# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Wa-Hung Leung' _publ_contact_author_email chleung@ust.hk _publ_section_title ; Synthesis, Structures and Reactivity of Ruthenium Nitrosyl Complexes Containing Klaui's Oxygen Tripodal Ligand ; loop_ _publ_author_name H.-F.Ip X.-Y.Yi W.-Y.Wong I.Williams 'Wa-Hung Leung' # Attachment '- cif-re3.cif' data_wy1942wm_Compound5 _database_code_depnum_ccdc_archive 'CCDC 725289' #TrackingRef '- cif-re3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H38 Cl2 Co N O9 P3 Ru' _chemical_formula_weight 748.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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)/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 11.9048(10) _cell_length_b 16.9791(14) _cell_length_c 14.2772(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.6600(10) _cell_angle_gamma 90.00 _cell_volume 2880.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7848 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16649 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.26 _reflns_number_total 6951 _reflns_number_gt 5134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0295P)^2^+1.0741P] 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 6951 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.004 _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 C1 C 0.4299(3) 0.0444(2) 0.2298(2) 0.0326(8) Uani 1 1 d . . . H1A H 0.3722 0.0024 0.2269 0.039 Uiso 1 1 calc R . . H1B H 0.4407 0.0623 0.1650 0.039 Uiso 1 1 calc R . . C2 C 0.3915(3) 0.1112(2) 0.2864(3) 0.0401(9) Uani 1 1 d . . . H2A H 0.3206 0.1319 0.2576 0.060 Uiso 1 1 calc R . . H2B H 0.4486 0.1529 0.2887 0.060 Uiso 1 1 calc R . . H2C H 0.3799 0.0931 0.3502 0.060 Uiso 1 1 calc R . . C3 C 0.5722(3) -0.11808(19) 0.0609(2) 0.0274(7) Uani 1 1 d . . . H3A H 0.6353 -0.0894 0.0344 0.033 Uiso 1 1 calc R . . H3B H 0.5029 -0.1075 0.0208 0.033 Uiso 1 1 calc R . . C4 C 0.5963(3) -0.2047(2) 0.0629(3) 0.0421(10) Uani 1 1 d . . . H4A H 0.6059 -0.2234 -0.0011 0.063 Uiso 1 1 calc R . . H4B H 0.5334 -0.2327 0.0888 0.063 Uiso 1 1 calc R . . H4C H 0.6654 -0.2147 0.1021 0.063 Uiso 1 1 calc R . . C5 C 0.6652(3) 0.13591(19) 0.4672(2) 0.0294(8) Uani 1 1 d . . . H5A H 0.6308 0.1617 0.4101 0.035 Uiso 1 1 calc R . . H5B H 0.7069 0.1763 0.5054 0.035 Uiso 1 1 calc R . . C6 C 0.5758(3) 0.1002(2) 0.5222(3) 0.0372(9) Uani 1 1 d . . . H6A H 0.5239 0.1414 0.5404 0.056 Uiso 1 1 calc R . . H6B H 0.6105 0.0750 0.5786 0.056 Uiso 1 1 calc R . . H6C H 0.5344 0.0607 0.4837 0.056 Uiso 1 1 calc R . . C7 C 0.9529(3) 0.1650(2) 0.4000(3) 0.0317(8) Uani 1 1 d . . . H7A H 0.9599 0.1667 0.4695 0.038 Uiso 1 1 calc R . . H7B H 0.8924 0.2018 0.3780 0.038 Uiso 1 1 calc R . . C8 C 1.0617(3) 0.1893(2) 0.3618(2) 0.0377(9) Uani 1 1 d . . . H8A H 1.0805 0.2430 0.3825 0.057 Uiso 1 1 calc R . . H8B H 1.0543 0.1877 0.2931 0.057 Uiso 1 1 calc R . . H8C H 1.1215 0.1532 0.3847 0.057 Uiso 1 1 calc R . . C9 C 1.0956(3) -0.00279(19) 0.2398(2) 0.0249(7) Uani 1 1 d . . . H9A H 1.0650 0.0513 0.2423 0.030 Uiso 1 1 calc R . . H9B H 1.1603 -0.0019 0.1996 0.030 Uiso 1 1 calc R . . C10 C 1.1350(3) -0.0288(2) 0.3374(2) 0.0312(8) Uani 1 1 d . . . H10A H 1.1927 0.0076 0.3634 0.047 Uiso 1 1 calc R . . H10B H 1.1666 -0.0820 0.3348 0.047 Uiso 1 1 calc R . . H10C H 1.0711 -0.0291 0.3775 0.047 Uiso 1 1 calc R . . C11 C 0.9085(3) -0.0939(2) 0.0115(2) 0.0321(8) Uani 1 1 d . . . H11A H 0.9867 -0.1121 0.0257 0.039 Uiso 1 1 calc R . . H11B H 0.9110 -0.0400 -0.0147 0.039 Uiso 1 1 calc R . . C12 C 0.8494(3) -0.1480(2) -0.0584(2) 0.0339(8) Uani 1 1 d . . . H12A H 0.8899 -0.1489 -0.1161 0.051 Uiso 1 1 calc R . . H12B H 0.7724 -0.1293 -0.0728 0.051 Uiso 1 1 calc R . . H12C H 0.8473 -0.2013 -0.0322 0.051 Uiso 1 1 calc R . . C13 C 0.8401(3) -0.0989(2) 0.4194(2) 0.0292(8) Uani 1 1 d . . . H13A H 0.8904 -0.0700 0.4665 0.035 Uiso 1 1 calc R . . C14 C 0.8754(3) -0.14598(18) 0.3453(2) 0.0293(8) Uani 1 1 d . . . H14A H 0.9550 -0.1561 0.3304 0.035 Uiso 1 1 calc R . . C15 C 0.7778(3) -0.17715(18) 0.2964(2) 0.0270(7) Uani 1 1 d . . . H15A H 0.7766 -0.2130 0.2407 0.032 Uiso 1 1 calc R . . C16 C 0.6835(3) -0.15013(18) 0.3411(2) 0.0274(7) Uani 1 1 d . . . H16A H 0.6032 -0.1631 0.3223 0.033 Uiso 1 1 calc R . . C17 C 0.7210(3) -0.10133(19) 0.4169(2) 0.0292(8) Uani 1 1 d . . . H17A H 0.6724 -0.0745 0.4617 0.035 Uiso 1 1 calc R . . C18 C 0.7342(3) 0.15289(17) -0.0831(2) 0.0219(7) Uani 1 1 d . . . C19 C 0.7175(3) 0.1722(2) -0.1828(2) 0.0358(9) Uani 1 1 d . . . H19A H 0.6600 0.1374 -0.2125 0.054 Uiso 1 1 calc R . . H19B H 0.7884 0.1652 -0.2130 0.054 Uiso 1 1 calc R . . H19C H 0.6927 0.2271 -0.1897 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.59554(7) 0.21656(4) 0.13548(5) 0.02339(16) Uani 1 1 d . . . Cl2 Cl 0.87951(7) 0.23558(4) 0.14235(5) 0.02443(17) Uani 1 1 d . . . N1 N 0.7439(2) 0.13999(14) -0.00520(17) 0.0192(5) Uani 1 1 d . . . O1 O 0.64391(17) 0.03846(11) 0.12508(13) 0.0182(4) Uani 1 1 d . . . O2 O 0.74560(17) 0.13104(11) 0.27990(13) 0.0186(4) Uani 1 1 d . . . O3 O 0.88092(17) 0.05182(11) 0.13771(13) 0.0177(4) Uani 1 1 d . . . O4 O 0.53521(17) 0.01365(13) 0.27185(14) 0.0228(5) Uani 1 1 d . . . O5 O 0.55777(18) -0.09109(12) 0.15689(14) 0.0248(5) Uani 1 1 d . . . O6 O 0.7413(2) 0.07467(13) 0.44120(14) 0.0272(5) Uani 1 1 d . . . O7 O 0.92447(18) 0.08459(12) 0.36822(14) 0.0233(5) Uani 1 1 d . . . O8 O 1.00953(17) -0.05525(11) 0.19903(14) 0.0200(4) Uani 1 1 d . . . O9 O 0.84762(17) -0.09353(12) 0.09717(13) 0.0202(5) Uani 1 1 d . . . P1 P 0.62644(7) -0.01943(4) 0.20480(5) 0.01701(16) Uani 1 1 d . . . P2 P 0.79432(7) 0.06580(4) 0.34265(5) 0.01610(16) Uani 1 1 d . . . P3 P 0.88030(6) -0.03125(4) 0.17796(5) 0.01525(15) Uani 1 1 d . . . Co1 Co 0.77374(3) -0.05421(2) 0.29258(3) 0.01563(9) Uani 1 1 d . . . Ru1 Ru 0.74957(2) 0.133138(13) 0.135074(15) 0.01475(6) 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 C1 0.0189(17) 0.039(2) 0.039(2) -0.0048(16) -0.0038(15) 0.0077(15) C2 0.033(2) 0.039(2) 0.048(2) -0.0057(17) 0.0014(17) 0.0110(17) C3 0.0295(19) 0.0258(18) 0.0262(16) -0.0034(13) -0.0029(14) -0.0040(14) C4 0.052(3) 0.0251(19) 0.047(2) -0.0102(16) -0.0142(19) 0.0009(17) C5 0.037(2) 0.0220(17) 0.0305(17) -0.0049(14) 0.0158(15) 0.0032(15) C6 0.038(2) 0.0283(19) 0.047(2) -0.0032(16) 0.0190(18) -0.0015(16) C7 0.0282(19) 0.0254(18) 0.040(2) -0.0137(15) -0.0107(16) 0.0012(14) C8 0.049(2) 0.032(2) 0.0304(18) -0.0004(15) -0.0037(17) -0.0149(17) C9 0.0187(17) 0.0272(17) 0.0286(17) 0.0008(13) 0.0006(13) -0.0015(13) C10 0.0274(19) 0.036(2) 0.0292(18) -0.0018(15) -0.0034(15) 0.0051(15) C11 0.041(2) 0.037(2) 0.0196(16) -0.0067(14) 0.0142(15) -0.0093(16) C12 0.045(2) 0.036(2) 0.0209(16) -0.0080(14) 0.0048(15) -0.0040(16) C13 0.040(2) 0.0261(18) 0.0208(16) 0.0114(13) -0.0036(14) 0.0006(15) C14 0.0296(19) 0.0241(18) 0.0349(18) 0.0165(14) 0.0071(15) 0.0103(14) C15 0.040(2) 0.0162(15) 0.0252(16) 0.0054(13) 0.0068(15) 0.0035(14) C16 0.0277(18) 0.0228(17) 0.0316(18) 0.0140(13) 0.0010(14) -0.0028(13) C17 0.043(2) 0.0254(17) 0.0210(16) 0.0100(13) 0.0131(15) 0.0030(15) C18 0.0274(18) 0.0161(15) 0.0224(16) -0.0006(12) 0.0039(13) -0.0014(12) C19 0.066(3) 0.0282(19) 0.0136(15) 0.0029(13) 0.0010(16) -0.0014(18) Cl1 0.0273(4) 0.0197(4) 0.0226(4) 0.0014(3) -0.0020(3) 0.0053(3) Cl2 0.0282(4) 0.0190(4) 0.0260(4) 0.0008(3) 0.0013(3) -0.0072(3) N1 0.0237(14) 0.0156(12) 0.0185(12) 0.0017(10) 0.0017(10) 0.0006(10) O1 0.0222(11) 0.0164(11) 