# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Masahiro Mikuriya' _publ_contact_author_email junpei@kwansei.ac.jp _publ_section_title ; Molecule-based magnetic materials based on dinuclear ruthenium carboxylate and octacyanotungstate ; _publ_contact_author_address ; Department of Chemistry, School of Science and Technology, Kwansei Gakuin University, Gakuen, Sanda, Hyogo 669-1337, JAPAN ; _publ_contact_author_fax +81-47-565-9077 _publ_contact_author_phone +81-79-565-8366 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category FM _publ_requested_coeditor_name ? loop_ _publ_author_name M.Mikuriya D.Yoshioka A.Borta D.Luneau D.Matoga ; J.Szklarzewicz ; M.Handa # Attachment 'PPh4RUPIVWC.CIF' data_pph4rupivwc _database_code_depnum_ccdc_archive 'CCDC 799276' #TrackingRef 'PPh4RUPIVWC.CIF' _audit_creation_method SHELXL-97 #--------------------------------------------------------------------- _chemical_name_systematic ; (PPh4)2[Ru2(piv)4W(CN)8].0.5H2O ; _chemical_name_common (PPh4)2(Ru2(piv)4W(CN)8).0.5H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H77 N8 O8.50 P2 Ru2 W' _chemical_formula_weight 1686.39 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.779(11) _cell_length_b 25.28(2) _cell_length_c 20.913(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.576(16) _cell_angle_gamma 90.00 _cell_volume 7271(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(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 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3396 _exptl_absorpt_coefficient_mu 2.094 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3664 _exptl_absorpt_correction_T_max 0.5724 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'psi 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 44741 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.58 _reflns_number_total 16877 _reflns_number_gt 13093 _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 SHELXL' _computing_publication_material 'Bruker SHELXL' _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^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16877 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.005 _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 W1 W 0.831240(7) 0.240445(4) 0.643647(4) 0.02504(3) Uani 1 1 d . . . Ru1 Ru 1.000382(14) 0.292209(8) 0.426393(9) 0.02667(5) Uani 1 1 d . . . Ru2 Ru 1.071524(14) 0.276793(8) 0.332887(9) 0.02746(5) Uani 1 1 d . . . P1 P 0.66831(5) -0.01709(3) 0.41440(3) 0.03433(16) Uani 1 1 d . . . P2 P 1.34995(5) 0.43481(3) 0.56136(3) 0.03646(16) Uani 1 1 d . . . O1 O 0.87214(11) 0.30072(7) 0.37701(8) 0.0367(4) Uani 1 1 d . . . O2 O 0.93887(12) 0.28354(7) 0.28561(8) 0.0365(4) Uani 1 1 d . . . O3 O 0.97560(12) 0.21408(7) 0.43187(8) 0.0348(4) Uani 1 1 d . . . O4 O 1.04445(12) 0.19934(6) 0.34040(8) 0.0344(4) Uani 1 1 d . . . O5 O 1.12812(12) 0.28025(7) 0.47508(8) 0.0344(4) Uani 1 1 d . . . O6 O 1.19770(12) 0.26264(7) 0.38466(8) 0.0340(4) Uani 1 1 d . . . O7 O 1.02433(12) 0.37074(6) 0.41626(8) 0.0349(4) Uani 1 1 d . . . O8 O 1.09287(12) 0.35572(7) 0.32472(8) 0.0350(4) Uani 1 1 d . . . N21 N 0.91992(14) 0.29671(8) 0.51727(9) 0.0326(5) Uani 1 1 d . . . N22 N 0.8380(2) 0.12068(10) 0.70740(12) 0.0588(7) Uani 1 1 d . . . N23 N 0.77199(19) 0.15661(10) 0.52770(12) 0.0605(7) Uani 1 1 d . . . N24 N 0.63722(18) 0.29361(12) 0.56843(13) 0.0646(8) Uani 1 1 d . . . N25 N 0.65637(15) 0.23673(9) 0.74482(10) 0.0368(5) Uani 1 1 d . . . N26 N 0.84220(19) 0.36743(10) 0.68162(13) 0.0557(7) Uani 1 1 d . . . N27 N 0.9531(2) 0.25065(10) 0.78344(12) 0.0574(7) Uani 1 1 d . . . N28 N 1.05123(19) 0.19858(11) 0.62001(14) 0.0684(8) Uani 1 1 d . . . C1 C 0.86537(18) 0.29089(10) 0.31740(12) 0.0343(6) Uani 1 1 d . . . C2 C 0.76403(19) 0.28762(12) 0.28496(14) 0.0450(7) Uani 1 1 d . . . C3 C 0.7214(3) 0.34214(15) 0.2810(2) 0.1019(16) Uani 1 1 d . . . H3A H 0.7601 0.3641 0.2550 0.153 Uiso 1 1 calc R . . H3B H 0.7208 0.3569 0.3232 0.153 Uiso 1 1 calc R . . H3C H 0.6562 0.3404 0.2621 0.153 Uiso 1 1 calc R . . C4 C 0.7037(2) 0.25283(17) 0.3261(2) 0.0991(16) Uani 1 1 d . . . H4A H 0.6390 0.2498 0.3067 0.149 Uiso 1 1 calc R . . H4B H 0.7013 0.2683 0.3680 0.149 Uiso 1 1 calc R . . H4C H 0.7327 0.2183 0.3298 0.149 Uiso 1 1 calc R . . C5 C 0.7667(3) 0.26391(16) 0.21858(17) 0.0816(12) Uani 1 1 d . . . H5A H 0.8046 0.2861 0.1925 0.122 Uiso 1 1 calc R . . H5B H 0.7016 0.2612 0.1995 0.122 Uiso 1 1 calc R . . H5C H 0.7954 0.2293 0.2216 0.122 Uiso 1 1 calc R . . C6 C 1.00034(17) 0.18326(10) 0.38847(13) 0.0342(6) Uani 1 1 d . . . C7 C 0.9741(2) 0.12529(10) 0.39271(14) 0.0424(7) Uani 1 1 d . . . C8 C 0.8648(2) 0.12224(13) 0.37668(16) 0.0656(10) Uani 1 1 d . . . H8A H 0.8502 0.1355 0.3342 0.098 Uiso 1 1 calc R . . H8B H 0.8316 0.1432 0.4068 0.098 Uiso 1 1 calc R . . H8C H 0.8439 0.0861 0.3790 0.098 Uiso 1 1 calc R . . C9 C 1.0262(3) 0.09331(13) 0.3446(2) 0.0985(15) Uani 1 1 d . . . H9A H 1.0110 0.1071 0.3024 0.148 Uiso 1 1 calc R . . H9B H 1.0057 0.0571 0.3463 0.148 Uiso 1 1 calc R . . H9C H 1.0951 0.0954 0.3544 0.148 Uiso 1 1 calc R . . C10 C 0.9973(3) 0.10532(13) 0.46008(16) 0.0741(11) Uani 1 1 d . . . H10A H 0.9639 0.1266 0.4897 0.111 Uiso 1 1 calc R . . H10B H 1.0662 0.1075 0.4701 0.111 Uiso 1 1 calc R . . H10C H 0.9766 0.0692 0.4631 0.111 Uiso 1 1 calc R . . C11 C 1.19760(18) 0.26223(10) 0.44505(12) 0.0327(6) Uani 1 1 d . . . C12 C 1.28005(19) 0.23473(11) 0.48392(13) 0.0400(6) Uani 1 1 d . . . C13 C 1.2390(2) 0.18082(12) 0.50001(17) 0.0689(10) Uani 1 1 d . . . H13A H 1.1814 0.1854 0.5230 0.103 Uiso 1 1 calc R . . H13B H 1.2866 0.1614 0.5260 0.103 Uiso 1 1 calc R . . H13C H 1.2232 0.1616 0.4611 0.103 Uiso 1 1 calc R . . C14 C 1.3688(2) 0.22810(17) 0.44574(19) 0.0928(14) Uani 1 1 d . . . H14A H 1.3938 0.2623 0.4354 0.139 Uiso 1 1 calc R . . H14B H 1.3513 0.2091 0.4070 0.139 Uiso 1 1 calc R . . H14C H 1.4177 0.2087 0.4706 0.139 Uiso 1 1 calc R . . C15 C 1.3046(3) 0.26459(13) 0.54582(16) 0.0772(12) Uani 1 1 d . . . H15A H 1.3304 0.2987 0.5361 0.116 Uiso 1 1 calc R . . H15B H 1.3521 0.2450 0.5717 0.116 Uiso 1 1 calc R . . H15C H 1.2469 0.2689 0.5687 0.116 Uiso 1 1 calc R . . C16 C 1.05991(17) 0.38669(10) 0.36531(12) 0.0337(6) Uani 1 1 d . . . C17 C 1.0575(2) 0.44575(11) 0.35006(14) 0.0444(7) Uani 1 1 d . . . C18 C 1.1432(2) 0.46174(13) 0.31175(19) 0.0795(12) Uani 1 1 d . . . H18A H 1.1425 0.4412 0.2731 0.119 Uiso 1 1 calc R . . H18B H 1.2028 0.4555 0.3368 0.119 Uiso 1 1 calc R . . H18C H 1.1382 0.4986 0.3011 0.119 Uiso 1 1 calc R . . C19 C 1.0545(3) 0.47855(12) 0.41117(16) 0.0687(10) Uani 1 1 d . . . H19A H 1.0003 0.4675 0.4346 0.103 Uiso 1 1 calc R . . H19B H 1.0475 0.5153 0.4002 0.103 Uiso 1 1 calc R . . H19C H 1.1137 0.4734 0.4371 0.103 Uiso 1 1 calc R . . C20 C 0.9632(2) 0.45355(13) 0.30891(15) 0.0640(9) Uani 1 1 d . . . H20A H 0.9092 0.4423 0.3324 0.096 Uiso 1 1 calc R . . H20B H 0.9654 0.4330 0.2704 0.096 Uiso 1 1 calc R . . H20C H 0.9558 0.4903 0.2980 0.096 Uiso 1 1 calc R . . C21 C 0.88623(17) 0.27837(10) 0.56067(12) 0.0298(5) Uani 1 1 d . . . C22 C 0.8353(2) 0.16180(11) 0.68557(12) 0.0379(6) Uani 1 1 d . . . C23 C 0.79282(19) 0.18547(11) 0.56787(13) 0.0388(6) Uani 1 1 d . . . C24 C 0.7042(2) 0.27472(11) 0.59340(13) 0.0392(6) Uani 1 1 d . . . C25 C 0.71565(18) 0.23926(10) 0.70984(12) 0.0310(5) Uani 1 1 d . . . C26 C 0.83818(18) 0.32338(11) 0.66847(12) 0.0369(6) Uani 1 1 d . . . C27 C 0.91067(19) 0.24725(10) 0.73512(13) 0.0367(6) Uani 1 1 d . . . C28 C 0.9752(2) 0.21263(12) 0.62851(13) 0.0438(7) Uani 1 1 d . . . C31 C 0.58231(18) -0.06901(10) 0.40055(13) 0.0369(6) Uani 1 1 d . . . C32 C 0.6042(2) -0.11347(11) 0.36694(14) 0.0457(7) Uani 1 1 d . . . H32A H 0.6659 -0.1177 0.3520 0.055 Uiso 1 1 calc R . . C33 C 0.5345(2) -0.15199(12) 0.35536(16) 0.0603(9) Uani 1 1 d . . . H33A H 0.5493 -0.1822 0.3325 0.072 Uiso 1 1 calc R . . C34 C 0.4440(2) -0.14605(13) 0.37723(17) 0.0658(10) Uani 1 1 d . . . H34A H 0.3971 -0.1721 0.3694 0.079 Uiso 1 1 calc R . . C35 C 0.4227(2) -0.10191(14) 0.41045(18) 0.0750(11) Uani 1 1 d . . . H35A H 0.3610 -0.0978 0.4253 0.090 Uiso 1 1 calc R . . C36 C 0.4911(2) -0.06354(12) 0.42224(17) 0.0624(9) Uani 1 1 d . . . H36A H 0.4757 -0.0335 0.4452 0.075 Uiso 1 1 calc R . . C37 C 0.60931(18) 0.04308(10) 0.38998(13) 0.0365(6) Uani 1 1 d . . . C38 C 0.5456(2) 0.04242(12) 0.33611(14) 0.0512(8) Uani 1 1 d . . . H38A H 0.5321 0.0108 0.3145 0.061 Uiso 1 1 calc R . . C39 C 0.5022(2) 0.08862(15) 0.31472(17) 0.0655(10) Uani 1 1 d . . . H39A H 0.4596 0.0881 0.2784 0.079 Uiso 1 1 calc R . . C40 C 0.5206(3) 0.13462(15) 0.3457(2) 0.0737(11) Uani 1 1 d . . . H40A H 0.4910 0.1656 0.3305 0.088 Uiso 1 1 calc R . . C41 C 0.5824(2) 0.13585(13) 0.39936(19) 0.0678(10) Uani 1 1 d . . . H41A H 0.5943 0.1676 0.4209 0.081 Uiso 1 1 calc R . . C42 C 0.6272(2) 0.09022(11) 0.42161(15) 0.0493(8) Uani 1 1 d . . . H42A H 0.6695 0.0912 0.4580 0.059 Uiso 1 1 calc R . . C43 C 0.71021(19) -0.01450(10) 0.49716(13) 0.0385(6) Uani 1 1 d . . . C44 C 0.7813(2) 0.02234(12) 0.51570(15) 0.0556(8) Uani 1 1 d . . . H44A H 0.8089 0.0432 0.4850 0.067 Uiso 1 1 calc R . . C45 C 0.8107(3) 0.02795(15) 0.57915(17) 0.0715(11) Uani 1 1 d . . . H45A H 0.8567 0.0535 0.5917 0.086 Uiso 1 1 calc R . . C46 C 0.7730(3) -0.00365(18) 0.62348(17) 0.0795(12) Uani 1 1 d . . . H46A H 0.7931 0.0004 0.6665 0.095 Uiso 1 1 calc R . . C47 C 0.7059(3) -0.04126(16) 0.60592(16) 0.0726(11) Uani 1 1 d . . . H47A H 0.6822 -0.0634 0.6368 0.087 Uiso 1 1 calc R . . C48 C 0.6727(2) -0.04681(12) 0.54237(15) 0.0517(8) Uani 1 1 d . . . H48A H 0.6258 -0.0720 0.5305 0.062 Uiso 1 1 calc R . . C49 C 0.77065(18) -0.02851(10) 0.36806(13) 0.0348(6) Uani 1 1 d . . . C50 C 0.7752(2) -0.00836(12) 0.30734(14) 0.0483(7) Uani 1 1 d . . . H50A H 0.7256 0.0132 0.2901 0.058 Uiso 1 1 calc R . . C51 C 0.8528(2) -0.02017(14) 0.27252(16) 0.0631(9) Uani 1 1 d . . . H51A H 0.8561 -0.0061 0.2316 0.076 Uiso 1 1 calc R . . C52 C 0.9260(2) -0.05242(13) 0.29692(18) 0.0618(9) Uani 1 1 d . . . H52A H 0.9784 -0.0603 0.2726 0.074 Uiso 1 1 calc R . . C53 C 0.9216(2) -0.07269(12) 0.35637(18) 0.0605(9) Uani 1 1 d . . . H53A H 0.9711 -0.0946 0.3730 0.073 Uiso 1 1 calc R . . C54 C 0.8448(2) -0.06116(12) 0.39241(15) 0.0527(8) Uani 1 1 d . . . H54A H 0.8423 -0.0753 0.4333 0.063 Uiso 1 1 calc R . . C61 C 1.25557(19) 0.40342(10) 0.60277(13) 0.0386(6) Uani 1 1 d . . . C62 C 1.2644(2) 0.39654(13) 0.66803(15) 0.0572(9) Uani 1 1 d . . . H62A H 1.3226 0.4051 0.6906 0.069 Uiso 1 1 calc R . . C63 C 1.1886(2) 0.37718(14) 0.70021(17) 0.0706(10) Uani 1 1 d . . . H63A H 1.1948 0.3738 0.7446 0.085 Uiso 1 1 calc R . . C64 C 1.1048(3) 0.36302(14) 0.66776(19) 0.0712(10) Uani 1 1 d . . . H64A H 1.0547 0.3480 0.6894 0.085 Uiso 1 1 calc R . . C65 C 1.0938(3) 0.37069(18) 0.6035(2) 0.0940(15) Uani 1 1 d . . . H65A H 1.0351 0.3624 0.5815 0.113 Uiso 1 1 calc R . . C66 C 1.1692(2) 0.39072(16) 0.57092(17) 0.0786(12) Uani 1 1 d . . . H66A H 1.1614 0.3956 0.5268 0.094 Uiso 1 1 calc R . . C67 C 1.30547(18) 0.49855(11) 0.53784(13) 0.0380(6) Uani 1 1 d . . . C68 C 1.2503(2) 0.52724(12) 0.57848(15) 0.0582(9) Uani 1 1 d . . . H68A H 1.2365 0.5133 0.6181 0.070 Uiso 1 1 calc R . . C69 C 1.2157(2) 0.57655(13) 0.56039(18) 0.0717(11) Uani 1 1 d . . . H69A H 1.1798 0.5961 0.5883 0.086 Uiso 1 1 calc R . . C70 C 1.2336(2) 0.59688(13) 0.50217(18) 0.0641(10) Uani 1 1 d . . . H70A H 1.2093 0.6299 0.4900 0.077 Uiso 1 1 calc R . . C71 C 1.2871(2) 0.56867(13) 0.46184(17) 0.0633(9) Uani 1 1 d . . . H71A H 1.2995 0.5825 0.4220 0.076 Uiso 1 1 calc R . . C72 C 1.3231(2) 0.51998(12) 0.47938(15) 0.0516(8) Uani 1 1 d . . . H72A H 1.3599 0.5012 0.4513 0.062 Uiso 1 1 calc R . . C73 C 1.45509(19) 0.43952(12) 0.61596(13) 0.0416(7) Uani 1 1 d . . . C74 C 1.4989(2) 0.39338(13) 0.63873(14) 0.0535(8) Uani 1 1 d . . . H74A H 1.4728 0.3608 0.6263 0.064 Uiso 1 1 calc R . . C75 C 1.5809(2) 0.39545(16) 0.67964(16) 0.0646(10) Uani 1 1 d . . . H75A H 1.6104 0.3645 0.6950 0.078 Uiso 1 1 calc R . . C76 C 1.6185(2) 0.44348(18) 0.69738(16) 0.0692(10) Uani 1 1 d . . . H76A H 1.6746 0.4448 0.7245 0.083 Uiso 1 1 calc R . . C77 C 1.5763(2) 0.48943(15) 0.67659(15) 0.0630(10) Uani 1 1 d . . . H77A H 1.6023 0.5217 0.6904 0.076 Uiso 1 1 calc R . . C78 C 1.4937(2) 0.48794(12) 0.63451(13) 0.0459(7) Uani 1 1 d . . . H78A H 1.4651 0.5191 0.6192 0.055 Uiso 1 1 calc R . . C79 C 1.38300(19) 0.40099(10) 0.49048(13) 0.0386(6) Uani 1 1 d . . . C80 C 1.3147(2) 0.39332(12) 0.43914(14) 0.0487(7) Uani 1 1 d . . . H80A H 1.2504 0.4033 0.4430 0.058 Uiso 1 1 calc R . . C81 C 1.3414(2) 0.37131(12) 0.38335(15) 0.0555(8) Uani 1 1 d . . . H81A H 1.2950 0.3661 0.3497 0.067 Uiso 1 1 calc R . . C82 C 1.4353(3) 0.35693(13) 0.37653(16) 0.0627(9) Uani 1 1 d . . . H82A H 1.4540 0.3430 0.3380 0.075 Uiso 1 1 calc R . . C83 C 1.5020(2) 0.36342(14) 0.42735(17) 0.0682(10) Uani 1 1 d . . . H83A H 1.5658 0.3525 0.4234 0.082 Uiso 1 1 calc R . . C84 C 1.4770(2) 0.38558(12) 0.48391(15) 0.0542(8) Uani 1 1 d . . . H84A H 1.5237 0.3901 0.5176 0.065 Uiso 1 1 calc R . . O9 O 0.7454(3) -0.1471(2) 0.6906(2) 0.0839(16) Uani 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 W1 0.02441(5) 0.02910(5) 0.02218(5) -0.00032(4) 0.00606(4) -0.00256(4) Ru1 0.02729(10) 0.03073(11) 0.02277(10) 0.00275(8) 0.00781(8) 0.00211(8) Ru2 0.02515(10) 0.03537(12) 0.02258(10) 0.00279(8) 0.00726(8) 0.00157(8) P1 0.0351(4) 0.0307(4) 0.0374(4) -0.0014(3) 0.0039(3) -0.0023(3) P2 0.0339(4) 0.0375(4) 0.0383(4) -0.0042(3) 0.0042(3) 0.0013(3) O1 0.0258(9) 0.0528(12) 0.0321(10) 0.0025(9) 0.0059(8) 0.0051(8) O2 0.0286(9) 0.0541(12) 0.0268(9) 0.0034(8) 0.0022(8) 0.0018(8) O3 0.0412(10) 0.0325(10) 0.0323(10) 0.0000(8) 0.0138(8) -0.0006(8) O4 0.0409(10) 0.0331(10) 0.0305(9) -0.0019(8) 0.0125(8) 0.0017(8) O5 0.0325(10) 0.0433(11) 0.0276(9) 0.0005(8) 0.0017(8) 0.0046(8) O6 0.0286(9) 0.0456(11) 0.0282(9) 0.0025(8) 0.0054(7) 0.0031(8) O7 0.0405(10) 0.0322(10) 0.0330(10) 0.0037(8) 0.0092(8) 0.0013(8) O8 0.0357(10) 0.0347(10) 0.0356(10) 0.0069(8) 0.0108(8) 0.0004(8) N21 0.0326(12) 0.0389(13) 0.0276(11) 0.0020(10) 0.0113(9) 0.0032(10) N22 0.081(2) 0.0407(15) 0.0553(17) 0.0053(13) 0.0102(15) -0.0027(14) N23 0.0707(19) 0.0615(18) 0.0505(16) -0.0212(14) 0.0134(14) -0.0245(14) N24 0.0437(16) 0.088(2) 0.0607(18) 0.0073(16) -0.0060(14) 0.0152(15) N25 0.0339(12) 0.0478(14) 0.0298(11) -0.0035(10) 0.0101(10) -0.0045(10) N26 0.0661(18) 0.0362(15) 0.0638(18) -0.0059(13) -0.0050(14) 0.0003(13) N27 0.0694(18) 0.0527(17) 0.0471(16) 0.0012(13) -0.0197(14) -0.0032(13) N28 0.0448(16) 0.079(2) 0.083(2) 0.0194(17) 0.0192(15) 0.0234(15) C1 0.0307(14) 0.0367(15) 0.0358(15) 0.0076(12) 0.0047(12) 0.0004(11) C2 0.0291(15) 0.0569(19) 0.0484(18) 0.0080(15) -0.0036(13) 0.0007(13) C3 0.081(3) 0.084(3) 0.134(4) -0.009(3) -0.049(3) 0.032(2) C4 0.044(2) 0.156(4) 0.096(3) 0.041(3) -0.007(2) -0.037(2) C5 0.054(2) 0.117(3) 0.071(3) -0.017(2) -0.016(2) -0.010(2) C6 0.0263(13) 0.0356(15) 0.0407(16) 0.0025(12) 0.0031(12) 0.0015(11) C7 0.0441(17) 0.0322(15) 0.0522(18) -0.0020(13) 0.0129(14) -0.0044(13) C8 0.061(2) 0.061(2) 0.074(2) 0.0001(18) -0.0039(19) -0.0194(17) C9 0.122(3) 0.043(2) 0.140(4) -0.023(2) 0.078(3) -0.008(2) C10 0.085(3) 0.051(2) 0.084(3) 0.0271(19) -0.019(2) -0.0175(19) C11 0.0321(14) 0.0309(14) 0.0349(14) 0.0032(12) 0.0009(12) -0.0032(11) C12 0.0353(15) 0.0458(17) 0.0384(15) 0.0082(13) -0.0023(12) 0.0065(13) C13 