# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Datong Song' _publ_contact_author_email DSONG@CHEM.UTORONTO.CA _publ_section_title ; Reversible H2 Splitting between Ru(II) and a Remote Carbanion in a Zwitterionic Compound ; loop_ _publ_author_name 'Datong Song.' 'Huiling Jiang.' 'Elzbieta Stepowska' # Attachment 'cif_revised.txt' data_2 _database_code_depnum_ccdc_archive 'CCDC 743623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H44 N4 P2 Ru' _chemical_formula_weight 899.93 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 18.4215(5) _cell_length_b 9.9438(2) _cell_length_c 25.1806(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.4570(10) _cell_angle_gamma 90.00 _cell_volume 4321.68(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68492 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8371 _exptl_absorpt_correction_T_max 0.9403 _exptl_absorpt_process_details 'Bruker Apex2' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68492 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9914 _reflns_number_gt 8445 _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^)+(0.0229P)^2^+2.7788P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9914 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Ru1 Ru 0.350490(7) 0.229909(12) 0.078779(5) 0.01616(4) Uani 1 1 d . . . P1 P 0.41644(2) 0.16102(4) 0.172112(17) 0.01717(9) Uani 1 1 d . . . P2 P 0.29986(2) 0.33752(4) -0.009739(17) 0.01661(9) Uani 1 1 d . . . N1 N 0.26419(8) 0.32617(14) 0.10258(6) 0.0216(3) Uani 1 1 d . . . N2 N 0.26025(8) 0.06214(14) 0.05582(6) 0.0205(3) Uani 1 1 d . . . N3 N 0.42544(8) 0.13580(15) 0.05485(6) 0.0233(3) Uani 1 1 d . . . N4 N 0.46802(9) 0.07999(17) 0.04107(7) 0.0337(4) Uani 1 1 d . . . C1 C 0.25637(12) 0.44614(18) 0.12437(7) 0.0311(4) Uani 1 1 d . . . H1A H 0.2976 0.5093 0.1333 0.037 Uiso 1 1 calc R . . C1S C 0.85892(13) 0.1431(2) 0.20718(9) 0.0428(5) Uani 1 1 d . . . H1SA H 0.8415 0.1112 0.2362 0.051 Uiso 1 1 calc R . . C2 C 0.18730(13) 0.4799(2) 0.13422(8) 0.0395(5) Uani 1 1 d . . . H2A H 0.1836 0.5659 0.1496 0.047 Uiso 1 1 calc R . . C2S C 0.86754(13) 0.2797(2) 0.20084(9) 0.0442(5) Uani 1 1 d . . . H2SA H 0.8558 0.3415 0.2255 0.053 Uiso 1 1 calc R . . C3 C 0.12528(13) 0.3930(2) 0.12243(8) 0.0381(5) Uani 1 1 d . . . H3A H 0.0799 0.4187 0.1296 0.046 Uiso 1 1 calc R . . C3S C 0.89317(11) 0.3265(2) 0.15876(8) 0.0354(5) Uani 1 1 d . . . H3SA H 0.8999 0.4202 0.1549 0.042 Uiso 1 1 calc R . . C4 C 0.13036(11) 0.2656(2) 0.09957(8) 0.0304(4) Uani 1 1 d . . . C4S C 0.90897(11) 0.2367(2) 0.12220(9) 0.0333(4) Uani 1 1 d . . . H4SA H 0.9257 0.2688 0.0929 0.040 Uiso 1 1 calc R . . C5 C 0.08421(11) 0.1486(2) 0.08149(8) 0.0362(5) Uani 1 1 d . . . H5A H 0.0335 0.1355 0.0822 0.043 Uiso 1 1 calc R . . C5S C 0.90032(12) 0.0999(2) 0.12848(9) 0.0363(5) Uani 1 1 d . . . H5SA H 0.9113 0.0382 0.1034 0.044 Uiso 1 1 calc R . . C6 C 0.12742(11) 0.0543(2) 0.06210(8) 0.0295(4) Uani 1 1 d . . . C6S C 0.87577(12) 0.0527(2) 0.17117(9) 0.0380(5) Uani 1 1 d . . . H6SA H 0.8705 -0.0412 0.1757 0.046 Uiso 1 1 calc R . . C7 C 0.11843(12) -0.0775(2) 0.04015(9) 0.0386(5) Uani 1 1 d . . . H7A H 0.0719 -0.1264 0.0342 0.046 Uiso 1 1 calc R . . C8 C 0.17883(13) -0.1335(2) 0.02758(8) 0.0382(5) Uani 1 1 d . . . H8A H 0.1735 -0.2227 0.0132 0.046 Uiso 1 1 calc R . . C9 C 0.24843(11) -0.06329(18) 0.03529(8) 0.0285(4) Uani 1 1 d . . . H9A H 0.2881 -0.1065 0.0256 0.034 Uiso 1 1 calc R . . C10 C 0.20093(10) 0.11473(17) 0.06866(7) 0.0210(3) Uani 1 1 d . . . C11 C 0.20278(10) 0.24270(17) 0.09132(7) 0.0219(3) Uani 1 1 d . . . C12 C 0.52162(10) 0.19498(16) 0.19971(7) 0.0212(3) Uani 1 1 d . . . C13 C 0.55711(11) 0.2725(2) 0.16970(8) 0.0328(4) Uani 1 1 d . . . H13A H 0.5271 0.3077 0.1336 0.039 Uiso 1 1 calc R . . C14 C 0.63636(12) 0.2988(2) 0.19220(9) 0.0422(5) Uani 1 1 d . . . H14A H 0.6599 0.3518 0.1713 0.051 Uiso 1 1 calc R . . C15 C 0.68089(11) 0.2487(2) 0.24451(9) 0.0368(5) Uani 1 1 d . . . H15A H 0.7348 0.2675 0.2597 0.044 Uiso 1 1 calc R . . C16 C 0.64652(11) 0.1710(2) 0.27461(9) 0.0362(5) Uani 1 1 d . . . H16A H 0.6770 0.1358 0.3106 0.043 Uiso 1 1 calc R . . C17 C 0.56758(11) 0.14413(19) 0.25249(8) 0.0298(4) Uani 1 1 d . . . H17A H 0.5445 0.0905 0.2735 0.036 Uiso 1 1 calc R . . C18 C 0.41492(9) -0.01930(16) 0.18815(7) 0.0196(3) Uani 1 1 d . . . C19 C 0.41744(11) -0.11122(17) 0.14692(8) 0.0264(4) Uani 1 1 d . . . H19A H 0.4172 -0.0794 0.1113 0.032 Uiso 1 1 calc R . . C20 C 0.42031(12) -0.24842(18) 0.15734(8) 0.0315(4) Uani 1 1 d . . . H20A H 0.4221 -0.3098 0.1289 0.038 Uiso 1 1 calc R . . C21 C 0.42056(11) -0.29636(18) 0.20907(8) 0.0310(4) Uani 1 1 d . . . H21A H 0.4228 -0.3904 0.2162 0.037 Uiso 1 1 calc R . . C22 C 0.41756(10) -0.20698(18) 0.25027(8) 0.0278(4) Uani 1 1 d . . . H22A H 0.4176 -0.2397 0.2857 0.033 Uiso 1 1 calc R . . C23 C 0.41455(10) -0.06927(17) 0.24006(7) 0.0242(4) Uani 1 1 d . . . H23A H 0.4122 -0.0086 0.2686 0.029 Uiso 1 1 calc R . . C24 C 0.38297(10) 0.24169(16) 0.22477(7) 0.0208(3) Uani 1 1 d . . . C25 C 0.42333(11) 0.34648(17) 0.25905(7) 0.0268(4) Uani 1 1 d . . . H25A H 0.4717 0.3747 0.2572 0.032 Uiso 1 1 calc R . . C26 C 0.39321(13) 0.4105(2) 0.29614(8) 0.0378(5) Uani 1 1 d . . . H26A H 0.4210 0.4820 0.3194 0.045 Uiso 1 1 calc R . . C27 C 0.32319(13) 0.3701(2) 0.29912(8) 0.0416(5) Uani 1 1 d . . . H27A H 0.3031 0.4131 0.3247 0.050 Uiso 1 1 calc R . . C28 C 0.28216(12) 0.2668(2) 0.26483(9) 0.0382(5) Uani 1 1 d . . . H28A H 0.2338 0.2395 0.2668 0.046 Uiso 1 1 calc R . . C29 C 0.31135(10) 0.20271(19) 0.22753(7) 0.0275(4) Uani 1 1 d . . . H29A H 0.2827 0.1324 0.2039 0.033 Uiso 1 1 calc R . . C30 C 0.19363(9) 0.34884(16) -0.03870(7) 0.0197(3) Uani 1 1 d . . . C31 C 0.14833(11) 0.25859(19) -0.07867(9) 0.0390(5) Uani 1 1 d . . . H31A H 0.1725 0.1928 -0.0942 0.047 Uiso 1 1 calc R . . C32 C 0.06797(13) 0.2636(2) -0.09613(12) 0.0552(7) Uani 1 1 d . . . H32A H 0.0378 0.2010 -0.1235 0.066 Uiso 1 1 calc R . . C33 C 0.03183(12) 0.3578(2) -0.07426(10) 0.0454(6) Uani 1 1 d . . . H33A H -0.0231 0.3603 -0.0862 0.054 Uiso 1 1 calc R . . C34 C 0.07569(11) 0.4490(2) -0.03484(9) 0.0355(5) Uani 1 1 d . . . H34A H 0.0509 0.5152 -0.0199 0.043 Uiso 1 1 calc R . . C35 C 0.15602(10) 0.44417(19) -0.01690(7) 0.0278(4) Uani 1 1 d . . . H35A H 0.1858 0.5067 0.0106 0.033 Uiso 1 1 calc R . . C36 C 0.33002(9) 0.51182(16) -0.01398(7) 0.0190(3) Uani 1 1 d . . . C37 C 0.28197(10) 0.60092(17) -0.05350(8) 0.0254(4) Uani 1 1 d . . . H37A H 0.2310 0.5737 -0.0759 0.031 Uiso 1 1 calc R . . C38 C 0.30748(11) 0.72882(18) -0.06060(8) 0.0287(4) Uani 1 1 d . . . H38A H 0.2738 0.7888 -0.0874 0.034 Uiso 1 1 calc R . . C39 C 0.38194(11) 0.76884(17) -0.02862(8) 0.0268(4) Uani 1 1 d . . . H39A H 0.3995 0.8563 -0.0334 0.032 Uiso 1 1 calc R . . C40 C 0.43054(11) 0.68102(19) 0.01021(8) 0.0303(4) Uani 1 1 d . . . H40A H 0.4819 0.7080 0.0318 0.036 Uiso 1 1 calc R . . C41 C 0.40483(10) 0.55313(18) 0.01792(7) 0.0261(4) Uani 1 1 d . . . H41A H 0.4385 0.4939 0.0450 0.031 Uiso 1 1 calc R . . C42 C 0.32611(10) 0.25983(16) -0.06706(7) 0.0200(3) Uani 1 1 d . . . C43 C 0.31576(11) 0.12154(18) -0.07680(7) 0.0273(4) Uani 1 1 d . . . H43A H 0.2928 0.0698 -0.0552 0.033 Uiso 1 1 calc R . . C44 C 0.33867(12) 0.05868(19) -0.11782(8) 0.0329(4) Uani 1 1 d . . . H44A H 0.3293 -0.0347 -0.1250 0.039 Uiso 1 1 calc R . . C45 C 0.37507(11) 0.1319(2) -0.14809(8) 0.0325(4) Uani 1 1 d . . . H45A H 0.3928 0.0882 -0.1748 0.039 Uiso 1 1 calc R . . C46 C 0.38550(11) 0.2685(2) -0.13928(8) 0.0320(4) Uani 1 1 d . . . H46A H 0.4098 0.3191 -0.1604 0.038 Uiso 1 1 calc R . . C47 C 0.36046(10) 0.33278(18) -0.09951(7) 0.0245(4) Uani 1 1 d . . . H47A H 0.3668 0.4273 -0.0944 0.029 Uiso 1 1 calc R . . H1 H 0.4037(12) 0.356(2) 0.0981(8) 0.037(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01549(7) 0.01842(6) 0.01433(7) 0.00126(5) 0.00490(5) 0.00075(5) P1 0.0161(2) 0.0202(2) 0.0148(2) 0.00130(15) 0.00486(16) 0.00021(15) P2 0.0162(2) 0.01826(19) 0.0152(2) 0.00079(15) 0.00534(16) 0.00072(15) N1 0.0262(8) 0.0232(7) 0.0138(7) 0.0014(5) 0.0052(6) 0.0058(6) N2 0.0210(7) 0.0238(7) 0.0167(7) 0.0013(5) 0.0065(6) 0.0014(6) N3 0.0201(8) 0.0289(7) 0.0199(7) 0.0035(6) 0.0057(6) -0.0010(6) N4 