0.0157(10) 0.0014(8) -0.0017(8) -0.0024(8) O2 0.0269(12) 0.0143(10) 0.0144(9) 0.0010(8) 0.0001(8) 0.0020(9) O3 0.0208(11) 0.0150(10) 0.0177(10) 0.0013(8) 0.0037(8) 0.0004(8) O4 0.0186(12) 0.0287(12) 0.0211(11) 0.0015(9) 0.0023(9) 0.0045(9) O5 0.0285(13) 0.0221(12) 0.0239(11) -0.0014(9) 0.0030(9) -0.0092(9) O6 0.0391(14) 0.0291(13) 0.0143(10) 0.0023(9) 0.0084(10) 0.0159(10) O7 0.0225(12) 0.0204(11) 0.0265(11) -0.0046(9) -0.0034(9) 0.0026(9) O8 0.0184(11) 0.0172(10) 0.0243(11) -0.0021(8) 0.0006(9) 0.0006(8) O9 0.0254(12) 0.0194(11) 0.0162(10) -0.0032(8) 0.0051(9) -0.0030(9) P1 0.0187(4) 0.0153(4) 0.0171(4) 0.0014(3) 0.0016(3) -0.0010(3) P2 0.0202(4) 0.0168(4) 0.0114(3) 0.0003(3) 0.0015(3) 0.0031(3) P3 0.0181(4) 0.0141(4) 0.0137(3) -0.0007(3) 0.0023(3) 0.0001(3) Co1 0.0192(2) 0.01404(19) 0.01388(18) 0.00264(15) 0.00316(15) 0.00194(16) Ru1 0.01961(12) 0.01255(11) 0.01193(10) 0.00109(9) -0.00016(8) -0.00068(10) _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 C1 O4 1.452(4) . ? C1 C2 1.481(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O5 1.466(4) . ? C3 C4 1.499(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O6 1.443(4) . ? C5 C6 1.491(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O7 1.471(4) . ? C7 C8 1.495(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O8 1.451(4) . ? C9 C10 1.508(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O9 1.461(3) . ? C11 C12 1.499(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.411(5) . ? C13 C17 1.416(5) . ? C13 Co1 2.072(3) . ? C13 H13A 1.0000 . ? C14 C15 1.419(5) . ? C14 Co1 2.084(3) . ? C14 H14A 1.0000 . ? C15 C16 1.404(5) . ? C15 Co1 2.089(3) . ? C15 H15A 1.0000 . ? C16 C17 1.413(5) . ? C16 Co1 2.093(3) . ? C16 H16A 1.0000 . ? C17 Co1 2.080(3) . ? C17 H17A 1.0000 . ? C18 N1 1.133(4) . ? C18 C19 1.461(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Cl1 Ru1 2.3173(8) . ? Cl2 Ru1 2.3257(8) . ? N1 Ru1 2.003(2) . ? O1 P1 1.528(2) . ? O1 Ru1 2.0406(19) . ? O2 P2 1.516(2) . ? O2 Ru1 2.0716(18) . ? O3 P3 1.523(2) . ? O3 Ru1 2.085(2) . ? O4 P1 1.595(2) . ? O5 P1 1.595(2) . ? O6 P2 1.586(2) . ? O7 P2 1.601(2) . ? O8 P3 1.601(2) . ? O9 P3 1.595(2) . ? P1 Co1 2.1712(9) . ? P2 Co1 2.1681(8) . ? P3 Co1 2.1690(8) . ? 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 O4 C1 C2 109.8(3) . . ? O4 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O4 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O5 C3 C4 108.8(3) . . ? O5 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? O5 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O6 C5 C6 108.9(3) . . ? O6 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O6 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O7 C7 C8 109.4(3) . . ? O7 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O7 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? 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 . . ? O8 C9 C10 111.1(3) . . ? O8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? O8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C11 C12 108.9(3) . . ? O9 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O9 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 108.0(3) . . ? C14 C13 Co1 70.61(18) . . ? C17 C13 Co1 70.36(18) . . ? C14 C13 H13A 126.0 . . ? C17 C13 H13A 126.0 . . ? Co1 C13 H13A 126.0 . . ? C13 C14 C15 107.9(3) . . ? C13 C14 Co1 69.69(18) . . ? C15 C14 Co1 70.30(18) . . ? C13 C14 H14A 126.1 . . ? C15 C14 H14A 126.1 . . ? Co1 C14 H14A 126.1 . . ? C16 C15 C14 107.9(3) . . ? C16 C15 Co1 70.57(18) . . ? C14 C15 Co1 69.94(18) . . ? C16 C15 H15A 126.0 . . ? C14 C15 H15A 126.0 . . ? Co1 C15 H15A 126.0 . . ? C15 C16 C17 108.5(3) . . ? C15 C16 Co1 70.20(18) . . ? C17 C16 Co1 69.69(18) . . ? C15 C16 H16A 125.8 . . ? C17 C16 H16A 125.8 . . ? Co1 C16 H16A 125.8 . . ? C16 C17 C13 107.7(3) . . ? C16 C17 Co1 70.74(17) . . ? C13 C17 Co1 69.76(17) . . ? C16 C17 H17A 126.1 . . ? C13 C17 H17A 126.1 . . ? Co1 C17 H17A 126.1 . . ? N1 C18 C19 177.3(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 N1 Ru1 171.2(2) . . ? P1 O1 Ru1 124.56(11) . . ? P2 O2 Ru1 124.75(11) . . ? P3 O3 Ru1 126.76(12) . . ? C1 O4 P1 118.80(19) . . ? C3 O5 P1 123.50(19) . . ? C5 O6 P2 126.05(19) . . ? C7 O7 P2 117.11(19) . . ? C9 O8 P3 124.35(19) . . ? C11 O9 P3 119.84(19) . . ? O1 P1 O5 105.17(11) . . ? O1 P1 O4 110.54(12) . . ? O5 P1 O4 100.14(12) . . ? O1 P1 Co1 117.49(9) . . ? O5 P1 Co1 114.39(9) . . ? O4 P1 Co1 107.76(8) . . ? O2 P2 O6 107.22(11) . . ? O2 P2 O7 108.50(12) . . ? O6 P2 O7 102.28(12) . . ? O2 P2 Co1 117.44(8) . . ? O6 P2 Co1 109.81(9) . . ? O7 P2 Co1 110.48(8) . . ? O3 P3 O9 110.37(11) . . ? O3 P3 O8 106.19(11) . . ? O9 P3 O8 98.87(11) . . ? O3 P3 Co1 117.92(8) . . ? O9 P3 Co1 107.41(8) . . ? O8 P3 Co1 114.44(8) . . ? C13 Co1 C17 39.88(13) . . ? C13 Co1 C14 39.71(13) . . ? C17 Co1 C14 66.67(13) . . ? C13 Co1 C15 66.73(13) . . ? C17 Co1 C15 66.50(13) . . ? C14 Co1 C15 39.77(13) . . ? C13 Co1 C16 66.51(14) . . ? C17 Co1 C16 39.57(13) . . ? C14 Co1 C16 66.26(13) . . ? C15 Co1 C16 39.24(13) . . ? C13 Co1 P2 91.55(10) . . ? C17 Co1 P2 96.56(10) . . ? C14 Co1 P2 122.20(10) . . ? C15 Co1 P2 158.26(9) . . ? C16 Co1 P2 132.20(10) . . ? C13 Co1 P3 121.09(10) . . ? C17 Co1 P3 159.36(10) . . ? C14 Co1 P3 93.03(9) . . ? C15 Co1 P3 100.68(9) . . ? C16 Co1 P3 136.61(10) . . ? P2 Co1 P3 91.18(3) . . ? C13 Co1 P1 148.50(10) . . ? C17 Co1 P1 108.70(10) . . ? C14 Co1 P1 147.23(10) . . ? C15 Co1 P1 107.66(10) . . ? C16 Co1 P1 89.41(10) . . ? P2 Co1 P1 90.27(3) . . ? P3 Co1 P1 90.30(3) . . ? N1 Ru1 O1 89.69(9) . . ? N1 Ru1 O2 176.01(9) . . ? O1 Ru1 O2 90.17(8) . . ? N1 Ru1 O3 91.94(9) . . ? O1 Ru1 O3 86.43(8) . . ? O2 Ru1 O3 92.03(8) . . ? N1 Ru1 Cl1 89.48(7) . . ? O1 Ru1 Cl1 89.85(6) . . ? O2 Ru1 Cl1 86.53(6) . . ? O3 Ru1 Cl1 176.01(6) . . ? N1 Ru1 Cl2 88.92(7) . . ? O1 Ru1 Cl2 176.05(6) . . ? O2 Ru1 Cl2 91.48(6) . . ? O3 Ru1 Cl2 89.92(6) . . ? Cl1 Ru1 Cl2 93.84(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.766 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.103 ### end data_ip21cult_Compound10 _database_code_depnum_ccdc_archive 'CCDC 725291' #TrackingRef '- cif-re3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H42 Cl2 Co N O9 P3 Ru' _chemical_formula_weight 800.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1030(3) _cell_length_b 12.3909(3) _cell_length_c 22.2152(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.052(4) _cell_angle_gamma 90.00 _cell_volume 3245.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4396 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 71.40 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 11.