(12) 0.012(9) -0.007(9) 0.007(8) O20' 0.41(9) 0.06(2) 0.10(3) 0.01(2) 0.17(5) 0.00(4) O21 0.066(9) 0.072(9) 0.076(10) 0.004(7) 0.008(7) 0.026(7) O22 0.04(2) 0.27(6) 0.25(6) 0.14(5) 0.01(3) 0.05(3) O22' 0.08(3) 0.15(4) 0.32(7) -0.07(4) 0.00(3) 0.09(3) O23 0.10(3) 0.16(4) 0.21(5) 0.05(4) -0.04(3) 0.00(3) O24 0.12(2) 0.19(3) 0.13(2) 0.12(2) 0.084(19) 0.10(2) O24' 0.13(2) 0.19(3) 0.13(2) 0.12(2) 0.085(19) 0.10(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O3 2.321(11) . ? Er1 O1 2.332(10) . ? Er1 O2 2.346(11) . ? Er1 N3 2.348(12) . ? Er1 N10 2.371(12) . ? Er1 O4 2.389(10) . ? Er1 N19 2.564(11) . ? Er1 N20 2.581(12) 2_566 ? Er1 H2C 2.3686 . ? Er2 O6 2.314(11) . ? Er2 N9 2.368(12) . ? Er2 O5 2.374(8) . ? Er2 N15 2.377(12) . ? Er2 O7 2.383(9) . ? Er2 N4 2.418(11) . ? Er2 N22 2.536(11) 2 ? Er2 N21 2.573(10) . ? Ru1 C13 1.968(14) . ? Ru1 C14 1.990(16) . ? Ru1 C16 2.010(16) . ? Ru1 C15 2.048(16) . ? Ru1 N2 2.108(11) . ? Ru1 N1 2.128(11) . ? Ru2 C30 1.956(16) . ? Ru2 C29 2.000(16) . ? Ru2 C31 2.004(15) . ? Ru2 C32 2.064(18) . ? Ru2 N7 2.120(11) . ? Ru2 N8 2.138(13) . ? Ru3 C49 1.96(3) . ? Ru3 C46 2.013(16) . ? Ru3 C48 2.01(3) . ? Ru3 C47 2.02(2) . ? Ru3 N14 2.125(16) . ? Ru3 N13 2.127(15) . ? C1 N1 1.313(19) . ? C1 C2 1.46(2) . ? C1 H1 0.9500 . ? C2 C3 1.34(3) . ? C2 H2 0.9500 . ? C3 C4 1.37(3) . ? C3 H3 0.9500 . ? C4 C5 1.40(3) . ? C4 C12 1.44(2) . ? C5 C6 1.35(3) . ? C5 H5 0.9500 . ? C6 C7 1.46(2) . ? C6 H6 0.9500 . ? C7 C8 1.37(3) . ? C7 C11 1.43(2) . ? C8 C9 1.38(2) . ? C8 H8 0.9500 . ? C9 C10 1.38(2) . ? C9 H9 0.9500 . ? C10 N2 1.326(19) . ? C10 H10 0.9500 . ? C11 N2 1.355(17) . ? C11 C12 1.44(2) . ? C12 N1 1.360(19) . ? C13 N3 1.146(17) . ? C14 N4 1.158(18) . ? C15 N5 1.159(18) . ? C16 N6 1.174(19) . ? C17 N7 1.343(19) . ? C17 C18 1.40(2) . ? C17 H17 0.9500 . ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 C20 1.40(2) . ? C19 H19 0.9500 . ? C20 C21 1.41(3) . ? C20 C28 1.42(2) . ? C21 C22 1.33(3) . ? C21 H21 0.9500 . ? C22 C23 1.42(2) . ? C22 H22 0.9500 . ? C23 C24 1.41(2) . ? C23 C27 1.42(2) . ? C24 C25 1.37(2) . ? C24 H24 0.9500 . ? C25 C26 1.40(2) . ? C25 H25 0.9500 . ? C26 N8 1.332(19) . ? C26 H26 0.9500 . ? C27 N8 1.369(18) . ? C27 C28 1.41(2) . ? C28 N7 1.355(19) . ? C29 N9 1.147(18) . ? C30 N10 1.186(18) . ? C31 N11 1.162(19) . ? C32 N12 1.148(19) . ? C33 N13 1.33(2) . ? C33 C34 1.41(3) . ? C33 H33 0.9500 . ? C34 C36 1.38(3) . ? C34 H34 0.9500 . ? C36 C37 1.35(3) . ? C36 H36 0.9500 . ? C37 C38 1.41(4) . ? C37 C45 1.41(3) . ? C38 C39 1.31(5) . ? C38 H38 0.9500 . ? C39 C40 1.42(5) . ? C39 H39 0.9500 . ? C40 C41 1.36(5) . ? C40 C44 1.41(3) . ? C41 C42 1.37(5) . ? C41 H41 0.9500 . ? C42 C43 1.42(4) . ? C42 H42 0.9500 . ? C43 N14 1.37(3) . ? C43 H43 0.9500 . ? C44 N14 1.38(3) . ? C44 C45 1.41(3) . ? C45 N13 1.36(2) . ? C46 N15 1.142(18) . ? C47 N16 1.14(2) . ? C48 N17 1.19(3) . ? C49 N18 1.18(3) . ? C50 N19 1.352(16) . ? C50 C51 1.36(2) . ? C50 H50 0.9500 . ? C51 C35 1.38(2) . ? C51 H51 0.9500 . ? C52 N20 1.306(17) . ? C52 N19 1.319(17) . ? C52 C52 1.50(2) 2_566 ? C53 C54 1.359(19) . ? C53 C56 1.38(2) . ? C53 H53 0.9500 . ? C54 N21 1.347(15) . ? C54 H54 0.9500 . ? C55 N22 1.325(17) . ? C55 N21 1.343(17) . ? C55 C55 1.49(2) 2 ? N22 C56 1.371(16) . ? N22 Er2 2.536(11) 2 ? C56 H56 0.9500 . ? C35 N20 1.363(17) . ? N20 Er1 2.581(12) 2_566 ? N20 H35 0.8800 . ? O1 H1B 0.8504 . ? O1 H1C 0.8503 . ? O2 H2B 0.8501 . ? O2 H2C 0.8000 . ? O3 H3B 0.8500 . ? O3 H3C 0.8499 . ? O4 H4B 0.8438 . ? O4 H4C 0.8499 . ? O5 H5B 0.8501 . ? O5 H5C 0.8505 . ? O6 H6B 0.8693 . ? O6 H6C 0.8499 . ? O7 H7B 0.8500 . ? O7 H7C 0.8500 . ? O20 O20' 1.44(7) . ? 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 O3 Er1 O1 79.4(4) . . ? O3 Er1 O2 78.7(4) . . ? O1 Er1 O2 79.1(4) . . ? O3 Er1 N3 77.6(4) . . ? O1 Er1 N3 150.1(4) . . ? O2 Er1 N3 114.3(4) . . ? O3 Er1 N10 80.4(4) . . ? O1 Er1 N10 76.5(4) . . ? O2 Er1 N10 150.3(4) . . ? N3 Er1 N10 81.1(4) . . ? O3 Er1 O4 121.2(4) . . ? O1 Er1 O4 137.3(4) . . ? O2 Er1 O4 70.4(4) . . ? N3 Er1 O4 71.9(4) . . ? N10 Er1 O4 139.1(4) . . ? O3 Er1 N19 147.7(4) . . ? O1 Er1 N19 109.7(4) . . ? O2 Er1 N19 132.9(4) . . ? N3 Er1 N19 81.5(4) . . ? N10 Er1 N19 72.3(4) . . ? O4 Er1 N19 73.8(4) . . ? O3 Er1 N20 144.3(4) . 2_566 ? O1 Er1 N20 69.8(4) . 2_566 ? O2 Er1 N20 78.4(4) . 2_566 ? N3 Er1 N20 137.2(4) . 2_566 ? N10 Er1 N20 108.3(4) . 2_566 ? O4 Er1 N20 75.2(3) . 2_566 ? N19 Er1 N20 63.4(3) . 2_566 ? O3 Er1 H2C 65.1 . . ? O1 Er1 H2C 63.9 . . ? O2 Er1 H2C 19.5 . . ? N3 Er1 H2C 120.9 . . ? N10 Er1 H2C 130.8 . . ? O4 Er1 H2C 89.8 . . ? N19 Er1 H2C 147.1 . . ? N20 Er1 H2C 85.1 2_566 . ? O6 Er2 N9 75.5(4) . . ? O6 Er2 O5 117.2(4) . . ? N9 Er2 O5 72.4(3) . . ? O6 Er2 N15 74.9(4) . . ? N9 Er2 N15 117.1(4) . . ? O5 Er2 N15 74.1(4) . . ? O6 Er2 O7 80.7(4) . . ? N9 Er2 O7 145.3(4) . . ? O5 Er2 O7 142.0(3) . . ? N15 Er2 O7 79.5(4) . . ? O6 Er2 N4 85.4(4) . . ? N9 Er2 N4 80.2(4) . . ? O5 Er2 N4 137.4(3) . . ? N15 Er2 N4 148.5(4) . . ? O7 Er2 N4 73.0(4) . . ? O6 Er2 N22 142.8(4) . 2 ? N9 Er2 N22 140.4(4) . 2 ? O5 Er2 N22 77.8(3) . 2 ? N15 Er2 N22 77.6(4) . 2 ? O7 Er2 N22 70.1(4) . 2 ? N4 Er2 N22 106.5(4) . 