0.0286(9) 0.0419(9) 0.0337(9) 0.0008(7) 0.0148(8) 0.0033(7) C1 0.0411(12) 0.0268(9) 0.0204(9) -0.0012(7) 0.0044(8) 0.0083(8) C1S 0.0448(13) 0.0556(14) 0.0286(11) -0.0026(9) 0.0134(10) -0.0069(10) C2 0.0568(14) 0.0380(11) 0.0233(10) -0.0006(8) 0.0138(10) 0.0250(10) C2S 0.0475(14) 0.0504(13) 0.0313(11) -0.0160(10) 0.0098(10) 0.0001(11) C3 0.0415(12) 0.0538(13) 0.0252(10) 0.0107(9) 0.0195(9) 0.0256(10) C3S 0.0289(11) 0.0330(10) 0.0341(11) -0.0069(8) -0.0019(9) -0.0018(8) C4 0.0289(10) 0.0465(11) 0.0202(9) 0.0119(8) 0.0143(8) 0.0156(8) C4S 0.0246(10) 0.0393(11) 0.0358(11) 0.0015(8) 0.0103(8) 0.0014(8) C5 0.0220(10) 0.0567(13) 0.0351(11) 0.0141(9) 0.0163(9) 0.0042(9) C5S 0.0357(11) 0.0357(10) 0.0389(11) -0.0038(9) 0.0149(9) 0.0067(9) C6 0.0227(9) 0.0425(11) 0.0228(9) 0.0100(8) 0.0073(8) -0.0032(8) C6S 0.0392(12) 0.0349(11) 0.0368(11) -0.0006(9) 0.0094(9) -0.0043(9) C7 0.0312(11) 0.0441(12) 0.0356(11) 0.0048(9) 0.0057(9) -0.0163(9) C8 0.0482(13) 0.0305(10) 0.0326(11) -0.0043(8) 0.0100(10) -0.0121(9) C9 0.0356(11) 0.0257(9) 0.0244(9) -0.0017(7) 0.0108(8) 0.0007(8) C10 0.0206(9) 0.0271(8) 0.0158(8) 0.0045(6) 0.0068(7) 0.0009(7) C11 0.0219(9) 0.0296(9) 0.0154(8) 0.0060(6) 0.0082(7) 0.0066(7) C12 0.0178(8) 0.0231(8) 0.0219(8) -0.0027(6) 0.0057(7) -0.0008(6) C13 0.0245(10) 0.0477(11) 0.0239(9) 0.0035(8) 0.0055(8) -0.0070(8) C14 0.0277(11) 0.0641(15) 0.0350(11) -0.0009(10) 0.0113(9) -0.0155(10) C15 0.0170(9) 0.0521(13) 0.0374(11) -0.0118(9) 0.0047(8) -0.0057(8) C16 0.0225(10) 0.0425(11) 0.0347(11) 0.0011(9) -0.0010(8) 0.0038(8) C17 0.0230(10) 0.0326(10) 0.0290(10) 0.0062(8) 0.0030(8) -0.0005(7) C18 0.0152(8) 0.0221(8) 0.0204(8) 0.0028(6) 0.0048(7) 0.0009(6) C19 0.0305(10) 0.0267(9) 0.0239(9) 0.0031(7) 0.0121(8) 0.0016(7) C20 0.0379(11) 0.0248(9) 0.0330(10) -0.0020(7) 0.0141(9) 0.0013(8) C21 0.0285(10) 0.0232(9) 0.0397(11) 0.0078(8) 0.0100(8) 0.0009(7) C22 0.0249(10) 0.0307(9) 0.0266(9) 0.0101(7) 0.0074(8) -0.0012(7) C23 0.0234(9) 0.0279(9) 0.0213(9) 0.0031(7) 0.0077(7) -0.0008(7) C24 0.0227(9) 0.0252(8) 0.0138(8) 0.0037(6) 0.0055(7) 0.0066(7) C25 0.0304(10) 0.0259(9) 0.0212(9) 0.0020(7) 0.0051(8) 0.0060(7) C26 0.0507(13) 0.0338(10) 0.0232(10) -0.0039(8) 0.0060(9) 0.0156(9) C27 0.0529(14) 0.0504(13) 0.0242(10) 0.0050(9) 0.0170(10) 0.0292(11) C28 0.0325(11) 0.0550(13) 0.0326(11) 0.0134(9) 0.0184(9) 0.0185(10) C29 0.0232(9) 0.0372(10) 0.0225(9) 0.0045(7) 0.0087(7) 0.0038(8) C30 0.0166(8) 0.0228(8) 0.0179(8) 0.0058(6) 0.0035(6) 0.0004(6) C31 0.0246(10) 0.0301(10) 0.0497(13) -0.0099(9) -0.0027(9) 0.0017(8) C32 0.0264(12) 0.0363(12) 0.0797(18) -0.0069(11) -0.0107(11) -0.0047(9) C33 0.0176(10) 0.0423(12) 0.0683(16) 0.0214(11) 0.0051(10) -0.0001(9) C34 0.0255(10) 0.0495(12) 0.0364(11) 0.0150(9) 0.0171(9) 0.0110(9) C35 0.0229(9) 0.0393(10) 0.0216(9) 0.0021(7) 0.0082(7) 0.0039(8) C36 0.0199(8) 0.0196(8) 0.0190(8) 0.0003(6) 0.0086(7) -0.0002(6) C37 0.0180(9) 0.0255(9) 0.0298(10) 0.0046(7) 0.0046(7) -0.0002(7) C38 0.0236(9) 0.0237(8) 0.0373(10) 0.0076(8) 0.0088(8) 0.0035(7) C39 0.0285(10) 0.0217(8) 0.0329(10) 0.0009(7) 0.0139(8) -0.0031(7) C40 0.0234(10) 0.0340(10) 0.0285(10) 0.0018(8) 0.0028(8) -0.0088(8) C41 0.0229(9) 0.0287(9) 0.0230(9) 0.0058(7) 0.0033(7) -0.0011(7) C42 0.0180(8) 0.0267(8) 0.0142(8) 0.0027(6) 0.0042(6) 0.0054(6) C43 0.0366(11) 0.0263(9) 0.0203(9) 0.0021(7) 0.0117(8) 0.0048(8) C44 0.0453(12) 0.0297(10) 0.0221(9) -0.0013(7) 0.0100(9) 0.0107(8) C45 0.0317(11) 0.0482(12) 0.0178(9) -0.0020(8) 0.0089(8) 0.0165(9) C46 0.0280(10) 0.0496(12) 0.0204(9) 0.0045(8) 0.0112(8) 0.0036(9) C47 0.0219(9) 0.0320(9) 0.0194(8) 0.0014(7) 0.0071(7) 0.0012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 1.9305(15) . ? Ru1 N1 2.1139(14) . ? Ru1 N2 2.2823(14) . ? Ru1 P1 2.3394(4) . ? Ru1 P2 2.3516(4) . ? P1 C24 1.8311(17) . ? P1 C18 1.8403(16) . ? P1 C12 1.8467(17) . ? P2 C36 1.8345(16) . ? P2 C30 1.8376(17) . ? P2 C42 1.8445(17) . ? N1 C1 1.342(2) . ? N1 C11 1.351(2) . ? N2 C9 1.339(2) . ? N2 C10 1.349(2) . ? N3 N4 1.111(2) . ? C1 C2 1.419(3) . ? C1S C2S 1.383(3) . ? C1S C6S 1.387(3) . ? C2 C3 1.380(3) . ? C2S C3S 1.383(3) . ? C3 C4 1.408(3) . ? C3S C4S 1.385(3) . ? C4 C5 1.419(3) . ? C4 C11 1.438(2) . ? C4S C5S 1.385(3) . ? C5 C6 1.422(3) . ? C5S C6S 1.386(3) . ? C6 C7 1.409(3) . ? C6 C10 1.437(2) . ? C7 C8 1.376(3) . ? C8 C9 1.412(3) . ? C10 C11 1.390(2) . ? C12 C13 1.392(2) . ? C12 C17 1.397(2) . ? C13 C14 1.394(3) . ? C14 C15 1.379(3) . ? C15 C16 1.381(3) . ? C16 C17 1.389(3) . ? C18 C19 1.396(2) . ? C18 C23 1.401(2) . ? C19 C20 1.387(2) . ? C20 C21 1.385(3) . ? C21 C22 1.382(3) . ? C22 C23 1.391(2) . ? C24 C25 1.391(2) . ? C24 C29 1.400(2) . ? C25 C26 1.395(3) . ? C26 C27 1.378(3) . ? C27 C28 1.384(3) . ? C28 C29 1.389(3) . ? C30 C31 1.388(2) . ? C30 C35 1.395(2) . ? C31 C32 1.390(3) . ? C32 C33 1.372(3) . ? C33 C34 1.378(3) . ? C34 C35 1.389(3) . ? C36 C41 1.393(2) . ? C36 C37 1.394(2) . ? C37 C38 1.389(2) . ? C38 C39 1.384(3) . ? C39 C40 1.381(3) . ? C40 C41 1.394(2) . ? C42 C43 1.398(2) . ? C42 C47 1.398(2) . ? C43 C44 1.393(2) . ? C44 C45 1.385(3) . ? C45 C46 1.379(3) . ? C46 C47 1.395(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 N1 177.16(6) . . ? N3 Ru1 N2 95.95(5) . . ? N1 Ru1 N2 81.34(5) . . ? N3 Ru1 P1 89.69(4) . . ? N1 Ru1 P1 91.47(4) . . ? N2 Ru1 P1 96.72(3) . . ? N3 Ru1 P2 90.85(4) . . ? N1 Ru1 P2 88.52(4) . . ? N2 Ru1 P2 94.59(4) . . ? P1 Ru1 P2 168.561(15) . . ? C24 P1 C18 103.48(7) . . ? C24 P1 C12 102.83(8) . . ? C18 P1 C12 100.95(7) . . ? C24 P1 Ru1 114.28(5) . . ? C18 P1 Ru1 117.60(5) . . ? C12 P1 Ru1 115.63(6) . . ? C36 P2 C30 102.78(7) . . ? C36 P2 C42 100.52(7) . . ? C30 P2 C42 104.43(7) . . ? C36 P2 Ru1 117.21(5) . . ? C30 P2 Ru1 114.75(5) . . ? C42 P2 Ru1 115.19(5) . . ? C1 N1 C11 115.48(16) . . ? C1 N1 Ru1 135.84(13) . . ? C11 N1 Ru1 108.66(11) . . ? C9 N2 C10 114.70(15) . . ? C9 N2 Ru1 141.70(12) . . ? C10 N2 Ru1 103.60(10) . . ? N4 N3 Ru1 179.01(15) . . ? N1 C1 C2 120.87(19) . . ? C2S C1S C6S 120.0(2) . . ? C3 C2 C1 122.65(18) . . ? C3S C2S C1S 120.2(2) . . ? C2 C3 C4 118.91(18) . . ? C2S C3S C4S 120.0(2) . . ? C3 C4 C5 138.67(18) . . ? C3 C4 C11 113.51(18) . . ? C5 C4 C11 107.82(16) . . ? C3S C4S C5S 119.9(2) . . ? C4 C5 C6 107.83(16) . . ? C4S C5S C6S 120.18(19) . . ? C7 C6 C5 138.11(18) . . ? C7 C6 C10 114.25(17) . . ? C5 C6 C10 107.63(17) . . ? C5S C6S C1S 119.8(2) . . ? C8 C7 C6 118.21(18) . . ? C7 C8 C9 122.46(18) . . ? N2 C9 C8 122.06(18) . . ? N2 C10 C11 123.21(15) . . ? N2 C10 C6 128.32(16) . . ? C11 C10 C6 108.47(15) . . ? N1 C11 C10 123.16(15) . . ? N1 C11 C4 128.58(16) . . ? C10 C11 C4 108.26(16) . . ? C13 C12 C17 118.25(16) . . ? C13 C12 P1 121.81(13) . . ? C17 C12 P1 119.93(13) . . ? C12 C13 C14 120.49(18) . . ? C15 C14 C13 120.60(19) . . ? C14 C15 C16 119.52(18) . . ? C15 C16 C17 120.27(18) . . ? C16 C17 C12 120.86(18) . . ? C19 C18 C23 118.29(15) . . ? C19 C18 P1 117.88(12) . . ? C23 C18 P1 123.77(13) . . ? C20 C19 C18 120.81(17) . . ? C21 C20 C19 120.26(18) . . ? C22 C21 C20 119.78(17) . . ? C21 C22 C23 120.26(17) . . ? C22 C23 C18 120.59(17) . . ? C25 C24 C29 119.02(16) . . ? C25 C24 P1 122.37(14) . . ? C29 C24 P1 118.45(13) . . ? C24 C25 C26 120.37(19) . . ? C27 C26 C25 120.16(19) . . ? C26 C27 C28 120.00(18) . . ? C27 C28 C29 120.4(2) . . ? C28 C29 C24 120.05(18) . . ? C31 C30 C35 117.99(16) . . ? C31 C30 P2 122.34(14) . . ? C35 C30 P2 119.47(13) . . ? C30 C31 C32 120.7(2) . . ? C33 C32 C31 120.7(2) . . ? C32 C33 C34 119.60(19) . . ? C33 C34 C35 120.12(19) . . ? C34 C35 C30 120.96(18) . . ? C41 C36 C37 118.54(15) . . ? C41 C36 P2 120.26(12) . . ? C37 C36 P2 120.82(13) . . ? C38 C37 C36 120.98(16) . . ? C39 C38 C37 119.97(17) . . ? C40 C39 C38 119.69(16) . . ? C39 C40 C41 120.50(17) . . ? C36 C41 C40 120.31(16) . . ? C43 C42 C47 118.01(16) . . ? C43 C42 P2 119.48(13) . . ? C47 C42 P2 122.40(13) . . ? C44 C43 C42 120.88(17) . . ? C45 C44 C43 120.18(18) . . ? C46 C45 C44 119.76(17) . . ? C45 C46 C47 120.27(18) . . ? C46 C47 C42 120.83(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.384 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.054 #===>END data_3 _database_code_depnum_ccdc_archive 'CCDC 