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16253 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 72.42 _reflns_number_total 6117 _reflns_number_gt 4956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. In this complex, the Cp ring of the LOEt- ligand was found to be rotationa- lly disordered. The distance between carbon atoms of Cp ring is restrained by SADI commend. ; _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^)+(0.0850P)^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 6117 _refine_ls_number_parameters 356 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.69385(2) 0.33795(2) 0.275276(13) 0.01921(11) Uani 1 1 d . A . Co1 Co 0.47373(6) 0.33019(6) 0.38040(3) 0.02752(19) Uani 1 1 d . . . Cl1 Cl 0.81388(8) 0.48145(8) 0.26828(5) 0.0291(2) Uani 1 1 d . . . Cl2 Cl 0.64911(9) 0.31375(9) 0.16854(5) 0.0299(2) Uani 1 1 d . . . P1 P 0.46541(9) 0.44390(9) 0.30616(5) 0.0260(2) Uani 1 1 d . A . P2 P 0.65313(9) 0.36468(9) 0.41271(5) 0.0259(2) Uani 1 1 d . A . P3 P 0.50557(9) 0.19717(9) 0.32315(5) 0.0238(2) Uani 1 1 d . A . O1 O 0.3488(3) 0.4330(3) 0.25583(16) 0.0385(8) Uani 1 1 d . . . O2 O 0.4511(3) 0.5608(3) 0.33411(16) 0.0371(8) Uani 1 1 d . . . O3 O 0.6757(3) 0.4824(3) 0.44233(16) 0.0361(8) Uani 1 1 d . . . O4 O 0.6996(3) 0.2903(3) 0.47113(15) 0.0374(8) Uani 1 1 d . . . O5 O 0.5282(3) 0.0882(3) 0.36222(15) 0.0318(7) Uani 1 1 d . . . O6 O 0.3915(3) 0.1656(2) 0.27570(15) 0.0294(7) Uani 1 1 d . . . O7 O 0.5610(2) 0.4479(2) 0.27308(14) 0.0271(7) Uani 1 1 d . . . O8 O 0.7324(2) 0.3506(2) 0.36973(13) 0.0250(6) Uani 1 1 d . . . O9 O 0.5988(2) 0.2078(2) 0.28801(14) 0.0247(6) Uani 1 1 d . . . N1 N 0.8248(3) 0.2266(3) 0.27529(16) 0.0245(7) Uani 1 1 d . . . H1B H 0.7914 0.1624 0.2602 0.029 Uiso 1 1 calc R A . H1C H 0.8648 0.2508 0.2473 0.029 Uiso 1 1 calc R . . C1 C 0.3479(11) 0.4119(10) 0.4134(6) 0.044(3) Uiso 0.50 1 d PD A 1 H1A H 0.3191 0.4870 0.4038 0.053 Uiso 0.50 1 calc PR A 1 C2 C 0.4323(11) 0.3767(10) 0.4628(6) 0.043(3) Uiso 0.50 1 d PD A 1 H2A H 0.4801 0.4268 0.4933 0.051 Uiso 0.50 1 calc PR A 1 C3 C 0.4483(9) 0.2650(9) 0.4638(5) 0.038(3) Uiso 0.50 1 d PD A 1 H3A H 0.5028 0.2214 0.4950 0.045 Uiso 0.50 1 calc PR A 1 C4 C 0.3649(9) 0.2274(7) 0.4146(5) 0.0276(19) Uiso 0.50 1 d PD A 1 H4A H 0.3498 0.1499 0.4029 0.033 Uiso 0.50 1 calc PR A 1 C5 C 0.3060(10) 0.3157(11) 0.3840(5) 0.044(3) Uiso 0.50 1 d PD A 1 H5A H 0.2413 0.3108 0.3470 0.053 Uiso 0.50 1 calc PR A 1 C1A C 0.4543(9) 0.3488(9) 0.4718(5) 0.030(2) Uiso 0.50 1 d PD A 2 H1AA H 0.5135 0.3656 0.5100 0.036 Uiso 0.50 1 calc PR A 2 C2A C 0.4161(10) 0.2452(8) 0.4464(6) 0.037(2) Uiso 0.50 1 d PD A 2 H2AA H 0.4490 0.1749 0.4641 0.044 Uiso 0.50 1 calc PR A 2 C3A C 0.3266(8) 0.2542(9) 0.3930(5) 0.0279(19) Uiso 0.50 1 d PD A 2 H3AA H 0.2854 0.1935 0.3679 0.034 Uiso 0.50 1 calc PR A 2 C4A C 0.3047(8) 0.3659(9) 0.3832(4) 0.030(2) Uiso 0.50 1 d PD A 2 H4AA H 0.2458 0.3996 0.3497 0.035 Uiso 0.50 1 calc PR A 2 C5A C 0.3813(8) 0.4207(7) 0.4322(5) 0.024(2) Uiso 0.50 1 d PD A 2 H5AA H 0.3859 0.5010 0.4363 0.029 Uiso 0.50 1 calc PR A 2 C11 C 0.3414(5) 0.4036(5) 0.1933(3) 0.0530(15) Uani 1 1 d . A . H11A H 0.3038 0.3325 0.1849 0.064 Uiso 1 1 calc R . . H11B H 0.4185 0.3975 0.1855 0.064 Uiso 1 1 calc R . . C12 C 0.2763(7) 0.4853(6) 0.1521(3) 0.078(2) Uani 1 1 d . . . H12A H 0.2721 0.4650 0.1090 0.117 Uiso 1 1 calc R A . H12B H 0.3138 0.5556 0.1605 0.117 Uiso 1 1 calc R . . H12C H 0.1995 0.4899 0.1593 0.117 Uiso 1 1 calc R . . C13 C 0.4323(5) 0.6540(4) 0.2933(3) 0.0432(13) Uani 1 1 d . A . H13A H 0.3507 0.6601 0.2732 0.052 Uiso 1 1 calc R . . H13B H 0.4754 0.6459 0.2607 0.052 Uiso 1 1 calc R . . C14 C 0.4705(7) 0.7528(5) 0.3305(4) 0.0686(19) Uani 1 1 d . . . H14A H 0.4580 0.8163 0.3035 0.103 Uiso 1 1 calc R A . H14B H 0.5514 0.7466 0.3499 0.103 Uiso 1 1 calc R . . H14C H 0.4272 0.7605 0.3626 0.103 Uiso 1 1 calc R . . C15 C 0.7297(4) 0.5679(4) 0.4152(2) 0.0381(11) Uani 1 1 d . . . H15A H 0.7023 0.6385 0.4267 0.046 Uiso 1 1 calc R . . H15B H 0.7083 0.5616 0.3696 0.046 Uiso 1 1 calc R . . C16 C 0.8579(5) 0.5630(5) 0.4367(3) 0.0481(13) Uani 1 1 d . . . H16A H 0.8919 0.6214 0.4173 0.072 Uiso 1 1 calc R . . H16B H 0.8852 0.4933 0.4249 0.072 Uiso 1 1 calc R . . H16C H 0.8793 0.5710 0.4817 0.072 Uiso 1 1 calc R . . C17 C 0.8213(5) 0.2961(5) 0.5010(2) 0.0460(13) Uani 1 1 d . . . H17A H 0.8372 0.3626 0.5262 0.055 Uiso 1 1 calc R . . H17B H 0.8670 0.2978 0.4693 0.055 Uiso 1 1 calc R . . C18 C 0.8515(6) 0.1999(5) 0.5409(3) 0.0588(16) Uani 1 1 d . . . H18A H 0.9322 0.2026 0.5612 0.088 Uiso 1 1 calc R . . H18B H 0.8359 0.1345 0.5156 0.088 Uiso 1 1 calc R . . H18C H 0.8062 0.1990 0.5723 0.088 Uiso 1 1 calc R . . C19 C 0.6405(4) 0.0487(4) 0.3889(2) 0.0403(12) Uani 1 1 d . A . H19A H 0.6928 0.1101 0.4020 0.048 Uiso 1 1 calc R . . H19B H 0.6691 0.0060 0.3580 0.048 Uiso 1 1 calc R . . C20 C 0.6356(6) -0.0196(6) 0.4429(3) 0.070(2) Uani 1 1 d . . . H20A H 0.7116 -0.0470 0.4615 0.105 Uiso 1 1 calc R A . H20B H 0.5841 -0.0804 0.4296 0.105 Uiso 1 1 calc R . . H20C H 0.6078 0.0234 0.4735 0.105 Uiso 1 1 calc R . . C21 C 0.3954(4) 0.0741(4) 0.2344(2) 0.0332(10) Uani 1 1 d . A . H21A H 0.3302 0.0258 0.2341 0.040 Uiso 1 1 calc R . . H21B H 0.4659 0.0324 0.2499 0.040 Uiso 1 1 calc R . . C22 C 0.3918(5) 0.1118(5) 0.1700(2) 0.0467(13) Uani 1 1 d . . . H22A H 0.3939 0.0492 0.1433 0.070 Uiso 1 1 calc R A . H22B H 0.4575 0.1581 0.1700 0.070 Uiso 1 1 calc R . . H22C H 0.3219 0.1526 0.1545 0.070 Uiso 1 1 calc R . . C31 C 0.9057(3) 0.2027(4) 0.3317(2) 0.0261(9) Uani 1 1 d . A . C32 C 0.9808(4) 0.2819(4) 0.3607(2) 0.0359(11) Uani 1 1 d . . . H32A H 0.9799 0.3517 0.3429 0.043 Uiso 1 1 calc R A . C33 C 1.0566(4) 0.2582(5) 0.4157(3) 0.0457(14) Uani 1 1 d . A . H33A H 1.1079 0.3121 0.4355 0.055 Uiso 1 1 calc R . . C34 C 1.0586(5) 0.1577(5) 0.4418(3) 0.0531(16) Uani 1 1 d . . . H34A H 1.1101 0.1421 0.4798 0.064 Uiso 1 1 calc R A . C35 C 0.9841(5) 0.0789(5) 0.4119(3) 0.0508(14) Uani 1 1 d . A . H35A H 0.9856 0.0089 0.4295 0.061 Uiso 1 1 calc R . . C36 C 0.9089(4) 0.1009(4) 0.3574(2) 0.0365(11) Uani 1 1 d . . . H36A H 0.8589 0.0462 0.3373 0.044 Uiso 1 1 calc R A . 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 0.02141(17) 0.02147(18) 0.01621(18) -0.00068(11) 0.00730(12) -0.00084(11) Co1 0.0302(4) 0.0313(4) 0.0260(4) -0.0041(3) 0.0168(3) -0.0036(3) Cl1 0.0303(5) 0.0266(5) 0.0321(6) 0.0016(4) 0.0108(4) -0.0069(4) Cl2 0.0387(5) 0.0352(6) 0.0158(5) -0.0029(4) 0.0065(4) -0.0013(4) P1 0.0257(5) 0.0268(6) 0.0271(6) -0.0027(4) 0.0095(4) 0.0034(4) P2 0.0320(5) 0.0292(6) 0.0184(5) -0.0035(4) 0.0097(4) -0.0028(4) P3 0.0258(5) 0.0238(5) 0.0239(6) -0.0011(4) 0.0101(4) -0.0034(4) O1 0.0247(16) 0.051(2) 0.038(2) -0.0014(16) 0.0041(14) 0.0050(14) O2 0.0466(19) 0.0296(17) 0.040(2) -0.0068(14) 0.0196(16) 0.0035(15) O3 0.0462(19) 0.0344(18) 0.0318(19) -0.0134(14) 0.0175(15) -0.0088(15) O4 0.0433(19) 0.044(2) 0.0244(18) 0.0033(15) 0.0074(15) -0.0059(16) O5 0.0345(16) 0.0331(17) 0.0295(17) 0.0061(14) 0.0108(13) -0.0026(13) O6 0.0261(15) 0.0293(16) 0.0330(18) -0.0067(13) 0.0073(13) -0.0046(12) O7 0.0280(15) 0.0262(16) 0.0293(17) 0.0055(12) 0.0115(13) 0.0084(12) O8 0.0263(14) 0.0298(16) 0.0190(15) -0.0047(12) 0.0057(12) -0.0014(12) O9 0.0308(15) 0.0220(14) 0.0251(16) -0.0019(12) 0.0140(13) -0.0017(12) N1 0.0288(18) 0.0240(18) 0.0218(19) -0.0033(14) 0.0079(15) 0.0047(14) C11 0.048(3) 0.064(4) 0.043(3) -0.011(3) 0.001(3) 0.017(3) C12 0.103(6) 0.095(5) 0.043(4) 0.014(4) 0.029(4) 0.061(5) C13 0.047(3) 0.031(3) 0.055(4) 0.008(2) 0.020(3) 0.002(2) C14 0.090(5) 0.036(3) 0.078(5) -0.008(3) 0.017(4) 0.001(3) C15 0.049(3) 0.028(2) 0.038(3) -0.009(2) 0.012(2) -0.005(2) C16 0.048(3) 0.050(3) 0.045(3) -0.006(3) 0.007(3) -0.016(3) C17 0.049(3) 0.061(3) 0.024(3) 0.008(2) 0.000(2) -0.006(3) C18 0.072(4) 0.061(4) 0.035(3) 0.007(3) -0.004(3) 0.001(3) C19 0.041(3) 0.040(3) 0.039(3) 0.006(2) 0.007(2) 0.009(2) C20 0.081(5) 0.063(4) 0.055(4) 0.030(3) -0.005(3) 0.000(4) C21 0.030(2) 0.033(2) 0.037(3) -0.009(2) 0.011(2) -0.0096(19) C22 0.064(3) 0.044(3) 0.035(3) -0.005(2) 0.016(3) -0.008(3) C31 0.0186(18) 0.030(2) 0.029(2) -0.0049(18) 0.0037(17) 0.0034(16) C32 0.031(2) 0.042(3) 0.037(3) -0.009(2) 0.013(2) -0.001(2) C33 0.027(2) 