2 ? O6 Er2 N21 151.6(4) . . ? N9 Er2 N21 82.9(4) . . ? O5 Er2 N21 72.2(3) . . ? N15 Er2 N21 132.4(4) . . ? O7 Er2 N21 108.9(4) . . ? N4 Er2 N21 72.7(4) . . ? N22 Er2 N21 63.2(3) 2 . ? C13 Ru1 C14 91.1(5) . . ? C13 Ru1 C16 85.9(6) . . ? C14 Ru1 C16 94.7(6) . . ? C13 Ru1 C15 93.1(5) . . ? C14 Ru1 C15 85.5(5) . . ? C16 Ru1 C15 178.9(6) . . ? C13 Ru1 N2 92.9(5) . . ? C14 Ru1 N2 175.9(5) . . ? C16 Ru1 N2 86.7(5) . . ? C15 Ru1 N2 93.1(5) . . ? C13 Ru1 N1 170.2(5) . . ? C14 Ru1 N1 97.8(5) . . ? C16 Ru1 N1 89.1(5) . . ? C15 Ru1 N1 91.9(5) . . ? N2 Ru1 N1 78.3(5) . . ? C30 Ru2 C29 89.4(6) . . ? C30 Ru2 C31 88.0(6) . . ? C29 Ru2 C31 91.3(6) . . ? C30 Ru2 C32 88.5(5) . . ? C29 Ru2 C32 85.2(6) . . ? C31 Ru2 C32 175.1(5) . . ? C30 Ru2 N7 95.9(5) . . ? C29 Ru2 N7 174.4(5) . . ? C31 Ru2 N7 90.6(5) . . ? C32 Ru2 N7 93.2(5) . . ? C30 Ru2 N8 172.4(5) . . ? C29 Ru2 N8 97.2(5) . . ? C31 Ru2 N8 88.2(5) . . ? C32 Ru2 N8 95.7(5) . . ? N7 Ru2 N8 77.6(5) . . ? C49 Ru3 C46 89.4(7) . . ? C49 Ru3 C48 89.0(10) . . ? C46 Ru3 C48 89.3(8) . . ? C49 Ru3 C47 89.1(8) . . ? C46 Ru3 C47 88.4(7) . . ? C48 Ru3 C47 177.1(9) . . ? C49 Ru3 N14 96.4(8) . . ? C46 Ru3 N14 173.0(8) . . ? C48 Ru3 N14 94.7(8) . . ? C47 Ru3 N14 87.8(7) . . ? C49 Ru3 N13 173.5(7) . . ? C46 Ru3 N13 97.0(6) . . ? C48 Ru3 N13 90.5(9) . . ? C47 Ru3 N13 91.6(6) . . ? N14 Ru3 N13 77.2(7) . . ? N1 C1 C2 119.3(17) . . ? N1 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C3 C2 C1 119.9(18) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 123.1(16) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C3 C4 C5 124.9(17) . . ? C3 C4 C12 113.7(17) . . ? C5 C4 C12 121.3(18) . . ? C6 C5 C4 120.2(17) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 122.6(18) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C11 117.3(15) . . ? C8 C7 C6 124.9(17) . . ? C11 C7 C6 117.7(17) . . ? C7 C8 C9 119.2(15) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 119.7(17) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 123.6(15) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N2 C11 C7 123.0(14) . . ? N2 C11 C12 117.4(13) . . ? C7 C11 C12 119.6(14) . . ? N1 C12 C4 125.0(16) . . ? N1 C12 C11 116.5(13) . . ? C4 C12 C11 118.4(15) . . ? N3 C13 Ru1 171.9(11) . . ? N4 C14 Ru1 176.5(13) . . ? N5 C15 Ru1 176.4(12) . . ? N6 C16 Ru1 175.9(15) . . ? N7 C17 C18 124.8(16) . . ? N7 C17 H17 117.6 . . ? C18 C17 H17 117.6 . . ? C19 C18 C17 117.3(17) . . ? C19 C18 H18 121.4 . . ? C17 C18 H18 121.4 . . ? C18 C19 C20 121.4(15) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 124.1(16) . . ? C19 C20 C28 116.3(14) . . ? C21 C20 C28 119.5(16) . . ? C22 C21 C20 119.0(17) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 125.5(17) . . ? C21 C22 H22 117.2 . . ? C23 C22 H22 117.2 . . ? C24 C23 C27 119.3(15) . . ? C24 C23 C22 125.2(16) . . ? C27 C23 C22 115.4(16) . . ? C25 C24 C23 117.9(16) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C24 C25 C26 120.2(18) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N8 C26 C25 123.0(16) . . ? N8 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? N8 C27 C28 117.8(13) . . ? N8 C27 C23 121.0(15) . . ? C28 C27 C23 121.2(14) . . ? N7 C28 C27 117.2(13) . . ? N7 C28 C20 123.5(14) . . ? C27 C28 C20 119.2(14) . . ? N9 C29 Ru2 171.4(13) . . ? N10 C30 Ru2 175.8(12) . . ? N11 C31 Ru2 177.3(13) . . ? N12 C32 Ru2 174.0(12) . . ? N13 C33 C34 121.4(19) . . ? N13 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C36 C34 C33 120(2) . . ? C36 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C37 C36 C34 119(2) . . ? C37 C36 H36 120.6 . . ? C34 C36 H36 120.6 . . ? C36 C37 C38 122(3) . . ? C36 C37 C45 120(2) . . ? C38 C37 C45 118(3) . . ? C39 C38 C37 120(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 126(3) . . ? C38 C39 H39 116.8 . . ? C40 C39 H39 116.8 . . ? C41 C40 C44 117(4) . . ? C41 C40 C39 129(3) . . ? C44 C40 C39 114(3) . . ? C40 C41 C42 122(3) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C41 C42 C43 121(3) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? N14 C43 C42 117(3) . . ? N14 C43 H43 121.3 . . ? C42 C43 H43 121.3 . . ? N14 C44 C45 115.6(19) . . ? N14 C44 C40 123(3) . . ? C45 C44 C40 122(3) . . ? N13 C45 C37 122(2) . . ? N13 C45 C44 118(2) . . ? C37 C45 C44 120(2) . . ? N15 C46 Ru3 177.0(16) . . ? N16 C47 Ru3 176.6(16) . . ? N17 C48 Ru3 177(2) . . ? N18 C49 Ru3 174.3(19) . . ? N19 C50 C51 121.9(13) . . ? N19 C50 H50 119.1 . . ? C51 C50 H50 119.1 . . ? C50 C51 C35 118.9(13) . . ? C50 C51 H51 120.6 . . ? C35 C51 H51 120.6 . . ? N20 C52 N19 125.4(12) . . ? N20 C52 C52 117.9(15) . 2_566 ? N19 C52 C52 116.7(15) . 2_566 ? C54 C53 C56 116.6(12) . . ? C54 C53 H53 121.7 . . ? C56 C53 H53 121.7 . . ? N21 C54 C53 123.4(13) . . ? N21 C54 H54 118.3 . . ? C53 C54 H54 118.3 . . ? N22 C55 N21 127.0(11) . . ? N22 C55 C55 117.7(15) . 2 ? N21 C55 C55 115.2(15) . 2 ? C1 N1 C12 118.8(13) . . ? C1 N1 Ru1 127.6(11) . . ? C12 N1 Ru1 113.6(10) . . ? C10 N2 C11 117.1(12) . . ? C10 N2 Ru1 128.8(10) . . ? C11 N2 Ru1 114.0(10) . . ? C13 N3 Er1 151.9(11) . . ? C14 N4 Er2 154.3(11) . . ? C17 N7 C28 116.6(13) . . ? C17 N7 Ru2 128.9(10) . . ? C28 N7 Ru2 114.4(10) . . ? C26 N8 C27 118.4(14) . . ? C26 N8 Ru2 128.3(10) . . ? C27 N8 Ru2 113.0(10) . . ? C29 N9 Er2 155.8(11) . . ? C30 N10 Er1 154.4(11) . . ? C33 N13 C45 118.4(17) . . ? C33 N13 Ru3 127.8(13) . . ? C45 N13 Ru3 113.8(13) . . ? C43 N14 C44 120(2) . . ? C43 N14 Ru3 125.7(19) . . ? C44 N14 Ru3 114.2(14) . . ? C46 N15 Er2 177.0(13) . . ? C52 N19 C50 116.4(12) . . ? C52 N19 Er1 121.3(8) . . ? C50 N19 Er1 122.2(9) . . ? C55 N21 C54 115.4(11) . . ? C55 N21 Er2 121.5(8) . . ? C54 N21 Er2 123.1(9) . . ? C55 N22 C56 114.9(12) . . ? C55 N22 Er2 122.3(8) . 