743624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H40 N2 P2 Ru' _chemical_formula_weight 795.82 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 13.8338(4) _cell_length_b 17.7363(6) _cell_length_c 15.9357(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.9974(16) _cell_angle_gamma 90.00 _cell_volume 3758.57(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25385 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25385 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8519 _reflns_number_gt 6283 _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^)+(0.0300P)^2^+3.6170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8519 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ru1 Ru 0.847265(15) 0.215306(12) 0.850831(13) 0.02240(7) Uani 1 1 d . . . P1 P 0.74777(5) 0.23004(4) 0.94366(4) 0.02340(15) Uani 1 1 d . . . P2 P 0.97022(5) 0.23541(4) 0.78500(4) 0.02359(15) Uani 1 1 d . . . N1 N 0.71661(16) 0.19579(13) 0.73791(13) 0.0263(5) Uani 1 1 d . . . N2 N 0.84044(16) 0.09040(13) 0.85215(14) 0.0276(5) Uani 1 1 d . . . C1 C 0.6491(2) 0.23719(19) 0.67768(19) 0.0373(7) Uani 1 1 d . . . H1A H 0.6579 0.2903 0.6772 0.045 Uiso 1 1 calc R . . C2 C 0.5677(2) 0.2055(2) 0.61664(19) 0.0439(8) Uani 1 1 d . . . H2A H 0.5240 0.2372 0.5749 0.053 Uiso 1 1 calc R . . C3 C 0.5485(2) 0.1287(2) 0.61493(19) 0.0434(8) Uani 1 1 d . . . H3A H 0.4915 0.1074 0.5743 0.052 Uiso 1 1 calc R . . C4 C 0.6160(2) 0.08464(18) 0.67480(18) 0.0357(7) Uani 1 1 d . . . C5 C 0.6234(2) 0.00168(19) 0.6974(2) 0.0448(8) Uani 1 1 d . . . H5A H 0.6295 -0.0291 0.6474 0.054 Uiso 1 1 calc R . . H5B H 0.5639 -0.0154 0.7154 0.054 Uiso 1 1 calc R . . C6 C 0.7180(2) -0.00320(17) 0.7727(2) 0.0380(7) Uani 1 1 d . . . C7 C 0.7674(3) -0.06072(19) 0.8249(2) 0.0502(9) Uani 1 1 d . . . H7A H 0.7428 -0.1110 0.8179 0.060 Uiso 1 1 calc R . . C8 C 0.8551(3) -0.04177(19) 0.8885(2) 0.0465(8) Uani 1 1 d . . . H8A H 0.8925 -0.0802 0.9248 0.056 Uiso 1 1 calc R . . C9 C 0.8892(2) 0.03207(17) 0.89998(19) 0.0365(7) Uani 1 1 d . . . H9A H 0.9500 0.0421 0.9438 0.044 Uiso 1 1 calc R . . C10 C 0.7577(2) 0.06865(16) 0.78994(17) 0.0286(6) Uani 1 1 d . . . C11 C 0.6964(2) 0.12189(16) 0.73207(17) 0.0283(6) Uani 1 1 d . . . C12 C 0.6723(2) 0.31644(16) 0.93790(17) 0.0307(6) Uani 1 1 d . . . C13 C 0.6972(3) 0.38057(19) 0.8991(3) 0.0593(11) Uani 1 1 d . . . H13A H 0.7538 0.3796 0.8763 0.071 Uiso 1 1 calc R . . C14 C 0.6412(4) 0.4465(2) 0.8928(3) 0.0835(16) Uani 1 1 d . . . H14A H 0.6600 0.4898 0.8659 0.100 Uiso 1 1 calc R . . C15 C 0.5597(3) 0.4493(2) 0.9247(2) 0.0618(11) Uani 1 1 d . . . H15A H 0.5218 0.4945 0.9208 0.074 Uiso 1 1 calc R . . C16 C 0.5325(2) 0.38593(18) 0.9630(2) 0.0419(8) Uani 1 1 d . . . H16A H 0.4754 0.3874 0.9851 0.050 Uiso 1 1 calc R . . C17 C 0.5879(2) 0.32025(17) 0.96958(17) 0.0314(6) Uani 1 1 d . . . H17A H 0.5681 0.2771 0.9960 0.038 Uiso 1 1 calc R . . C18 C 0.64842(19) 0.15742(15) 0.92747(17) 0.0251(6) Uani 1 1 d . . . C19 C 0.6614(2) 0.09121(18) 0.9754(2) 0.0440(8) Uani 1 1 d . . . H19A H 0.7177 0.0860 1.0250 0.053 Uiso 1 1 calc R . . C20 C 0.5935(3) 0.0326(2) 0.9521(3) 0.0653(12) Uani 1 1 d . . . H20A H 0.6039 -0.0123 0.9859 0.078 Uiso 1 1 calc R . . C21 C 0.5113(2) 0.0384(2) 0.8809(3) 0.0559(10) Uani 1 1 d . . . H21A H 0.4651 -0.0022 0.8650 0.067 Uiso 1 1 calc R . . C22 C 0.4966(2) 0.10362(19) 0.8330(2) 0.0420(8) Uani 1 1 d . . . H22A H 0.4395 0.1084 0.7838 0.050 Uiso 1 1 calc R . . C23 C 0.5644(2) 0.16277(17) 0.85557(17) 0.0317(6) Uani 1 1 d . . . H23A H 0.5533 0.2075 0.8216 0.038 Uiso 1 1 calc R . . C24 C 0.8082(2) 0.21956(18) 1.06197(17) 0.0332(7) Uani 1 1 d . . . C25 C 0.7871(2) 0.2650(2) 1.12558(19) 0.0433(8) Uani 1 1 d . . . H25A H 0.7413 0.3058 1.1092 0.052 Uiso 1 1 calc R . . C26 C 0.8336(3) 0.2506(3) 1.2138(2) 0.0593(11) Uani 1 1 d . . . H26A H 0.8199 0.2823 1.2572 0.071 Uiso 1 1 calc R . . C27 C 0.8989(3) 0.1911(3) 1.2382(2) 0.0655(13) Uani 1 1 d . . . H27A H 0.9287 0.1810 1.2984 0.079 Uiso 1 1 calc R . . C28 C 0.9213(2) 0.1462(2) 1.1761(2) 0.0569(11) Uani 1 1 d . . . H28A H 0.9669 0.1053 1.1931 0.068 Uiso 1 1 calc R . . C29 C 0.8771(2) 0.1606(2) 1.08781(19) 0.0412(8) Uani 1 1 d . . . H29A H 0.8940 0.1302 1.0449 0.049 Uiso 1 1 calc R . . C30 C 0.9269(2) 0.25088(17) 0.66626(17) 0.0306(6) Uani 1 1 d . . . C31 C 0.8659(2) 0.1947(2) 0.6183(2) 0.0478(9) Uani 1 1 d . . . H31A H 0.8534 0.1504 0.6472 0.057 Uiso 1 1 calc R . . C32 C 0.8230(3) 0.2021(3) 0.5290(2) 0.0625(12) Uani 1 1 d . . . H32A H 0.7803 0.1636 0.4976 0.075 Uiso 1 1 calc R . . C33 C 0.8422(3) 0.2648(3) 0.4861(2) 0.0650(12) Uani 1 1 d . . . H33A H 0.8134 0.2697 0.4249 0.078 Uiso 1 1 calc R . . C34 C 0.9032(4) 0.3204(2) 0.5319(2) 0.0687(13) Uani 1 1 d . . . H34A H 0.9179 0.3634 0.5020 0.082 Uiso 1 1 calc R . . C35 C 0.9440(3) 0.3144(2) 0.6218(2) 0.0495(9) Uani 1 1 d . . . H35A H 0.9839 0.3543 0.6531 0.059 Uiso 1 1 calc R . . C36 C 1.06444(19) 0.16014(15) 0.79315(17) 0.0264(6) Uani 1 1 d . . . C37 C 1.0953(3) 0.13210(19) 0.7240(2) 0.0460(8) Uani 1 1 d . . . H37A H 1.0676 0.1521 0.6671 0.055 Uiso 1 1 calc R . . C38 C 1.1669(3) 0.0746(2) 0.7368(2) 0.0593(10) Uani 1 1 d . . . H38A H 1.1876 0.0561 0.6886 0.071 Uiso 1 1 calc R . . C39 C 1.2074(2) 0.04465(18) 0.8180(2) 0.0447(8) Uani 1 1 d . . . H39A H 1.2550 0.0048 0.8260 0.054 Uiso 1 1 calc R . . C40 C 1.1787(2) 0.07259(19) 0.8876(2) 0.0458(8) Uani 1 1 d . . . H40A H 1.2075 0.0528 0.9444 0.055 Uiso 1 1 calc R . . C41 C 1.1076(2) 0.12970(18) 0.87528(19) 0.0383(7) Uani 1 1 d . . . H41A H 1.0881 0.1484 0.9240 0.046 Uiso 1 1 calc R . . C42 C 1.0561(2) 0.31591(16) 0.82333(17) 0.0271(6) Uani 1 1 d . . . C43 C 1.1358(2) 0.33139(18) 0.7879(2) 0.0393(7) Uani 1 1 d . . . H43A H 1.1480 0.2990 0.7444 0.047 Uiso 1 1 calc R . . C44 C 1.1973(3) 0.39348(19) 0.8154(2) 0.0479(8) Uani 1 1 d . . . H44A H 1.2501 0.4039 0.7896 0.057 Uiso 1 1 calc R . . C45 C 1.1825(2) 0.44027(18) 0.8797(2) 0.0446(8) Uani 1 1 d . . . H45A H 1.2239 0.4833 0.8977 0.053 Uiso 1 1 calc R . . C46 C 1.1070(2) 0.42382(17) 0.9175(2) 0.0368(7) Uani 1 1 d . . . H46A H 1.0978 0.4548 0.9633 0.044 Uiso 1 1 calc R . . C47 C 1.0441(2) 0.36250(16) 0.88969(18) 0.0303(6) Uani 1 1 d . . . H47A H 0.9921 0.3523 0.9164 0.036 Uiso 1 1 calc R . . H2 H 0.941(2) 0.2188(17) 0.932(2) 0.049(9) Uiso 1 1 d . . . H1 H 0.846(2) 0.3084(18) 0.8438(18) 0.043(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02169(11) 0.02290(12) 0.02375(11) 0.00091(9) 0.00818(8) -0.00066(9) P1 0.0232(3) 0.0264(4) 0.0219(3) 0.0007(3) 0.0083(3) -0.0032(3) P2 0.0243(3) 0.0235(4) 0.0249(3) 0.0020(3) 0.0099(3) 0.0013(3) N1 0.0257(12) 0.0314(13) 0.0237(11) 0.0020(10) 0.0098(9) 0.0033(10) N2 0.0261(12) 0.0241(12) 0.0321(12) 0.0025(10) 0.0076(10) 0.0014(10) C1 0.0353(17) 0.0434(19) 0.0331(15) 0.0077(14) 0.0093(13) 0.0062(14) C2 0.0363(17) 0.061(2) 0.0297(15) 0.0044(15) 0.0015(13) 0.0116(16) C3 0.0312(16) 0.062(2) 0.0317(16) -0.0123(15) 0.0001(13) 0.0056(16) C4 0.0301(15) 0.0434(19) 0.0331(15) -0.0129(14) 0.0081(13) 0.0008(14) C5 0.0339(17) 0.0396(19) 0.058(2) -0.0230(16) 0.0080(15) -0.0034(14) C6 0.0335(16) 0.0291(17) 0.0513(18) -0.0096(14) 0.0117(14) 0.0005(13) C7 0.047(2) 0.0265(18) 0.077(2) -0.0041(17) 0.0166(18) -0.0003(15) C8 0.0450(19) 0.0317(18) 0.060(2) 0.0092(16) 0.0102(16) 0.0073(15) C9 0.0319(15) 0.0325(17) 0.0412(17) 0.0045(14) 0.0036(13) 0.0032(13) C10 0.0274(14) 0.0272(16) 0.0324(14) -0.0036(12) 0.0104(12) 0.0016(12) C11 0.0268(14) 0.0327(16) 0.0266(13) -0.0059(12) 0.0092(11) 0.0033(12) C12 0.0409(17) 0.0269(15) 0.0278(14) -0.0036(12) 0.0156(12) -0.0019(13) C13 0.085(3) 0.0295(19) 0.091(3) 0.0039(18) 0.070(2) 0.0072(19) C14 0.140(4) 0.031(2) 0.122(4) 0.017(2) 0.108(4) 0.022(2) C15 0.097(3) 0.034(2) 0.075(3) 0.0037(18) 0.058(2) 0.025(2) C16 0.0479(19) 0.0398(19) 0.0457(18) -0.0070(15) 0.0261(15) 0.0071(16) C17 0.0370(16) 0.0315(16) 0.0289(14) -0.0024(12) 0.0146(12) -0.0025(13) C18 0.0221(13) 0.0233(14) 0.0333(14) -0.0010(12) 0.0132(11) 0.0010(11) C19 0.0273(16) 0.0360(19) 0.065(2) 0.0154(16) 0.0064(15) -0.0021(14) C20 0.0378(19) 0.034(2) 0.122(4) 0.027(2) 0.018(2) -0.0031(16) C21 0.0333(18) 0.032(2) 0.102(3) -0.006(2) 0.0183(19) -0.0082(15) C22 0.0272(16) 0.051(2) 