0.070(4) 0.036(3) -0.019(3) -0.002(2) 0.002(2) C34 0.042(3) 0.081(5) 0.030(3) 0.002(3) -0.004(2) 0.023(3) C35 0.053(3) 0.053(3) 0.042(3) 0.009(3) 0.001(3) 0.010(3) C36 0.036(2) 0.037(3) 0.036(3) 0.002(2) 0.007(2) 0.008(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 O9 2.038(3) . ? Ru1 O8 2.050(3) . ? Ru1 O7 2.100(3) . ? Ru1 N1 2.102(3) . ? Ru1 Cl1 2.3234(10) . ? Ru1 Cl2 2.3292(10) . ? Co1 C2A 2.052(11) . ? Co1 C5 2.057(11) . ? Co1 C2 2.086(13) . ? Co1 C3A 2.089(9) . ? Co1 C1 2.094(12) . ? Co1 C4 2.094(9) . ? Co1 C5A 2.101(9) . ? Co1 C3 2.106(11) . ? Co1 C4A 2.107(9) . ? Co1 C1A 2.110(11) . ? Co1 P1 2.1541(14) . ? Co1 P3 2.1688(13) . ? P1 O7 1.505(3) . ? P1 O1 1.596(3) . ? P1 O2 1.601(3) . ? P2 O8 1.509(3) . ? P2 O4 1.588(4) . ? P2 O3 1.598(3) . ? P3 O9 1.516(3) . ? P3 O6 1.585(3) . ? P3 O5 1.596(3) . ? O1 C11 1.420(6) . ? O2 C13 1.454(6) . ? O3 C15 1.446(6) . ? O4 C17 1.474(6) . ? O5 C19 1.441(6) . ? O6 C21 1.466(5) . ? N1 C31 1.436(5) . ? C1 C2 1.390(12) . ? C1 C5 1.398(12) . ? C2 C3 1.397(12) . ? C3 C4 1.390(11) . ? C4 C5 1.396(12) . ? C1A C5A 1.415(11) . ? C1A C2A 1.437(11) . ? C2A C3A 1.419(11) . ? C3A C4A 1.417(11) . ? C4A C5A 1.430(10) . ? C11 C12 1.469(8) . ? C13 C14 1.491(8) . ? C15 C16 1.518(7) . ? C17 C18 1.481(8) . ? C19 C20 1.480(7) . ? C21 C22 1.496(7) . ? C31 C36 1.382(7) . ? C31 C32 1.392(6) . ? C32 C33 1.384(7) . ? C33 C34 1.372(8) . ? C34 C35 1.392(8) . ? C35 C36 1.367(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Ru1 O8 85.61(12) . . ? O9 Ru1 O7 93.65(11) . . ? O8 Ru1 O7 88.32(12) . . ? O9 Ru1 N1 85.96(13) . . ? O8 Ru1 N1 93.00(12) . . ? O7 Ru1 N1 178.59(13) . . ? O9 Ru1 Cl1 175.01(9) . . ? O8 Ru1 Cl1 90.50(8) . . ? O7 Ru1 Cl1 89.36(8) . . ? N1 Ru1 Cl1 91.12(10) . . ? O9 Ru1 Cl2 91.76(9) . . ? O8 Ru1 Cl2 176.95(8) . . ? O7 Ru1 Cl2 93.39(9) . . ? N1 Ru1 Cl2 85.27(10) . . ? Cl1 Ru1 Cl2 92.04(4) . . ? C2A Co1 C5 55.2(4) . . ? C2A Co1 C2 47.6(4) . . ? C5 Co1 C2 63.6(5) . . ? C2A Co1 C3A 40.1(3) . . ? C5 Co1 C3A 22.6(3) . . ? C2 Co1 C3A 68.0(4) . . ? C2A Co1 C1 66.8(4) . . ? C5 Co1 C1 39.4(3) . . ? C2 Co1 C1 38.9(3) . . ? C3A Co1 C1 57.4(4) . . ? C2A Co1 C4 23.8(3) . . ? C5 Co1 C4 39.3(3) . . ? C2 Co1 C4 63.5(4) . . ? C3A Co1 C4 18.6(3) . . ? C1 Co1 C4 66.5(4) . . ? C2A Co1 C5A 64.8(4) . . ? C5 Co1 C5A 51.2(4) . . ? C2 Co1 C5A 27.0(3) . . ? C3A Co1 C5A 65.9(4) . . ? C1 Co1 C5A 14.3(3) . . ? C4 Co1 C5A 70.7(3) . . ? C2A Co1 C3 14.9(3) . . ? C5 Co1 C3 65.9(4) . . ? C2 Co1 C3 38.9(3) . . ? C3A Co1 C3 53.9(4) . . ? C1 Co1 C3 67.4(4) . . ? C4 Co1 C3 38.6(3) . . ? C5A Co1 C3 61.4(4) . . ? C2A Co1 C4A 66.3(4) . . ? C5 Co1 C4A 17.1(3) . . ? C2 Co1 C4A 59.2(4) . . ? C3A Co1 C4A 39.5(3) . . ? C1 Co1 C4A 25.9(3) . . ? C4 Co1 C4A 54.7(3) . . ? C5A Co1 C4A 39.7(3) . . ? C3 Co1 C4A 73.7(4) . . ? C2A Co1 C1A 40.4(3) . . ? C5 Co1 C1A 69.3(4) . . ? C2 Co1 C1A 12.4(4) . . ? C3A Co1 C1A 68.7(4) . . ? C1 Co1 C1A 50.4(4) . . ? C4 Co1 C1A 60.1(3) . . ? C5A Co1 C1A 39.3(3) . . ? C3 Co1 C1A 29.0(3) . . ? C4A Co1 C1A 68.2(4) . . ? C2A Co1 P1 156.7(3) . . ? C5 Co1 P1 102.2(4) . . ? C2 Co1 P1 120.8(3) . . ? C3A Co1 P1 120.2(3) . . ? C1 Co1 P1 92.3(3) . . ? C4 Co1 P1 138.7(3) . . ? C5A Co1 P1 97.5(3) . . ? C3 Co1 P1 159.0(3) . . ? C4A Co1 P1 90.4(3) . . ? C1A Co1 P1 132.0(3) . . ? C2A Co1 P3 99.4(3) . . ? C5 Co1 P3 105.3(4) . . ? C2 Co1 P3 146.5(3) . . ? C3A Co1 P3 90.3(3) . . ? C1 Co1 P3 144.3(4) . . ? C4 Co1 P3 87.7(3) . . ? C5A Co1 P3 156.0(3) . . ? C3 Co1 P3 107.7(3) . . ? C4A Co1 P3 118.6(3) . . ? C1A Co1 P3 136.1(3) . . ? P1 Co1 P3 91.83(5) . . ? O7 P1 O1 108.43(18) . . ? O7 P1 O2 108.76(18) . . ? O1 P1 O2 101.09(19) . . ? O7 P1 Co1 119.17(13) . . ? O1 P1 Co1 111.24(14) . . ? O2 P1 Co1 106.58(14) . . ? O8 P2 O4 106.93(18) . . ? O8 P2 O3 107.01(17) . . ? O4 P2 O3 101.39(19) . . ? O8 P2 Co1 119.98(13) . . ? O4 P2 Co1 107.43(13) . . ? O3 P2 Co1 112.39(14) . . ? O9 P3 O6 108.46(17) . . ? O9 P3 O5 107.30(17) . . ? O6 P3 O5 99.73(17) . . ? O9 P3 Co1 119.19(12) . . ? O6 P3 Co1 109.53(12) . . ? O5 P3 Co1 110.84(13) . . ? C11 O1 P1 123.9(3) . . ? C13 O2 P1 119.5(3) . . ? C15 O3 P2 123.2(3) . . ? C17 O4 P2 118.3(3) . . ? C19 O5 P3 122.8(3) . . ? C21 O6 P3 117.5(3) . . ? P1 O7 Ru1 129.50(17) . . ? P2 O8 Ru1 128.75(18) . . ? P3 O9 Ru1 130.48(17) . . ? C31 N1 Ru1 120.0(3) . . ? C2 C1 C5 103.1(10) . . ? C2 C1 Co1 70.3(7) . . ? C5 C1 Co1 68.9(7) . . ? C1 C2 C3 113.4(10) . . ? C1 C2 Co1 70.9(7) . . ? C3 C2 Co1 71.3(7) . . ? C4 C3 C2 104.3(9) . . ? C4 C3 Co1 70.2(6) . . ? C2 C3 Co1 69.8(7) . . ? C3 C4 C5 108.7(9) . . ? C3 C4 Co1 71.1(6) . . ? C5 C4 Co1 68.9(6) . . ? C4 C5 C1 110.4(10) . . ? C4 C5 Co1 71.8(6) . . ? C1 C5 Co1 71.8(7) . . ? C5A C1A C2A 102.5(9) . . ? C5A C1A Co1 70.0(6) . . ? C2A C1A Co1 67.6(6) . . ? C3A C2A C1A 112.1(9) . . ? C3A C2A Co1 71.4(6) . . ? C1A C2A Co1 72.0(6) . . ? C4A C3A C2A 106.6(8) . . ? C4A C3A Co1 71.0(5) . . ? C2A C3A Co1 68.6(6) . . ? C3A C4A C5A 106.3(8) . . ? C3A C4A Co1 69.6(5) . . ? C5A C4A Co1 69.9(5) . . ? C1A C5A C4A 112.4(8) . . ? C1A C5A Co1 70.7(5) . . ? C4A C5A Co1 70.4(5) . . ? O1 C11 C12 109.8(5) . . ? O2 C13 C14 108.7(5) . . ? O3 C15 C16 111.4(4) . . ? O4 C17 C18 108.5(5) . . ? O5 C19 C20 108.7(4) . . ? O6 C21 C22 111.1(4) . . ? C36 C31 C32 119.9(4) . . ? C36 C31 N1 119.9(4) . . ? C32 C31 N1 120.3(4) . . ? C33 C32 C31 119.5(5) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 119.2(5) . . ? C36 C35 C34 120.8(6) . . ? C35 C36 C31 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 72.42 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.119 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.146 ###END data_yxy137compound6 _database_code_depnum_ccdc_archive 'CCDC 725292' #TrackingRef '- cif-re3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H35 Cl2 Co O9 P3 Ru' _chemical_formula_weight 707.26 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2031(14) _cell_length_b 10.7139(14) _cell_length_c 12.5190(17) _cell_angle_alpha 89.323(2) _cell_angle_beta 79.401(2) _cell_angle_gamma 85.973(3) _cell_volume 1341.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10486 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5203 _reflns_number_gt 3852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. In this complex, the carbon atoms C21 and C22 of an ethoxy group were found to be 60:40 and 50:50 disordered, respectively.The bond distance of C21-C22 is fixed as 1.50 A. ; _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^)+(0.0570P)^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 constrain _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5203 _refine_ls_number_parameters 296 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _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 0.09950(4) 0.11669(4) 0.44198(3) 0.01704(13) Uani 1 1 d . . . Co1 Co 0.30568(7) 0.20926(6) 0.16078(5) 0.01683(17) Uani 1 1 d . . . Cl1 Cl -0.13048(12) 0.07578(11) 0.47042(10) 0.0199(3) Uani 1 1 d . . . Cl2 Cl 0.07784(13) 0.22812(11) 0.60199(10) 0.0232(3) Uani 1 1 d . . . P1 P 0.17513(14) 0.05806(12) 0.18559(11) 0.0188(3) Uani 1 1 d . . . P2 P 0.15933(13) 0.32951(12) 0.26519(11) 0.0182(3) Uani 1 1 d . A . P3 P 0.39091(14) 0.14399(12) 0.29886(11) 0.0193(3) Uani 1 1 d . . . O1 O 0.0504(4) 0.0946(3) 0.1284(3) 0.0254(9) Uani 1 1 d . . . O2 O 0.2397(4) -0.0660(3) 0.1215(3) 0.0260(9) Uani 1 1 d . . . O3 O 0.4605(4) 0.0067(3) 0.2699(3) 0.0226(8) Uani 1 1 d . . . O4 O 0.5162(3) 0.2179(3) 0.3122(3) 