0.066(2) 0.047(2) 0.092(3) 0.0149(19) -0.010(2) 0.0093(17) C14 0.043(2) 0.150(4) 0.087(3) 0.051(3) 0.014(2) 0.037(2) C15 0.093(3) 0.068(2) 0.065(2) -0.0022(19) -0.042(2) 0.017(2) C16 0.0273(13) 0.0380(15) 0.0356(15) 0.0062(12) 0.0018(12) 0.0001(11) C17 0.0460(17) 0.0352(16) 0.0520(18) 0.0102(14) 0.0030(14) 0.0014(13) C18 0.071(2) 0.052(2) 0.119(3) 0.035(2) 0.033(2) -0.0034(18) C19 0.089(3) 0.0363(18) 0.079(3) 0.0002(17) -0.007(2) 0.0025(18) C20 0.067(2) 0.057(2) 0.066(2) 0.0218(17) -0.0043(18) 0.0128(17) C21 0.0261(13) 0.0330(14) 0.0309(14) -0.0010(11) 0.0056(11) 0.0027(11) C22 0.0471(17) 0.0332(16) 0.0345(15) -0.0020(12) 0.0099(13) -0.0033(13) C23 0.0366(15) 0.0427(17) 0.0380(15) -0.0027(13) 0.0092(12) -0.0087(13) C24 0.0359(15) 0.0476(17) 0.0348(15) 0.0008(13) 0.0083(12) -0.0020(13) C25 0.0310(13) 0.0331(14) 0.0290(13) -0.0017(11) 0.0031(11) -0.0080(11) C26 0.0343(15) 0.0445(18) 0.0323(14) 0.0021(13) 0.0039(12) 0.0017(12) C27 0.0406(16) 0.0307(15) 0.0381(15) -0.0003(12) -0.0022(13) -0.0006(11) C28 0.0387(17) 0.0531(19) 0.0405(16) 0.0097(14) 0.0103(13) 0.0052(14) C31 0.0359(15) 0.0318(15) 0.0433(16) -0.0051(12) 0.0045(13) -0.0040(11) C32 0.0410(16) 0.0424(17) 0.0544(19) -0.0104(14) 0.0090(14) -0.0028(13) C33 0.064(2) 0.049(2) 0.068(2) -0.0274(17) 0.0093(18) -0.0111(16) C34 0.055(2) 0.063(2) 0.080(3) -0.0230(19) 0.0117(19) -0.0271(17) C35 0.046(2) 0.073(3) 0.109(3) -0.028(2) 0.032(2) -0.0196(18) C36 0.0508(19) 0.0465(19) 0.093(3) -0.0269(18) 0.0289(18) -0.0129(15) C37 0.0341(14) 0.0343(15) 0.0414(16) 0.0028(12) 0.0056(12) 0.0008(12) C38 0.0551(19) 0.054(2) 0.0443(18) -0.0008(15) 0.0010(15) 0.0081(15) C39 0.057(2) 0.079(3) 0.061(2) 0.026(2) 0.0065(18) 0.0177(19) C40 0.064(2) 0.057(2) 0.104(3) 0.039(2) 0.031(2) 0.0219(19) C41 0.067(2) 0.0323(18) 0.107(3) 0.0000(19) 0.027(2) 0.0023(16) C42 0.0464(18) 0.0381(17) 0.064(2) -0.0055(15) 0.0078(15) -0.0041(14) C43 0.0405(16) 0.0377(16) 0.0371(15) 0.0019(12) 0.0023(13) 0.0030(12) C44 0.057(2) 0.058(2) 0.0501(19) 0.0046(16) -0.0072(16) -0.0073(16) C45 0.077(3) 0.079(3) 0.055(2) -0.006(2) -0.022(2) -0.003(2) C46 0.085(3) 0.107(3) 0.044(2) 0.000(2) -0.012(2) 0.026(3) C47 0.081(3) 0.091(3) 0.047(2) 0.026(2) 0.0157(19) 0.020(2) C48 0.0520(19) 0.0510(19) 0.0532(19) 0.0097(15) 0.0119(16) 0.0066(15) C49 0.0330(14) 0.0301(14) 0.0415(16) -0.0022(12) 0.0042(12) -0.0030(11) C50 0.0469(18) 0.0522(19) 0.0460(18) 0.0031(14) 0.0059(15) 0.0060(14) C51 0.068(2) 0.077(3) 0.0470(19) 0.0005(17) 0.0222(18) -0.0025(19) C52 0.049(2) 0.058(2) 0.081(3) -0.0144(19) 0.0276(18) -0.0015(17) C53 0.0424(18) 0.047(2) 0.093(3) 0.0068(18) 0.0126(19) 0.0079(15) C54 0.0448(18) 0.0515(19) 0.062(2) 0.0156(16) 0.0077(16) 0.0033(15) C61 0.0362(15) 0.0355(15) 0.0446(17) -0.0060(13) 0.0066(13) -0.0021(12) C62 0.0418(18) 0.074(2) 0.055(2) 0.0153(17) 0.0036(16) -0.0050(16) C63 0.059(2) 0.090(3) 0.064(2) 0.022(2) 0.0140(19) -0.009(2) C64 0.061(2) 0.072(2) 0.084(3) -0.007(2) 0.027(2) -0.0213(19) C65 0.060(2) 0.142(4) 0.081(3) -0.041(3) 0.015(2) -0.052(3) C66 0.063(2) 0.125(3) 0.049(2) -0.022(2) 0.0092(18) -0.034(2) C67 0.0326(15) 0.0385(16) 0.0428(16) -0.0041(13) 0.0024(12) 0.0010(12) C68 0.073(2) 0.053(2) 0.0513(19) 0.0055(16) 0.0218(17) 0.0188(17) C69 0.075(2) 0.056(2) 0.088(3) 0.003(2) 0.033(2) 0.0273(19) C70 0.057(2) 0.048(2) 0.088(3) 0.0208(19) 0.013(2) 0.0123(16) C71 0.068(2) 0.056(2) 0.068(2) 0.0222(18) 0.0204(19) 0.0053(18) C72 0.0532(19) 0.0490(19) 0.0552(19) 0.0049(15) 0.0235(16) 0.0034(15) C73 0.0327(15) 0.0530(19) 0.0398(16) -0.0043(14) 0.0075(12) 0.0008(13) C74 0.0434(18) 0.065(2) 0.0524(19) -0.0001(16) 0.0024(15) 0.0056(16) C75 0.051(2) 0.091(3) 0.052(2) 0.0041(19) 0.0016(17) 0.0153(19) C76 0.045(2) 0.119(3) 0.043(2) -0.004(2) 0.0002(16) 0.004(2) C77 0.050(2) 0.091(3) 0.050(2) -0.0211(19) 0.0129(17) -0.0244(19) C78 0.0407(17) 0.060(2) 0.0384(16) -0.0066(14) 0.0106(14) -0.0059(14) C79 0.0401(16) 0.0366(15) 0.0395(15) -0.0050(12) 0.0063(13) 0.0017(12) C80 0.0434(17) 0.057(2) 0.0457(18) -0.0048(15) 0.0010(14) 0.0082(14) C81 0.059(2) 0.058(2) 0.0489(19) -0.0123(16) -0.0018(16) -0.0009(17) C82 0.072(2) 0.059(2) 0.058(2) -0.0258(17) 0.0203(19) -0.0047(18) C83 0.047(2) 0.084(3) 0.075(2) -0.032(2) 0.0132(18) 0.0059(18) C84 0.0426(18) 0.064(2) 0.056(2) -0.0215(16) 0.0047(15) 0.0014(15) O9 0.084(4) 0.085(4) 0.085(4) 0.037(3) 0.019(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C28 2.147(3) . ? W1 C23 2.149(3) . ? W1 C27 2.151(3) . ? W1 C26 2.161(3) . ? W1 C21 2.161(3) . ? W1 C24 2.166(3) . ? W1 C22 2.172(3) . ? W1 C25 2.175(3) . ? Ru1 O5 2.001(2) . ? Ru1 O1 2.002(2) . ? Ru1 O3 2.009(2) . ? Ru1 O7 2.026(2) . ? Ru1 N21 2.262(2) . ? Ru1 Ru2 2.2751(15) . ? Ru2 O4 2.001(2) . ? Ru2 O6 2.022(2) . ? Ru2 O8 2.026(2) . ? Ru2 O2 2.030(2) . ? Ru2 N25 2.268(3) 4_665 ? P1 C31 1.780(3) . ? P1 C49 1.784(3) . ? P1 C37 1.784(3) . ? P1 C43 1.791(3) . ? P2 C67 1.782(3) . ? P2 C73 1.792(3) . ? P2 C61 1.792(3) . ? P2 C79 1.794(3) . ? O1 C1 1.269(3) . ? O2 C1 1.259(3) . ? O3 C6 1.259(3) . ? O4 C6 1.273(3) . ? O5 C11 1.262(3) . ? O6 C11 1.263(3) . ? O7 C16 1.266(3) . ? O8 C16 1.260(3) . ? N21 C21 1.143(3) . ? N22 C22 1.135(3) . ? N23 C23 1.136(3) . ? N24 C24 1.137(3) . ? N25 C25 1.132(3) . ? N25 Ru2 2.268(3) 4_566 ? N26 C26 1.147(3) . ? N27 C27 1.139(3) . ? N28 C28 1.131(3) . ? C1 C2 1.516(4) . ? C2 C3 1.498(4) . ? C2 C5 1.515(4) . ? C2 C4 1.515(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.513(4) . ? C7 C9 1.507(4) . ? C7 C10 1.512(4) . ? C7 C8 1.525(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.523(4) . ? C12 C14 1.511(4) . ? C12 C15 1.518(4) . ? C12 C13 1.521(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.527(4) . ? C17 C18 1.521(4) . ? C17 C20 1.526(4) . ? C17 C19 1.526(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C31 C36 1.369(4) . ? C31 C32 1.369(4) . ? C32 C33 1.378(4) . ? C32 H32A 0.9300 . ? C33 C34 1.363(4) . ? C33 H33A 0.9300 . ? C34 C35 1.356(4) . ? C34 H34A 0.9300 . ? C35 C36 1.364(4) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C42 1.378(4) . ? C37 C38 1.385(4) . ? C38 C39 1.374(4) . ? C38 H38A 0.9300 . ? C39 C40 1.347(5) . ? C39 H39A 0.9300 . ? C40 C41 1.367(5) . ? C40 H40A 0.9300 . ? C41 C42 1.375(4) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C48 1.374(4) . ? C43 C44 1.389(4) . ? C44 C45 1.371(4) . ? C44 H44A 0.9300 . ? C45 C46 1.352(5) . ? C45 H45A 0.9300 . ? C46 C47 1.360(5) . ? C46 H46A 0.9300 . ? C47 C48 1.386(4) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C50 1.373(4) . ? C49 C54 1.385(4) . ? C50 C51 1.364(4) . ? C50 H50A 0.9300 . ? C51 C52 1.370(4) . ? C51 H51A 0.9300 . ? C52 C53 1.349(5) . ? C52 H52A 0.9300 . ? C53 C54 1.368(4) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C61 C66 1.365(4) . ? C61 C62 1.374(4) . ? C62 C63 1.368(4) . ? C62 H62A 0.9300 . ? C63 C64 1.350(4) . ? C63 H63A 0.9300 . ? C64 C65 1.357(5) . ? C64 H64A 0.9300 . ? C65 C66 1.374(5) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C67 C72 1.373(4) . ? C67 C68 1.381(4) . ? C68 C69 1.379(4) . ? C68 H68A 0.9300 . ? C69 C70 1.358(5) . ? C69 H69A 0.9300 . ? C70 C71 1.357(4) . ? C70 H70A 0.9300 . ? C71 C72 1.368(4) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C73 C78 1.381(4) . ? C73 C74 1.384(4) . ? C74 C75 1.375(4) . ? C74 H74A 0.9300 . ? C75 C76 1.362(5) . ? C75 H75A 0.9300 . ? C76 C77 1.359(5) . ? C76 H76A 0.9300 . ? C77 C78 1.395(4) . ? C77 H77A 0.9300 . ? C78 H78A 0.9300 . ? C79 C84 1.368(4) . ? C79 C80 1.396(4) . ? C80 C81 1.363(4) . ? C80 H80A 0.9300 . ? C81 C82 1.361(4) . ? C81 H81A 0.9300 . ? C82 C83 1.370(4) . ? C82 H82A 0.9300 . ? C83 C84 1.372(4) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? 