0.0474(18) -0.0122(16) 0.0102(14) -0.0070(15) C23 0.0297(15) 0.0366(17) 0.0300(14) -0.0011(13) 0.0101(12) -0.0038(13) C24 0.0270(14) 0.0478(19) 0.0248(13) 0.0023(13) 0.0070(11) -0.0122(14) C25 0.0346(17) 0.066(2) 0.0284(15) -0.0072(15) 0.0069(13) -0.0152(16) C26 0.047(2) 0.104(3) 0.0271(16) -0.0087(19) 0.0108(15) -0.027(2) C27 0.049(2) 0.113(4) 0.0266(17) 0.015(2) -0.0034(16) -0.033(2) C28 0.0346(18) 0.086(3) 0.044(2) 0.027(2) -0.0005(15) -0.0124(19) C29 0.0315(16) 0.056(2) 0.0328(16) 0.0141(15) 0.0038(13) -0.0048(15) C30 0.0280(15) 0.0387(17) 0.0279(14) -0.0014(13) 0.0122(12) 0.0076(13) C31 0.0417(18) 0.074(3) 0.0327(16) -0.0075(16) 0.0191(14) -0.0171(18) C32 0.0376(19) 0.114(4) 0.0375(19) -0.025(2) 0.0130(15) -0.010(2) C33 0.069(3) 0.095(3) 0.0273(17) 0.000(2) 0.0083(17) 0.037(3) C34 0.117(4) 0.053(2) 0.0369(19) 0.0115(18) 0.021(2) 0.036(3) C35 0.082(3) 0.0356(19) 0.0297(16) 0.0040(14) 0.0141(17) 0.0163(18) C36 0.0246(14) 0.0237(14) 0.0330(14) 0.0008(12) 0.0116(11) -0.0003(11) C37 0.057(2) 0.044(2) 0.0409(17) 0.0049(15) 0.0214(16) 0.0192(17) C38 0.072(3) 0.054(2) 0.061(2) -0.0031(19) 0.034(2) 0.026(2) C39 0.0379(18) 0.0301(18) 0.066(2) 0.0013(16) 0.0150(16) 0.0119(14) C40 0.0373(18) 0.049(2) 0.0477(19) 0.0086(16) 0.0062(15) 0.0139(16) C41 0.0320(16) 0.0452(19) 0.0366(16) 0.0006(14) 0.0078(13) 0.0132(14) C42 0.0244(14) 0.0247(15) 0.0329(14) 0.0053(12) 0.0090(11) 0.0000(11) C43 0.0400(17) 0.0355(18) 0.0500(18) 0.0007(14) 0.0249(15) -0.0021(14) C44 0.0436(19) 0.042(2) 0.066(2) 0.0080(17) 0.0275(17) -0.0103(16) C45 0.0423(19) 0.0316(18) 0.059(2) 0.0012(16) 0.0131(16) -0.0135(15) C46 0.0362(17) 0.0279(16) 0.0439(17) -0.0002(14) 0.0071(14) -0.0012(13) C47 0.0272(14) 0.0286(16) 0.0346(15) 0.0045(12) 0.0078(12) 0.0004(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.198(2) . ? Ru1 N2 2.218(2) . ? Ru1 P2 2.2593(7) . ? Ru1 P1 2.2964(7) . ? Ru1 H2 1.56(3) . ? Ru1 H1 1.66(3) . ? P1 C12 1.842(3) . ? P1 C24 1.849(3) . ? P1 C18 1.849(3) . ? P2 C30 1.841(3) . ? P2 C36 1.845(3) . ? P2 C42 1.850(3) . ? N1 C11 1.338(4) . ? N1 C1 1.356(4) . ? N2 C10 1.348(3) . ? N2 C9 1.350(4) . ? C1 C2 1.388(4) . ? C1 H1A 0.9500 . ? C2 C3 1.387(5) . ? C2 H2A 0.9500 . ? C3 C4 1.378(4) . ? C3 H3A 0.9500 . ? C4 C11 1.396(4) . ? C4 C5 1.512(5) . ? C5 C6 1.515(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.373(4) . ? C6 C10 1.385(4) . ? C7 C8 1.391(5) . ? C7 H7A 0.9500 . ? C8 C9 1.387(4) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.424(4) . ? C12 C13 1.383(4) . ? C12 C17 1.396(4) . ? C13 C14 1.391(5) . ? C13 H13A 0.9500 . ? C14 C15 1.360(5) . ? C14 H14A 0.9500 . ? C15 C16 1.380(5) . ? C15 H15A 0.9500 . ? C16 C17 1.382(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.385(4) . ? C18 C23 1.393(4) . ? C19 C20 1.381(5) . ? C19 H19A 0.9500 . ? C20 C21 1.372(5) . ? C20 H20A 0.9500 . ? C21 C22 1.370(5) . ? C21 H21A 0.9500 . ? C22 C23 1.387(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.387(4) . ? C24 C29 1.398(4) . ? C25 C26 1.399(4) . ? C25 H25A 0.9500 . ? C26 C27 1.375(6) . ? C26 H26A 0.9500 . ? C27 C28 1.371(6) . ? C27 H27A 0.9500 . ? C28 C29 1.394(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.386(4) . ? C30 C31 1.390(4) . ? C31 C32 1.389(5) . ? C31 H31A 0.9500 . ? C32 C33 1.370(6) . ? C32 H32A 0.9500 . ? C33 C34 1.370(6) . ? C33 H33A 0.9500 . ? C34 C35 1.393(5) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.380(4) . ? C36 C41 1.389(4) . ? C37 C38 1.396(5) . ? C37 H37A 0.9500 . ? C38 C39 1.367(5) . ? C38 H38A 0.9500 . ? C39 C40 1.370(5) . ? C39 H39A 0.9500 . ? C40 C41 1.387(4) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C47 1.388(4) . ? C42 C43 1.398(4) . ? C43 C44 1.387(4) . ? C43 H43A 0.9500 . ? C44 C45 1.377(5) . ? C44 H44A 0.9500 . ? C45 C46 1.373(4) . ? C45 H45A 0.9500 . ? C46 C47 1.387(4) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N2 79.80(8) . . ? N1 Ru1 P2 101.49(6) . . ? N2 Ru1 P2 101.62(6) . . ? N1 Ru1 P1 92.39(6) . . ? N2 Ru1 P1 94.19(6) . . ? P2 Ru1 P1 160.52(3) . . ? N1 Ru1 H2 173.2(11) . . ? N2 Ru1 H2 93.4(11) . . ? P2 Ru1 H2 79.9(12) . . ? P1 Ru1 H2 88.0(11) . . ? N1 Ru1 H1 96.3(10) . . ? N2 Ru1 H1 176.1(10) . . ? P2 Ru1 H1 78.9(10) . . ? P1 Ru1 H1 86.1(10) . . ? H2 Ru1 H1 90.5(15) . . ? C12 P1 C24 103.02(13) . . ? C12 P1 C18 100.55(13) . . ? C24 P1 C18 100.48(12) . . ? C12 P1 Ru1 119.65(9) . . ? C24 P1 Ru1 117.55(10) . . ? C18 P1 Ru1 112.66(8) . . ? C30 P2 C36 101.76(12) . . ? C30 P2 C42 102.82(13) . . ? C36 P2 C42 99.10(12) . . ? C30 P2 Ru1 115.29(9) . . ? C36 P2 Ru1 117.43(9) . . ? C42 P2 Ru1 117.75(9) . . ? C11 N1 C1 113.0(2) . . ? C11 N1 Ru1 108.66(17) . . ? C1 N1 Ru1 138.1(2) . . ? C10 N2 C9 112.8(2) . . ? C10 N2 Ru1 107.98(17) . . ? C9 N2 Ru1 139.01(19) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 121.7(3) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C4 C3 C2 117.0(3) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? C3 C4 C11 116.7(3) . . ? C3 C4 C5 134.8(3) . . ? C11 C4 C5 108.4(3) . . ? C4 C5 C6 103.4(2) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C10 117.4(3) . . ? C7 C6 C5 134.3(3) . . ? C10 C6 C5 108.2(3) . . ? C6 C7 C8 116.7(3) . . ? C6 C7 H7A 121.6 . . ? C8 C7 H7A 121.6 . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? N2 C9 C8 123.4(3) . . ? N2 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? N2 C10 C6 128.2(3) . . ? N2 C10 C11 121.3(3) . . ? C6 C10 C11 110.5(2) . . ? N1 C11 C4 128.5(3) . . ? N1 C11 C10 121.9(2) . . ? C4 C11 C10 109.5(3) . . ? C13 C12 C17 117.3(3) . . ? C13 C12 P1 119.9(2) . . ? C17 C12 P1 122.8(2) . . ? C12 C13 C14 121.4(3) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C16 C17 C12 121.0(3) . . ? C16 C17 H17A 119.5 . . ? C12 C17 H17A 119.5 . . ? C19 C18 C23 117.6(3) . . ? C19 C18 P1 122.4(2) . . ? C23 C18 P1 119.2(2) . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C21 C20 C19 120.9(3) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C22 C21 C20 119.1(3) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C22 C23 C18 120.9(3) . . ? C22 C23 H23A 119.5 . . ? C18 C23 H23A 119.5 . . ? C25 C24 C29 118.8(3) . . ? C25 C24 P1 124.0(2) . . ? C29 C24 P1 117.1(2) . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C27 C26 C25 120.5(4) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C24 120.6(3) . . ? C28 C29 H29A 119.7 . . ? C24 C29 H29A 119.7 . . ? C35 C30 C31 117.7(3) . . ? C35 C30 P2 126.4(2) . . ? C31 C30 P2 115.7(2) . . ? C32 C31 C30 121.2(4) . . ? C32 C31 H31A 119.4 . . ? C30 C31 H31A 119.4 . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C30 C35 C34 120.7(4) . . ? C30 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C37 C36 C41 117.7(3) . . ? C37 C36 P2 124.9(2) . . ? C41 C36 P2 117.3(2) . . ? C36 C37 C38 120.6(3) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C40 119.4(3) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C39 C40 C41 120.2(3) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C36 121.4(3) . . ? C40 C41 H41A 119.3 . . ? C36 C41 H41A 119.3 . . ? C47 C42 C43 117.7(3) . . ? C47 C42 P2 120.7(2) . . ? C43 C42 P2 121.6(2) . . ? C44 C43 C42 120.8(3) . . ? C44 C43 H43A 119.6 . . ? C42 C43 H43A 119.6 . . ? C45 C44 C43 120.7(3) . . ? C45 C44 H44A 119.7 . . ? C43 C44 H44A 119.7 . . ? C46 C45 C44 119.1(3) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C45 C46 C47 120.8(3) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C47 C42 121.0(3) . . ? C46 C47 H47A 119.5 . . ? C42 C47 H47A 119.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.046 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.082 #===>END data_4 _database_code_depnum_ccdc_archive 'CCDC 743625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H55 N2 Na O2 P2 Ru' _chemical_formula_weight 962.01 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 20.9478(4) _cell_length_b 21.7547(3) _cell_length_c 23.2295(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.8897(8) _cell_angle_gamma 90.00 _cell_volume 9523.