0.0260(9) Uani 1 1 d . . . O5 O 0.2362(3) 0.4316(3) 0.3156(3) 0.0229(8) Uani 1 1 d . . . O6 O 0.0717(4) 0.4113(3) 0.1939(3) 0.0270(9) Uani 1 1 d . . . O7 O 0.1257(3) 0.0177(3) 0.3017(3) 0.0214(8) Uani 1 1 d . . . O8 O 0.3018(3) 0.1453(3) 0.4101(3) 0.0198(8) Uani 1 1 d . . . O9 O 0.0605(3) 0.2731(3) 0.3555(3) 0.0186(8) Uani 1 1 d . . . C1 C 0.2936(7) 0.2558(7) 0.0014(5) 0.0443(18) Uani 1 1 d . . . H1A H 0.2112 0.2592 -0.0313 0.053 Uiso 1 1 calc R . . C2 C 0.3821(7) 0.1554(6) 0.0022(4) 0.0399(17) Uani 1 1 d . . . H2A H 0.3747 0.0715 -0.0295 0.048 Uiso 1 1 calc R . . C3 C 0.4851(6) 0.1875(7) 0.0522(5) 0.0440(18) Uani 1 1 d . . . H3A H 0.5657 0.1329 0.0616 0.053 Uiso 1 1 calc R . . C4 C 0.4572(7) 0.3150(7) 0.0828(5) 0.0459(19) Uani 1 1 d . . . H4A H 0.5144 0.3672 0.1184 0.055 Uiso 1 1 calc R . . C5 C 0.3412(8) 0.3544(6) 0.0505(6) 0.053(2) Uani 1 1 d . . . H5A H 0.2974 0.4410 0.0600 0.063 Uiso 1 1 calc R . . C11 C -0.0643(6) 0.0184(6) 0.1497(5) 0.0388(15) Uani 1 1 d . . . H11A H -0.0617 -0.0386 0.0876 0.047 Uiso 1 1 calc R . . H11B H -0.0606 -0.0331 0.2153 0.047 Uiso 1 1 calc R . . C12 C -0.1873(7) 0.0976(8) 0.1658(6) 0.064(2) Uani 1 1 d . . . H12A H -0.2637 0.0453 0.1800 0.097 Uiso 1 1 calc R . . H12B H -0.1914 0.1477 0.1003 0.097 Uiso 1 1 calc R . . H12C H -0.1902 0.1533 0.2278 0.097 Uiso 1 1 calc R . . C13 C 0.2649(7) -0.1843(5) 0.1740(5) 0.0345(15) Uani 1 1 d . . . H13A H 0.2335 -0.1760 0.2534 0.041 Uiso 1 1 calc R . . H13B H 0.3621 -0.2078 0.1607 0.041 Uiso 1 1 calc R . . C14 C 0.1941(8) -0.2827(6) 0.1308(6) 0.053(2) Uani 1 1 d . . . H14A H 0.2113 -0.3623 0.1667 0.079 Uiso 1 1 calc R . . H14B H 0.2263 -0.2914 0.0524 0.079 Uiso 1 1 calc R . . H14C H 0.0979 -0.2595 0.1447 0.079 Uiso 1 1 calc R . . C15 C 0.5211(6) -0.0599(5) 0.3535(5) 0.0334(14) Uani 1 1 d . . . H15A H 0.4520 -0.0733 0.4184 0.040 Uiso 1 1 calc R . . H15B H 0.5897 -0.0097 0.3753 0.040 Uiso 1 1 calc R . . C16 C 0.5840(6) -0.1834(5) 0.3082(5) 0.0356(15) Uani 1 1 d . . . H16A H 0.6252 -0.2287 0.3634 0.053 Uiso 1 1 calc R . . H16B H 0.6526 -0.1693 0.2442 0.053 Uiso 1 1 calc R . . H16C H 0.5154 -0.2328 0.2874 0.053 Uiso 1 1 calc R . . C17 C 0.5162(6) 0.3126(5) 0.3945(5) 0.0292(13) Uani 1 1 d . . . H17A H 0.5721 0.2810 0.4472 0.035 Uiso 1 1 calc R . . H17B H 0.4240 0.3319 0.4345 0.035 Uiso 1 1 calc R . . C18 C 0.5705(6) 0.4283(5) 0.3407(5) 0.0393(16) Uani 1 1 d . . . H18A H 0.5703 0.4926 0.3958 0.059 Uiso 1 1 calc R . . H18B H 0.5145 0.4594 0.2889 0.059 Uiso 1 1 calc R . . H18C H 0.6621 0.4089 0.3020 0.059 Uiso 1 1 calc R . . C19 C 0.1677(7) 0.4992(6) 0.4126(6) 0.0490(19) Uani 1 1 d . . . H19A H 0.0771 0.5299 0.4023 0.059 Uiso 1 1 calc R . . H19B H 0.1581 0.4416 0.4755 0.059 Uiso 1 1 calc R . . C20 C 0.2409(7) 0.6045(6) 0.4349(5) 0.0427(17) Uani 1 1 d . . . H20A H 0.1935 0.6472 0.5012 0.064 Uiso 1 1 calc R . . H20B H 0.2478 0.6630 0.3738 0.064 Uiso 1 1 calc R . . H20C H 0.3307 0.5742 0.4450 0.064 Uiso 1 1 calc R . . C21 C -0.0560(11) 0.4729(10) 0.2403(8) 0.039(3) Uiso 0.60 1 d PD A 1 C22 C -0.1189(13) 0.5347(12) 0.1567(10) 0.028(3) Uiso 0.50 1 d PD A 1 C21A C -0.0557(18) 0.3915(15) 0.1786(14) 0.051(5) Uiso 0.40 1 d PD A 2 C22A C -0.1256(13) 0.5002(12) 0.1360(11) 0.027(3) Uiso 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0188(2) 0.0168(2) 0.0138(2) -0.00093(16) 0.00135(17) -0.00056(17) Co1 0.0168(4) 0.0160(3) 0.0152(4) 0.0018(3) 0.0025(3) 0.0016(3) Cl1 0.0196(7) 0.0188(6) 0.0201(6) 0.0029(5) -0.0014(5) 0.0008(5) Cl2 0.0270(7) 0.0227(7) 0.0185(7) -0.0053(5) -0.0012(6) 0.0003(6) P1 0.0208(8) 0.0187(7) 0.0150(7) 0.0001(5) 0.0012(6) -0.0005(6) P2 0.0182(7) 0.0159(6) 0.0186(7) 0.0011(5) 0.0003(6) 0.0020(5) P3 0.0175(7) 0.0185(7) 0.0206(7) 0.0004(5) -0.0005(6) 0.0011(6) O1 0.021(2) 0.032(2) 0.024(2) 0.0031(16) -0.0041(17) -0.0037(17) O2 0.038(2) 0.0188(19) 0.0171(19) -0.0019(15) 0.0049(17) 0.0003(17) O3 0.027(2) 0.0192(19) 0.0187(19) 0.0024(15) 0.0008(16) 0.0026(16) O4 0.017(2) 0.028(2) 0.030(2) -0.0050(17) 0.0022(17) -0.0007(16) O5 0.020(2) 0.0186(19) 0.028(2) -0.0074(15) 0.0024(16) 0.0004(15) O6 0.019(2) 0.030(2) 0.028(2) 0.0081(17) 0.0022(17) 0.0036(16) O7 0.025(2) 0.0220(19) 0.0161(18) -0.0040(15) 0.0018(16) -0.0037(16) O8 0.018(2) 0.0245(19) 0.0162(18) -0.0009(15) -0.0029(15) 0.0022(15) O9 0.0157(19) 0.0166(18) 0.0207(19) 0.0018(14) 0.0025(15) 0.0021(14) C1 0.030(4) 0.072(5) 0.028(3) 0.036(3) -0.001(3) -0.004(4) C2 0.073(5) 0.029(3) 0.014(3) 0.003(2) 0.006(3) -0.016(3) C3 0.027(4) 0.075(5) 0.019(3) 0.021(3) 0.017(3) 0.022(3) C4 0.049(5) 0.072(5) 0.017(3) 0.000(3) 0.008(3) -0.041(4) C5 0.064(5) 0.030(4) 0.043(4) 0.016(3) 0.038(4) 0.016(4) C11 0.033(4) 0.051(4) 0.035(4) 0.005(3) -0.009(3) -0.010(3) C12 0.028(4) 0.099(7) 0.065(5) 0.037(5) -0.009(4) -0.001(4) C13 0.054(4) 0.020(3) 0.023(3) 0.001(2) 0.009(3) 0.001(3) C14 0.076(6) 0.023(3) 0.057(5) 0.001(3) 0.001(4) -0.012(3) C15 0.043(4) 0.032(3) 0.024(3) 0.003(3) -0.009(3) 0.014(3) C16 0.037(4) 0.034(3) 0.034(3) 0.001(3) -0.008(3) 0.015(3) C17 0.030(3) 0.028(3) 0.032(3) -0.002(2) -0.011(3) -0.007(3) C18 0.034(4) 0.035(4) 0.049(4) 0.005(3) -0.005(3) -0.007(3) C19 0.038(4) 0.052(4) 0.049(4) -0.030(3) 0.018(3) -0.013(3) C20 0.046(4) 0.040(4) 0.044(4) -0.017(3) -0.016(3) 0.006(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 Ru1 O7 2.028(3) . ? Ru1 O9 2.039(3) . ? Ru1 O8 2.073(3) . ? Ru1 Cl2 2.3116(12) . ? Ru1 Cl1 2.3531(13) 2_556 ? Ru1 Cl1 2.3786(13) . ? Co1 C2 2.068(6) . ? Co1 C3 2.070(6) . ? Co1 C4 2.072(6) . ? Co1 C5 2.074(6) . ? Co1 C1 2.074(6) . ? Co1 P1 2.1528(15) . ? Co1 P2 2.1563(15) . ? Co1 P3 2.1616(15) . ? Cl1 Ru1 2.3531(13) 2_556 ? P1 O7 1.517(4) . ? P1 O1 1.595(4) . ? P1 O2 1.598(4) . ? P2 O9 1.520(4) . ? P2 O5 1.591(3) . ? P2 O6 1.591(4) . ? P3 O8 1.516(4) . ? P3 O4 1.585(4) . ? P3 O3 1.603(4) . ? O1 C11 1.456(7) . ? O2 C13 1.449(6) . ? O3 C15 1.464(6) . ? O4 C17 1.455(6) . ? O5 C19 1.457(6) . ? O6 C21A 1.378(17) . ? O6 C21 1.442(11) . ? C1 C2 1.356(9) . ? C1 C5 1.388(10) . ? C2 C3 1.383(9) . ? C3 C4 1.418(9) . ? C4 C5 1.357(10) . ? C11 C12 1.448(9) . ? C13 C14 1.479(8) . ? C15 C16 1.499(7) . ? C17 C18 1.496(8) . ? C19 C20 1.453(8) . ? C21 C22 1.455(13) . ? C21A C22A 1.469(15) . ? 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 O7 Ru1 O9 88.19(14) . . ? O7 Ru1 O8 88.73(13) . . ? O9 Ru1 O8 90.47(13) . . ? O7 Ru1 Cl2 177.90(11) . . ? O9 Ru1 Cl2 92.63(10) . . ? O8 Ru1 Cl2 89.32(10) . . ? O7 Ru1 Cl1 86.81(10) . 2_556 ? O9 Ru1 Cl1 173.52(10) . 2_556 ? O8 Ru1 Cl1 93.55(10) . 2_556 ? Cl2 Ru1 Cl1 92.50(5) . 