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 C28 W1 C23 82.35(11) . . ? C28 W1 C27 74.55(11) . . ? C23 W1 C27 142.74(10) . . ? C28 W1 C26 109.02(11) . . ? C23 W1 C26 144.09(10) . . ? C27 W1 C26 72.32(9) . . ? C28 W1 C21 69.72(10) . . ? C23 W1 C21 77.13(11) . . ? C27 W1 C21 119.63(11) . . ? C26 W1 C21 75.52(10) . . ? C28 W1 C24 141.82(11) . . ? C23 W1 C24 75.31(11) . . ? C27 W1 C24 138.65(10) . . ? C26 W1 C24 75.57(10) . . ? C21 W1 C24 75.30(10) . . ? C28 W1 C22 76.06(11) . . ? C23 W1 C22 72.82(11) . . ? C27 W1 C22 73.46(10) . . ? C26 W1 C22 142.33(11) . . ? C21 W1 C22 136.79(9) . . ? C24 W1 C22 124.16(10) . . ? C28 W1 C25 144.06(10) . . ? C23 W1 C25 107.70(10) . . ? C27 W1 C25 77.71(11) . . ? C26 W1 C25 83.31(9) . . ? C21 W1 C25 145.57(9) . . ? C24 W1 C25 73.28(11) . . ? C22 W1 C25 74.44(10) . . ? O5 Ru1 O1 177.46(7) . . ? O5 Ru1 O3 88.26(7) . . ? O1 Ru1 O3 89.28(7) . . ? O5 Ru1 O7 93.29(7) . . ? O1 Ru1 O7 89.14(7) . . ? O3 Ru1 O7 177.26(7) . . ? O5 Ru1 N21 92.39(9) . . ? O1 Ru1 N21 87.99(9) . . ? O3 Ru1 N21 84.70(7) . . ? O7 Ru1 N21 97.48(7) . . ? O5 Ru1 Ru2 89.95(7) . . ? O1 Ru1 Ru2 89.35(7) . . ? O3 Ru1 Ru2 87.96(5) . . ? O7 Ru1 Ru2 89.79(5) . . ? N21 Ru1 Ru2 172.23(5) . . ? O4 Ru2 O6 86.74(7) . . ? O4 Ru2 O8 177.61(7) . . ? O6 Ru2 O8 95.45(7) . . ? O4 Ru2 O2 87.35(7) . . ? O6 Ru2 O2 173.49(7) . . ? O8 Ru2 O2 90.42(7) . . ? O4 Ru2 N25 91.39(7) . 4_665 ? O6 Ru2 N25 86.48(9) . 4_665 ? O8 Ru2 N25 89.72(7) . 4_665 ? O2 Ru2 N25 96.39(9) . 4_665 ? O4 Ru2 Ru1 90.44(5) . . ? O6 Ru2 Ru1 88.41(7) . . ? O8 Ru2 Ru1 88.64(5) . . ? O2 Ru2 Ru1 88.92(7) . . ? N25 Ru2 Ru1 174.46(5) 4_665 . ? C31 P1 C49 109.45(13) . . ? C31 P1 C37 107.17(14) . . ? C49 P1 C37 110.12(13) . . ? C31 P1 C43 110.82(13) . . ? C49 P1 C43 108.23(14) . . ? C37 P1 C43 111.05(13) . . ? C67 P2 C73 111.49(13) . . ? C67 P2 C61 106.64(13) . . ? C73 P2 C61 107.67(14) . . ? C67 P2 C79 107.67(13) . . ? C73 P2 C79 108.75(14) . . ? C61 P2 C79 114.67(13) . . ? C1 O1 Ru1 119.62(16) . . ? C1 O2 Ru2 118.98(17) . . ? C6 O3 Ru1 120.84(17) . . ? C6 O4 Ru2 118.34(16) . . ? C11 O5 Ru1 118.15(17) . . ? C11 O6 Ru2 118.84(16) . . ? C16 O7 Ru1 118.30(16) . . ? C16 O8 Ru2 119.67(17) . . ? C21 N21 Ru1 153.0(2) . . ? C25 N25 Ru2 164.3(2) . 4_566 ? O2 C1 O1 122.4(2) . . ? O2 C1 C2 120.3(2) . . ? O1 C1 C2 117.4(2) . . ? C3 C2 C5 110.2(3) . . ? C3 C2 C4 109.8(3) . . ? C5 C2 C4 109.7(3) . . ? C3 C2 C1 108.7(3) . . ? C5 C2 C1 111.0(2) . . ? C4 C2 C1 107.4(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 122.4(2) . . ? O3 C6 C7 118.7(2) . . ? O4 C6 C7 118.9(2) . . ? C9 C7 C10 111.2(3) . . ? C9 C7 C6 110.8(2) . . ? C10 C7 C6 109.9(2) . . ? C9 C7 C8 109.3(3) . . ? C10 C7 C8 109.7(3) . . ? C6 C7 C8 105.8(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 122.9(2) . . ? O5 C11 C12 117.6(2) . . ? O6 C11 C12 119.3(2) . . ? C14 C12 C15 111.2(3) . . ? C14 C12 C13 110.0(3) . . ? C15 C12 C13 108.8(3) . . ? C14 C12 C11 111.7(2) . . ? C15 C12 C11 110.3(2) . . ? C13 C12 C11 104.6(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 122.9(2) . . ? O8 C16 C17 118.1(2) . . ? O7 C16 C17 118.9(2) . . ? C18 C17 C20 109.2(3) . . ? C18 C17 C19 111.1(3) . . ? C20 C17 C19 109.6(3) . . ? C18 C17 C16 111.3(2) . . ? C20 C17 C16 104.5(2) . . ? C19 C17 C16 111.0(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N21 C21 W1 176.1(2) . . ? N22 C22 W1 179.5(3) . . ? N23 C23 W1 179.5(3) . . ? N24 C24 W1 178.1(3) . . ? N25 C25 W1 177.4(2) . . ? N26 C26 W1 179.8(3) . . ? N27 C27 W1 179.6(3) . . ? N28 C28 W1 179.0(3) . . ? C36 C31 C32 119.3(3) . . ? C36 C31 P1 119.1(2) . . ? C32 C31 P1 121.5(2) . . ? C31 C32 C33 119.8(3) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 120.6(3) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C31 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C42 C37 C38 119.1(3) . . ? C42 C37 P1 122.4(2) . . ? C38 C37 P1 118.5(2) . . ? C39 C38 C37 119.7(3) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C40 C39 C38 120.8(3) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C39 C40 C41 120.2(3) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C41 C42 C37 120.0(3) . . ? C41 C42 H42A 120.0 . . ? C37 C42 H42A 120.0 . . ? C48 C43 C44 119.7(3) . . ? C48 C43 P1 122.1(2) . . ? C44 C43 P1 118.2(2) . . ? C45 C44 C43 120.1(3) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 119.9(4) . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C47 120.8(3) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C47 C48 120.5(3) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C43 C48 C47 118.9(3) . . ? C43 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C54 119.1(3) . . ? C50 C49 P1 121.7(2) . . ? C54 C49 P1 119.1(2) . . ? C51 C50 C49 119.6(3) . . ? C51 C50 H50A 120.2 . . ? C49 C50 H50A 120.2 . . ? C50 C51 C52 121.0(3) . . ? C50 C51 H51A 119.5 . . ? C52 C51 H51A 119.5 . . ? C53 C52 C51 119.7(3) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? C52 C53 C54 120.5(3) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C53 C54 C49 120.1(3) . . ? C53 C54 H54A 119.9 . . ? C49 C54 H54A 119.9 . . ? C66 C61 C62 118.4(3) . . ? C66 C61 P2 120.3(2) . . ? C62 C61 P2 120.9(2) . . ? C63 C62 C61 120.7(3) . . ? C63 C62 H62A 119.6 . . ? C61 C62 H62A 119.6 . . ? C64 C63 C62 120.2(3) . . ? C64 C63 H63A 119.9 . . ? C62 C63 H63A 119.9 . . ? C63 C64 C65 119.9(3) . . ? C63 C64 H64A 120.0 . . ? C65 C64 H64A 120.0 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65A 119.9 . . ? C66 C65 H65A 119.9 . . ? C61 C66 C65 120.5(3) . . ? C61 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C72 C67 C68 118.4(3) . . ? C72 C67 P2 121.7(2) . . ? C68 C67 P2 119.9(2) . . ? C69 C68 C67 120.0(3) . . ? C69 C68 H68A 120.0 . . ? C67 C68 H68A 120.0 . . ? C70 C69 C68 120.6(3) . . ? C70 C69 H69A 119.7 . . ? C68 C69 H69A 119.7 . . ? C71 C70 C69 119.6(3) . . ? C71 C70 H70A 120.2 . . ? C69 C70 H70A 120.2 . . ? C70 C71 C72 120.5(3) . . ? C70 C71 H71A 119.7 . . ? C72 C71 H71A 119.7 . . ? C71 C72 C67 120.9(3) . . ? C71 C72 H72A 119.6 . . ? C67 C72 H72A 119.6 . . ? C78 C73 C74 119.9(3) . . ? C78 C73 P2 121.3(2) . . ? C74 C73 P2 118.8(2) . . ? C75 C74 C73 120.4(3) . . ? C75 C74 H74A 119.8 . . ? C73 C74 H74A 119.8 . . ? C76 C75 C74 119.1(3) . . ? C76 C75 H75A 120.4 . . ? C74 C75 H75A 120.4 . . ? C77 C76 C75 121.8(3) . . ? C77 C76 H76A 119.1 . . ? C75 C76 H76A 119.1 . . ? C76 C77 C78 119.7(3) . . ? C76 C77 H77A 120.2 . . ? C78 C77 H77A 120.2 . . ? C73 C78 C77 119.1(3) . . ? C73 C78 H78A 120.5 . . ? C77 C78 H78A 120.5 . . ? C84 C79 C80 118.7(3) . . ? C84 C79 P2 120.6(2) . . ? C80 C79 P2 120.5(2) . . ? C81 C80 C79 120.7(3) . . ? C81 C80 H80A 119.7 . . ? C79 C80 H80A 119.7 . . ? C82 C81 C80 120.5(3) . . ? C82 C81 H81A 119.8 . . ? C80 C81 H81A 119.8 . . ? C81 C82 C83 118.8(3) . . ? C81 C82 H82A 120.6 . . ? C83 C82 H82A 120.6 . . ? C82 C83 C84 121.7(3) . . ? C82 C83 H83A 119.1 . . ? C84 C83 H83A 119.1 . . ? C79 C84 C83 119.5(3) . . ? C79 C84 H84A 120.2 . . ? C83 C84 H84A 120.2 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.122 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.073 data_rupivwc _database_code_depnum_ccdc_archive 'CCDC 799277' _audit_creation_method SHELXL-97 #--------------------------------------------------------------------- _chemical_name_systematic ; [{Ru2(piv)4}3W(CN)8(H2O)] ; _chemical_name_common ((Ru2(piv)4)3W(CN)8(H2O)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H110 N8 O25 Ru6 W' _chemical_formula_weight 2229.91 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' _cell_length_a 24.609(2) _cell_length_b 24.609(2) _cell_length_c 15.7876(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9561.