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 67962 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67962 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.37 _reflns_number_total 21347 _reflns_number_gt 11611 _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^)+(0.0681P)^2^+2.4260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21347 _refine_ls_number_parameters 1103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ru1 Ru 0.371029(18) 0.277841(14) 0.096120(16) 0.03970(11) Uani 1 1 d . . . H1 H 0.4285(19) 0.2237(14) 0.1218(17) 0.038(10) Uiso 1 1 d . . . H2 H 0.307(2) 0.2283(15) 0.0667(18) 0.046(11) Uiso 1 1 d . . . Ru2 Ru 0.137179(19) 0.732159(15) 0.775973(16) 0.04214(11) Uani 1 1 d . . . H3 H 0.067(2) 0.695(2) 0.777(2) 0.080(15) Uiso 1 1 d . . . H4 H 0.1939(19) 0.6792(16) 0.8157(17) 0.046(11) Uiso 1 1 d . . . P1 P 0.38236(6) 0.26711(5) 0.00344(5) 0.0421(3) Uani 1 1 d . . . P2 P 0.36758(6) 0.26444(5) 0.19232(5) 0.0424(3) Uani 1 1 d . . . P3 P 0.10912(6) 0.66821(5) 0.69038(5) 0.0440(3) Uani 1 1 d . . . P4 P 0.15598(6) 0.77522(5) 0.87190(6) 0.0446(3) Uani 1 1 d . . . Na1 Na 0.35829(10) 0.13820(8) 0.08963(9) 0.0589(5) Uani 1 1 d . . . Na2 Na 0.11900(10) 0.61890(8) 0.84048(9) 0.0583(5) Uani 1 1 d . . . O1 O 0.2675(2) 0.08085(18) 0.0137(2) 0.0959(8) Uani 1 1 d . . . O2 O 0.43183(19) 0.06084(15) 0.14650(18) 0.0738(6) Uani 1 1 d . . . O3 O 0.04117(18) 0.58939(16) 0.88049(17) 0.0695(9) Uani 1 1 d . . . O4 O 0.20098(18) 0.54538(14) 0.86580(16) 0.0666(9) Uani 1 1 d . . . N1 N 0.29462(18) 0.35497(15) 0.06854(16) 0.0418(8) Uani 1 1 d . . . N2 N 0.44671(19) 0.35593(16) 0.12678(16) 0.0465(9) Uani 1 1 d . . . N3 N 0.0744(2) 0.81032(15) 0.71957(17) 0.0472(9) Uani 1 1 d . . . N4 N 0.2227(2) 0.78564(16) 0.76718(18) 0.0501(9) Uani 1 1 d . . . C1 C 0.2251(2) 0.3636(2) 0.0457(2) 0.0489(11) Uani 1 1 d . . . H1A H 0.1947 0.3288 0.0320 0.059 Uiso 1 1 calc R . . C1S C 0.2318(3) 0.0240(3) 0.0124(3) 0.0959(8) Uani 1 1 d . . . H1SA H 0.2227 0.0198 0.0506 0.115 Uiso 1 1 calc R . . H1SB H 0.2596 -0.0118 0.0099 0.115 Uiso 1 1 calc R . . C2 C 0.1950(3) 0.4217(2) 0.0412(2) 0.0572(12) Uani 1 1 d . . . H2A H 0.1449 0.4248 0.0241 0.069 Uiso 1 1 calc R . . C2S C 0.1627(3) 0.0306(3) -0.0485(3) 0.0959(8) Uani 1 1 d . . . H2SA H 0.1468 -0.0101 -0.0689 0.115 Uiso 1 1 calc R . . H2SB H 0.1251 0.0477 -0.0382 0.115 Uiso 1 1 calc R . . C3 C 0.2347(3) 0.4745(2) 0.0603(2) 0.0552(12) Uani 1 1 d . . . H3A H 0.2128 0.5134 0.0575 0.066 Uiso 1 1 calc R . . C3S C 0.1756(3) 0.0713(3) -0.0910(3) 0.0959(8) Uani 1 1 d . . . H3SA H 0.1748 0.0486 -0.1283 0.115 Uiso 1 1 calc R . . H3SB H 0.1398 0.1045 -0.1065 0.115 Uiso 1 1 calc R . . C4 C 0.3087(3) 0.46907(19) 0.0841(2) 0.0510(11) Uani 1 1 d . . . C4S C 0.2449(3) 0.0956(3) -0.0525(3) 0.0959(8) Uani 1 1 d . . . H4SA H 0.2441 0.1408 -0.0577 0.115 Uiso 1 1 calc R . . H4SB H 0.2790 0.0784 -0.0671 0.115 Uiso 1 1 calc R . . C5 C 0.3687(3) 0.5081(2) 0.1082(2) 0.0571(13) Uani 1 1 d . . . H5A H 0.3683 0.5515 0.1122 0.069 Uiso 1 1 calc R . . C5S C 0.4987(3) 0.0679(2) 0.2005(3) 0.0738(6) Uani 1 1 d . . . H5SA H 0.4923 0.0735 0.2400 0.089 Uiso 1 1 calc R . . H5SB H 0.5242 0.1041 0.1950 0.089 Uiso 1 1 calc R . . C6 C 0.4300(3) 0.4703(2) 0.1255(2) 0.0536(12) Uani 1 1 d . . . C6S C 0.5394(3) 0.0095(2) 0.2042(3) 0.0738(6) Uani 1 1 d . . . H6SA H 0.5650 0.0123 0.1772 0.089 Uiso 1 1 calc R . . H6SB H 0.5737 0.0004 0.2488 0.089 Uiso 1 1 calc R . . C7 C 0.5033(3) 0.4780(2) 0.1496(2) 0.0677(15) Uani 1 1 d . . . H7A H 0.5236 0.5179 0.1577 0.081 Uiso 1 1 calc R . . C7S C 0.4819(3) -0.0379(2) 0.1791(3) 0.0738(6) Uani 1 1 d . . . H7SA H 0.4938 -0.0708 0.1560 0.089 Uiso 1 1 calc R . . H7SB H 0.4740 -0.0566 0.2143 0.089 Uiso 1 1 calc R . . C8 C 0.5461(3) 0.4261(2) 0.1615(2) 0.0628(14) Uani 1 1 d . . . H8A H 0.5959 0.4310 0.1769 0.075 Uiso 1 1 calc R . . C8S C 0.4186(3) -0.0029(2) 0.1352(3) 0.0738(6) Uani 1 1 d . . . H8SA H 0.4080 -0.0125 0.0902 0.089 Uiso 1 1 calc R . . H8SB H 0.3770 -0.0147 0.1423 0.089 Uiso 1 1 calc R . . C9 C 0.5166(3) 0.3657(2) 0.1509(2) 0.0532(12) Uani 1 1 d . . . H9A H 0.5476 0.3313 0.1613 0.064 Uiso 1 1 calc R . . C9S C -0.0338(3) 0.6005(3) 0.8494(3) 0.0700(14) Uani 1 1 d . . . H9SA H -0.0593 0.5633 0.8260 0.084 Uiso 1 1 calc R . . H9SB H -0.0447 0.6348 0.8185 0.084 Uiso 1 1 calc R . . C10 C 0.4067(2) 0.40756(18) 0.1132(2) 0.0449(10) Uani 1 1 d . . . C10S C -0.0556(3) 0.6163(3) 0.9002(3) 0.0894(19) Uani 1 1 d . . . H10A H -0.1060 0.6060 0.8872 0.107 Uiso 1 1 calc R . . H10B H -0.0480 0.6605 0.9113 0.107 Uiso 1 1 calc R . . C11 C 0.3337(2) 0.40702(18) 0.0870(2) 0.0438(10) Uani 1 1 d . . . C11S C -0.0072(3) 0.5768(2) 0.9548(3) 0.0803(17) Uani 1 1 d . . . H11A H 0.0000 0.5944 0.9965 0.096 Uiso 1 1 calc R . . H11B H -0.0261 0.5345 0.9512 0.096 Uiso 1 1 calc R . . C12 C 0.4500(3) 0.31595(19) -0.0046(2) 0.0504(11) Uani 1 1 d . . . C12S C 0.0594(3) 0.5777(3) 0.9470(3) 0.0812(17) Uani 1 1 d . . . H12A H 0.0914 0.6103 0.9741 0.097 Uiso 1 1 calc R . . H12B H 0.0841 0.5377 0.9602 0.097 Uiso 1 1 calc R . . C13 C 0.4349(3) 0.3780(2) -0.0177(2) 0.0594(13) Uani 1 1 d . . . H13A H 0.3902 0.3938 -0.0236 0.071 Uiso 1 1 calc R . . C13S C 0.1944(3) 0.4881(2) 0.8936(3) 0.0792(17) Uani 1 1 d . . . H13B H 0.1593 0.4611 0.8607 0.095 Uiso 1 1 calc R . . H13C H 0.1791 0.4953 0.9278 0.095 Uiso 1 1 calc R . . C14 C 0.4851(4) 0.4171(2) -0.0223(3) 0.0753(17) Uani 1 1 d . . . H14A H 0.4736 0.4592 -0.0325 0.090 Uiso 1 1 calc R . . C14S C 0.2669(3) 0.4599(3) 0.9205(3) 0.0862(19) Uani 1 1 d . . . H14B H 0.2965 0.4744 0.9646 0.103 Uiso 1 1 calc R . . H14C H 0.2642 0.4145 0.9205 0.103 Uiso 1 1 calc R . . C15S C 0.2952(4) 0.4821(2) 0.8754(3) 0.0870(18) Uani 1 1 d . . . H15A H 0.3477 0.4830 0.8963 0.104 Uiso 1 1 calc R . . H15B H 0.2788 0.4556 0.8369 0.104 Uiso 1 1 calc R . . C15 C 0.5495(4) 0.3965(3) -0.0128(3) 0.095(2) Uani 1 1 d . . . H15C H 0.5828 0.4235 -0.0172 0.114 Uiso 1 1 calc R . . C16 C 0.5666(4) 0.3359(3) 0.0036(4) 0.109(3) Uani 1 1 d . . . H16A H 0.6128 0.3213 0.0126 0.131 Uiso 1 1 calc R . . C16S C 0.2655(3) 0.5452(2) 0.8585(3) 0.0701(15) Uani 1 1 d . . . H16B H 0.2993 0.5759 0.8873 0.084 Uiso 1 1 calc R . . H16C H 0.2557 0.5552 0.8138 0.084 Uiso 1 1 calc R . . C17 C 0.5172(3) 0.2961(2) 0.0069(3) 0.0793(17) Uani 1 1 d . . . H17A H 0.5296 0.2542 0.0174 0.095 Uiso 1 1 calc R . . C18 C 0.3025(3) 0.28308(19) -0.0715(2) 0.0486(11) Uani 1 1 d . . . C19 C 0.2382(3) 0.2716(2) -0.0714(2) 0.0561(12) Uani 1 1 d . . . H19A H 0.2367 0.2555 -0.0339 0.067 Uiso 1 1 calc R . . C20 C 0.1750(3) 0.2831(2) -0.1253(3) 0.0723(15) Uani 1 1 d . . . H20A H 0.1307 0.2744 -0.1249 0.087 Uiso 1 1 calc R . . C21 C 0.1771(3) 0.3075(3) -0.1797(2) 0.0704(15) Uani 1 1 d . . . H21A H 0.1342 0.3157 -0.2166 0.084 Uiso 1 1 calc R . . C22 C 0.2414(3) 0.3199(2) -0.1800(2) 0.0647(14) Uani 1 1 d . . . H22A H 0.2426 0.3374 -0.2170 0.078 Uiso 1 1 calc R . . C23 C 0.3041(3) 0.3071(2) -0.1272(2) 0.0535(12) Uani 1 1 d . . . H23A H 0.3482 0.3144 -0.1284 0.064 Uiso 1 1 calc R . . C24 C 0.4089(2) 0.19098(18) -0.0143(2) 0.0421(10) Uani 1 1 d . . . C25 C 0.4632(2) 0.1578(2) 0.0341(2) 0.0510(11) Uani 1 1 d . . . H25A H 0.4848 0.1741 0.0763 0.061 Uiso 1 1 calc R . . C26 C 0.4859(3) 0.1019(2) 0.0219(2) 0.0599(13) Uani 1 1 d . . . H26A H 0.5230 0.0804 0.0555 0.072 Uiso 1 1 calc R . . C27 C 0.4556(3) 0.0773(2) -0.0384(2) 0.0565(12) Uani 1 1 d . . . H27A H 0.4717 0.0389 -0.0466 0.068 Uiso 1 1 calc R . . C28 C 0.4018(3) 0.10813(19) -0.0868(2) 0.0553(12) Uani 1 1 d . . . H28A H 0.3801 0.0910 -0.1286 0.066 Uiso 1 1 calc R . . C29 C 0.3789(2) 0.16452(19) -0.0748(2) 0.0473(11) Uani 1 1 d . . . H29A H 0.3417 0.1855 -0.1088 0.057 Uiso 1 1 calc R . . C30 C 0.3133(2) 0.31708(19) 0.21531(19) 0.0447(10) Uani 1 1 d . . . C31 C 0.2577(2) 0.2988(2) 0.2284(2) 0.0538(12) Uani 1 1 d . . . H31A H 0.2462 0.2564 0.2264 0.065 Uiso 1 1 calc R . . C32 C 0.2185(3) 0.3413(2) 0.2444(3) 0.0663(14) Uani 1 1 d . . . H32A H 0.1815 0.3278 0.2546 0.080 Uiso 1 1 calc R . . C33 C 0.2332(3) 0.4029(2) 0.2454(2) 0.0627(14) Uani 1 1 d . . . H33A H 0.2054 0.4321 0.2549 0.075 Uiso 1 1 calc R . . C34 C 0.2885(3) 0.4223(2) 0.2326(2) 0.0565(12) Uani 1 1 d . . . H34A H 0.2992 0.4649 0.2337 0.068 Uiso 1 1 calc R . . C35 C 0.3284(3) 0.3794(2) 0.2182(2) 0.0523(12) Uani 1 1 d . . . H35A H 0.3668 0.3930 0.2100 0.063 Uiso 1 1 calc R . . C36 C 0.3336(2) 0.18848(19) 0.2025(2) 0.0455(10) Uani 