2_556 ? O7 Ru1 Cl1 88.12(10) . . ? O9 Ru1 Cl1 89.97(10) . . ? O8 Ru1 Cl1 176.81(9) . . ? Cl2 Ru1 Cl1 93.81(5) . . ? Cl1 Ru1 Cl1 85.74(5) 2_556 . ? C2 Co1 C3 39.1(3) . . ? C2 Co1 C4 65.7(2) . . ? C3 Co1 C4 40.0(3) . . ? C2 Co1 C5 64.6(2) . . ? C3 Co1 C5 65.3(3) . . ? C4 Co1 C5 38.2(3) . . ? C2 Co1 C1 38.2(3) . . ? C3 Co1 C1 65.3(2) . . ? C4 Co1 C1 65.4(3) . . ? C5 Co1 C1 39.1(3) . . ? C2 Co1 P1 92.42(17) . . ? C3 Co1 P1 119.7(2) . . ? C4 Co1 P1 157.81(19) . . ? C5 Co1 P1 136.3(3) . . ? C1 Co1 P1 100.0(2) . . ? C2 Co1 P2 145.6(2) . . ? C3 Co1 P2 149.1(2) . . ? C4 Co1 P2 109.1(2) . . ? C5 Co1 P2 90.04(18) . . ? C1 Co1 P2 107.6(2) . . ? P1 Co1 P2 90.84(6) . . ? C2 Co1 P3 123.8(2) . . ? C3 Co1 P3 94.20(17) . . ? C4 Co1 P3 100.0(2) . . ? C5 Co1 P3 134.5(3) . . ? C1 Co1 P3 159.49(19) . . ? P1 Co1 P3 89.16(6) . . ? P2 Co1 P3 90.47(6) . . ? Ru1 Cl1 Ru1 94.26(5) 2_556 . ? O7 P1 O1 109.5(2) . . ? O7 P1 O2 105.91(19) . . ? O1 P1 O2 102.2(2) . . ? O7 P1 Co1 117.50(14) . . ? O1 P1 Co1 108.07(15) . . ? O2 P1 Co1 112.59(15) . . ? O9 P2 O5 109.1(2) . . ? O9 P2 O6 106.0(2) . . ? O5 P2 O6 102.9(2) . . ? O9 P2 Co1 119.87(14) . . ? O5 P2 Co1 108.02(14) . . ? O6 P2 Co1 109.68(15) . . ? O8 P3 O4 105.83(19) . . ? O8 P3 O3 110.67(19) . . ? O4 P3 O3 100.9(2) . . ? O8 P3 Co1 118.72(15) . . ? O4 P3 Co1 111.93(15) . . ? O3 P3 Co1 107.38(14) . . ? C11 O1 P1 118.8(3) . . ? C13 O2 P1 123.7(3) . . ? C15 O3 P3 117.7(3) . . ? C17 O4 P3 124.9(3) . . ? C19 O5 P2 118.7(3) . . ? C21A O6 C21 49.0(8) . . ? C21A O6 P2 127.2(7) . . ? C21 O6 P2 122.1(5) . . ? P1 O7 Ru1 129.9(2) . . ? P3 O8 Ru1 125.96(19) . . ? P2 O9 Ru1 125.3(2) . . ? C2 C1 C5 107.5(6) . . ? C2 C1 Co1 70.7(3) . . ? C5 C1 Co1 70.4(4) . . ? C1 C2 C3 109.4(6) . . ? C1 C2 Co1 71.1(4) . . ? C3 C2 Co1 70.5(3) . . ? C2 C3 C4 106.5(6) . . ? C2 C3 Co1 70.4(4) . . ? C4 C3 Co1 70.1(3) . . ? C5 C4 C3 107.2(6) . . ? C5 C4 Co1 71.0(4) . . ? C3 C4 Co1 69.9(3) . . ? C4 C5 C1 109.3(6) . . ? C4 C5 Co1 70.8(4) . . ? C1 C5 Co1 70.5(4) . . ? C12 C11 O1 110.2(6) . . ? O2 C13 C14 109.8(5) . . ? O3 C15 C16 108.8(4) . . ? O4 C17 C18 109.2(5) . . ? C20 C19 O5 111.2(5) . . ? O6 C21 C22 111.0(9) . . ? O6 C21A C22A 114.4(13) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.591 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.135 ### end data_yxy168cult_Compound11 _database_code_depnum_ccdc_archive 'CCDC 725293' #TrackingRef '- cif-re3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 Cl6 Co O9 P3 Ru' _chemical_formula_weight 862.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1126(4) _cell_length_b 12.8269(4) _cell_length_c 13.2733(5) _cell_angle_alpha 76.350(3) _cell_angle_beta 88.177(3) _cell_angle_gamma 89.410(3) _cell_volume 1672.24(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7277 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 71.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 13.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9500 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 71.47 _reflns_number_total 6109 _reflns_number_gt 5631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. CHCl3 molecule was cocrystallized in this compound. The carbon atoms C14, C17 and C18 in the ethoxy group was found disordered with 45/55, 50/50 and 50/50 occupations, respectively. ; _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^)+(0.0927P)^2^+0.5156P] 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 6109 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _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 0.47156(2) 0.322765(19) 0.282103(17) 0.01546(11) Uani 1 1 d . C . Co1 Co 0.09179(5) 0.36219(4) 0.26169(4) 0.01909(15) Uani 1 1 d . . . Cl1 Cl 0.57358(8) 0.19032(7) 0.40057(6) 0.0271(2) Uani 1 1 d . . . Cl2 Cl 0.60699(8) 0.45156(7) 0.31103(6) 0.02548(19) Uani 1 1 d . . . Cl3 Cl 0.60134(8) 0.29047(7) 0.14887(6) 0.02433(19) Uani 1 1 d . . . P1 P 0.20891(8) 0.39871(7) 0.38164(6) 0.01841(19) Uani 1 1 d . . . P2 P 0.19145(8) 0.20961(7) 0.27938(7) 0.01947(19) Uani 1 1 d . C . P3 P 0.23533(8) 0.43519(7) 0.14289(6) 0.01707(18) Uani 1 1 d . C . O1 O 0.2215(3) 0.5249(2) 0.36204(19) 0.0250(5) Uani 1 1 d . . . O2 O 0.1399(3) 0.3700(2) 0.4949(2) 0.0290(6) Uani 1 1 d . B . O3 O 0.1609(3) 0.1408(2) 0.3936(2) 0.0289(6) Uani 1 1 d . . . O4 O 0.1346(3) 0.1352(2) 0.2110(2) 0.0348(6) Uani 1 1 d . . . O5 O 0.2332(2) 0.3778(2) 0.04982(19) 0.0248(5) Uani 1 1 d . . . O6 O 0.2016(3) 0.5552(2) 0.0840(2) 0.0290(6) Uani 1 1 d . . . O7 O 0.3471(2) 0.3469(2) 0.39629(18) 0.0211(5) Uani 1 1 d . . . O8 O 0.3416(2) 0.2124(2) 0.25675(19) 0.0224(5) Uani 1 1 d . . . O9 O 0.3775(2) 0.43911(19) 0.17888(18) 0.0193(5) Uani 1 1 d . . . C1 C -0.0684(4) 0.4313(4) 0.3239(3) 0.0361(9) Uani 1 1 d . . . H1A H -0.0656 0.4713 0.3799 0.043 Uiso 1 1 calc R . . C2 C -0.0888(4) 0.3196(4) 0.3376(4) 0.0466(13) Uani 1 1 d . . . H2A H -0.1031 0.2663 0.4053 0.056 Uiso 1 1 calc R . . C3 C -0.0898(4) 0.2974(4) 0.2370(6) 0.0573(16) Uani 1 1 d . . . H3A H -0.1034 0.2254 0.2221 0.069 Uiso 1 1 calc R . . C4 C -0.0660(4) 0.3940(4) 0.1626(4) 0.0418(11) Uani 1 1 d . . . H4A H -0.0614 0.4035 0.0856 0.050 Uiso 1 1 calc R . . C5 C -0.0550(4) 0.4755(3) 0.2167(3) 0.0336(9) Uani 1 1 d . . . H5A H -0.0395 0.5531 0.1838 0.040 Uiso 1 1 calc R . . C11 C 0.3039(5) 0.5700(4) 0.4317(3) 0.0390(10) Uani 1 1 d . . . H11A H 0.2490 0.5802 0.4917 0.047 Uiso 1 1 calc R . . H11B H 0.3759 0.5190 0.4583 0.047 Uiso 1 1 calc R . . C12 C 0.3602(10) 0.6717(6) 0.3771(5) 0.089(3) Uani 1 1 d . . . H12A H 0.4142 0.7002 0.4244 0.133 Uiso 1 1 calc R . . H12B H 0.2889 0.7224 0.3516 0.133 Uiso 1 1 calc R . . H12C H 0.4157 0.6613 0.3184 0.133 Uiso 1 1 calc R . . C13 C 0.1622(7) 0.2732(5) 0.5718(4) 0.073(2) Uani 1 1 d . . . H13A H 0.2543 0.2488 0.5640 0.087 Uiso 1 1 calc R A 1 H13B H 0.1022 0.2167 0.5607 0.087 Uiso 1 1 calc R A 1 C14 C 0.1405(14) 0.2874(10) 0.6748(10) 0.049(3) Uiso 0.45 1 d P B 1 C14A C 0.0816(11) 0.2712(8) 0.6652(7) 0.044(2) Uiso 0.55 1 d P B 2 C15 C 0.2318(4) 0.0406(3) 0.4364(4) 0.0384(10) Uani 1 1 d . . . H15A H 0.2476 0.0349 0.5107 0.046 Uiso 1 1 calc R . . H15B H 0.3188 0.0414 0.3999 0.046 Uiso 1 1 calc R . . C16 C 0.1546(6) -0.0544(4) 0.4252(6) 0.0644(16) Uani 1 1 d . . . H16A H 0.2041 -0.1202 0.4542 0.097 Uiso 1 1 calc R . . H16B H 0.1400 -0.0494 0.3515 0.097 Uiso 1 1 calc R . . H16C H 0.0691 -0.0560 0.4624 0.097 Uiso 1 1 calc R . . C17 C 0.1772(10) 0.1318(8) 0.1095(8) 0.040(2) Uiso 0.50 1 d P C 1 C18 C 0.1336(14) 0.0271(12) 0.0908(11) 0.059(3) Uiso 0.50 1 d P C 1 C17A C 0.2163(9) 0.0923(8) 0.1355(7) 0.0341(18) Uiso 0.50 1 d P C 2 C18A C 0.1157(13) 0.0630(12) 0.0603(11) 0.057(3) Uiso 0.50 1 d P C 2 C19 C 0.3297(4) 0.4100(3) -0.0377(3) 0.0300(8) Uani 1 1 d . . . H19A H 0.4158 0.4272 -0.0122 0.036 Uiso 1 1 calc R . . H19B H 0.2975 0.4745 -0.0877 0.036 Uiso 1 1 calc R . . C20 C 0.3454(6) 0.3187(4) -0.0893(4) 0.0509(13) Uani 1 1 d . . . H20A H 0.4094 0.3381 -0.1476 0.076 Uiso 1 1 calc R . . H20B H 0.2599 0.3027 -0.1148 0.076 Uiso 1 1 calc R . . H20C H 0.3772 0.2552 -0.0392 0.076 Uiso 1 1 calc R . . C21 C 0.2525(8) 0.6467(4) 0.1126(4) 0.0583(16) Uani 1 1 d . . . H21A H 0.3459 0.6582 0.0883 0.070 Uiso 1 1 calc R . . H21B H 0.2488 0.6353 0.1891 0.070 Uiso 1 1 calc R . . C22 C 0.1714(9) 0.7429(5) 0.0646(6) 0.083(3) Uani 1 1 d . . . H22A H 0.2065 0.8064 0.0835 0.124 Uiso 1 1 calc R . . H22B H 0.0794 0.7316 0.0900 0.124 Uiso 1 1 calc R . . H22C H 0.1753 0.7536 -0.0110 0.124 Uiso 1 1 calc R . . C1S C 0.6106(5) 0.0141(4) 0.2326(4) 0.0456(11) Uani 1 1 d . . . H1SA H 0.5755 0.0855 0.2390 0.055 Uiso 1 1 calc R . . Cl11 Cl 0.78369(16) 0.01677(12) 0.23681(15) 0.0712(4) Uani 1 1 d . . . Cl12 Cl 0.5628(3) -0.0073(3) 0.11415(18) 0.1175(9) Uani 1 1 d . . . Cl13 Cl 0.54777(15) -0.08455(11) 0.33854(14) 0.0692(4) 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 Ru1 0.01101(15) 0.02045(16) 0.01523(15) -0.00426(10) -0.00384(9) -0.00219(9) Co1 0.0104(3) 0.0221(3) 0.0238(3) -0.0028(2) -0.0041(2) -0.0037(2) Cl1 0.0248(4) 0.0307(4) 0.0237(4) -0.0015(3) -0.0089(3) 0.0046(3) Cl2 0.0186(4) 0.0316(4) 0.0285(4) -0.0104(3) -0.0061(3) -0.0080(3) Cl3 0.0194(4) 0.0324(4) 0.0219(4) -0.0083(3) 0.0018(3) -0.0009(3) P1 0.0151(4) 0.0228(4) 0.0170(4) -0.0039(3) -0.0002(3) -0.0021(3) P2 0.0151(4) 0.0191(4) 0.0241(4) -0.0042(3) -0.0032(3) -0.0062(3) P3 0.0134(4) 0.0197(4) 0.0176(4) -0.0027(3) -0.0059(3) -0.0027(3) O1 