2 ? C56 N22 Er2 122.8(9) . 2 ? N22 C56 C53 122.7(14) . . ? N22 C56 H56 118.7 . . ? C53 C56 H56 118.7 . . ? N20 C35 C51 118.2(14) . . ? C52 N20 C35 119.2(13) . . ? C52 N20 Er1 120.4(8) . 2_566 ? C35 N20 Er1 120.2(10) . 2_566 ? C52 N20 H35 120.4 . . ? C35 N20 H35 120.4 . . ? Er1 N20 H35 3.8 2_566 . ? Er1 O1 H1B 106.5 . . ? Er1 O1 H1C 134.5 . . ? H1B O1 H1C 106.1 . . ? Er1 O2 H2B 112.3 . . ? Er1 O2 H2C 81.8 . . ? H2B O2 H2C 93.3 . . ? Er1 O3 H3B 126.3 . . ? Er1 O3 H3C 104.8 . . ? H3B O3 H3C 105.8 . . ? Er1 O4 H4B 101.0 . . ? Er1 O4 H4C 98.6 . . ? H4B O4 H4C 115.7 . . ? Er2 O5 H5B 129.5 . . ? Er2 O5 H5C 127.8 . . ? H5B O5 H5C 95.2 . . ? Er2 O6 H6B 100.8 . . ? Er2 O6 H6C 140.4 . . ? H6B O6 H6C 115.3 . . ? Er2 O7 H7B 100.1 . . ? Er2 O7 H7C 113.9 . . ? H7B O7 H7C 90.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.845 _refine_diff_density_min -2.991 _refine_diff_density_rms 0.224 #===END data_imw701s _database_code_depnum_ccdc_archive 'CCDC 636991' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H78 N22 O24 Ru3 Yb2' _chemical_formula_weight 2092.69 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 15.4596(6) _cell_length_b 15.7478(6) _cell_length_c 17.2375(7) _cell_angle_alpha 110.360(2) _cell_angle_beta 94.733(2) _cell_angle_gamma 94.567(2) _cell_volume 3894.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 3.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5552 _exptl_absorpt_correction_T_max 0.8632 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59145 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13714 _reflns_number_gt 11583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+4.4977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13714 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.962908(12) 1.479393(12) 0.300029(12) 0.01281(6) Uani 1 1 d . . . Yb2 Yb 1.077361(13) 0.997321(13) 0.188641(13) 0.01700(7) Uani 1 1 d . . . Ru1 Ru 0.78197(2) 1.15818(2) 0.21862(2) 0.01350(9) Uani 1 1 d . A . Ru2 Ru 1.25389(2) 1.32797(2) 0.31667(2) 0.01675(9) Uani 1 1 d . A . Ru3 Ru 1.29071(2) 0.72152(2) 0.12585(2) 0.01578(9) Uani 1 1 d . A . C1 C 0.7004(3) 0.9809(3) 0.2400(3) 0.0228(11) Uani 1 1 d . A . H1 H 0.7582 0.9650 0.2437 0.027 Uiso 1 1 calc R . . C2 C 0.6315(3) 0.9231(3) 0.2490(3) 0.0281(12) Uani 1 1 d . . . H2 H 0.6430 0.8694 0.2594 0.034 Uiso 1 1 calc R . . C3 C 0.5472(3) 0.9440(4) 0.2425(3) 0.0278(12) Uani 1 1 d . . . H3 H 0.5002 0.9053 0.2491 0.033 Uiso 1 1 calc R . . C4 C 0.5310(3) 1.0226(3) 0.2263(3) 0.0228(11) Uani 1 1 d . . . C5 C 0.4458(3) 1.0488(4) 0.2161(3) 0.0288(13) Uani 1 1 d . . . H5 H 0.3964 1.0119 0.2208 0.035 Uiso 1 1 calc R . . C6 C 0.4344(3) 1.1250(3) 0.1998(3) 0.0279(12) Uani 1 1 d . . . H6 H 0.3767 1.1396 0.1915 0.034 Uiso 1 1 calc R . . C7 C 0.5071(3) 1.1849(3) 0.1946(3) 0.0229(11) Uani 1 1 d . . . C8 C 0.4990(3) 1.2661(3) 0.1803(3) 0.0278(12) Uani 1 1 d . . . H8 H 0.4432 1.2857 0.1741 0.033 Uiso 1 1 calc R . . C9 C 0.5733(3) 1.3174(4) 0.1754(3) 0.0295(13) Uani 1 1 d . . . H9 H 0.5688 1.3735 0.1670 0.035 Uiso 1 1 calc R . . C10 C 0.6550(3) 1.2875(3) 0.1825(3) 0.0251(12) Uani 1 1 d . A . H10 H 0.7051 1.3222 0.1758 0.030 Uiso 1 1 calc R . . C11 C 0.5910(3) 1.1598(3) 0.2039(3) 0.0193(11) Uani 1 1 d . A . C12 C 0.6034(3) 1.0775(3) 0.2191(3) 0.0174(10) Uani 1 1 d . A . C13 C 0.8561(3) 1.2644(3) 0.2182(3) 0.0155(10) Uani 1 1 d . . . C14 C 0.8874(3) 1.0989(3) 0.2336(3) 0.0143(10) Uani 1 1 d . . . C15 C 0.7788(3) 1.0925(3) 0.0947(3) 0.0172(10) Uani 1 1 d . . . C16 C 0.7811(3) 1.2279(3) 0.3430(3) 0.0208(11) Uani 1 1 d . . . C17 C 1.3271(3) 1.5175(3) 0.3134(3) 0.0243(11) Uani 1 1 d . A . H17 H 1.2697 1.5213 0.2915 0.029 Uiso 1 1 calc R . . C18 C 1.3911(4) 1.5908(3) 0.3276(3) 0.0316(13) Uani 1 1 d . . . H18 H 1.3772 1.6432 0.3161 0.038 Uiso 1 1 calc R . . C19 C 1.4741(4) 1.5860(4) 0.3584(4) 0.0329(13) Uani 1 1 d . . . H19 H 1.5179 1.6358 0.3690 0.040 Uiso 1 1 calc R . . C20 C 1.4951(3) 1.5082(3) 0.3744(3) 0.0282(12) Uani 1 1 d . . . C21 C 1.5796(3) 1.4973(4) 0.4071(4) 0.0346(14) Uani 1 1 d . . . H21 H 1.6264 1.5441 0.4171 0.042 Uiso 1 1 calc R . . C22 C 1.5944(3) 1.4224(4) 0.4239(4) 0.0348(14) Uani 1 1 d . . . H22 H 1.6515 1.4174 0.4455 0.042 Uiso 1 1 calc R . . C23 C 1.5264(3) 1.3499(3) 0.4104(3) 0.0256(12) Uani 1 1 d . . . C24 C 1.5371(3) 1.2718(4) 0.4296(3) 0.0321(13) Uani 1 1 d . . . H24 H 1.5929 1.2634 0.4514 0.039 Uiso 1 1 calc R . . C25 C 1.4673(4) 1.2074(4) 0.4171(3) 0.0317(13) Uani 1 1 d . . . H25 H 1.4737 1.1548 0.4310 0.038 Uiso 1 1 calc R . . C26 C 1.3854(3) 1.2209(3) 0.3831(3) 0.0262(12) Uani 1 1 d . A . H26 H 1.3370 1.1761 0.3745 0.031 Uiso 1 1 calc R . . C27 C 1.4421(3) 1.3585(3) 0.3778(3) 0.0205(11) Uani 1 1 d . A . C28 C 1.4266(3) 1.4377(3) 0.3598(3) 0.0208(11) Uani 1 1 d . A . C29 C 1.1501(3) 1.3759(3) 0.2831(3) 0.0178(10) Uani 1 1 d . . . C30 C 1.1802(3) 1.2134(3) 0.3012(3) 0.0173(10) Uani 1 1 d . . . C31 C 1.2669(3) 1.2674(3) 0.1932(3) 0.0193(11) Uani 1 1 d . . . C32 C 1.2293(3) 1.3880(4) 0.4358(3) 0.0296(13) Uani 1 1 d . . . C33 C 1.3790(3) 0.8572(3) 0.0524(3) 0.0237(11) Uani 1 1 d . A . H33 H 1.3251 0.8826 0.0550 0.028 Uiso 1 1 calc R . . C34 C 1.4473(4) 0.8954(4) 0.0224(3) 0.0302(13) Uani 1 1 d . . . H34 H 1.4394 0.9454 0.0048 0.036 Uiso 1 1 calc R . . C35 C 1.5259(4) 0.8602(4) 0.0187(3) 0.0331(13) Uani 1 1 d . . . H35 H 1.5738 0.8873 0.0009 0.040 Uiso 1 1 calc R . . C36 C 1.5347(3) 0.7844(4) 0.0414(3) 0.0279(12) Uani 1 1 d . . . C37 C 1.6125(3) 0.7399(4) 0.0376(4) 0.0365(14) Uani 1 1 d . . . H37 H 1.6625 0.7638 0.0201 0.044 Uiso 1 1 calc R . . C38 C 1.6168(4) 0.6652(4) 0.0583(4) 0.0393(15) Uani 1 1 d . . . H38 H 1.6696 0.6380 0.0555 0.047 Uiso 1 1 calc R . . C39 C 1.5433(3) 0.6265(4) 0.0842(3) 0.0295(12) Uani 1 1 d . . . C40 C 1.5406(4) 0.5458(4) 0.1021(4) 0.0383(15) Uani 1 1 d . . . H40 H 1.5913 0.5152 0.1003 0.046 Uiso 1 1 calc R . . C41 C 1.4656(4) 0.5117(4) 0.1219(3) 0.0314(13) Uani 1 1 d . . . H41 H 1.4637 0.4572 0.1340 0.038 Uiso 1 1 calc R . . C42 C 1.3914(3) 0.5569(4) 0.1244(3) 0.0272(12) Uani 1 1 d . A . H42 H 1.3391 0.5312 0.1369 0.033 Uiso 1 1 calc R . . C43 C 1.4663(3) 0.6693(3) 0.0898(3) 0.0209(11) Uani 1 1 d . A . C44 C 1.4627(3) 0.7493(3) 0.0693(3) 0.0197(11) Uani 1 1 d . A . C45 C 1.2080(3) 0.8156(3) 0.1443(3) 0.0183(10) Uani 1 1 d . . . C46 C 1.2124(3) 0.6462(3) 0.1668(3) 0.0202(11) Uani 1 1 d . . . C47 C 1.2341(3) 0.6511(3) 0.0070(3) 0.0240(11) Uani 1 1 d . . . C48 C 1.3500(3) 0.7883(3) 0.2445(3) 0.0198(11) Uani 1 1 d . . . C53 C 0.9851(3) 1.6738(3) 0.4757(3) 0.0177(10) Uani 1 1 d . . . H53 H 0.9800 1.7012 0.4346 0.021 Uiso 1 1 calc R . . C54 C 0.9899(3) 1.7279(3) 0.5586(3) 0.0184(10) Uani 1 1 d . . . H54 H 0.9866 1.7916 0.5750 0.022 Uiso 1 1 calc R . . C55 C 1.0240(3) 0.8180(3) 0.0041(3) 0.0227(11) Uani 1 1 d . . . H55 H 1.0429 0.7869 0.0396 0.027 Uiso 1 1 calc R A . C56 C 0.9942(3) 0.7691(3) -0.0778(3) 0.0196(11) Uani 1 1 d . A . H56 H 0.9912 0.7045 -0.0995 0.024 Uiso 1 1 calc R . . N1 N 0.6877(2) 1.0572(2) 0.2264(2) 0.0157(8) Uani 1 1 d . . . N2 N 0.6651(2) 1.2113(2) 0.1985(2) 0.0172(9) Uani 1 1 d . . . N3 N 0.8967(2) 1.3332(3) 0.2269(2) 0.0164(8) Uani 1 1 d . . . N4 N 0.9496(2) 1.0636(3) 0.2369(2) 0.0184(9) Uani 1 1 d . A . N5 N 0.7752(3) 1.0517(3) 0.0233(3) 0.0270(10) Uani 1 1 d . A . N6 N 0.7788(3) 1.2705(3) 0.4115(3) 0.0309(11) Uani 1 1 d . A . N7 N 1.3427(2) 1.4422(3) 0.3292(3) 0.0199(9) Uani 1 1 d . . . N8 N 1.3730(2) 1.2932(3) 0.3628(2) 0.0194(9) Uani 1 1 d . . . N9 N 1.0879(2) 1.4057(3) 0.2665(2) 0.0175(9) Uani 1 1 d . . . N10 N 1.1374(3) 1.1433(3) 0.2811(3) 0.0203(9) Uani 1 1 d . A . N11 N 1.2632(3) 1.2308(3) 0.1219(3) 0.0249(10) Uani 1 1 d . A . N12 N 1.2127(3) 1.4247(4) 0.5026(3) 0.0553(17) Uani 1 1 d . A . N13 N 1.3859(2) 0.7878(3) 0.0771(2) 0.0189(9) Uani 1 1 d . . . N14 N 1.3908(3) 0.6342(3) 0.1103(2) 0.0206(9) Uani 1 1 d . . . N15 N 1.1609(3) 0.8720(3) 0.1575(2) 0.0203(9) Uani 1 1 d . A . N16 N 1.1687(3) 0.5968(3) 0.1882(3) 0.0285(10) Uani 1 1 d . A . N17 N 1.2060(3) 0.6091(3) -0.0609(3) 0.0382(12) Uani 1 1 d . A . N18 N 1.3847(3) 0.8238(3) 0.3113(3) 0.0261(10) Uani 1 1 d . A . N21 N 0.9874(2) 1.5833(2) 0.4516(2) 0.0143(8) Uani 1 1 d . . . N22 N 1.0270(2) 0.9097(3) 0.0353(3) 0.0193(9) Uani 1 1 d . A . C51 C 0.9996(3) 1.6874(3) 0.6162(3) 0.0168(10) Uani 1 1 d . . . H51 H 1.0022 1.7237 0.6735 0.020 Uiso 1 1 calc R . . C52 C 0.9976(3) 1.5498(3) 0.5125(3) 0.0135(10) Uani 1 1 d . . . N20 N 1.0057(2) 1.5975(2) 0.5945(2) 0.0139(8) Uani 1 1 d . . . C49 C 0.9688(3) 0.8170(3) -0.1276(3) 0.0166(10) Uani 1 1 d . . . H49 H 0.9493 0.7843 -0.1848 0.020 Uiso 1 1 calc R A . C50 C 0.9993(3) 0.9494(3) -0.0172(3) 0.0159(10) Uani 1 1 d . . . N19 N 0.9707(2) 0.9080(2) -0.0981(2) 0.0158(8) Uani 1 1 d . . . O1 O 1.1421(5) 0.9970(5) 0.3213(4) 0.0263(16) Uani 0.50 1 d PU A 1 O1' O 1.0839(5) 0.9676(4) 0.3062(4) 0.0172(14) Uani 0.50 1 d PU A 2 O2 O 1.2004(2) 1.0387(2) 0.13604(19) 0.0175(7) Uani 1 1 d . A . H2B H 1.2165 1.0884 0.1319 0.021 Uiso 1 1 d R . . H2C H 1.2123 1.0014 0.0858 0.021 Uiso 1 1 d R . . O3 O 0.9973(5) 0.8793(5) 0.2057(5) 0.0272(15) Uani 0.50 1 d PU A 1 O3' O 0.9515(4) 0.8778(4) 0.1583(4) 0.0156(13) Uani 0.50 1 d PU A 2 O4 O 1.0737(2) 1.5940(2) 0.3155(2) 0.0236(8) Uani 1 1 d . . . H4B H 1.0576 1.6433 0.3127 0.028 Uiso 1 1 d R . . H4C H 1.1105 1.5815 0.2725 0.028 Uiso 1 1 d R . . O5 O 0.8874(2) 1.6004(2) 0.2979(2) 0.0318(9) Uani 1 1 d . . . O6 O 0.9513(2) 1.4645(2) 0.1626(2) 0.0252(8) Uani 1 1 d . . . H6B H 0.8994 1.4414 0.1392 0.030 Uiso 1 1 d R . . H6C H 0.9655 1.5039 0.1488 0.030 Uiso 1 1 d R . . O7 O 0.8297(2) 1.4592(2) 0.3510(2) 0.0287(9) Uani 1 1 d . . . H7B H 0.8133 1.4994 0.3930 0.034 Uiso 1 1 d R . . H7C H 0.8044 1.4120 0.3429 0.034 Uiso 1 1 d R . . O8 O 0.8168(3) 0.8784(3) 0.0415(3) 0.0422(10) Uani 1 1 d . . . H8B H 0.8018 0.8327 -0.0031 0.051 Uiso 1 1 d R . . H8C H 0.8049 0.9321 0.0486 0.051 Uiso 1 1 d R . . O9 O 0.0076(2) 0.5688(3) 0.0762(2) 0.0375(10) Uani 1 1 d . . . O10 O 1.5662(3) 1.7829(3) 0.3472(3) 0.0521(12) Uani 1 1 d . . . H10B H 1.5154 1.7862 0.3264 0.062 Uiso 1 1 d R . . H10C H 1.5546 1.7709 0.3924 0.062 Uiso 1 1 d R . . O11 O 1.1913(3) 1.5896(3) 0.4361(3) 0.0529(13) Uani 1 1 d . . . H11B H 1.1647 1.5823 0.3887 0.063 Uiso 1 