1 1 d . . . C37 C 0.2680(3) 0.1682(2) 0.1550(2) 0.0554(12) Uani 1 1 d . . . H37A H 0.2407 0.1949 0.1205 0.067 Uiso 1 1 calc R . . C38 C 0.2424(3) 0.1103(2) 0.1575(3) 0.0662(14) Uani 1 1 d . . . H38A H 0.1972 0.0982 0.1256 0.079 Uiso 1 1 calc R . . C39 C 0.2810(3) 0.0703(2) 0.2053(3) 0.0821(19) Uani 1 1 d . . . H39A H 0.2641 0.0299 0.2060 0.099 Uiso 1 1 calc R . . C40 C 0.3450(3) 0.0898(3) 0.2526(3) 0.086(2) Uani 1 1 d . . . H40A H 0.3717 0.0626 0.2867 0.104 Uiso 1 1 calc R . . C41 C 0.3715(3) 0.1484(2) 0.2516(3) 0.0635(14) Uani 1 1 d . . . H41A H 0.4158 0.1608 0.2848 0.076 Uiso 1 1 calc R . . C42 C 0.4532(2) 0.26711(19) 0.2650(2) 0.0470(11) Uani 1 1 d . . . C43 C 0.4575(3) 0.2854(2) 0.3234(2) 0.0614(13) Uani 1 1 d . . . H43A H 0.4161 0.2989 0.3268 0.074 Uiso 1 1 calc R . . C44 C 0.5224(3) 0.2842(3) 0.3776(3) 0.0777(17) Uani 1 1 d . . . H44A H 0.5254 0.2978 0.4175 0.093 Uiso 1 1 calc R . . C45 C 0.5821(3) 0.2634(3) 0.3734(2) 0.0718(15) Uani 1 1 d . . . H45A H 0.6259 0.2614 0.4107 0.086 Uiso 1 1 calc R . . C46 C 0.5783(3) 0.2456(2) 0.3154(2) 0.0632(13) Uani 1 1 d . . . H46A H 0.6198 0.2317 0.3125 0.076 Uiso 1 1 calc R . . C47 C 0.5146(2) 0.2478(2) 0.2612(2) 0.0519(11) Uani 1 1 d . . . H47A H 0.5126 0.2362 0.2210 0.062 Uiso 1 1 calc R . . C48 C 0.0070(3) 0.8283(2) 0.6950(2) 0.0552(12) Uani 1 1 d . . . H48A H -0.0262 0.8048 0.7033 0.066 Uiso 1 1 calc R . . C49 C -0.0160(3) 0.8814(2) 0.6571(2) 0.0656(14) Uani 1 1 d . . . H49A H -0.0648 0.8923 0.6398 0.079 Uiso 1 1 calc R . . C50 C 0.0293(3) 0.9179(2) 0.6441(2) 0.0685(15) Uani 1 1 d . . . H50A H 0.0120 0.9533 0.6178 0.082 Uiso 1 1 calc R . . C51 C 0.1019(3) 0.9024(2) 0.6702(2) 0.0629(14) Uani 1 1 d . . . C52 C 0.1664(4) 0.9251(2) 0.6725(3) 0.0775(17) Uani 1 1 d . . . H52A H 0.1718 0.9618 0.6527 0.093 Uiso 1 1 calc R . . C53 C 0.2214(3) 0.8840(2) 0.7091(3) 0.0660(15) Uani 1 1 d . . . C54 C 0.2952(4) 0.8798(3) 0.7331(3) 0.0817(18) Uani 1 1 d . . . H54A H 0.3210 0.9097 0.7221 0.098 Uiso 1 1 calc R . . C55 C 0.3300(3) 0.8310(3) 0.7733(3) 0.0804(18) Uani 1 1 d . . . H55A H 0.3803 0.8285 0.7905 0.096 Uiso 1 1 calc R . . C56 C 0.2925(3) 0.7848(2) 0.7892(2) 0.0620(13) Uani 1 1 d . . . H56A H 0.3185 0.7523 0.8167 0.074 Uiso 1 1 calc R . . C57 C 0.1901(3) 0.8345(2) 0.7286(2) 0.0528(12) Uani 1 1 d . . . C58 C 0.1184(3) 0.84627(19) 0.7058(2) 0.0492(11) Uani 1 1 d . . . C59 C 0.0351(2) 0.69148(19) 0.6133(2) 0.0460(11) Uani 1 1 d . . . C60 C 0.0419(3) 0.7474(2) 0.5885(2) 0.0671(15) Uani 1 1 d . . . H60A H 0.0839 0.7708 0.6103 0.080 Uiso 1 1 calc R . . C61 C -0.0109(4) 0.7697(2) 0.5331(3) 0.084(2) Uani 1 1 d . . . H61A H -0.0044 0.8077 0.5162 0.101 Uiso 1 1 calc R . . C62 C -0.0724(3) 0.7381(3) 0.5020(3) 0.0798(18) Uani 1 1 d . . . H62A H -0.1090 0.7538 0.4636 0.096 Uiso 1 1 calc R . . C63 C -0.0809(3) 0.6840(4) 0.5266(3) 0.096(2) Uani 1 1 d . . . H63A H -0.1246 0.6625 0.5063 0.116 Uiso 1 1 calc R . . C64 C -0.0260(3) 0.6597(3) 0.5814(2) 0.0725(16) Uani 1 1 d . . . H64A H -0.0315 0.6204 0.5966 0.087 Uiso 1 1 calc R . . C65 C 0.0819(2) 0.5895(2) 0.7006(2) 0.0499(11) Uani 1 1 d . . . C66 C 0.1195(3) 0.53722(19) 0.6971(2) 0.0571(12) Uani 1 1 d . . . H66A H 0.1585 0.5417 0.6869 0.068 Uiso 1 1 calc R . . C67 C 0.1001(3) 0.4790(2) 0.7085(2) 0.0654(14) Uani 1 1 d . . . H67A H 0.1267 0.4441 0.7073 0.079 Uiso 1 1 calc R . . C68 C 0.0429(3) 0.4720(2) 0.7214(2) 0.0654(14) Uani 1 1 d . . . H68A H 0.0295 0.4319 0.7280 0.079 Uiso 1 1 calc R . . C69 C 0.0039(3) 0.5221(2) 0.7250(2) 0.0587(13) Uani 1 1 d . . . H69A H -0.0356 0.5166 0.7343 0.070 Uiso 1 1 calc R . . C70 C 0.0245(3) 0.5814(2) 0.7147(2) 0.0547(12) Uani 1 1 d . . . H70A H -0.0014 0.6162 0.7173 0.066 Uiso 1 1 calc R . . C71 C 0.1784(2) 0.65055(18) 0.6638(2) 0.0454(11) Uani 1 1 d . . . C72 C 0.2485(3) 0.65157(19) 0.7086(2) 0.0526(12) Uani 1 1 d . . . H72A H 0.2599 0.6610 0.7519 0.063 Uiso 1 1 calc R . . C73 C 0.3026(3) 0.6390(2) 0.6911(2) 0.0591(13) Uani 1 1 d . . . H73A H 0.3505 0.6399 0.7226 0.071 Uiso 1 1 calc R . . C74 C 0.2877(3) 0.6254(2) 0.6289(3) 0.0608(13) Uani 1 1 d . . . H74A H 0.3250 0.6172 0.6172 0.073 Uiso 1 1 calc R . . C75 C 0.2177(3) 0.6236(2) 0.5833(3) 0.0651(14) Uani 1 1 d . . . H75A H 0.2068 0.6138 0.5401 0.078 Uiso 1 1 calc R . . C76 C 0.1639(3) 0.6362(2) 0.6006(2) 0.0580(13) Uani 1 1 d . . . H76A H 0.1161 0.6351 0.5689 0.070 Uiso 1 1 calc R . . C77 C 0.0788(2) 0.8107(2) 0.8771(2) 0.0503(11) Uani 1 1 d . . . C78 C 0.0828(3) 0.8648(2) 0.9102(2) 0.0601(13) Uani 1 1 d . . . H78A H 0.1259 0.8875 0.9275 0.072 Uiso 1 1 calc R . . C79 C 0.0250(3) 0.8863(3) 0.9186(3) 0.0771(17) Uani 1 1 d . . . H79A H 0.0285 0.9236 0.9412 0.092 Uiso 1 1 calc R . . C80 C -0.0379(3) 0.8530(3) 0.8937(3) 0.0761(16) Uani 1 1 d . . . H80A H -0.0770 0.8666 0.9009 0.091 Uiso 1 1 calc R . . C81 C -0.0441(3) 0.8004(3) 0.8587(3) 0.0707(15) Uani 1 1 d . . . H81A H -0.0877 0.7785 0.8404 0.085 Uiso 1 1 calc R . . C82 C 0.0140(3) 0.7796(2) 0.8506(2) 0.0607(13) Uani 1 1 d . . . H82A H 0.0096 0.7433 0.8263 0.073 Uiso 1 1 calc R . . C83 C 0.2216(2) 0.83798(19) 0.9000(2) 0.0477(11) Uani 1 1 d . . . C84 C 0.2853(2) 0.8347(2) 0.9549(2) 0.0605(13) Uani 1 1 d . . . H84A H 0.2946 0.8003 0.9827 0.073 Uiso 1 1 calc R . . C85 C 0.3357(3) 0.8807(3) 0.9698(3) 0.0746(16) Uani 1 1 d . . . H85A H 0.3789 0.8777 1.0077 0.089 Uiso 1 1 calc R . . C86 C 0.3236(3) 0.9308(2) 0.9301(3) 0.0710(15) Uani 1 1 d . . . H86A H 0.3584 0.9622 0.9404 0.085 Uiso 1 1 calc R . . C87 C 0.2610(3) 0.9351(2) 0.8756(3) 0.0624(13) Uani 1 1 d . . . H87A H 0.2525 0.9695 0.8480 0.075 Uiso 1 1 calc R . . C88 C 0.2098(3) 0.8893(2) 0.8604(2) 0.0524(12) Uani 1 1 d . . . H88A H 0.1664 0.8930 0.8228 0.063 Uiso 1 1 calc R . . C89 C 0.1883(2) 0.72651(19) 0.9448(2) 0.0498(11) Uani 1 1 d . . . C90 C 0.1702(3) 0.7373(2) 0.9945(2) 0.0594(13) Uani 1 1 d . . . H90A H 0.1377 0.7692 0.9909 0.071 Uiso 1 1 calc R . . C91 C 0.1993(3) 0.7017(2) 1.0499(2) 0.0639(14) Uani 1 1 d . . . H91A H 0.1875 0.7105 1.0842 0.077 Uiso 1 1 calc R . . C92 C 0.2445(3) 0.6544(2) 1.0558(2) 0.0574(13) Uani 1 1 d . . . H92A H 0.2639 0.6302 1.0937 0.069 Uiso 1 1 calc R . . C93 C 0.2615(3) 0.6422(2) 1.0065(2) 0.0599(13) Uani 1 1 d . . . H93A H 0.2920 0.6088 1.0098 0.072 Uiso 1 1 calc R . . C94 C 0.2346(2) 0.6780(2) 0.9517(2) 0.0540(12) Uani 1 1 d . . . H94A H 0.2480 0.6694 0.9184 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0406(2) 0.04090(19) 0.0391(2) 0.00222(15) 0.01881(16) 0.00113(14) Ru2 0.0414(2) 0.0442(2) 0.0417(2) -0.00028(15) 0.01901(17) -0.00038(15) P1 0.0464(7) 0.0402(6) 0.0420(6) 0.0036(5) 0.0214(5) 0.0033(5) P2 0.0417(7) 0.0455(6) 0.0424(6) 0.0043(5) 0.0207(5) 0.0019(5) P3 0.0464(7) 0.0422(6) 0.0451(7) 0.0006(5) 0.0216(5) -0.0014(5) P4 0.0420(7) 0.0487(6) 0.0433(6) 0.0000(5) 0.0190(5) 0.0037(5) Na1 0.0580(12) 0.0452(9) 0.0694(12) 0.0017(9) 0.0240(10) 0.0011(8) Na2 0.0563(12) 0.0597(11) 0.0617(11) 0.0149(9) 0.0284(10) 0.0061(8) O1 0.0896(19) 0.0782(16) 0.114(2) -0.0114(16) 0.0386(17) -0.0145(14) O2 0.0694(15) 0.0583(11) 0.0854(16) 0.0027(12) 0.0262(12) 0.0025(10) O3 0.060(2) 0.090(2) 0.063(2) 0.0115(19) 0.0311(19) 0.0031(18) O4 0.067(2) 0.0521(19) 0.079(2) 0.0146(17) 0.031(2) 0.0086(16) N1 0.040(2) 0.0437(19) 0.044(2) 0.0038(16) 0.0203(17) 0.0009(15) N2 0.044(2) 0.054(2) 0.040(2) 0.0024(17) 0.0166(17) -0.0020(17) N3 0.050(2) 0.045(2) 0.047(2) -0.0019(17) 0.0218(19) 0.0004(17) N4 0.049(3) 0.054(2) 0.054(2) -0.0174(19) 0.029(2) -0.0130(18) C1 0.048(3) 0.050(3) 0.054(3) 0.009(2) 0.027(2) 0.002(2) C1S 0.0896(19) 0.0782(16) 0.114(2) -0.0114(16) 0.0386(17) -0.0145(14) C2 0.049(3) 0.062(3) 0.062(3) 0.014(2) 0.026(3) 0.012(2) C2S 0.0896(19) 0.0782(16) 0.114(2) -0.0114(16) 0.0386(17) -0.0145(14) C3 0.070(4) 0.052(3) 0.051(3) 0.010(2) 0.034(3) 0.015(2) C3S 0.0896(19) 0.0782(16) 0.114(2) -0.0114(16) 0.0386(17) -0.0145(14) C4 0.062(3) 0.045(2) 0.049(3) 0.003(2) 0.027(2) 0.002(2) C4S 0.0896(19) 0.0782(16) 0.114(2) -0.0114(16) 0.0386(17) -0.0145(14) C5 0.069(3) 0.044(2) 0.056(3) -0.004(2) 0.026(3) -0.003(2) C5S 0.0694(15) 0.0583(11) 0.0854(16) 0.0027(12) 0.0262(12) 0.0025(10) C6 0.055(3) 0.053(3) 0.047(3) -0.003(2) 0.016(2) -0.006(2) C6S 0.0694(15) 0.0583(11) 0.0854(16) 