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3793 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK(J\(Ba _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'psi 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 59819 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.1598 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 28.67 _reflns_number_total 22284 _reflns_number_gt 13019 _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 SHELXL' _computing_publication_material 'Bruker SHELXL' _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/[(J\(Bs^2^(Fo^2^)+(0.0212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.491(5) _refine_ls_number_reflns 22284 _refine_ls_number_parameters 972 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.766 _refine_ls_restrained_S_all 0.766 _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 W1 W 0.258271(12) 0.755649(12) 0.400648(15) 0.02326(6) Uani 1 1 d . . . Ru1 Ru 0.46037(3) 0.72915(3) 0.50358(5) 0.03384(19) Uani 1 1 d . . . Ru2 Ru 0.54170(3) 0.76750(3) 0.53872(5) 0.03470(19) Uani 1 1 d . . . Ru3 Ru 0.27184(3) 0.95960(3) 0.51030(5) 0.0357(2) Uani 1 1 d . . . Ru4 Ru 0.23343(3) 1.04141(3) 0.54232(5) 0.0393(2) Uani 1 1 d . . . Ru5 Ru 0.22816(5) 0.71815(4) 0.07587(4) 0.0714(3) Uani 1 1 d . . . Ru6 Ru 0.23536(4) 0.72912(3) -0.06646(4) 0.0589(2) Uani 1 1 d . . . O1 O 0.4430(2) 0.7978(2) 0.4397(4) 0.0391(16) Uani 1 1 d . . . O2 O 0.5219(2) 0.8347(2) 0.4726(4) 0.0437(17) Uani 1 1 d . . . O3 O 0.4276(2) 0.7614(2) 0.6086(4) 0.0430(16) Uani 1 1 d . . . O4 O 0.5067(2) 0.8007(2) 0.6430(4) 0.0432(17) Uani 1 1 d . . . O5 O 0.4813(2) 0.6611(2) 0.5678(4) 0.0453(17) Uani 1 1 d . . . O6 O 0.5591(2) 0.6998(2) 0.6053(4) 0.0445(16) Uani 1 1 d . . . O7 O 0.4946(2) 0.6978(2) 0.3988(4) 0.0435(15) Uani 1 1 d . . . O8 O 0.5731(2) 0.7359(2) 0.4330(4) 0.0438(16) Uani 1 1 d . . . O9 O 0.3086(2) 0.9934(2) 0.4084(4) 0.0428(15) Uani 1 1 d . . . O10 O 0.2711(2) 1.0732(2) 0.4401(4) 0.0488(17) Uani 1 1 d . . . O11 O 0.2068(2) 0.9434(2) 0.4370(4) 0.0494(18) Uani 1 1 d . . . O12 O 0.1702(2) 1.0242(2) 0.4674(4) 0.0496(18) Uani 1 1 d . . . O13 O 0.2341(2) 0.9277(2) 0.6106(4) 0.0463(16) Uani 1 1 d . . . O14 O 0.1951(2) 1.0059(2) 0.6427(4) 0.0497(18) Uani 1 1 d . . . O15 O 0.3363(2) 0.9784(2) 0.5835(4) 0.0471(16) Uani 1 1 d . . . O16 O 0.2979(2) 1.0577(2) 0.6155(4) 0.0533(18) Uani 1 1 d . . . O17 O 0.1582(3) 0.7620(3) 0.0731(4) 0.080(2) Uani 1 1 d . . . O18 O 0.1655(3) 0.7736(3) -0.0661(4) 0.071(2) Uani 1 1 d . . . O19 O 0.1868(3) 0.6480(3) 0.0572(4) 0.087(2) Uani 1 1 d . A . O20 O 0.1932(3) 0.6594(2) -0.0827(4) 0.0672(19) Uani 1 1 d . A . O21 O 0.3061(3) 0.6887(3) -0.0645(4) 0.074(2) Uani 1 1 d . . . O22 O 0.2975(3) 0.6789(3) 0.0759(4) 0.107(3) Uani 1 1 d . . . O23 O 0.2766(3) 0.7972(3) -0.0494(3) 0.070(2) Uani 1 1 d . . . O24 O 0.2701(3) 0.7863(3) 0.0911(3) 0.0702(19) Uani 1 1 d . . . O25 O 0.2456(3) 0.7465(3) -0.2130(3) 0.095(2) Uani 1 1 d . . . N61 N 0.3728(3) 0.7058(3) 0.4754(5) 0.042(2) Uani 1 1 d . . . N62 N 0.2131(3) 0.6295(3) 0.4323(5) 0.042(2) Uani 1 1 d . . . N63 N 0.2972(3) 0.8738(3) 0.4827(4) 0.042(2) Uani 1 1 d . . . N64 N 0.1294(3) 0.7860(3) 0.4292(5) 0.044(2) Uani 1 1 d . . . N65 N 0.2196(4) 0.7083(4) 0.2158(4) 0.097(3) Uani 1 1 d . . . N66 N 0.2303(5) 0.8566(4) 0.2682(6) 0.108(4) Uani 1 1 d . . . N67 N 0.2414(3) 0.7461(3) 0.6090(3) 0.0558(17) Uani 1 1 d . . . N68 N 0.3602(4) 0.7596(5) 0.2665(6) 0.102(4) Uani 1 1 d . . . C1 C 0.4757(4) 0.8356(3) 0.4342(6) 0.038(2) Uani 1 1 d . . . C2 C 0.4595(4) 0.8875(4) 0.3912(7) 0.054(3) Uani 1 1 d . . . C3 C 0.4139(5) 0.8806(5) 0.3322(11) 0.148(7) Uani 1 1 d . . . H3A H 0.4250 0.8580 0.2858 0.222 Uiso 1 1 calc R . . H3B H 0.4029 0.9155 0.3111 0.222 Uiso 1 1 calc R . . H3C H 0.3840 0.8639 0.3612 0.222 Uiso 1 1 calc R . . C4 C 0.4352(5) 0.9249(5) 0.4591(8) 0.102(4) Uani 1 1 d . . . C5 C 0.5057(5) 0.9116(6) 0.3513(12) 0.224(12) Uani 1 1 d . . . H5A H 0.5219 0.8858 0.3132 0.336 Uiso 1 1 calc R . . H5B H 0.5317 0.9219 0.3936 0.336 Uiso 1 1 calc R . . H5C H 0.4945 0.9432 0.3201 0.336 Uiso 1 1 calc R . . C6 C 0.4557(4) 0.7910(4) 0.6573(6) 0.047(3) Uani 1 1 d . . . C7 C 0.4279(4) 0.8143(4) 0.7330(7) 0.060(3) Uani 1 1 d . . . C8 C 0.3726(5) 0.8392(6) 0.7046(10) 0.141(8) Uani 1 1 d . . . H8A H 0.3505 0.8114 0.6793 0.212 Uiso 1 1 calc R . . H8B H 0.3790 0.8675 0.6640 0.212 Uiso 1 1 calc R . . H8C H 0.3541 0.8540 0.7529 0.212 Uiso 1 1 calc R . . C9 C 0.4625(4) 0.8582(4) 0.7721(7) 0.075(4) Uani 1 1 d . . . H9A H 0.4968 0.8430 0.7892 0.113 Uiso 1 1 calc R . . H9B H 0.4443 0.8729 0.8207 0.113 Uiso 1 1 calc R . . H9C H 0.4686 0.8865 0.7314 0.113 Uiso 1 1 calc R . . C10 C 0.4184(7) 0.7705(5) 0.7930(7) 0.166(8) Uani 1 1 d . . . H10A H 0.4526 0.7551 0.8099 0.249 Uiso 1 1 calc R . . H10B H 0.3964 0.7430 0.7669 0.249 Uiso 1 1 calc R . . H10C H 0.4000 0.7845 0.8419 0.249 Uiso 1 1 calc R . . C11 C 0.5275(4) 0.6596(4) 0.6051(6) 0.046(2) Uani 1 1 d . . . C12 C 0.5440(4) 0.6090(4) 0.6513(8) 0.073(4) Uani 1 1 d . . . C13 C 0.5015(5) 0.5906(7) 0.7047(13) 0.248(14) Uani 1 1 d . . . H13A H 0.4948 0.6171 0.7481 0.372 Uiso 1 1 calc R . . H13B H 0.5118 0.5568 0.7305 0.372 Uiso 1 1 calc R . . H13C H 0.4691 0.5854 0.6719 0.372 Uiso 1 1 calc R . . C14 C 0.5984(5) 0.6174(5) 0.6915(8) 0.100(5) Uani 1 1 d . . . H14A H 0.5955 0.6447 0.7348 0.150 Uiso 1 1 calc R . . H14B H 0.6240 0.6291 0.6494 0.150 Uiso 1 1 calc R . . H14C H 0.6105 0.5839 0.7163 0.150 Uiso 1 1 calc R . . C15 C 0.5535(6) 0.5636(5) 0.5812(9) 0.135(6) Uani 1 1 d . . . C16 C 0.5443(4) 0.7078(3) 0.3829(6) 0.037(2) Uani 1 1 d . . . C17 C 0.5717(4) 0.6863(5) 0.3038(7) 0.059(3) Uani 1 1 d . . . C18 C 0.5906(6) 0.7338(5) 0.2557(7) 0.114(5) Uani 1 1 d . . . H18A H 0.5599 0.7546 0.2371 0.171 Uiso 1 1 calc R . . H18B H 0.6110 0.7218 0.2073 0.171 Uiso 1 1 calc R . . H18C H 0.6133 0.7559 0.2911 0.171 Uiso 1 1 calc R . . C19 C 0.5349(5) 0.6510(6) 0.2549(8) 0.135(7) Uani 1 1 d . . . H19A H 0.5027 0.6708 0.2403 0.203 Uiso 1 1 calc R . . H19B H 0.5252 0.6199 0.2885 0.203 Uiso 1 1 calc R . . H19C H 0.5528 0.6391 0.2042 0.203 Uiso 1 1 calc R . . C20 C 0.6219(6) 0.6560(6) 0.3259(10) 0.133(6) Uani 1 1 d . . . H20A H 0.6472 0.6801 0.3528 0.199 Uiso 1 1 calc R . . H20B H 0.6379 0.6414 0.2754 0.199 Uiso 1 1 calc R . . H20C H 0.6131 0.6269 0.3640 0.199 Uiso 1 1 calc R . . C21 C 0.2998(3) 1.0430(4) 0.3918(6) 0.044(2) Uani 1 1 d . . . C22 C 0.3217(4) 1.0675(4) 0.3129(7) 0.057(3) Uani 1 1 d . . . C23 C 0.2755(6) 1.0769(7) 0.2509(9) 0.180(9) Uani 1 1 d . . . H23A H 0.2594 1.0427 0.2359 0.270 Uiso 1 1 calc R . . H23B H 0.2893 1.0942 0.2008 0.270 Uiso 1 1 calc R . . H23C H 0.2486 1.0998 0.2766 0.270 Uiso 1 1 calc R . . C24 C 0.3474(5) 1.1208(4) 0.3375(9) 0.109(5) Uani 1 1 d . . . H24A H 0.3767 1.1142 0.3762 0.164 Uiso 1 1 calc R . . H24B H 0.3207 1.1435 0.3642 0.164 Uiso 1 1 calc R . . H24C H 0.3611 1.1385 0.2877 0.164 Uiso 1 1 calc R . . C25 C 0.3606(4) 1.0323(4) 0.2701(7) 0.079(4) Uani 1 1 d . . . H25A H 0.3908 1.0254 0.3069 0.119 Uiso 1 1 calc R . . H25B H 0.3731 1.0497 0.2194 0.119 Uiso 1 1 calc R . . H25C H 0.3433 0.9985 0.2559 0.119 Uiso 1 1 calc R . . C26 C 0.1688(3) 0.9781(4) 0.4297(6) 0.042(2) Uani 1 1 d . . . C27 C 0.1211(4) 0.9656(4) 0.3753(7) 0.059(3) Uani 1 1 d . . . C28 C 0.1093(5) 0.9079(4) 0.3755(10) 0.141(7) Uani 1 1 d . . . H28A H 0.0960 0.8974 0.4303 0.212 Uiso 1 1 calc R . . H28B H 0.1418 0.8880 0.3629 0.212 Uiso 1 1 calc R . . H28C H 0.0822 0.9001 0.3335 0.212 Uiso 1 1 calc R . . C29 C 0.1417(5) 0.9749(6) 0.2832(8) 0.131(5) Uani 1 1 d . . . H29A H 0.1534 1.0119 0.2770 0.197 Uiso 1 1 calc R . . H29B H 0.1128 0.9676 0.2440 0.197 Uiso 1 1 calc R . . H29C H 0.1716 0.9509 0.2720 0.197 Uiso 1 1 calc R . . C30 