1 d R . . H11C H 1.2053 1.6411 0.4750 0.063 Uiso 1 1 d R . . O12 O 1.2006(3) 0.4018(3) 0.0888(3) 0.0573(13) Uani 1 1 d . . . H12B H 1.2201 0.3686 0.1144 0.069 Uiso 1 1 d R . . H12C H 1.1815 0.4352 0.1274 0.069 Uiso 1 1 d R . . O13 O 0.7717(3) 0.5724(3) 0.1595(3) 0.0555(13) Uani 1 1 d . . . H13B H 0.8041 0.5962 0.1333 0.067 Uiso 1 1 d R . . H13C H 0.7773 0.5163 0.1484 0.067 Uiso 1 1 d R . . O14 O 1.8416(5) 1.1742(5) 0.6633(5) 0.0294(15) Uani 0.50 1 d PU B 1 O14' O 1.7874(5) 1.1353(5) 0.6301(5) 0.0347(16) Uani 0.50 1 d PU C 2 O15 O 1.1342(5) 1.1276(5) 0.7071(4) 0.0274(17) Uani 0.50 1 d P . . O16 O 1.7785(5) 1.1449(5) 0.4974(5) 0.0319(18) Uiso 0.50 1 d P . . O17 O 2.1047(5) 0.9776(5) 0.5613(5) 0.0321(18) Uiso 0.50 1 d P . . O18 O 1.2697(5) 1.2636(5) 0.7125(5) 0.0356(19) Uani 0.50 1 d P . . O19 O 0.1351(4) 0.3419(5) 0.9271(4) 0.113(3) Uani 1 1 d . . . H19B H 0.6422 1.1838 0.2188 0.135 Uiso 1 1 d R . . H19C H 0.1533 0.3579 0.9786 0.135 Uiso 1 1 d R . . O20 O 2.0143(6) 1.2494(6) 0.7023(7) 0.062(2) Uani 0.50 1 d PU D 1 O20' O 1.9507(6) 1.2219(6) 0.6911(7) 0.055(2) Uani 0.50 1 d PU E 2 O21 O 1.3281(6) 1.0632(6) 0.5385(6) 0.0447(18) Uani 0.50 1 d PU F 1 O21' O 1.3382(6) 1.1097(6) 0.5122(6) 0.0521(19) Uani 0.50 1 d PU G 2 O22 O 1.3799(5) 0.9316(6) 0.4867(5) 0.053(2) Uani 0.50 1 d P H 1 O22' O 1.4548(6) 0.9985(6) 0.4332(6) 0.055(3) Uani 0.50 1 d P I 2 O23 O 0.8319(5) 0.8185(6) 0.1576(6) 0.050(2) Uani 0.50 1 d P . . O24 O 1.3447(6) 1.3503(7) 0.7150(6) 0.065(3) Uani 0.50 1 d P . . O25 O 1.9233(4) 1.9172(4) 0.5352(4) 0.0236(15) Uani 0.50 1 d P J 1 O25' O 1.8159(5) 1.8704(5) 0.5164(5) 0.0350(15) Uani 0.50 1 d PU K 2 O26 O 1.7980(5) 1.7669(5) 0.4555(5) 0.0320(13) Uani 0.50 1 d PU L 1 O26' O 1.7794(5) 1.6877(5) 0.4201(5) 0.0335(15) Uani 0.50 1 d PU M 2 O27 O 2.0730(6) 0.9620(6) 0.5958(6) 0.046(2) Uiso 0.50 1 d P . . O28 O 1.7714(5) 1.0941(6) 0.4594(6) 0.042(2) Uiso 0.50 1 d P . . 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 Yb1 0.01276(11) 0.01221(11) 0.01313(11) 0.00346(8) 0.00237(8) 0.00355(8) Yb2 0.02038(12) 0.01150(11) 0.02063(12) 0.00493(9) 0.01088(9) 0.00560(8) Ru1 0.00971(19) 0.01351(18) 0.0159(2) 0.00270(16) 0.00417(14) 0.00253(14) Ru2 0.00804(19) 0.01602(19) 0.0198(2) -0.00204(17) 0.00272(15) 0.00250(15) Ru3 0.0131(2) 0.0187(2) 0.0176(2) 0.00862(17) 0.00180(15) 0.00386(15) C1 0.020(3) 0.026(3) 0.023(3) 0.008(2) 0.003(2) 0.002(2) C2 0.035(3) 0.023(3) 0.031(3) 0.014(2) 0.007(2) 0.001(2) C3 0.025(3) 0.031(3) 0.025(3) 0.007(2) 0.009(2) -0.008(2) C4 0.017(3) 0.025(3) 0.020(3) 0.000(2) 0.006(2) -0.001(2) C5 0.015(3) 0.032(3) 0.029(3) -0.001(2) 0.008(2) -0.007(2) C6 0.009(2) 0.031(3) 0.032(3) -0.003(3) 0.005(2) 0.003(2) C7 0.014(3) 0.025(3) 0.023(3) -0.001(2) 0.004(2) 0.005(2) C8 0.016(3) 0.029(3) 0.033(3) 0.001(2) 0.001(2) 0.012(2) C9 0.022(3) 0.025(3) 0.040(3) 0.009(3) 0.001(2) 0.011(2) C10 0.019(3) 0.019(3) 0.036(3) 0.007(2) 0.005(2) 0.006(2) C11 0.010(2) 0.021(2) 0.019(3) -0.003(2) 0.0030(19) 0.0001(19) C12 0.016(2) 0.020(2) 0.013(2) 0.001(2) 0.0043(19) 0.002(2) C13 0.011(2) 0.022(3) 0.013(2) 0.004(2) 0.0037(18) 0.007(2) C14 0.017(3) 0.014(2) 0.009(2) 0.0015(19) 0.0042(18) -0.004(2) C15 0.013(2) 0.018(2) 0.021(3) 0.008(2) 0.0039(19) 0.0060(19) C16 0.014(2) 0.023(3) 0.024(3) 0.007(2) 0.003(2) 0.004(2) C17 0.018(3) 0.020(3) 0.028(3) 0.000(2) 0.002(2) 0.007(2) C18 0.036(3) 0.019(3) 0.036(3) 0.007(2) 0.003(3) 0.002(2) C19 0.028(3) 0.028(3) 0.036(3) 0.006(3) 0.002(2) -0.011(2) C20 0.016(3) 0.027(3) 0.034(3) 0.004(2) 0.002(2) -0.003(2) C21 0.016(3) 0.038(3) 0.042(4) 0.007(3) 0.001(2) -0.007(2) C22 0.012(3) 0.048(4) 0.038(3) 0.008(3) -0.002(2) 0.001(2) C23 0.012(3) 0.033(3) 0.029(3) 0.005(2) 0.004(2) 0.006(2) C24 0.020(3) 0.041(3) 0.033(3) 0.008(3) 0.000(2) 0.014(3) C25 0.032(3) 0.030(3) 0.033(3) 0.009(3) 0.003(2) 0.011(3) C26 0.022(3) 0.024(3) 0.029(3) 0.003(2) 0.005(2) 0.006(2) C27 0.012(2) 0.025(3) 0.021(3) 0.002(2) 0.006(2) 0.004(2) C28 0.014(2) 0.023(3) 0.021(3) 0.001(2) 0.004(2) 0.003(2) C29 0.016(3) 0.011(2) 0.018(3) -0.006(2) 0.006(2) -0.0026(19) C30 0.011(2) 0.027(3) 0.012(2) 0.004(2) 0.0024(18) 0.007(2) C31 0.012(2) 0.017(2) 0.034(3) 0.013(2) 0.011(2) 0.0055(19) C32 0.007(2) 0.037(3) 0.032(3) -0.003(3) 0.003(2) 0.003(2) C33 0.023(3) 0.028(3) 0.021(3) 0.010(2) 0.002(2) 0.004(2) C34 0.040(3) 0.027(3) 0.026(3) 0.012(2) 0.005(2) -0.003(2) C35 0.031(3) 0.040(3) 0.029(3) 0.012(3) 0.013(2) -0.004(3) C36 0.026(3) 0.036(3) 0.022(3) 0.011(2) 0.007(2) 0.001(2) C37 0.018(3) 0.058(4) 0.038(4) 0.019(3) 0.013(2) 0.008(3) C38 0.018(3) 0.066(4) 0.041(4) 0.023(3) 0.015(3) 0.016(3) C39 0.024(3) 0.040(3) 0.024(3) 0.010(3) 0.003(2) 0.011(2) C40 0.036(3) 0.051(4) 0.038(4) 0.022(3) 0.010(3) 0.030(3) C41 0.037(3) 0.034(3) 0.031(3) 0.017(3) 0.009(3) 0.017(3) C42 0.031(3) 0.033(3) 0.023(3) 0.014(2) 0.007(2) 0.009(2) C43 0.017(3) 0.028(3) 0.016(3) 0.004(2) 0.004(2) 0.005(2) C44 0.014(2) 0.028(3) 0.015(3) 0.005(2) 0.0041(19) 0.003(2) C45 0.019(3) 0.018(2) 0.017(3) 0.008(2) -0.002(2) -0.004(2) C46 0.017(3) 0.023(3) 0.017(3) 0.003(2) 0.001(2) 0.003(2) C47 0.019(3) 0.028(3) 0.025(3) 0.010(2) 0.001(2) 0.000(2) C48 0.013(2) 0.019(2) 0.032(3) 0.013(2) 0.007(2) 0.004(2) C53 0.019(3) 0.014(2) 0.022(3) 0.009(2) 0.005(2) 0.0039(19) C54 0.019(3) 0.015(2) 