0.0027(12) 0.0262(12) 0.0025(10) C7 0.078(4) 0.058(3) 0.061(3) -0.002(3) 0.025(3) -0.017(3) C7S 0.0694(15) 0.0583(11) 0.0854(16) 0.0027(12) 0.0262(12) 0.0025(10) C8 0.047(3) 0.078(4) 0.055(3) 0.004(3) 0.014(2) -0.018(3) C8S 0.0694(15) 0.0583(11) 0.0854(16) 0.0027(12) 0.0262(12) 0.0025(10) C9 0.048(3) 0.061(3) 0.049(3) 0.004(2) 0.020(2) 0.001(2) C9S 0.062(4) 0.085(4) 0.067(4) 0.003(3) 0.033(3) 0.003(3) C10 0.051(3) 0.044(2) 0.041(2) 0.0009(19) 0.021(2) -0.004(2) C10S 0.092(5) 0.113(5) 0.066(4) 0.005(3) 0.037(4) 0.024(4) C11 0.053(3) 0.041(2) 0.042(2) 0.0017(19) 0.026(2) 0.002(2) C11S 0.124(5) 0.063(3) 0.077(4) 0.010(3) 0.065(4) 0.010(3) C12 0.065(3) 0.041(2) 0.056(3) -0.001(2) 0.036(3) -0.002(2) C12S 0.077(4) 0.099(4) 0.063(4) 0.005(3) 0.026(3) 0.004(3) C13 0.072(4) 0.050(3) 0.051(3) 0.001(2) 0.023(3) -0.004(2) C13S 0.093(5) 0.062(3) 0.082(4) 0.028(3) 0.037(3) 0.004(3) C14 0.108(5) 0.051(3) 0.064(3) 0.000(3) 0.035(3) -0.024(3) C14S 0.122(5) 0.065(3) 0.093(4) 0.024(3) 0.068(4) 0.037(3) C15S 0.112(5) 0.069(4) 0.093(4) 0.019(3) 0.057(4) 0.026(3) C15 0.118(6) 0.082(4) 0.129(6) -0.024(4) 0.095(5) -0.036(4) C16 0.103(5) 0.069(4) 0.204(8) -0.030(4) 0.111(6) -0.024(4) C16S 0.065(4) 0.070(3) 0.079(4) 0.011(3) 0.035(3) 0.012(3) C17 0.087(4) 0.053(3) 0.132(5) -0.013(3) 0.080(4) -0.009(3) C18 0.056(3) 0.047(2) 0.044(3) 0.003(2) 0.023(2) 0.011(2) C19 0.055(3) 0.067(3) 0.042(3) 0.003(2) 0.018(2) 0.012(2) C20 0.053(3) 0.097(4) 0.058(3) 0.006(3) 0.016(3) 0.013(3) C21 0.065(4) 0.092(4) 0.041(3) 0.007(3) 0.012(3) 0.020(3) C22 0.076(4) 0.065(3) 0.049(3) 0.006(2) 0.024(3) 0.021(3) C23 0.065(3) 0.053(3) 0.043(3) 0.000(2) 0.024(2) 0.009(2) C24 0.044(3) 0.042(2) 0.043(2) 0.0031(19) 0.022(2) -0.0006(18) C25 0.051(3) 0.058(3) 0.051(3) 0.004(2) 0.028(2) 0.009(2) C26 0.070(4) 0.051(3) 0.060(3) 0.012(2) 0.031(3) 0.018(2) C27 0.074(4) 0.044(2) 0.065(3) -0.003(2) 0.042(3) 0.006(2) C28 0.070(3) 0.045(3) 0.053(3) -0.007(2) 0.029(3) -0.005(2) C29 0.051(3) 0.047(2) 0.043(3) 0.007(2) 0.019(2) 0.006(2) C30 0.045(3) 0.051(3) 0.038(2) 0.003(2) 0.018(2) 0.004(2) C31 0.054(3) 0.053(3) 0.063(3) 0.005(2) 0.033(3) 0.005(2) C32 0.058(3) 0.068(3) 0.083(4) -0.004(3) 0.040(3) 0.001(3) C33 0.057(3) 0.064(3) 0.062(3) -0.009(3) 0.022(3) 0.013(2) C34 0.063(3) 0.051(3) 0.052(3) -0.003(2) 0.023(3) 0.006(2) C35 0.057(3) 0.058(3) 0.044(3) 0.004(2) 0.025(2) 0.000(2) C36 0.048(3) 0.045(2) 0.052(3) 0.008(2) 0.030(2) 0.007(2) C37 0.055(3) 0.056(3) 0.062(3) 0.005(2) 0.032(3) 0.003(2) C38 0.067(4) 0.057(3) 0.090(4) 0.001(3) 0.048(3) -0.007(3) C39 0.067(4) 0.054(3) 0.150(6) 0.018(4) 0.069(4) 0.003(3) C40 0.058(4) 0.075(4) 0.132(5) 0.057(4) 0.046(4) 0.021(3) C41 0.046(3) 0.063(3) 0.087(4) 0.029(3) 0.034(3) 0.011(2) C42 0.046(3) 0.055(3) 0.041(3) 0.005(2) 0.019(2) 0.002(2) C43 0.058(3) 0.087(4) 0.039(3) 0.004(2) 0.022(3) 0.014(3) C44 0.072(4) 0.109(5) 0.049(3) -0.012(3) 0.023(3) 0.008(3) C45 0.049(3) 0.105(4) 0.050(3) 0.006(3) 0.011(3) 0.008(3) C46 0.047(3) 0.090(4) 0.051(3) 0.002(3) 0.020(3) 0.007(3) C47 0.042(3) 0.067(3) 0.047(3) -0.002(2) 0.020(2) 0.001(2) C48 0.058(3) 0.052(3) 0.054(3) 0.000(2) 0.023(2) 0.009(2) C49 0.069(4) 0.065(3) 0.060(3) 0.004(3) 0.026(3) 0.017(3) C50 0.097(5) 0.048(3) 0.057(3) 0.011(2) 0.031(3) 0.016(3) C51 0.091(4) 0.045(3) 0.059(3) -0.004(2) 0.039(3) -0.008(3) C52 0.123(5) 0.053(3) 0.069(4) -0.004(3) 0.053(4) -0.021(3) C53 0.086(4) 0.059(3) 0.068(3) -0.014(3) 0.047(3) -0.028(3) C54 0.106(5) 0.077(4) 0.086(4) -0.031(3) 0.065(4) -0.041(4) C55 0.066(4) 0.094(4) 0.101(5) -0.043(4) 0.055(4) -0.029(3) C56 0.054(3) 0.069(3) 0.068(3) -0.020(3) 0.031(3) -0.010(2) C57 0.065(3) 0.050(3) 0.054(3) -0.006(2) 0.035(3) -0.014(2) C58 0.058(3) 0.046(2) 0.047(3) -0.002(2) 0.026(2) -0.005(2) C59 0.045(3) 0.046(2) 0.048(3) 0.000(2) 0.022(2) 0.006(2) C60 0.100(4) 0.049(3) 0.046(3) 0.001(2) 0.026(3) 0.002(3) C61 0.131(6) 0.052(3) 0.054(3) 0.005(3) 0.026(4) 0.012(3) C62 0.081(5) 0.108(5) 0.048(3) 0.018(3) 0.025(3) 0.049(4) C63 0.051(4) 0.162(7) 0.064(4) 0.028(4) 0.012(3) -0.009(4) C64 0.056(3) 0.095(4) 0.053(3) 0.019(3) 0.012(3) -0.015(3) C65 0.055(3) 0.052(3) 0.040(3) 0.000(2) 0.018(2) -0.004(2) C66 0.065(3) 0.044(2) 0.063(3) -0.002(2) 0.029(3) -0.002(2) C67 0.073(4) 0.047(3) 0.077(4) 0.004(2) 0.034(3) 0.003(2) C68 0.083(4) 0.047(3) 0.064(3) 0.002(2) 0.031(3) -0.016(3) C69 0.067(3) 0.062(3) 0.048(3) -0.004(2) 0.025(3) -0.018(3) C70 0.056(3) 0.057(3) 0.053(3) -0.002(2) 0.026(2) -0.006(2) C71 0.053(3) 0.043(2) 0.044(3) -0.001(2) 0.024(2) 0.0005(19) C72 0.055(3) 0.052(3) 0.050(3) 0.000(2) 0.022(3) 0.001(2) C73 0.056(3) 0.065(3) 0.057(3) 0.003(2) 0.025(3) 0.006(2) C74 0.057(3) 0.062(3) 0.074(4) 0.009(3) 0.038(3) 0.015(2) C75 0.069(4) 0.073(3) 0.061(3) -0.005(3) 0.036(3) 0.014(3) C76 0.059(3) 0.061(3) 0.055(3) -0.001(2) 0.026(3) 0.007(2) C77 0.050(3) 0.059(3) 0.041(3) 0.010(2) 0.019(2) 0.010(2) C78 0.064(3) 0.057(3) 0.065(3) 0.000(2) 0.033(3) 0.012(2) C79 0.090(5) 0.079(4) 0.074(4) 0.007(3) 0.047(4) 0.032(3) C80 0.073(4) 0.089(4) 0.085(4) 0.023(3) 0.051(4) 0.028(3) C81 0.053(3) 0.092(4) 0.077(4) 0.011(3) 0.038(3) 0.009(3) C82 0.056(3) 0.073(3) 0.057(3) 0.001(2) 0.028(3) 0.003(3) C83 0.048(3) 0.048(2) 0.050(3) -0.003(2) 0.024(2) 0.002(2) C84 0.050(3) 0.065(3) 0.063(3) 0.003(3) 0.021(3) 0.001(2) C85 0.048(3) 0.081(4) 0.081(4) -0.009(3) 0.015(3) -0.004(3) C86 0.055(4) 0.069(3) 0.089(4) -0.015(3) 0.031(3) -0.010(3) C87 0.083(4) 0.049(3) 0.071(4) -0.005(2) 0.048(3) -0.002(3) C88 0.053(3) 0.052(3) 0.052(3) -0.009(2) 0.023(2) 0.000(2) C89 0.056(3) 0.047(2) 0.045(3) -0.002(2) 0.021(2) -0.001(2) C90 0.069(4) 0.057(3) 0.059(3) 0.006(2) 0.034(3) 0.011(2) C91 0.090(4) 0.065(3) 0.048(3) 0.006(2) 0.040(3) 0.014(3) C92 0.062(3) 0.057(3) 0.047(3) 0.007(2) 0.018(2) 0.005(2) C93 0.058(3) 0.067(3) 0.052(3) 0.006(2) 0.022(3) 0.014(2) C94 0.052(3) 0.060(3) 0.047(3) 0.005(2) 0.019(2) 0.012(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 Ru1 N1 2.212(3) . ? Ru1 N2 2.218(3) . ? Ru1 P1 2.2787(12) . ? Ru1 P2 2.2858(12) . ? Ru1 Na1 3.0476(17) . ? Ru2 N3 2.198(3) . ? Ru2 N4 2.218(4) . ? Ru2 P3 2.2834(12) . ? Ru2 P4 2.2874(12) . ? Ru2 Na2 2.9933(18) . ? P1 C12 1.845(5) . ? P1 C18 1.846(5) . ? P1 C24 1.849(4) . ? P2 C30 1.849(4) . ? P2 C42 1.850(4) . ? P2 C36 1.854(4) . ? P3 C71 1.850(5) . ? P3 C65 1.852(4) . ? P3 C59 1.856(4) . ? P4 C77 1.843(5) . ? P4 C83 1.842(4) . ? P4 C89 1.856(4) . ? Na1 O2 2.275(4) . ? Na1 O1 2.314(4) . ? Na1 C37 2.969(5) . ? Na1 C25 3.024(5) . ? Na1 C36 3.085(5) . ? Na2 O4 2.230(4) . ? Na2 O3 2.293(4) . ? Na2 C70 2.842(5) . ? Na2 C94 2.955(5) . ? Na2 C65 3.061(5) . ? O1 C4S 1.434(7) . ? O1 C1S 1.440(7) . ? O2 C8S 1.416(5) . ? O2 C5S 1.423(6) . ? O3 C9S 1.434(6) . ? O3 C12S 1.443(6) . ? O4 C16S 1.434(6) . ? O4 C13S 1.437(6) . ? N1 C1 1.327(5) . ? N1 C11 1.353(5) . ? N2 C9 1.336(5) . ? N2 C10 1.354(5) . ? N3 C48 1.329(5) . ? N3 C58 1.349(6) . ? N4 C56 1.322(6) . ? N4 C57 1.365(6) . ? C1 C2 1.396(6) . ? C1S C2S 1.526(8) . ? C2 C3 1.373(6) . ? C2S C3S 1.439(8) . ? C3 C4 1.406(6) . ? C3S C4S 1.432(8) . ? C4 C5 1.414(6) . ? C4 C11 1.439(6) . ? C5 C6 1.426(6) . ? C5S C6S 1.512(7) . ? C6 C7 1.396(7) . ? C6 C10 1.436(6) . ? C6S C7S 1.497(7) . ? C7 C8 1.392(7) . ? C7S C8S 1.483(7) . ? C8 C9 1.427(6) . ? C9S C10S 1.481(7) . ? C10 C11 1.376(6) . ? C10S C11S 1.501(7) . ? C11S C12S 1.485(8) . ? C12 C17 1.382(7) . ? C12 C13 1.390(6) . ? C13 C14 1.391(7) . ? C13S C14S 1.498(8) . ? C14 C15 1.345(8) . ? C14S C15S 1.492(8) . ? C15S C16S 1.487(7) . ? C15 C16 1.376(9) . ? C16 C17 1.376(7) . ? C18 C19 1.372(7) . ? C18 C23 1.409(6) . ? C19 C20 1.392(6) . ? C20 C21 1.388(7) . ? C21 C22 1.377(7) . ? C22 C23 1.378(6) . ? C24 C29 1.390(6) . ? C24 C25 1.401(6) . ? C25 C26 1.380(6) . ? C26 C27 1.369(6) . ? C27 C28 1.370(6) . ? C28 C29 1.389(6) . ? C30 C31 1.384(6) . ? C30 C35 1.387(6) . ? C31 C32 1.392(6) . ? C32 C33 1.373(7) . ? C33 C34 1.383(7) . ? C34 C35 1.389(6) . ? C36 C41 1.378(6) . ? C36 C37 1.407(6) . ? C37 C38 1.380(6) . ? C38 C39 1.364(7) . ? C39 C40 1.378(8) . ? C40 C41 1.397(7) . ? C42 C43 1.380(6) . ? C42 C47 1.392(6) . ? C43 C44 1.392(7) . ? C44 C45 1.370(8) . ? C45 C46 1.372(7) . ? C46 C47 1.379(6) . ? C48 C49 1.404(6) . ? C49 