C 0.0756(4) 1.0029(5) 0.3809(10) 0.145(7) Uani 1 1 d . . . H30A H 0.0552 0.9954 0.4314 0.218 Uiso 1 1 calc R . . H30B H 0.0527 0.9985 0.3323 0.218 Uiso 1 1 calc R . . H30C H 0.0889 1.0396 0.3829 0.218 Uiso 1 1 calc R . . C31 C 0.2032(4) 0.9563(4) 0.6562(6) 0.043(3) Uani 1 1 d . . . C32 C 0.1760(4) 0.9289(4) 0.7310(6) 0.056(3) Uani 1 1 d . . . C33 C 0.1280(5) 0.9624(5) 0.7644(7) 0.088(4) Uani 1 1 d . . . H33A H 0.1409 0.9972 0.7831 0.131 Uiso 1 1 calc R . . H33B H 0.1114 0.9437 0.8110 0.131 Uiso 1 1 calc R . . H33C H 0.1018 0.9673 0.7201 0.131 Uiso 1 1 calc R . . C34 C 0.2178(5) 0.9187(6) 0.7958(8) 0.127(6) Uani 1 1 d . . . H34A H 0.2318 0.9527 0.8161 0.191 Uiso 1 1 calc R . . H34B H 0.2468 0.8978 0.7714 0.191 Uiso 1 1 calc R . . H34C H 0.2021 0.8989 0.8420 0.191 Uiso 1 1 calc R . . C35 C 0.1554(5) 0.8717(5) 0.7011(9) 0.101(5) Uani 1 1 d . . . H35A H 0.1856 0.8506 0.6813 0.151 Uiso 1 1 calc R . . H35B H 0.1296 0.8762 0.6560 0.151 Uiso 1 1 calc R . . H35C H 0.1383 0.8533 0.7477 0.151 Uiso 1 1 calc R . . C36 C 0.3360(4) 1.0242(4) 0.6215(5) 0.042(2) Uani 1 1 d . . . C37 C 0.3854(4) 1.0411(5) 0.6756(8) 0.065(3) Uani 1 1 d . . . C38 C 0.3764(5) 1.0931(5) 0.7181(9) 0.147(7) Uani 1 1 d . . . H38A H 0.3637 1.1193 0.6777 0.221 Uiso 1 1 calc R . . H38B H 0.4098 1.1055 0.7427 0.221 Uiso 1 1 calc R . . H38C H 0.3497 1.0886 0.7619 0.221 Uiso 1 1 calc R . . C39 C 0.4294(6) 1.0472(11) 0.6168(14) 0.36(2) Uani 1 1 d . . . H39A H 0.4212 1.0760 0.5778 0.543 Uiso 1 1 calc R . . H39B H 0.4343 1.0139 0.5861 0.543 Uiso 1 1 calc R . . H39C H 0.4621 1.0557 0.6471 0.543 Uiso 1 1 calc R . . C40 C 0.3969(10) 0.9998(7) 0.7368(13) 0.293(17) Uani 1 1 d . . . H40A H 0.4028 0.9658 0.7085 0.439 Uiso 1 1 calc R . . H40B H 0.3667 0.9963 0.7749 0.439 Uiso 1 1 calc R . . H40C H 0.4289 1.0095 0.7682 0.439 Uiso 1 1 calc R . . C41 C 0.1412(5) 0.7834(5) 0.0043(7) 0.081(4) Uani 1 1 d . . . C42 C 0.0914(7) 0.8173(8) 0.0071(10) 0.136(6) Uani 1 1 d . . . C43 C 0.0511(7) 0.7919(9) 0.0520(18) 0.34(2) Uani 1 1 d . . . H43A H 0.0395 0.7600 0.0221 0.509 Uiso 1 1 calc R . . H43B H 0.0208 0.8162 0.0587 0.509 Uiso 1 1 calc R . . H43C H 0.0646 0.7817 0.1068 0.509 Uiso 1 1 calc R . . C44 C 0.0774(7) 0.8401(7) -0.0700(11) 0.214(10) Uani 1 1 d . . . H44A H 0.0711 0.8118 -0.1106 0.320 Uiso 1 1 calc R . . H44B H 0.1065 0.8630 -0.0894 0.320 Uiso 1 1 calc R . . H44C H 0.0450 0.8614 -0.0635 0.320 Uiso 1 1 calc R . . C45 C 0.1082(8) 0.8630(8) 0.0734(17) 0.342(19) Uani 1 1 d . . . H45A H 0.0784 0.8877 0.0811 0.513 Uiso 1 1 calc R . . H45B H 0.1392 0.8825 0.0524 0.513 Uiso 1 1 calc R . . H45C H 0.1171 0.8464 0.1266 0.513 Uiso 1 1 calc R . . C46 C 0.1789(5) 0.6326(5) -0.0173(6) 0.080(4) Uani 1 1 d . . . C47 C 0.1607(9) 0.5702(8) -0.0264(11) 0.076(5) Uiso 0.667(17) 1 d P A 3 C48 C 0.1294(7) 0.5676(7) -0.1179(10) 0.068(6) Uiso 0.667(17) 1 d P A 3 C49 C 0.1149(8) 0.5653(7) 0.0420(12) 0.095(6) Uiso 0.667(17) 1 d P A 3 C50 C 0.2065(9) 0.5335(9) -0.0130(12) 0.132(9) Uiso 0.667(17) 1 d P A 3 C47B C 0.1302(13) 0.5899(11) -0.0281(16) 0.040(8) Uiso 0.333(17) 1 d P A 4 C48B C 0.1515(13) 0.5563(12) -0.1175(18) 0.047(9) Uiso 0.333(17) 1 d P A 4 C49B C 0.1527(14) 0.5469(12) 0.049(2) 0.075(11) Uiso 0.333(17) 1 d P A 4 C50B C 0.0802(13) 0.6070(12) -0.0160(18) 0.073(12) Uiso 0.333(17) 1 d P A 4 C51 C 0.3237(5) 0.6717(4) 0.0063(7) 0.064(3) Uani 1 1 d . . . C52 C 0.3760(6) 0.6431(6) 0.0110(7) 0.106(4) Uani 1 1 d . . . C53 C 0.3663(7) 0.5836(7) 0.0382(13) 0.249(12) Uani 1 1 d . . . H53A H 0.4004 0.5647 0.0400 0.373 Uiso 1 1 calc R . . H53B H 0.3426 0.5662 -0.0017 0.373 Uiso 1 1 calc R . . H53C H 0.3499 0.5830 0.0934 0.373 Uiso 1 1 calc R . . C54 C 0.4076(5) 0.6421(5) -0.0725(8) 0.125(5) Uani 1 1 d . . . H54A H 0.4159 0.6786 -0.0895 0.188 Uiso 1 1 calc R . . H54B H 0.3860 0.6249 -0.1155 0.188 Uiso 1 1 calc R . . H54C H 0.4408 0.6221 -0.0650 0.188 Uiso 1 1 calc R . . C55 C 0.4125(6) 0.6657(9) 0.0790(11) 0.287(14) Uani 1 1 d . . . H55A H 0.4238 0.7017 0.0636 0.430 Uiso 1 1 calc R . . H55B H 0.4439 0.6429 0.0851 0.430 Uiso 1 1 calc R . . H55C H 0.3931 0.6670 0.1317 0.430 Uiso 1 1 calc R . . C56 C 0.2872(4) 0.8131(4) 0.0275(6) 0.070(3) Uani 1 1 d . . . C57 C 0.3185(5) 0.8650(5) 0.0404(6) 0.079(4) Uani 1 1 d . . . C58 C 0.2766(8) 0.9040(5) 0.0682(12) 0.239(12) Uani 1 1 d . . . H58A H 0.2931 0.9386 0.0789 0.358 Uiso 1 1 calc R . . H58B H 0.2597 0.8909 0.1191 0.358 Uiso 1 1 calc R . . H58C H 0.2496 0.9078 0.0247 0.358 Uiso 1 1 calc R . . C59 C 0.3403(6) 0.8887(5) -0.0354(7) 0.127(6) Uani 1 1 d . . . H59A H 0.3692 0.8663 -0.0566 0.191 Uiso 1 1 calc R . . H59B H 0.3541 0.9243 -0.0230 0.191 Uiso 1 1 calc R . . H59C H 0.3122 0.8914 -0.0773 0.191 Uiso 1 1 calc R . . C60 C 0.3527(8) 0.8617(7) 0.1124(13) 0.310(17) Uani 1 1 d . . . H60A H 0.3826 0.8378 0.1005 0.466 Uiso 1 1 calc R . . H60B H 0.3324 0.8478 0.1595 0.466 Uiso 1 1 calc R . . H60C H 0.3663 0.8972 0.1259 0.466 Uiso 1 1 calc R . . C61 C 0.3325(3) 0.7202(3) 0.4512(6) 0.034(2) Uani 1 1 d . . . C62 C 0.2293(3) 0.6738(3) 0.4198(5) 0.032(2) Uani 1 1 d . . . C63 C 0.2867(3) 0.8320(3) 0.4567(6) 0.037(2) Uani 1 1 d . . . C64 C 0.1736(3) 0.7756(3) 0.4204(5) 0.036(2) Uani 1 1 d . . . C65 C 0.2298(5) 0.7237(4) 0.2823(5) 0.059(3) Uani 1 1 d . . . C66 C 0.2406(4) 0.8229(4) 0.3131(6) 0.046(2) Uani 1 1 d . . . C67 C 0.2453(3) 0.7486(3) 0.5379(4) 0.0372(16) Uani 1 1 d . . . C68 C 0.3239(4) 0.7605(4) 0.3117(6) 0.063(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02286(19) 0.02352(19) 0.02342(12) -0.00019(14) 0.00028(14) -0.00040(14) Ru1 0.0222(4) 0.0317(4) 0.0477(5) 0.0001(4) -0.0048(4) 0.0002(3) Ru2 0.0235(4) 0.0365(4) 0.0441(5) -0.0034(3) -0.0041(3) 0.0004(3) Ru3 0.0378(4) 0.0232(4) 0.0462(5) -0.0035(4) 0.0013(4) 0.0003(3) Ru4 0.0416(4) 0.0223(4) 0.0541(5) -0.0028(4) 0.0042(4) -0.0004(3) Ru5 0.1099(8) 0.0810(7) 0.0231(4) -0.0016(4) 0.0007(5) -0.0341(5) Ru6 0.0877(7) 0.0651(6) 0.0240(3) -0.0006(4) 0.0005(5) -0.0133(4) O1 0.026(3) 0.039(4) 0.053(4) 0.003(3) -0.019(3) -0.004(3) O2 0.033(4) 0.034(3) 0.064(5) 0.007(3) -0.006(3) -0.010(3) O3 0.025(3) 0.053(4) 0.051(4) -0.014(3) 0.004(3) -0.005(3) O4 0.034(4) 0.048(4) 0.048(4) -0.010(3) 0.001(3) 0.001(3) O5 0.029(3) 0.035(3) 0.072(5) 0.014(3) -0.009(3) -0.005(3) O6 0.023(3) 0.047(4) 0.063(4) 0.007(3) -0.008(3) 0.002(3) O7 0.037(4) 0.045(4) 0.048(4) -0.003(3) -0.011(3) -0.007(3) O8 0.033(4) 0.049(4) 0.050(4) -0.013(3) 0.004(3) -0.005(3) O9 0.048(3) 0.029(4) 0.051(4) -0.003(3) 0.003(3) 0.004(3) O10 0.053(4) 0.029(4) 0.065(5) -0.007(3) 0.009(4) -0.001(3) O11 0.045(4) 0.033(4) 0.070(5) 0.002(3) 0.007(3) 0.007(3) O12 0.037(4) 0.039(4) 0.073(5) 0.001(3) 0.002(3) 0.009(3) O13 0.057(4) 0.035(4) 0.047(4) -0.004(3) 0.006(3) 0.002(3) O14 0.060(4) 0.034(4) 0.055(5) -0.001(3) 0.018(3) 0.006(3) O15 0.043(3) 0.029(3) 0.070(5) -0.001(3) 0.000(3) 0.000(3) O16 0.050(4) 0.035(4) 0.075(5) -0.007(4) -0.004(4) 0.005(3) O17 0.083(5) 0.101(6) 0.056(5) -0.021(4) 0.025(4) -0.010(4) O18 0.104(6) 0.085(5) 0.025(4) -0.011(3) 0.011(4) 0.000(4) O19 0.140(7) 0.092(5) 0.029(4) 0.008(4) -0.004(4) -0.052(5) O20 0.106(5) 0.064(4) 0.031(4) 0.010(3) -0.001(4) -0.029(4) O21 0.085(5) 0.109(6) 0.028(4) 0.009(4) -0.011(4) -0.019(4) O22 0.129(7) 0.174(8) 0.018(4) 0.017(5) -0.012(4) -0.057(6) O23 0.100(5) 0.100(6) 0.010(3) 0.007(3) 0.005(4) -0.020(4) O24 0.108(5) 0.083(5) 0.019(3) 0.005(3) 0.000(4) -0.043(4) O25 0.169(11) 0.089(8) 0.025(3) 0.000(4) 0.010(4) -0.037(7) N61 0.021(4) 0.041(4) 0.065(6) -0.004(4) -0.004(4) 0.007(3) N62 0.042(4) 0.023(4) 0.061(6) 0.006(4) -0.014(4) 0.004(3) N63 0.041(4) 0.029(5) 0.056(6) -0.013(4) 0.002(4) 0.000(3) N64 0.032(5) 0.039(4) 0.061(6) 0.004(4) 0.000(4) 0.000(4) N65 0.147(9) 