0.020(3) 0.004(2) 0.003(2) 0.0054(19) C55 0.019(3) 0.015(2) 0.032(3) 0.007(2) -0.002(2) 0.002(2) C56 0.013(2) 0.014(2) 0.030(3) 0.005(2) 0.000(2) 0.0021(19) N1 0.012(2) 0.016(2) 0.015(2) 0.0006(17) 0.0029(16) -0.0008(16) N2 0.016(2) 0.0136(19) 0.020(2) 0.0018(17) 0.0055(16) 0.0024(16) N3 0.017(2) 0.016(2) 0.015(2) 0.0025(17) 0.0045(16) 0.0033(17) N4 0.013(2) 0.023(2) 0.021(2) 0.0087(18) 0.0029(16) 0.0058(18) N5 0.030(3) 0.029(2) 0.025(3) 0.012(2) 0.0059(19) 0.011(2) N6 0.024(2) 0.035(3) 0.026(3) 0.001(2) 0.006(2) 0.005(2) N7 0.012(2) 0.017(2) 0.025(2) -0.0003(18) 0.0025(17) 0.0035(16) N8 0.014(2) 0.016(2) 0.023(2) 0.0002(18) 0.0047(17) 0.0033(16) N9 0.014(2) 0.018(2) 0.020(2) 0.0047(18) 0.0052(17) -0.0007(17) N10 0.015(2) 0.022(2) 0.022(2) 0.0052(19) 0.0045(17) 0.0018(18) N11 0.023(2) 0.025(2) 0.028(3) 0.008(2) 0.0133(19) 0.0094(19) N12 0.014(2) 0.076(4) 0.037(3) -0.029(3) 0.004(2) 0.003(2) N13 0.018(2) 0.025(2) 0.015(2) 0.0097(18) 0.0006(16) 0.0005(17) N14 0.024(2) 0.022(2) 0.017(2) 0.0075(18) 0.0014(17) 0.0080(18) N15 0.025(2) 0.016(2) 0.020(2) 0.0064(18) -0.0010(18) 0.0053(18) N16 0.023(2) 0.035(3) 0.031(3) 0.015(2) 0.007(2) 0.002(2) N17 0.035(3) 0.049(3) 0.028(3) 0.013(3) -0.004(2) -0.003(2) N18 0.024(2) 0.024(2) 0.027(3) 0.006(2) -0.002(2) -0.0011(19) N21 0.0113(19) 0.0155(19) 0.017(2) 0.0060(17) 0.0044(16) 0.0036(15) N22 0.014(2) 0.017(2) 0.027(2) 0.0074(18) -0.0028(17) 0.0061(16) C51 0.013(2) 0.017(2) 0.018(3) 0.002(2) 0.0041(19) 0.0023(19) C52 0.006(2) 0.017(2) 0.017(3) 0.005(2) 0.0034(18) 0.0009(18) N20 0.0098(19) 0.0153(19) 0.017(2) 0.0051(17) 0.0024(15) 0.0027(15) C49 0.009(2) 0.018(2) 0.021(3) 0.003(2) 0.0036(19) 0.0034(18) C50 0.005(2) 0.016(2) 0.024(3) 0.004(2) 0.0034(19) 0.0010(18) N19 0.0105(19) 0.0142(19) 0.022(2) 0.0036(17) 0.0064(16) 0.0037(16) O1 0.038(4) 0.021(4) 0.020(3) 0.006(3) 0.000(3) 0.008(3) O1' 0.022(4) 0.017(3) 0.014(3) 0.007(3) 0.003(3) 0.006(3) O2 0.0192(17) 0.0151(16) 0.0204(18) 0.0066(14) 0.0111(14) 0.0050(13) O3 0.024(4) 0.022(3) 0.036(4) 0.009(3) 0.008(3) 0.000(3) O3' 0.016(3) 0.012(3) 0.018(4) 0.006(3) -0.001(3) -0.001(3) O4 0.0254(19) 0.0123(16) 0.033(2) 0.0045(15) 0.0146(16) 0.0045(14) O5 0.047(2) 0.0223(19) 0.025(2) 0.0043(16) -0.0019(17) 0.0198(17) O6 0.031(2) 0.0233(18) 0.0228(19) 0.0126(16) -0.0016(15) -0.0030(15) O7 0.0160(18) 0.030(2) 0.028(2) -0.0067(16) 0.0086(15) 0.0017(15) O8 0.050(3) 0.024(2) 0.045(3) 0.0026(19) 0.007(2) 0.0081(19) O9 0.034(2) 0.047(2) 0.039(2) 0.024(2) 0.0052(18) 0.0017(19) O10 0.040(3) 0.056(3) 0.075(3) 0.047(3) -0.001(2) -0.007(2) O11 0.031(2) 0.064(3) 0.030(2) -0.024(2) -0.0046(18) 0.009(2) O12 0.069(3) 0.050(3) 0.071(3) 0.036(3) 0.028(3) 0.026(2) O13 0.053(3) 0.082(3) 0.035(3) 0.017(2) 0.007(2) 0.046(3) O14 0.037(4) 0.026(4) 0.028(4) 0.009(3) 0.008(3) 0.014(3) O14' 0.040(4) 0.031(4) 0.032(4) 0.008(3) 0.009(3) 0.011(3) O15 0.032(4) 0.033(4) 0.022(4) 0.012(3) 0.008(3) 0.020(3) O18 0.036(5) 0.041(5) 0.027(4) 0.006(4) 0.003(3) 0.019(4) O19 0.145(6) 0.182(7) 0.073(4) 0.087(5) 0.063(4) 0.131(5) O20 0.040(4) 0.038(4) 0.118(6) 0.043(4) -0.006(5) 0.006(4) O20' 0.035(4) 0.036(4) 0.108(6) 0.044(4) -0.001(5) 0.009(4) O21 0.044(4) 0.046(5) 0.051(5) 0.024(3) 0.005(3) 0.009(4) O21' 0.049(4) 0.050(5) 0.058(5) 0.020(4) 0.002(4) 0.012(4) O22 0.039(5) 0.062(6) 0.038(5) -0.004(5) 0.009(4) -0.007(4) O22' 0.046(6) 0.056(6) 0.045(6) -0.002(5) 0.008(4) -0.010(4) O23 0.035(5) 0.051(5) 0.068(6) 0.029(5) -0.003(4) 0.007(4) O24 0.037(5) 0.088(7) 0.051(6) 0.001(5) 0.007(4) 0.011(5) O25 0.034(4) 0.016(3) 0.021(4) 0.007(3) 0.000(3) 0.007(3) O25' 0.038(3) 0.031(3) 0.035(3) 0.010(3) 0.002(3) 0.007(3) O26 0.033(3) 0.029(3) 0.035(3) 0.011(2) 0.003(2) 0.008(2) O26' 0.035(3) 0.031(3) 0.035(3) 0.010(3) 0.005(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O6 2.289(3) . ? Yb1 N3 2.308(4) . ? Yb1 O4 2.315(3) . ? Yb1 O5 2.322(3) . ? Yb1 N9 2.342(4) . ? Yb1 O7 2.347(3) . ? Yb1 N21 2.531(4) . ? Yb1 N20 2.546(4) 2_786 ? Yb1 H6B 2.7037 . ? Yb2 O1' 2.229(6) . ? Yb2 O3 2.268(7) . ? Yb2 O2 2.316(3) . ? Yb2 N10 2.357(4) . ? Yb2 N15 2.374(4) . ? Yb2 N4 2.383(4) . ? Yb2 O1 2.421(7) . ? Yb2 O3' 2.483(6) . ? Yb2 N22 2.540(4) . ? Yb2 N19 2.610(4) 2_775 ? Ru1 C13 1.954(5) . ? Ru1 C14 1.984(5) . ? Ru1 C15 2.018(5) . ? Ru1 C16 2.043(5) . ? Ru1 N2 2.104(4) . ? Ru1 N1 2.118(4) . ? Ru2 C29 1.955(5) . ? Ru2 C30 1.978(5) . ? Ru2 C32 2.022(5) . ? Ru2 C31 2.042(5) . ? Ru2 N7 2.110(4) . ? Ru2 N8 2.132(4) . ? Ru3 C46 1.966(5) . ? Ru3 C45 1.993(5) . ? Ru3 C47 2.040(5) . ? Ru3 C48 2.042(5) . ? Ru3 N14 2.122(4) . ? Ru3 N13 2.129(4) . ? C1 N1 1.327(6) . ? C1 C2 1.399(7) . ? C1 H1 0.9500 . ? C2 C3 1.376(7) . ? C2 H2 0.9500 . ? C3 C4 1.397(7) . ? C3 H3 0.9500 . ? C4 C12 1.401(6) . ? C4 C5 1.426(7) . ? C5 C6 1.344(8) . ? C5 H5 0.9500 . ? C6 C7 1.437(7) . ? C6 H6 0.9500 . ? C7 C8 1.398(7) . ? C7 C11 1.398(7) . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.394(7) . ? C9 H9 0.9500 . ? C10 N2 1.339(6) . ? C10 H10 0.9500 . ? C11 N2 1.379(6) . ? C11 C12 1.433(7) . ? C11 H19B 0.8289 . ? C12 N1 1.372(6) . ? C13 N3 1.163(6) . ? C14 N4 1.156(6) . ? C15 N5 1.168(6) . ? C16 N6 1.141(6) . ? C17 N7 1.342(6) . ? C17 C18 1.398(7) . ? C17 H17 0.9500 . ? C18 C19 1.365(8) . ? C18 H18 0.9500 . ? C19 C20 1.402(8) . ? C19 H19 0.9500 . ? C20 C28 1.411(7) . ? C20 C21 1.427(7) . ? C21 C22 1.340(8) . ? C21 H21 0.9500 . ? C22 C23 1.431(7) . ? C22 H22 0.9500 . ? C23 C24 1.399(7) . ? C23 C27 1.412(7) . ? C24 C25 1.370(8) . ? C24 H24 0.9500 . ? C25 C26 1.413(7) . ? C25 H25 0.9500 . ? C26 N8 1.325(6) . ? C26 H26 0.9500 . ? C27 N8 1.365(6) . ? C27 C28 1.418(7) . ? C28 N7 1.376(6) . ? C29 N9 1.161(6) . ? C30 N10 1.164(6) . ? C31 N11 1.156(6) . ? C32 N12 1.156(7) . ? C33 N13 1.312(6) . ? C33 C34 1.395(7) . ? C33 H33 0.9500 . ? C34 C35 1.373(8) . ? C34 H34 0.9500 . ? C35 C36 1.393(8) . ? C35 H35 0.9500 . ? C36 C44 1.397(7) . ? C36 C37 1.435(8) . ? C37 C38 1.347(8) . ? C37 H37 0.9500 . ? C38 C39 1.423(8) . ? C38 H38 0.9500 . ? C39 C40 1.406(8) . ? C39 C43 1.408(7) . ? C40 C41 1.358(8) . ? C40 H40 0.9500 . ? C41 C42 1.393(7) . ? C41 H41 0.9500 . ? C42 N14 1.324(6) . ? C42 H42 0.9500 . ? C43 N14 1.375(6) . ? C43 C44 1.426(7) . ? C44 N13 1.370(6) . ? C45 N15 1.167(6) . ? C46 N16 1.164(6) . ? C47 N17 1.151(7) . ? C48 N18 1.153(6) . ? C53 N21 1.343(5) . ? C53 C54 1.378(7) . ? C53 H53 0.9500 . ? C54 C51 1.359(7) . ? C54 H54 0.9500 . ? C55 N22 1.348(6) . ? C55 C56 1.371(7) . ? C55 H55 0.9500 . ? C56 C49 1.379(7) . ? C56 H56 0.9500 . ? N2 H19B 0.7334 . ? N21 C52 1.334(6) . ? N22 C50 1.328(6) . ? C51 N20 1.346(6) . ? C51 H51 0.9500 . ? C52 N20 1.340(6) . ? C52 C52 1.484(8) 2_786 ? N20 Yb1 2.546(4) 2_786 ? C49 N19 1.341(6) . ? C49 H49 0.9500 . ? C50 N19 1.336(6) . ? C50 C50 1.493(9) 2_775 ? N19 Yb2 2.610(4) 2_775 ? O2 H2B 0.8315 . ? O2 H2C 0.9053 . ? O4 H4B 0.8500 . ? O4 H4C 0.9473 . ? O6 H6B 0.8592 . ? O6 H6C 0.7599 . ? O7 H7B 0.8507 . ? O7 H7C 0.7729 . ? O8 H8B 0.8500 . ? O8 H8C 0.8499 . ? O10 H10B 0.8500 . ? O10 H10C 0.8908 . ? O11 H11B 0.8500 . ? O11 H11C 0.8500 . ? O12 H12B 0.8503 . ? O12 H12C 0.7862 . ? O13 H13B 0.8500 . ? O13 H13C 0.8501 . ? O16 O28 0.831(9) . ? O17 O27 0.885(9) . ? O18 O24 1.705(13) . ? O19 H19C 0.8501 . ? 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 O6 Yb1 N3 74.23(12) . . ? O6 Yb1 O4 84.07(12) . . ? N3 Yb1 O4 148.92(12) . . ? O6 Yb1 O5 76.99(12) . . ? N3 Yb1 O5 118.08(13) . . ? O4 Yb1 O5 76.93(13) . . ? O6 Yb1 N9 82.73(13) . . ? N3 Yb1 N9 80.84(13) . . ? O4 Yb1 N9 74.46(12) . . ? O5 Yb1 N9 146.33(14) . . ? O6 Yb1 O7 114.93(12) . . ? N3 Yb1 O7 71.11(12) . . ? O4 Yb1 O7 139.49(11) . . ? O5 Yb1 O7 73.58(13) . . ? N9 Yb1 O7 139.95(13) . . ? O6 Yb1 N21 148.40(12) . . ? N3 Yb1 N21 135.59(12) . . ? O4 Yb1 N21 71.60(12) . . ? O5 Yb1 N21 78.07(12) . . ? N9 Yb1 N21 108.75(13) . . ? O7 Yb1 N21 75.58(12) . . ? O6 Yb1 N20 146.27(11) . 2_786 ? N3 Yb1 N20 79.03(13) . 2_786 ? O4 Yb1 N20 110.56(12) . 2_786 ? O5 Yb1 N20 134.88(12) . 2_786 ? N9 Yb1 N20 72.95(12) . 2_786 ? O7 Yb1 N20 74.06(12) . 2_786 ? N21 Yb1 N20 63.97(11) . 2_786 ? O6 Yb1 H6B 17.4 . . ? N3 Yb1 H6B 63.1 . . ? O4 Yb1 H6B 99.8 . . ? O5 Yb1 H6B 73.7 . . ? N9 Yb1 H6B 94.0 . . ? O7 Yb1 H6B 97.9 . . ? N21 Yb1 H6B 151.7 . . ? N20 Yb1 H6B 141.6 2_786 . ? O1' Yb2 O3 55.4(3) . . ? O1' Yb2 O2 122.9(2) . . ? O3 Yb2 O2 144.54(19) . . ? O1' Yb2 N10 82.0(2) . . ? O3 Yb2 N10 133.1(2) . . ? O2 Yb2 N10 72.86(12) . . ? O1' Yb2 N15 77.74(19) . . ? O3 Yb2 N15 71.9(2) . . ? O2 Yb2 N15 73.42(12) . . ? N10 Yb2 N15 121.08(14) . . ? O1' Yb2 N4 83.07(19) . . ? O3 Yb2 N4 78.0(2) . . ? O2 Yb2 N4 136.83(12) . . ? N10 Yb2 N4 78.42(13) . . ? N15 Yb2 N4 149.72(14) . . ? O1' Yb2 O1 23.1(2) . . ? O3 Yb2 O1 76.5(3) . . ? O2 Yb2 O1 100.6(2) . . ? N10 Yb2 O1 66.85(19) . . ? N15 Yb2 O1 73.77(19) . . ? N4 Yb2 O1 96.9(2) . . ? O1' Yb2 O3' 78.1(2) . . ? O3 Yb2 O3' 24.5(2) . . ? O2 Yb2 O3' 143.22(16) . . ? N10 Yb2 O3' 143.69(17) . . ? N15 Yb2 O3' 83.87(17) . . ? N4 Yb2 O3' 69.30(17) . . ? O1 Yb2 O3' 100.3(2) . . ? O1' Yb2 N22 136.58(19) . . ? O3 Yb2 N22 83.2(2) . . ? O2 Yb2 N22 82.33(12) . . ? N10 Yb2 N22 141.42(13) . . ? N15 Yb2 N22 77.27(12) . . ? N4 Yb2 N22 102.14(13) . . ? O1 Yb2 N22 148.59(18) . . ? O3' Yb2 N22 64.39(17) . . ? O1' Yb2 N19 152.10(18) . 2_775 ? O3 Yb2 N19 127.1(2) . 2_775 ? O2 Yb2 N19 72.69(11) . 2_775 ? N10 Yb2 N19 81.44(13) . 2_775 ? N15 Yb2 N19 130.15(12) . 2_775 ? N4 Yb2 N19 71.71(12) . 2_775 ? O1 Yb2 N19 148.01(18) . 2_775 ? O3' Yb2 N19 102.99(17) . 2_775 ? N22 Yb2 N19 62.93(11) . 2_775 ? C13 Ru1 C14 90.06(18) . . ? C13 Ru1 C15 93.30(18) . . ? C14 Ru1 C15 87.79(18) . . ? C13 Ru1 C16 86.26(19) . . ? C14 Ru1 C16 94.63(18) . . ? C15 Ru1 C16 177.53(18) . . ? C13 Ru1 N2 93.72(16) . . ? C14 Ru1 N2 175.76(16) . . ? C15 Ru1 N2 90.08(16) . . ? C16 Ru1 N2 87.52(17) . . ? C13 Ru1 N1 171.23(16) . . ? C14 Ru1 N1 97.66(16) . . ? C15 Ru1 N1 91.18(16) . . ? C16 Ru1 N1 88.95(17) . . ? N2 Ru1 N1 78.72(14) . . ? C29 Ru2 C30 88.86(18) . . ? C29 Ru2 C32 87.4(2) . . ? C30 Ru2 C32 93.3(2) . . ? C29 Ru2 C31 87.80(19) . . ? C30 Ru2 C31 84.58(18) . . ? C32 Ru2 C31 174.74(19) . . ? C29 Ru2 N7 95.89(17) . . ? C30 Ru2 N7 174.30(16) . . ? C32 Ru2 N7 90.11(19) . . ? C31 Ru2 N7 92.42(17) . . ? C29 Ru2 N8 172.75(16) . . ? C30 Ru2 N8 97.41(17) . . ? C32 Ru2 N8 88.64(18) . . ? C31 Ru2 N8 96.40(17) . . ? N7 Ru2 N8 78.07(15) . . ? C46 Ru3 C45 91.30(19) . . ? C46 Ru3 C47 89.8(2) . . ? C45 Ru3 C47 92.81(19) . . ? C46 Ru3 C48 89.83(19) . . ? C45 Ru3 C48 89.20(18) . . ? C47 Ru3 C48 177.97(19) . . ? C46 Ru3 N14 94.24(17) . . ? C45 Ru3 N14 