C50 1.369(7) . ? C50 C51 1.412(7) . ? C51 C52 1.418(8) . ? C51 C58 1.429(6) . ? C52 C53 1.412(8) . ? C53 C54 1.398(8) . ? C53 C57 1.435(6) . ? C54 C55 1.390(8) . ? C55 C56 1.421(7) . ? C57 C58 1.381(6) . ? C59 C64 1.355(6) . ? C59 C60 1.379(6) . ? C60 C61 1.367(7) . ? C61 C62 1.356(8) . ? C62 C63 1.353(8) . ? C63 C64 1.396(7) . ? C65 C70 1.389(6) . ? C65 C66 1.404(6) . ? C66 C67 1.389(6) . ? C67 C68 1.364(7) . ? C68 C69 1.386(7) . ? C69 C70 1.413(6) . ? C71 C72 1.381(6) . ? C71 C76 1.398(6) . ? C72 C73 1.387(7) . ? C73 C74 1.372(7) . ? C74 C75 1.384(7) . ? C75 C76 1.379(7) . ? C77 C78 1.389(6) . ? C77 C82 1.395(6) . ? C78 C79 1.389(7) . ? C79 C80 1.391(8) . ? C80 C81 1.377(8) . ? C81 C82 1.386(7) . ? C83 C84 1.389(6) . ? C83 C88 1.399(6) . ? C84 C85 1.384(7) . ? C85 C86 1.379(7) . ? C86 C87 1.372(7) . ? C87 C88 1.391(6) . ? C89 C90 1.385(6) . ? C89 C94 1.395(6) . ? C90 C91 1.394(6) . ? C91 C92 1.365(6) . ? C92 C93 1.365(7) . ? C93 C94 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N2 80.64(13) . . ? N1 Ru1 P1 99.49(9) . . ? N2 Ru1 P1 91.55(10) . . ? N1 Ru1 P2 92.99(9) . . ? N2 Ru1 P2 96.14(9) . . ? P1 Ru1 P2 166.27(4) . . ? N1 Ru1 Na1 134.84(9) . . ? N2 Ru1 Na1 144.51(10) . . ? P1 Ru1 Na1 83.93(5) . . ? P2 Ru1 Na1 83.21(5) . . ? N3 Ru2 N4 80.58(14) . . ? N3 Ru2 P3 95.32(9) . . ? N4 Ru2 P3 98.66(9) . . ? N3 Ru2 P4 93.87(9) . . ? N4 Ru2 P4 94.15(10) . . ? P3 Ru2 P4 165.29(4) . . ? N3 Ru2 Na2 139.57(11) . . ? N4 Ru2 Na2 139.65(11) . . ? P3 Ru2 Na2 83.90(5) . . ? P4 Ru2 Na2 81.65(5) . . ? C12 P1 C18 102.5(2) . . ? C12 P1 C24 100.1(2) . . ? C18 P1 C24 101.26(19) . . ? C12 P1 Ru1 116.00(15) . . ? C18 P1 Ru1 116.53(16) . . ? C24 P1 Ru1 117.83(14) . . ? C30 P2 C42 100.9(2) . . ? C30 P2 C36 101.36(19) . . ? C42 P2 C36 100.64(19) . . ? C30 P2 Ru1 119.29(14) . . ? C42 P2 Ru1 117.15(15) . . ? C36 P2 Ru1 114.55(14) . . ? C71 P3 C65 100.4(2) . . ? C71 P3 C59 100.4(2) . . ? C65 P3 C59 101.6(2) . . ? C71 P3 Ru2 118.45(14) . . ? C65 P3 Ru2 115.36(15) . . ? C59 P3 Ru2 117.59(14) . . ? C77 P4 C83 101.9(2) . . ? C77 P4 C89 99.2(2) . . ? C83 P4 C89 100.4(2) . . ? C77 P4 Ru2 116.88(15) . . ? C83 P4 Ru2 115.70(15) . . ? C89 P4 Ru2 119.59(14) . . ? O2 Na1 O1 99.58(15) . . ? O2 Na1 C37 106.69(15) . . ? O1 Na1 C37 90.77(16) . . ? O2 Na1 C25 85.29(14) . . ? O1 Na1 C25 105.00(16) . . ? C37 Na1 C25 158.54(14) . . ? O2 Na1 Ru1 133.34(11) . . ? O1 Na1 Ru1 126.89(12) . . ? C37 Na1 Ru1 79.45(10) . . ? C25 Na1 Ru1 79.43(9) . . ? O2 Na1 C36 95.23(14) . . ? O1 Na1 C36 116.90(16) . . ? C37 Na1 C36 26.79(12) . . ? C25 Na1 C36 137.29(13) . . ? Ru1 Na1 C36 69.39(8) . . ? O4 Na2 O3 107.12(14) . . ? O4 Na2 C70 100.12(15) . . ? O3 Na2 C70 92.12(15) . . ? O4 Na2 C94 80.70(13) . . ? O3 Na2 C94 102.92(15) . . ? C70 Na2 C94 164.04(15) . . ? O4 Na2 Ru2 118.09(12) . . ? O3 Na2 Ru2 134.57(11) . . ? C70 Na2 Ru2 84.58(10) . . ? C94 Na2 Ru2 81.07(10) . . ? O4 Na2 C65 86.52(14) . . ? O3 Na2 C65 118.44(14) . . ? C70 Na2 C65 26.90(13) . . ? C94 Na2 C65 138.63(15) . . ? Ru2 Na2 C65 70.69(9) . . ? C4S O1 C1S 104.1(5) . . ? C4S O1 Na1 118.3(3) . . ? C1S O1 Na1 136.5(4) . . ? C8S O2 C5S 107.9(4) . . ? C8S O2 Na1 126.1(3) . . ? C5S O2 Na1 126.0(3) . . ? C9S O3 C12S 106.8(4) . . ? C9S O3 Na2 124.4(3) . . ? C12S O3 Na2 125.5(3) . . ? C16S O4 C13S 109.4(4) . . ? C16S O4 Na2 128.9(3) . . ? C13S O4 Na2 121.7(3) . . ? C1 N1 C11 114.6(4) . . ? C1 N1 Ru1 138.7(3) . . ? C11 N1 Ru1 106.3(3) . . ? C9 N2 C10 114.8(4) . . ? C9 N2 Ru1 139.0(3) . . ? C10 N2 Ru1 106.1(3) . . ? C48 N3 C58 115.7(4) . . ? C48 N3 Ru2 136.9(3) . . ? C58 N3 Ru2 107.3(3) . . ? C56 N4 C57 114.6(4) . . ? C56 N4 Ru2 139.3(3) . . ? C57 N4 Ru2 106.0(3) . . ? N1 C1 C2 122.5(4) . . ? O1 C1S C2S 102.3(5) . . ? C3 C2 C1 123.0(5) . . ? C3S C2S C1S 107.9(6) . . ? C2 C3 C4 117.7(4) . . ? C4S C3S C2S 104.0(6) . . ? C3 C4 C5 138.0(4) . . ? C3 C4 C11 114.5(4) . . ? C5 C4 C11 107.6(4) . . ? C3S C4S O1 111.0(6) . . ? C4 C5 C6 107.5(4) . . ? O2 C5S C6S 105.8(4) . . ? C7 C6 C5 137.8(4) . . ? C7 C6 C10 114.3(4) . . ? C5 C6 C10 107.8(4) . . ? C7S C6S C5S 102.7(4) . . ? C8 C7 C6 118.9(4) . . ? C8S C7S C6S 103.8(4) . . ? C7 C8 C9 121.3(5) . . ? O2 C8S C7S 109.4(4) . . ? N2 C9 C8 122.1(4) . . ? O3 C9S C10S 106.7(4) . . ? N2 C10 C11 123.4(4) . . ? N2 C10 C6 128.4(4) . . ? C11 C10 C6 108.1(4) . . ? C9S C10S C11S 102.2(5) . . ? N1 C11 C10 123.3(4) . . ? N1 C11 C4 127.7(4) . . ? C10 C11 C4 108.9(4) . . ? C12S C11S C10S 102.3(5) . . ? C17 C12 C13 117.5(4) . . ? C17 C12 P1 124.3(3) . . ? C13 C12 P1 118.0(4) . . ? O3 C12S C11S 108.1(4) . . ? C12 C13 C14 120.2(5) . . ? O4 C13S C14S 105.3(5) . . ? C15 C14 C13 121.5(5) . . ? C15S C14S C13S 102.4(5) . . ? C16S C15S C14S 103.7(5) . . ? C14 C15 C16 119.0(6) . . ? C15 C16 C17 120.5(6) . . ? O4 C16S C15S 106.1(4) . . ? C16 C17 C12 121.3(5) . . ? C19 C18 C23 119.2(4) . . ? C19 C18 P1 116.7(3) . . ? C23 C18 P1 124.1(4) . . ? C18 C19 C20 120.9(5) . . ? C21 C20 C19 119.5(5) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C23 120.8(5) . . ? C22 C23 C18 119.7(5) . . ? C29 C24 C25 116.6(4) . . ? C29 C24 P1 123.3(3) . . ? C25 C24 P1 120.1(3) . . ? C26 C25 C24 121.5(4) . . ? C26 C25 Na1 110.2(3) . . ? C24 C25 Na1 85.9(3) . . ? C27 C26 C25 120.5(4) . . ? C26 C27 C28 119.7(4) . . ? C27 C28 C29 120.0(4) . . ? C28 C29 C24 121.7(4) . . ? C31 C30 C35 117.8(4) . . ? C31 C30 P2 124.6(3) . . ? C35 C30 P2 117.6(3) . . ? C30 C31 C32 121.3(4) . . ? C33 C32 C31 119.9(5) . . ? C32 C33 C34 119.8(5) . . ? C33 C34 C35 119.8(5) . . ? C30 C35 C34 121.3(5) . . ? C41 C36 C37 117.6(4) . . ? C41 C36 P2 123.7(4) . . ? C37 C36 P2 118.5(3) . . ? C41 C36 Na1 103.3(3) . . ? C37 C36 Na1 72.0(3) . . ? P2 C36 Na1 89.56(16) . . ? C38 C37 C36 121.1(5) . . ? C38 C37 Na1 99.7(3) . . ? C36 C37 Na1 81.2(3) . . ? C39 C38 C37 121.0(5) . . ? C38 C39 C40 118.5(5) . . ? C39 C40 C41 121.5(5) . . ? C36 C41 C40 120.2(5) . . ? C43 C42 C47 119.0(4) . . ? C43 C42 P2 121.9(4) . . ? C47 C42 P2 119.1(3) . . ? C42 C43 C44 120.1(5) . . ? C45 C44 C43 120.3(5) . . ? C44 C45 C46 119.9(5) . . ? C45 C46 C47 120.4(5) . . ? C46 C47 C42 120.3(5) . . ? N3 C48 C49 121.4(5) . . ? C50 C49 C48 122.3(5) . . ? C49 C50 C51 119.2(5) . . ? C50 C51 C52 139.8(5) . . ? C50 C51 C58 113.3(5) . . ? C52 C51 C58 107.0(5) . . ? C53 C52 C51 108.3(5) . . ? C54 C53 C52 138.7(5) . . ? C54 C53 C57 113.8(5) . . ? C52 C53 C57 107.5(5) . . ? C55 C54 C53 118.9(5) . . ? C54 C55 C56 121.7(5) . . ? N4 C56 C55 122.3(5) . . ? N4 C57 C58 123.0(4) . . ? N4 C57 C53 128.7(5) . . ? C58 C57 C53 108.1(5) . . ? N3 C58 C57 122.8(4) . . ? N3 C58 C51 128.0(5) . . ? C57 C58 C51 109.1(4) . . ? C64 C59 C60 117.9(4) . . ? C64 C59 P3 125.4(4) . . ? C60 C59 P3 116.7(4) . . ? C61 C60 C59 121.1(5) . . ? C62 C61 C60 120.8(5) . . ? C63 C62 C61 119.0(5) . . ? C62 C63 C64 120.5(6) . . ? C59 C64 C63 120.6(5) . . ? C70 C65 C66 118.3(4) . . ? C70 C65 P3 119.6(3) . . ? C66 C65 P3 122.0(4) . . ? C70 C65 Na2 67.7(3) . . ? C66 C65 Na2 109.9(3) . . ? P3 C65 Na2 89.61(16) . . ? C67 C66 C65 120.7(5) . . ? C68 C67 C66 120.0(5) . . ? C67 C68 C69 121.6(5) . . ? C68 C69 C70 118.4(5) . . ? C65 C70 C69 121.0(5) . . ? C65 C70 Na2 85.4(3) . . ? C69 C70 Na2 102.4(3) . . ? C72 C71 C76 117.9(4) . . ? C72 C71 P3 118.4(3) . . ? C76 C71 P3 123.7(4) . . ? C71 C72 C73 120.7(5) . . ? C74 C73 C72 120.8(5) . . ? C73 C74 C75 119.4(5) . . ? C76 C75 C74 119.9(5) . . ? C75 C76 C71 121.3(5) . . ? C78 C77 C82 117.9(5) . . ? C78 C77 P4 123.3(4) . . ? C82 C77 P4 118.7(4) . . ? C77 C78 C79 121.2(5) . . ? C78 C79 C80 119.4(5) . . ? C81 C80 C79 120.5(5) . . ? C80 C81 C82 119.4(5) . . ? C81 C82 C77 121.6(5) . . ? C84 C83 C88 117.9(4) . . ? C84 C83 P4 123.8(4) . . ? C88 C83 P4 117.9(3) . . ? C85 C84 C83 121.0(5) . . ? C86 C85 C84 120.5(5) . . ? C87 C86 C85 119.5(5) . . ? C86 C87 C88 120.4(5) . . ? C87 C88 C83 120.7(5) . . ? C90 C89 C94 117.5(4) . . ? C90 C89 P4 122.7(3) . . ? C94 C89 P4 119.7(4) . . ? C89 C90 C91 120.5(4) . . ? C92 C91 C90 121.1(5) . . ? C91 C92 C93 119.0(4) . . ? C92 C93 C94 120.8(5) . . ? C93 C94 C89 121.0(5) . . ? C93 C94 Na2 114.1(3) . . ? C89 C94 Na2 88.0(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.091 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.083