0.127(9) 0.018(4) 0.003(5) 0.000(5) -0.078(7) N66 0.186(11) 0.078(8) 0.059(7) 0.033(6) 0.008(6) 0.064(7) N67 0.055(6) 0.073(7) 0.039(3) 0.007(5) 0.008(4) -0.006(5) N68 0.054(7) 0.196(11) 0.057(7) 0.020(6) 0.016(5) 0.014(7) C1 0.034(6) 0.033(5) 0.049(6) 0.004(4) -0.003(5) 0.001(4) C2 0.039(6) 0.039(6) 0.085(8) 0.030(6) -0.011(6) -0.006(4) C3 0.103(12) 0.105(12) 0.236(18) 0.102(12) -0.058(12) -0.021(9) C4 0.128(11) 0.074(8) 0.102(9) -0.007(7) 0.027(8) 0.036(7) C5 0.079(11) 0.170(15) 0.42(3) 0.243(18) 0.027(13) 0.025(10) C6 0.041(7) 0.049(7) 0.052(7) -0.002(5) 0.003(6) 0.012(5) C7 0.047(7) 0.071(8) 0.061(8) -0.021(6) 0.008(6) -0.015(5) C8 0.052(9) 0.196(17) 0.175(17) -0.128(14) -0.019(9) 0.028(9) C9 0.065(8) 0.079(8) 0.082(9) -0.039(7) 0.019(6) -0.009(6) C10 0.34(3) 0.100(12) 0.053(10) -0.007(8) 0.087(12) -0.014(13) C11 0.032(6) 0.050(6) 0.056(6) 0.008(5) 0.004(5) -0.003(4) C12 0.047(7) 0.050(7) 0.121(11) 0.044(7) -0.049(7) -0.007(5) C13 0.051(10) 0.31(2) 0.39(3) 0.30(2) 0.034(13) 0.027(12) C14 0.090(10) 0.074(9) 0.137(12) 0.041(8) -0.016(8) 0.024(7) C15 0.217(16) 0.077(9) 0.111(11) -0.030(8) -0.044(11) 0.066(9) C16 0.032(5) 0.028(5) 0.049(6) -0.009(4) -0.006(5) 0.002(4) C17 0.054(8) 0.074(8) 0.050(7) -0.023(6) 0.003(6) -0.001(6) C18 0.193(15) 0.098(10) 0.051(8) -0.002(7) 0.050(8) -0.052(10) C19 0.061(9) 0.263(19) 0.082(9) -0.104(11) 0.020(7) -0.047(10) C20 0.117(14) 0.178(16) 0.103(12) -0.073(11) 0.003(10) 0.029(12) C21 0.028(5) 0.060(7) 0.044(6) -0.006(6) -0.010(5) -0.009(5) C22 0.065(8) 0.049(7) 0.058(8) 0.014(6) 0.020(6) 0.005(5) C23 0.113(13) 0.29(2) 0.136(16) 0.105(15) -0.006(11) 0.055(14) C24 0.127(12) 0.060(9) 0.141(13) 0.015(8) 0.081(9) -0.003(8) C25 0.084(9) 0.075(9) 0.079(9) 0.003(7) 0.037(7) 0.017(7) C26 0.041(5) 0.035(6) 0.049(6) 0.002(5) -0.008(5) 0.005(4) C27 0.057(7) 0.047(7) 0.073(8) -0.001(5) -0.007(6) 0.020(5) C28 0.132(11) 0.042(7) 0.249(19) 0.019(10) -0.096(12) -0.042(7) C29 0.076(10) 0.167(15) 0.150(14) -0.008(11) -0.052(10) 0.017(9) C30 0.072(9) 0.100(10) 0.263(19) -0.074(12) -0.067(11) 0.026(8) C31 0.035(6) 0.044(7) 0.049(7) -0.008(5) -0.005(5) 0.002(5) C32 0.063(7) 0.062(8) 0.044(7) 0.019(6) 0.011(6) -0.005(5) C33 0.092(9) 0.089(10) 0.081(9) -0.004(7) 0.057(7) -0.010(7) C34 0.115(12) 0.171(15) 0.095(12) 0.060(10) -0.009(9) 0.028(10) C35 0.125(11) 0.061(9) 0.118(12) 0.007(8) 0.049(9) -0.021(8) C36 0.044(6) 0.041(6) 0.041(6) 0.003(5) -0.007(4) -0.008(5) C37 0.034(6) 0.074(8) 0.087(9) -0.027(7) -0.003(6) -0.006(5) C38 0.153(14) 0.087(11) 0.202(16) -0.085(11) -0.111(12) 0.039(10) C39 0.063(10) 0.62(5) 0.40(3) -0.42(4) 0.073(16) -0.111(19) C40 0.44(3) 0.125(16) 0.32(3) 0.107(17) -0.32(3) -0.117(19) C41 0.112(11) 0.093(9) 0.037(7) 0.014(7) 0.002(7) -0.030(7) C42 0.111(13) 0.203(18) 0.095(12) 0.019(12) 0.050(11) 0.077(13) C43 0.152(18) 0.36(3) 0.50(4) 0.25(3) 0.19(3) 0.14(2) C44 0.22(2) 0.25(2) 0.171(19) 0.096(17) 0.108(17) 0.138(17) C45 0.29(3) 0.29(3) 0.45(4) -0.32(3) -0.12(3) 0.10(2) C46 0.129(11) 0.088(9) 0.022(7) -0.011(5) -0.001(6) -0.033(7) C51 0.080(8) 0.064(7) 0.046(7) 0.001(6) -0.025(7) -0.003(6) C52 0.141(13) 0.133(13) 0.043(8) 0.011(8) -0.018(8) 0.013(10) C53 0.176(18) 0.23(2) 0.35(3) 0.17(2) 0.053(19) 0.091(16) C54 0.130(12) 0.151(13) 0.095(11) 0.022(10) -0.023(9) 0.051(9) C55 0.186(18) 0.49(4) 0.180(18) -0.20(2) -0.133(16) 0.10(2) C56 0.092(8) 0.070(8) 0.047(7) -0.009(6) 0.014(6) -0.015(6) C57 0.101(10) 0.095(10) 0.039(6) -0.001(6) 0.010(6) -0.047(8) C58 0.42(3) 0.088(12) 0.21(2) -0.012(13) 0.15(2) -0.092(17) C59 0.196(15) 0.102(11) 0.083(10) -0.003(8) 0.057(10) -0.080(10) C60 0.38(3) 0.21(2) 0.33(3) 0.17(2) -0.27(3) -0.23(2) C61 0.022(5) 0.036(5) 0.045(6) 0.006(4) -0.006(4) 0.002(4) C62 0.034(5) 0.033(5) 0.030(5) 0.000(4) -0.018(4) 0.015(4) C63 0.044(6) 0.028(5) 0.039(6) 0.011(5) 0.003(4) 0.015(4) C64 0.040(6) 0.044(5) 0.025(5) 0.005(4) -0.005(4) -0.021(4) C65 0.083(7) 0.053(6) 0.039(5) 0.004(5) -0.003(6) -0.053(5) C66 0.059(6) 0.042(7) 0.036(6) 0.000(5) 0.006(5) 0.000(5) C67 0.031(7) 0.039(7) 0.043(4) -0.006(5) 0.009(4) -0.003(5) C68 0.055(8) 0.101(9) 0.031(6) 0.002(5) 0.012(5) 0.006(6) _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 W1 C68 2.144(10) . ? W1 C65 2.144(8) . ? W1 C62 2.158(9) . ? W1 C64 2.162(9) . ? W1 C61 2.177(8) . ? W1 C63 2.191(9) . ? W1 C67 2.197(6) . ? W1 C66 2.199(10) . ? Ru1 O3 2.008(6) . ? Ru1 O7 2.010(6) . ? Ru1 O1 2.014(5) . ? Ru1 O5 2.024(5) . ? Ru1 N61 2.276(7) . ? Ru1 Ru2 2.2811(9) . ? Ru2 O8 1.997(6) . ? Ru2 O6 2.015(6) . ? Ru2 O2 2.016(5) . ? Ru2 O4 2.029(6) . ? Ru2 N62 2.259(6) 3_566 ? Ru3 O13 1.997(6) . ? Ru3 O11 2.015(6) . ? Ru3 O15 2.017(6) . ? Ru3 O9 2.025(6) . ? Ru3 N63 2.244(7) . ? Ru3 Ru4 2.2809(10) . ? Ru4 O12 2.000(6) . ? Ru4 O16 2.003(6) . ? Ru4 O10 2.018(6) . ? Ru4 O14 2.041(6) . ? Ru4 N64 2.263(7) 4_666 ? Ru5 O22 1.960(9) . ? Ru5 O24 1.985(5) . ? Ru5 O19 2.026(6) . ? Ru5 O17 2.032(7) . ? Ru5 N65 2.233(7) . ? Ru5 Ru6 2.2701(9) . ? Ru6 O23 1.978(6) . ? Ru6 O21 2.006(7) . ? Ru6 O20 2.022(6) . ? Ru6 O18 2.037(7) . ? Ru6 O25 2.367(4) . ? O1 C1 1.233(9) . ? O2 C1 1.288(9) . ? O3 C6 1.264(10) . ? O4 C6 1.296(10) . ? O5 C11 1.279(10) . ? O6 C11 1.260(9) . ? O7 C16 1.273(9) . ? O8 C16 1.266(9) . ? O9 C21 1.265(10) . ? O10 C21 1.279(10) . ? O11 C26 1.272(9) . ? O12 C26 1.281(10) . ? O13 C31 1.261(10) . ? O14 C31 1.256(10) . ? O15 C36 1.276(10) . ? O16 C36 1.254(10) . ? O17 C41 1.278(11) . ? O18 C41 1.286(12) . ? O19 C46 1.251(10) . ? O20 C46 1.275(10) . ? O21 C51 1.269(10) . ? O22 C51 1.287(11) . ? O23 C56 1.303(10) . ? O24 C56 1.272(10) . ? N61 C61 1.118(9) . ? N62 C62 1.178(9) . ? N62 Ru2 2.259(6) 4_656 ? N63 C63 1.138(9) . ? N64 C64 1.127(9) . ? N64 Ru4 2.263(7) 3_466 ? N65 C65 1.144(9) . ? N66 C66 1.121(10) . ? N67 C67 1.127(7) . ? N68 C68 1.143(11) . ? C1 C2 1.500(11) . ? C2 C5 1.428(14) . ? C2 C3 1.468(15) . ? C2 C4 1.535(14) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.492(13) . ? C7 C10 1.455(15) . ? C7 C9 1.508(13) . ? C7 C8 1.559(15) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.499(12) . ? C12 C13 1.420(16) . ? C12 C14 1.495(14) . ? C12 C15 1.591(16) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C17 1.515(12) . ? C17 C18 1.470(14) . ? C17 C19 1.474(14) . ? C17 C20 1.484(16) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.485(13) . ? C22 C25 1.457(13) . ? C22 C24 1.506(14) . ? C22 C23 1.518(16) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.487(12) . ? C27 C28 1.450(13) . ? C27 C30 1.450(13) . ? C27 C29 1.557(15) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.515(13) . ? C32 C34 1.473(14) . ? C32 C33 1.533(14) . ? C32 C35 1.569(14) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.541(12) . ? C37 C40 1.431(16) . ? C37 C39 1.434(19) . ? C37 C38 1.462(13) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.484(17) . ? C42 C43 1.37(2) . ? C42 C44 1.383(19) . ? C42 C45 1.59(2) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47B 1.60(3) . ? C46 C47 1.605(19) . ? C47 C50 1.46(2) . ? C47 C49 1.56(3) . ? C47 C48 1.64(2) . ? C47B C50B 1.31(4) . ? C47B C49B 1.71(5) . ? C47B C48B 1.72(4) . ? C51 C52 1.469(16) . ? C52 C55 1.509(17) . ? C52 C54 1.532(16) . ? C52 C53 1.543(18) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.505(13) . ? C57 C60 1.417(17) . ? C57 C59 1.435(13) . ? C57 C58 1.477(18) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? 