173.26(17) . . ? C47 Ru3 N14 91.04(17) . . ? C48 Ru3 N14 86.99(17) . . ? C46 Ru3 N13 172.13(17) . . ? C45 Ru3 N13 96.51(17) . . ? C47 Ru3 N13 88.84(17) . . ? C48 Ru3 N13 91.21(17) . . ? N14 Ru3 N13 78.03(15) . . ? N1 C1 C2 122.2(5) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.8(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.6(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C12 117.1(4) . . ? C3 C4 C5 123.9(5) . . ? C12 C4 C5 119.0(5) . . ? C6 C5 C4 121.1(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 121.7(5) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C11 118.0(5) . . ? C8 C7 C6 124.1(5) . . ? C11 C7 C6 117.8(5) . . ? C9 C8 C7 119.0(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N2 C10 C9 122.0(5) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? N2 C11 C7 122.7(4) . . ? N2 C11 C12 116.7(4) . . ? C7 C11 C12 120.6(4) . . ? N2 C11 H19B 26.2 . . ? C7 C11 H19B 139.5 . . ? C12 C11 H19B 96.4 . . ? N1 C12 C4 123.3(4) . . ? N1 C12 C11 117.1(4) . . ? C4 C12 C11 119.6(4) . . ? N3 C13 Ru1 171.8(4) . . ? N4 C14 Ru1 175.5(4) . . ? N5 C15 Ru1 177.4(4) . . ? N6 C16 Ru1 176.4(4) . . ? N7 C17 C18 123.2(5) . . ? N7 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 120.6(5) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C28 117.1(5) . . ? C19 C20 C21 124.6(5) . . ? C28 C20 C21 118.3(5) . . ? C22 C21 C20 121.4(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 121.8(5) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C24 C23 C27 117.5(5) . . ? C24 C23 C22 124.4(5) . . ? C27 C23 C22 118.1(5) . . ? C25 C24 C23 120.1(5) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 118.7(5) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? N8 C26 C25 122.9(5) . . ? N8 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? N8 C27 C23 122.5(5) . . ? N8 C27 C28 117.5(4) . . ? C23 C27 C28 120.0(4) . . ? N7 C28 C20 122.7(5) . . ? N7 C28 C27 116.9(4) . . ? C20 C28 C27 120.4(4) . . ? N9 C29 Ru2 177.1(4) . . ? N10 C30 Ru2 171.1(4) . . ? N11 C31 Ru2 171.6(4) . . ? N12 C32 Ru2 176.9(5) . . ? N13 C33 C34 123.0(5) . . ? N13 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C35 C34 C33 119.4(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 119.2(5) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C44 117.6(5) . . ? C35 C36 C37 124.3(5) . . ? C44 C36 C37 118.0(5) . . ? C38 C37 C36 121.9(5) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C39 121.0(5) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C40 C39 C43 116.8(5) . . ? C40 C39 C38 124.6(5) . . ? C43 C39 C38 118.6(5) . . ? C41 C40 C39 120.1(5) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 119.7(5) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? N14 C42 C41 122.8(5) . . ? N14 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? N14 C43 C39 122.6(5) . . ? N14 C43 C44 117.2(4) . . ? C39 C43 C44 120.2(5) . . ? N13 C44 C36 122.8(4) . . ? N13 C44 C43 116.9(4) . . ? C36 C44 C43 120.3(4) . . ? N15 C45 Ru3 177.9(4) . . ? N16 C46 Ru3 175.6(4) . . ? N17 C47 Ru3 176.5(5) . . ? N18 C48 Ru3 177.9(4) . . ? N21 C53 C54 121.6(4) . . ? N21 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C51 C54 C53 118.0(4) . . ? C51 C54 H54 121.0 . . ? C53 C54 H54 121.0 . . ? N22 C55 C56 121.2(5) . . ? N22 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C55 C56 C49 117.6(4) . . ? C55 C56 H56 121.2 . . ? C49 C56 H56 121.2 . . ? C1 N1 C12 117.9(4) . . ? C1 N1 Ru1 128.6(3) . . ? C12 N1 Ru1 113.5(3) . . ? C10 N2 C11 117.8(4) . . ? C10 N2 Ru1 128.2(3) . . ? C11 N2 Ru1 113.9(3) . . ? C10 N2 H19B 137.6 . . ? C11 N2 H19B 30.0 . . ? Ru1 N2 H19B 90.2 . . ? C13 N3 Yb1 155.8(3) . . ? C14 N4 Yb2 156.0(4) . . ? C17 N7 C28 117.4(4) . . ? C17 N7 Ru2 128.6(3) . . ? C28 N7 Ru2 114.0(3) . . ? C26 N8 C27 118.2(4) . . ? C26 N8 Ru2 128.2(3) . . ? C27 N8 Ru2 113.4(3) . . ? C29 N9 Yb1 153.0(4) . . ? C30 N10 Yb2 155.6(4) . . ? C33 N13 C44 117.8(4) . . ? C33 N13 Ru3 128.5(3) . . ? C44 N13 Ru3 113.6(3) . . ? C42 N14 C43 117.9(4) . . ? C42 N14 Ru3 128.5(3) . . ? C43 N14 Ru3 113.3(3) . . ? C45 N15 Yb2 174.5(4) . . ? C52 N21 C53 116.1(4) . . ? C52 N21 Yb1 121.2(3) . . ? C53 N21 Yb1 122.5(3) . . ? C50 N22 C55 116.7(4) . . ? C50 N22 Yb2 123.1(3) . . ? C55 N22 Yb2 120.2(3) . . ? N20 C51 C54 122.1(4) . . ? N20 C51 H51 118.9 . . ? C54 C51 H51 118.9 . . ? N21 C52 N20 126.4(4) . . ? N21 C52 C52 117.1(5) . 2_786 ? N20 C52 C52 116.5(5) . 2_786 ? C52 N20 C51 115.7(4) . . ? C52 N20 Yb1 120.8(3) . 2_786 ? C51 N20 Yb1 123.4(3) . 2_786 ? N19 C49 C56 122.4(4) . . ? N19 C49 H49 118.8 . . ? C56 C49 H49 118.8 . . ? N22 C50 N19 126.7(4) . . ? N22 C50 C50 117.0(5) . 2_775 ? N19 C50 C50 116.3(5) . 2_775 ? C50 N19 C49 115.5(4) . . ? C50 N19 Yb2 120.6(3) . 2_775 ? C49 N19 Yb2 123.9(3) . 2_775 ? Yb2 O2 H2B 129.0 . . ? Yb2 O2 H2C 118.3 . . ? H2B O2 H2C 98.5 . . ? Yb1 O4 H4B 116.0 . . ? Yb1 O4 H4C 115.5 . . ? H4B O4 H4C 98.1 . . ? Yb1 O6 H6B 109.8 . . ? Yb1 O6 H6C 122.0 . . ? H6B O6 H6C 108.9 . . ? Yb1 O7 H7B 122.7 . . ? Yb1 O7 H7C 123.6 . . ? H7B O7 H7C 110.5 . . ? H8B O8 H8C 124.3 . . ? H10B O10 H10C 101.7 . . ? H11B O11 H11C 124.2 . . ? H12B O12 H12C 95.2 . . ? H13B O13 H13C 112.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.645 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.132 #===END