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 C68 W1 C65 72.3(3) . . ? C68 W1 C62 113.1(3) . . ? C65 W1 C62 70.9(3) . . ? C68 W1 C64 143.8(3) . . ? C65 W1 C64 83.9(4) . . ? C62 W1 C64 82.7(3) . . ? C68 W1 C61 68.3(4) . . ? C65 W1 C61 116.5(4) . . ? C62 W1 C61 81.5(3) . . ? C64 W1 C61 147.9(3) . . ? C68 W1 C63 88.6(4) . . ? C65 W1 C63 140.4(3) . . ? C62 W1 C63 148.1(3) . . ? C64 W1 C63 93.2(3) . . ? C61 W1 C63 85.8(3) . . ? C68 W1 C67 139.5(3) . . ? C65 W1 C67 141.5(3) . . ? C62 W1 C67 74.9(3) . . ? C64 W1 C67 74.7(3) . . ? C61 W1 C67 74.2(3) . . ? C63 W1 C67 73.5(3) . . ? C68 W1 C66 72.3(4) . . ? C65 W1 C66 70.4(3) . . ? C62 W1 C66 136.5(3) . . ? C64 W1 C66 74.3(3) . . ? C61 W1 C66 134.3(3) . . ? C63 W1 C66 70.9(3) . . ? C67 W1 C66 130.6(3) . . ? O3 Ru1 O7 178.8(2) . . ? O3 Ru1 O1 89.8(2) . . ? O7 Ru1 O1 89.9(2) . . ? O3 Ru1 O5 90.9(2) . . ? O7 Ru1 O5 89.3(2) . . ? O1 Ru1 O5 177.4(2) . . ? O3 Ru1 N61 83.1(2) . . ? O7 Ru1 N61 98.0(2) . . ? O1 Ru1 N61 85.0(2) . . ? O5 Ru1 N61 97.5(2) . . ? O3 Ru1 Ru2 89.32(16) . . ? O7 Ru1 Ru2 89.52(15) . . ? O1 Ru1 Ru2 87.74(15) . . ? O5 Ru1 Ru2 89.81(16) . . ? N61 Ru1 Ru2 169.57(17) . . ? O8 Ru2 O6 91.8(2) . . ? O8 Ru2 O2 88.9(2) . . ? O6 Ru2 O2 178.3(2) . . ? O8 Ru2 O4 177.3(2) . . ? O6 Ru2 O4 90.0(2) . . ? O2 Ru2 O4 89.2(2) . . ? O8 Ru2 N62 83.2(2) . 3_566 ? O6 Ru2 N62 82.3(2) . 3_566 ? O2 Ru2 N62 99.4(2) . 3_566 ? O4 Ru2 N62 99.0(2) . 3_566 ? O8 Ru2 Ru1 88.54(16) . . ? O6 Ru2 Ru1 88.37(16) . . ? O2 Ru2 Ru1 90.07(16) . . ? O4 Ru2 Ru1 89.47(17) . . ? N62 Ru2 Ru1 167.31(17) 3_566 . ? O13 Ru3 O11 90.5(2) . . ? O13 Ru3 O15 90.1(2) . . ? O11 Ru3 O15 178.1(2) . . ? O13 Ru3 O9 178.5(2) . . ? O11 Ru3 O9 88.8(2) . . ? O15 Ru3 O9 90.6(2) . . ? O13 Ru3 N63 85.0(2) . . ? O11 Ru3 N63 85.6(2) . . ? O15 Ru3 N63 96.2(2) . . ? O9 Ru3 N63 96.2(2) . . ? O13 Ru3 Ru4 88.76(16) . . ? O11 Ru3 Ru4 88.44(16) . . ? O15 Ru3 Ru4 89.80(16) . . ? O9 Ru3 Ru4 89.89(15) . . ? N63 Ru3 Ru4 171.34(17) . . ? O12 Ru4 O16 178.7(3) . . ? O12 Ru4 O10 88.1(2) . . ? O16 Ru4 O10 91.2(2) . . ? O12 Ru4 O14 90.5(2) . . ? O16 Ru4 O14 90.2(3) . . ? O10 Ru4 O14 177.4(2) . . ? O12 Ru4 N64 99.0(2) . 4_666 ? O16 Ru4 N64 82.0(2) . 4_666 ? O10 Ru4 N64 83.4(2) . 4_666 ? O14 Ru4 N64 99.1(3) . 4_666 ? O12 Ru4 Ru3 90.22(16) . . ? O16 Ru4 Ru3 88.66(17) . . ? O10 Ru4 Ru3 88.58(16) . . ? O14 Ru4 Ru3 89.19(17) . . ? N64 Ru4 Ru3 167.50(17) 4_666 . ? O22 Ru5 O24 87.9(3) . . ? O22 Ru5 O19 91.0(3) . . ? O24 Ru5 O19 178.2(3) . . ? O22 Ru5 O17 177.2(3) . . ? O24 Ru5 O17 89.7(3) . . ? O19 Ru5 O17 91.3(3) . . ? O22 Ru5 N65 91.7(4) . . ? O24 Ru5 N65 91.2(3) . . ? O19 Ru5 N65 90.2(3) . . ? O17 Ru5 N65 89.9(4) . . ? O22 Ru5 Ru6 89.48(19) . . ? O24 Ru5 Ru6 88.76(16) . . ? O19 Ru5 Ru6 89.81(17) . . ? O17 Ru5 Ru6 89.0(2) . . ? N65 Ru5 Ru6 178.9(3) . . ? O23 Ru6 O21 88.5(3) . . ? O23 Ru6 O20 179.5(2) . . ? O21 Ru6 O20 91.5(3) . . ? O23 Ru6 O18 88.7(3) . . ? O21 Ru6 O18 177.1(3) . . ? O20 Ru6 O18 91.3(3) . . ? O23 Ru6 Ru5 90.37(15) . . ? O21 Ru6 Ru5 89.62(18) . . ? O20 Ru6 Ru5 89.12(17) . . ? O18 Ru6 Ru5 89.74(18) . . ? O23 Ru6 O25 85.7(2) . . ? O21 Ru6 O25 90.7(3) . . ? O20 Ru6 O25 94.8(2) . . ? O18 Ru6 O25 89.7(3) . . ? Ru5 Ru6 O25 176.03(16) . . ? C1 O1 Ru1 122.0(6) . . ? C1 O2 Ru2 118.1(5) . . ? C6 O3 Ru1 120.6(6) . . ? C6 O4 Ru2 118.6(6) . . ? C11 O5 Ru1 118.8(5) . . ? C11 O6 Ru2 121.1(6) . . ? C16 O7 Ru1 119.3(5) . . ? C16 O8 Ru2 121.2(6) . . ? C21 O9 Ru3 119.0(6) . . ? C21 O10 Ru4 120.3(6) . . ? C26 O11 Ru3 120.2(6) . . ? C26 O12 Ru4 118.9(5) . . ? C31 O13 Ru3 120.9(6) . . ? C31 O14 Ru4 118.3(6) . . ? C36 O15 Ru3 117.9(5) . . ? C36 O16 Ru4 120.3(6) . . ? C41 O17 Ru5 121.0(8) . . ? C41 O18 Ru6 119.8(7) . . ? C46 O19 Ru5 118.2(7) . . ? C46 O20 Ru6 118.5(6) . . ? C51 O21 Ru6 118.2(7) . . ? C51 O22 Ru5 120.3(7) . . ? C56 O23 Ru6 118.9(6) . . ? C56 O24 Ru5 121.0(6) . . ? C61 N61 Ru1 145.6(7) . . ? C62 N62 Ru2 148.0(6) . 4_656 ? C63 N63 Ru3 149.1(7) . . ? C64 N64 Ru4 154.3(7) . 3_466 ? C65 N65 Ru5 148.4(7) . . ? O1 C1 O2 122.0(8) . . ? O1 C1 C2 120.0(8) . . ? O2 C1 C2 117.6(8) . . ? C5 C2 C3 112.1(12) . . ? C5 C2 C1 110.0(8) . . ? C3 C2 C1 113.1(8) . . ? C5 C2 C4 111.7(11) . . ? C3 C2 C4 102.4(10) . . ? C1 C2 C4 107.3(9) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 122.0(9) . . ? O3 C6 C7 117.2(9) . . ? O4 C6 C7 120.9(9) . . ? C10 C7 C6 108.1(10) . . ? C10 C7 C9 110.7(10) . . ? C6 C7 C9 110.1(9) . . ? C10 C7 C8 109.8(12) . . ? C6 C7 C8 108.8(10) . . ? C9 C7 C8 109.3(10) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 121.8(8) . . ? O6 C11 C12 118.9(9) . . ? O5 C11 C12 119.3(8) . . ? C13 C12 C14 116.8(12) . . ? C13 C12 C11 110.7(10) . . ? C14 C12 C11 109.6(8) . . ? C13 C12 C15 107.3(12) . . ? C14 C12 C15 105.2(10) . . ? C11 C12 C15 106.6(10) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O8 C16 O7 121.4(8) . . ? O8 C16 C17 117.1(8) . . ? O7 C16 C17 121.5(8) . . ? C18 C17 C19 113.1(11) . . ? C18 C17 C20 104.9(12) . . ? C19 C17 C20 109.8(11) . . ? C18 C17 C16 106.8(9) . . ? C19 C17 C16 111.4(9) . . ? C20 C17 C16 110.7(10) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 122.2(9) . . ? O9 C21 C22 120.2(9) . . ? O10 C21 C22 117.6(9) . . ? C25 C22 C21 112.6(9) . . ? C25 C22 C24 111.2(10) . . ? C21 C22 C24 106.9(9) . . ? C25 C22 C23 106.4(11) . . ? C21 C22 C23 109.4(9) . . ? C24 C22 C23 110.3(12) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 122.1(8) . . ? O11 C26 C27 119.7(9) . . ? O12 C26 C27 118.2(8) . . ? C28 C27 C30 117.8(11) . . ? C28 C27 C26 111.0(9) . . ? C30 C27 C26 116.3(9) . . ? C28 C27 C29 102.2(10) . . ? C30 C27 C29 102.5(10) . . ? C26 C27 C29 104.6(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O14 C31 O13 122.8(9) . . ? O14 C31 C32 119.6(9) . . ? O13 C31 C32 117.6(9) . . ? C34 C32 C31 108.0(9) . . ? C34 C32 C33 113.0(10) . . ? C31 C32 C33 111.7(9) . . ? C34 C32 C35 106.3(10) . . ? C31 C32 C35 107.8(9) . . ? C33 C32 C35 109.7(9) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 O15 123.4(8) . . ? O16 C36 C37 117.0(9) . . ? O15 C36 C37 119.6(8) . . ? C40 C37 C39 111.2(14) . . ? C40 C37 C38 109.9(14) . . ? C39 C37 C38 108.7(13) . . ? C40 C37 C36 109.8(10) . . ? C39 C37 C36 105.4(11) . . ? C38 C37 C36 111.8(9) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O17 C41 O18 120.3(12) . . ? O17 C41 C42 118.5(12) . . ? O18 C41 C42 121.1(11) . . ? C43 C42 C44 117.5(19) . . ? C43 C42 C41 110.9(16) . . ? C44 C42 C41 114.0(12) . . ? C43 C42 C45 99.8(16) . . ? C44 C42 C45 110.9(19) . . ? C41 C42 C45 101.6(14) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O19 C46 O20 124.3(10) . . ? O19 C46 C47B 114.5(12) . . ? O20 C46 C47B 117.2(12) . . ? O19 C46 C47 114.6(10) . . ? O20 C46 C47 119.9(9) . . ? C47B C46 C47 32.4(10) . . ? C50 C47 C49 114.0(17) . . ? C50 C47 C46 111.3(16) . . ? C49 C47 C46 102.4(13) . . ? C50 C47 C48 117.8(17) . . ? C49 C47 C48 105.5(16) . . ? C46 C47 C48 104.3(13) . . ? C50B C47B C46 118(2) . . ? C50B C47B C49B 113(2) . . ? C46 C47B C49B 95.0(19) . . ? C50B C47B C48B 124(3) . . ? C46 C47B C48B 100.1(19) . . ? C49B C47B C48B 101(2) . . ? O21 C51 O22 122.4(10) . . ? O21 C51 C52 120.0(11) . . ? O22 C51 C52 117.6(10) . . ? C51 C52 C55 112.4(13) . . ? C51 C52 C54 114.2(10) . . ? C55 C52 C54 108.4(14) . . ? C51 C52 C53 109.5(13) . . ? C55 C52 C53 104.1(13) . . ? C54 C52 C53 107.7(13) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O24 C56 O23 120.9(9) . . ? O24 C56 C57 120.2(9) . . ? O23 C56 C57 118.9(9) . . ? C60 C57 C59 118.1(12) . . ? C60 C57 C58 102.3(14) . . ? C59 C57 C58 104.1(13) . . ? C60 C57 C56 111.3(11) . . ? C59 C57 C56 115.1(10) . . ? C58 C57 C56 103.5(11) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N61 C61 W1 174.3(7) . . ? N62 C62 W1 178.4(8) . . ? N63 C63 W1 173.5(7) . . ? N64 C64 W1 178.8(8) . . ? N65 C65 W1 173.0(9) . . ? N66 C66 W1 178.3(10) . . ? N67 C67 W1 176.3(7) . . ? N68 C68 W1 175.1(10) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.963 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.112