0.0297(13) 0.0243(13) 0.0227(12) -0.0080(10) -0.0054(10) -0.0034(10) O2 0.0265(13) 0.0345(14) 0.0228(12) -0.0008(11) 0.0040(10) 0.0019(11) O3 0.0275(13) 0.0250(13) 0.0293(13) 0.0029(10) 0.0015(11) -0.0041(10) O4 0.0281(14) 0.0391(16) 0.0437(16) -0.0222(13) -0.0040(12) -0.0114(12) O5 0.0229(12) 0.0334(14) 0.0203(12) -0.0099(10) -0.0043(10) -0.0065(10) O6 0.0259(13) 0.0238(13) 0.0333(14) 0.0022(11) -0.0085(11) 0.0003(10) O7 0.0142(11) 0.0301(13) 0.0193(11) -0.0066(9) -0.0016(9) -0.0008(9) O8 0.0208(12) 0.0217(12) 0.0253(12) -0.0064(9) -0.0023(9) -0.0014(9) O9 0.0153(11) 0.0228(12) 0.0194(11) -0.0029(9) -0.0065(9) -0.0043(9) C1 0.0186(18) 0.050(3) 0.040(2) -0.0116(19) 0.0012(16) 0.0052(17) C2 0.0145(18) 0.049(3) 0.063(3) 0.015(2) 0.0076(19) -0.0037(17) C3 0.0128(19) 0.045(3) 0.121(5) -0.031(3) -0.020(2) -0.0061(18) C4 0.0218(19) 0.062(3) 0.044(2) -0.016(2) -0.0162(17) 0.0051(19) C5 0.0170(17) 0.035(2) 0.044(2) -0.0005(17) -0.0026(16) 0.0029(15) C11 0.051(3) 0.040(2) 0.031(2) -0.0181(18) -0.0086(18) -0.012(2) C12 0.156(8) 0.064(4) 0.053(3) -0.021(3) -0.018(4) -0.054(5) C13 0.095(5) 0.068(4) 0.036(3) 0.022(3) 0.028(3) 0.030(4) C15 0.032(2) 0.033(2) 0.042(2) 0.0081(18) -0.0084(18) -0.0016(17) C16 0.069(4) 0.027(2) 0.091(4) 0.002(3) -0.019(3) -0.005(2) C19 0.032(2) 0.037(2) 0.0216(17) -0.0071(15) -0.0025(15) -0.0016(16) C20 0.073(4) 0.047(3) 0.036(2) -0.018(2) 0.014(2) -0.003(3) C21 0.122(5) 0.020(2) 0.034(2) -0.0054(17) -0.022(3) -0.006(3) C22 0.135(7) 0.031(3) 0.074(4) -0.001(3) 0.031(4) 0.023(3) C1S 0.059(3) 0.035(2) 0.045(3) -0.015(2) 0.000(2) -0.001(2) Cl11 0.0594(8) 0.0476(8) 0.1015(12) -0.0096(7) 0.0155(8) -0.0074(6) Cl12 0.1336(19) 0.165(2) 0.0797(13) -0.0791(16) -0.0298(13) 0.0254(17) Cl13 0.0587(8) 0.0408(7) 0.0950(11) 0.0089(7) 0.0081(8) -0.0066(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 Ru1 O7 2.017(2) . ? Ru1 O9 2.024(2) . ? Ru1 O8 2.034(3) . ? Ru1 Cl2 2.2654(8) . ? Ru1 Cl3 2.2822(8) . ? Ru1 Cl1 2.2868(8) . ? Co1 C5 2.068(4) . ? Co1 C2 2.071(4) . ? Co1 C4 2.076(4) . ? Co1 C1 2.078(4) . ? Co1 C3 2.090(4) . ? Co1 P1 2.1541(10) . ? Co1 P3 2.1577(10) . ? Co1 P2 2.1585(10) . ? P1 O7 1.539(2) . ? P1 O1 1.583(3) . ? P1 O2 1.600(3) . ? P2 O8 1.537(2) . ? P2 O3 1.586(3) . ? P2 O4 1.587(3) . ? P3 O9 1.534(2) . ? P3 O5 1.581(2) . ? P3 O6 1.593(3) . ? O1 C11 1.482(5) . ? O2 C13 1.431(5) . ? O3 C15 1.467(5) . ? O4 C17 1.411(10) . ? O4 C17A 1.478(9) . ? O5 C19 1.477(4) . ? O6 C21 1.422(6) . ? C1 C5 1.404(6) . ? C1 C2 1.417(7) . ? C2 C3 1.430(9) . ? C3 C4 1.409(8) . ? C4 C5 1.408(7) . ? C11 C12 1.447(8) . ? C13 C14 1.431(14) . ? C13 C14A 1.457(10) . ? C15 C16 1.493(7) . ? C17 C18 1.495(18) . ? C17A C18A 1.556(17) . ? C19 C20 1.494(6) . ? C21 C22 1.497(8) . ? C1S Cl12 1.742(5) . ? C1S Cl11 1.754(6) . ? C1S Cl13 1.761(5) . ? 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 O7 Ru1 O9 89.95(10) . . ? O7 Ru1 O8 88.04(10) . . ? O9 Ru1 O8 90.01(10) . . ? O7 Ru1 Cl2 89.73(8) . . ? O9 Ru1 Cl2 87.87(7) . . ? O8 Ru1 Cl2 176.93(7) . . ? O7 Ru1 Cl3 176.30(7) . . ? O9 Ru1 Cl3 88.91(7) . . ? O8 Ru1 Cl3 88.44(7) . . ? Cl2 Ru1 Cl3 93.74(3) . . ? O7 Ru1 Cl1 89.03(7) . . ? O9 Ru1 Cl1 178.76(7) . . ? O8 Ru1 Cl1 89.25(7) . . ? Cl2 Ru1 Cl1 92.83(3) . . ? Cl3 Ru1 Cl1 92.06(3) . . ? C5 Co1 C2 66.53(17) . . ? C5 Co1 C4 39.74(19) . . ? C2 Co1 C4 67.3(2) . . ? C5 Co1 C1 39.59(17) . . ? C2 Co1 C1 39.9(2) . . ? C4 Co1 C1 67.25(18) . . ? C5 Co1 C3 66.07(19) . . ? C2 Co1 C3 40.2(2) . . ? C4 Co1 C3 39.5(2) . . ? C1 Co1 C3 66.9(2) . . ? C5 Co1 P1 111.54(13) . . ? C2 Co1 P1 102.68(17) . . ? C4 Co1 P1 151.19(14) . . ? C1 Co1 P1 87.61(13) . . ? C3 Co1 P1 142.2(2) . . ? C5 Co1 P3 96.06(12) . . ? C2 Co1 P3 160.45(14) . . ? C4 Co1 P3 93.73(14) . . ? C1 Co1 P3 129.50(13) . . ? C3 Co1 P3 125.9(2) . . ? P1 Co1 P3 91.76(4) . . ? C5 Co1 P2 157.06(13) . . ? C2 Co1 P2 102.67(14) . . ? C4 Co1 P2 117.99(15) . . ? C1 Co1 P2 140.24(13) . . ? C3 Co1 P2 92.42(15) . . ? P1 Co1 P2 90.22(4) . . ? P3 Co1 P2 90.23(4) . . ? O7 P1 O1 109.73(14) . . ? O7 P1 O2 104.81(14) . . ? O1 P1 O2 100.90(14) . . ? O7 P1 Co1 116.93(10) . . ? O1 P1 Co1 108.65(10) . . ? O2 P1 Co1 114.60(12) . . ? O8 P2 O3 109.59(14) . . ? O8 P2 O4 104.88(15) . . ? O3 P2 O4 101.92(16) . . ? O8 P2 Co1 116.92(10) . . ? O3 P2 Co1 108.14(11) . . ? O4 P2 Co1 114.32(12) . . ? O9 P3 O5 109.84(14) . . ? O9 P3 O6 105.21(14) . . ? O5 P3 O6 100.44(15) . . ? O9 P3 Co1 115.63(10) . . ? O5 P3 Co1 109.91(10) . . ? O6 P3 Co1 114.67(11) . . ? C11 O1 P1 118.8(3) . . ? C13 O2 P1 124.7(3) . . ? C15 O3 P2 121.7(3) . . ? C17 O4 C17A 26.9(4) . . ? C17 O4 P2 126.7(5) . . ? C17A O4 P2 123.5(4) . . ? C19 O5 P3 119.4(2) . . ? C21 O6 P3 123.3(3) . . ? P1 O7 Ru1 125.90(14) . . ? P2 O8 Ru1 126.81(14) . . ? P3 O9 Ru1 126.58(14) . . ? C5 C1 C2 107.2(4) . . ? C5 C1 Co1 69.8(2) . . ? C2 C1 Co1 69.8(2) . . ? C1 C2 C3 107.7(4) . . ? C1 C2 Co1 70.3(2) . . ? C3 C2 Co1 70.6(3) . . ? C4 C3 C2 108.2(4) . . ? C4 C3 Co1 69.7(3) . . ? C2 C3 Co1 69.2(3) . . ? C5 C4 C3 107.2(4) . . ? C5 C4 Co1 69.8(2) . . ? C3 C4 Co1 70.8(3) . . ? C1 C5 C4 109.8(4) . . ? C1 C5 Co1 70.6(2) . . ? C4 C5 Co1 70.4(2) . . ? C12 C11 O1 110.7(4) . . ? O2 C13 C14 112.1(7) . . ? O2 C13 C14A 110.7(5) . . ? C14 C13 C14A 26.4(6) . . ? O3 C15 C16 111.1(4) . . ? O4 C17 C18 107.8(8) . . ? O4 C17A C18A 104.9(7) . . ? O5 C19 C20 108.0(4) . . ? O6 C21 C22 109.0(5) . . ? Cl12 C1S Cl11 110.2(3) . . ? Cl12 C1S Cl13 112.2(3) . . ? Cl11 C1S Cl13 109.4(3) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 71.47 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.257 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.134 ### end # Attachment '- cpd13-updated.cif' data_ip16 _database_code_depnum_ccdc_archive 'CCDC 795120' #TrackingRef '- cpd13-updated.cif' _audit_creation_date 2011-07-05 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H86 Co2 N6 O18 P6 Ru2, 4(B0.5 F2), 0.5(C4 H10 O)' _chemical_formula_sum 'C56 H91 B2 Co2 F8 N6 O18.50 P6 Ru2' _chemical_formula_weight 1823.79 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 _space_group_IT_number 5 _space_group_name_Hall 'C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' _cell_length_a 21.501(3) _cell_length_b 14.5812(19) _cell_length_c 26.604(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.057(2) _cell_angle_gamma 90.00 _cell_volume 8124.9(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5309 _cell_measurement_temperature 173.0 _cell_measurement_theta_max 23.68 _cell_measurement_theta_min 2.21 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.846418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0396 before and 0.0282 after correction. The Ratio of minimum to maximum transmission is 0.846418. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3724 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_unetI/netI 0.0912 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 29502 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.78 _diffrn_ambient_temperature 175.0 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_current 40.0 _diffrn_source_power 2.0 _diffrn_source_target MO _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 11008 _reflns_number_total 15493 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.869 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.081 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(17) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 885 _refine_ls_number_reflns 15493 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0541 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.1050 _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. All the BF4- ions be restrained with DFIX 1.35 for B-F bonds and DANG 2.20 for all F-F 1,3-distances. In addition, for B(3) of BF4, the two parts are refined with F(5) to F(8) and F(5A) to F(8A) with occupancies of 0.65:0.35 respectively. In LOET ligand, One of Cp ring are found to be rotational disorder with occ- upancies of 0.52:0.48. The bonds of the disordered diethyl ether have been restrained with DFIX 1.50 and 1.40 for C-C and C-O bonds repectively and the answer definitely shows it is a diethyl ether with half occupancy (or more precise it can't be more than half). Besides the above restrains applied mentioned, all the bonds related to the disordered OEt groups of the tripod ligand have be restrained and the partial occupancies for those disordered atoms have been tested before fixed. C(13A)-O(2) bond has been restrained with DFIX 1.40 for C-O bond. The non-hydrogen atoms (F5-F8, F5A-F8A) in BF4 containing B3 are disordered over two overlapping positions. So, F5-F8, F5A-F8A atoms were left isotropic. o.5 mmol of solvate ethyl ether are situated inside large space among BF4- and {[LoetRu(bpy)]2(m-N2)}+ species. It was not possible to refined the atoms (C1S-C5S, O3S) in this co-cystallized solvent as antiiso- tropic due to the high U(eq). The non-hydrogen atoms C1-C5, C1A-C5A, C13, C14, C16, C18, C20, C22, C32, C40, C41, C42, C13A, C14A, C16A, C18A, C20A, C22A, C32A, C40A, C41A, C42 in the Loet liangd were left isotropic due to their serious disorder and high U(eq). ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.28316(3) 0.22067(3) 0.338551(19) 0.03983(14) Uani 1 1 d . B . Ru2 Ru 0.23924(3) 0.07083(3) 0.170073(18) 0.03724(13) Uani 1 1 d . B . Co1 Co 0.20534(5) 0.44345(6) 0.37874(3) 0.0515(3) Uani 1 1 d . . . Co2 Co 0.32728(4) -0.15383(6) 0.14693(3) 0.0394(2) Uani 1 1 d . . . P1 P 0.15689(10) 0.34706(14) 0.32125(7) 0.0541(5) Uani 1 1 d . B . P2 P 0.24405(10) 0.33252(14) 0.42999(6) 0.0511(5) Uani 1 1 d . B . P3 P 0.28798(10) 0.44275(12) 0.34502(7) 0.0505(5) Uani 1 1 d . B . P4 P 0.25226(8) -0.08886(11) 0.09065(6) 0.0382(4) Uani 1 1 d . . . P5 P 0.37411(9) -0.02427(12) 0.16963(7) 0.0409(4) Uani 1 1 d . . . P6 P 0.27113(9) -0.13987(11) 0.20457(7) 0.0431(4) Uani 1 1 d . L . O1 O 0.1468(3) 0.3980(3) 0.26649(18) 0.0691(15) Uani 1 1 d . . . O2 O 0.0837(2) 0.3332(4) 0.3221(2) 0.0836(17) Uani 1 1 d D . . O3 O 0.1845(3) 0.2817(4) 0.4447(2) 0.0744(16) Uani 1 1 d . . . O4 O 0.2810(3) 0.3650(4) 0.48538(17) 0.0743(17) Uani 1 1 d . . . O5 O 0.3460(3) 0.4766(4) 0.38901(19) 0.0677(15) Uani 1 1 d . B . O6 O 0.2850(3) 0.5209(3) 0.3042(2) 0.0788(18) Uani 1 1 d . B . O7 O 0.1861(2) 0.2542(3) 0.31881(16) 0.0497(12) Uani 1 1 d . . . O8 O 0.2869(2) 0.2626(3) 0.41288(15) 0.0436(11) Uani 1 1 d . . . O9 O 0.3054(2) 0.3559(3) 0.32076(16) 0.0474(11) Uani 1 1 d . . . N10 N 0.2753(3) 0.1773(3) 0.2705(2) 0.0390(13) Uani 1 1 d . . . N20 N 0.2639(3) 0.1446(3) 0.2309(2) 0.0414(14) Uani 1 1 d . B . O11 O 0.2033(2) -0.1615(3) 0.05796(17) 0.0551(12) Uani 1 1 d . J . O12 O 0.2835(2) -0.0483(3) 0.04599(15) 0.0450(11) Uani 1 1 d . . . O13 O 0.4324(2) -0.0057(3) 0.14422(17) 0.0523(12) Uani 1 1 d . . . O14 O 0.4108(2) -0.0361(3) 0.22785(17) 0.0576(13) Uani 1 1 d . . . O15 O 0.3005(3) -0.1924(3) 0.25637(18) 0.0687(16) Uani 1 1 d . L . O16 O 0.2094(2) -0.1993(3) 0.18566(19) 0.0614(14) Uani 1 1 d . . . O17 O 0.2112(2) -0.0164(3) 0.10753(15) 0.0394(11) Uani 1 1 d . . . O18 O 0.3336(2) 0.0616(3) 0.16238(15) 0.0432(10) Uani 1 1 d . . . O19 O 0.2533(2) -0.0450(3) 0.21932(15) 0.0428(11) Uani 1 1 d . . . N1 N 0.3738(3) 0.1811(3) 0.36538(19) 0.0447(14) Uani 1 1 d . . . N2 N 0.2691(3) 0.0932(3) 0.36395(19) 0.0434(14) Uani 1 1 d . . . N3 N 0.2177(3) 0.1740(4) 0.1190(2) 0.0428(14) Uani 1 1 d . . . N4 N 0.1463(2) 0.0869(3) 0.16870(18) 0.0402(13) Uani 1 1 d . . . B1 B 0.5000 0.8922(9) 0.0000 0.063(4) Uani 1 2 d SD . . F1 F 0.4886(2) 0.8379(4) 0.03922(19) 0.1053(18) Uani 1 1 d D . . F2 F 0.5528(2) 0.9441(3) 0.01764(18) 0.0867(14) Uani 1 1 d D . . B2 B 0.5000 0.8551(7) 0.5000 0.056(3) Uani 1 2 d SD . . F3 F 0.5444(3) 0.9106(4) 0.4873(3) 0.131(2) Uani 1 1 d D . . F4 F 0.4747(4) 0.8043(7) 0.4592(3) 0.254(5) Uani 1 1 d D . . B3 B 0.0461(6) 0.8877(10) 0.3099(5) 0.185(10) Uani 1 1 d D . . F5 F 0.0905(4) 0.9372(7) 0.2928(4) 0.099(3) Uiso 0.65 1 d PD A 1 F6 F 0.0521(4) 0.8952(5) 0.3602(3) 0.079(2) Uiso 0.65 1 d PD A 1 F7 F -0.0121(5) 0.9357(9) 0.2881(4) 0.153(4) Uiso 0.65 1 d PD A 1 F8 F 0.0341(9) 0.8043(10) 0.2908(6) 0.220(7) Uiso 0.65 1 d PD A 1 F5A F 0.0838(8) 0.9015(13) 0.2740(7) 0.110(7) Uiso 0.35 1 d PD A 2 F6A F 0.0838(9) 0.8094(12) 0.3280(8) 0.149(7) Uiso 0.35 1 d PD A 2 F7A F 0.0536(16) 0.9714(16) 0.3315(13) 0.281(17) Uiso 0.35 1 d PD A 2 F8A F -0.0105(7) 0.8618(14) 0.2891(6) 0.117(6) Uiso 0.35 1 d PD A 2 C1 C 0.1668(10) 0.5081(11) 0.4313(5) 0.056(4) Uiso 0.52 1 d PD B 1 H1 H 0.1610 0.4809 0.4644 0.067 Uiso 0.52 1 d PR B 1 C2 C 0.2135(8) 0.5517(14) 0.4247(7) 0.090(6) Uiso 0.52 1 d PD B 1 H2 H 0.2517 0.5673 0.4526 0.108 Uiso 0.52 1 d PR B 1 C3 C 0.2011(9) 0.5814(11) 0.3791(7) 0.064(4) Uiso 0.52 1 d PD B 1 H3 H 0.2290 0.6236 0.3643 0.077 Uiso 0.52 1 d PR B 1 C4 C 0.1464(8) 0.5537(11) 0.3578(5) 0.048(4) Uiso 0.52 1 d PD B 1 H4 H 0.1240 0.5694 0.3216 0.058 Uiso 0.52 1 d PR B 1 C5 C 0.1257(9) 0.5043(14) 0.3894(8) 0.091(7) Uiso 0.52 1 d PD B 1 H5 H 0.0822 0.4762 0.3828 0.109 Uiso 0.52 1 d PR B 1 C1A C 0.2087(5) 0.5300(8) 0.4428(4) 0.020(3) Uiso 0.48 1 d PD B 2 H1A H 0.2375 0.5209 0.4777 0.024 Uiso 0.48 1 d PR B 2 C2A C 0.2259(6) 0.5826(8) 0.3990(5) 0.030(3) Uiso 0.48 1 d PD B 2 H2A H 0.2671 0.6152 0.4000 0.035 Uiso 0.48 1 d PR B 2 C3A C 0.1678(7) 0.5770(10) 0.3532(5) 0.043(4) Uiso 0.48 1 d PD B 2 H3A H 0.1651 0.6042 0.3183 0.052 Uiso 0.48 1 d PR B 2 C4A C 0.1172(7) 0.5154(12) 0.3699(6) 0.055(5) Uiso 0.48 1 d PD B 2 H4A H 0.0757 0.4968 0.3468 0.066 Uiso 0.48 1 d PR B 2 C5A C 0.1412(7) 0.4874(9) 0.4259(5) 0.036(4) Uiso 0.48 1 d PD B 2 H5A H 0.1184 0.4481 0.4467 0.044 Uiso 0.48 1 d PR B 2 C6 C 0.3720(4) -0.2721(5) 0.1810(3) 0.060(2) Uani 1 1 d . . . H6 H 0.3762 -0.2904 0.2179 0.072 Uiso 1 1 calc R . . C7 C 0.3220(4) -0.2964(4) 0.1404(3) 0.054(2) Uani 1 1 d . . . H7 H 0.2845 -0.3349 0.1432 0.065 Uiso 1 1 calc R . . C8 C 0.3335(4) -0.2592(4) 0.0942(3) 0.0530(19) Uani 1 1 d . . . H8 H 0.3067 -0.2670 0.0585 0.064 Uiso 1 1 calc R . . C9 C 0.3913(4) -0.2117(5) 0.1090(4) 0.066(2) Uani 1 1 d . . . H9 H 0.4128 -0.1782 0.0848 0.080 Uiso 1 1 calc R . . C10 C 0.4151(4) -0.2183(5) 0.1624(4) 0.069(2) Uani 1 1 d . . . H10 H 0.4564 -0.1929 0.1827 0.083 Uiso 1 1 calc R . . C11 C 0.1203(5) 0.3451(7) 0.2200(3) 0.104(3) Uani 1 1 d . B . H11A H 0.1530 0.3023 0.2129 0.125 Uiso 1 1 calc R . . H11B H 0.0835 0.3084 0.2252 0.125 Uiso 1 1 calc R . . C12 C 0.0999(5) 0.4058(7) 0.1767(3) 0.099(3) Uani 1 1 d . . . H12A H 0.0824 0.3697 0.1456 0.148 Uiso 1 1 calc R B . H12B H 0.1364 0.4417 0.1715 0.148 Uiso 1 1 calc R . . H12C H 0.0669 0.4473 0.1835 0.148 Uiso 1 1 calc R . . C13 C 0.0580(15) 0.2667(18) 0.3506(10) 0.132(14) Uiso 0.60 1 d PD B 1 H13A H 0.0295 0.2957 0.3706 0.159 Uiso 0.60 1 calc PR B 1 H13B H 0.0923 0.2331 0.3746 0.159 Uiso 0.60 1 calc PR B 1 C14 C 0.0208(11) 0.2035(14) 0.3094(8) 0.117(7) Uiso 0.60 1 d PD B 1 H14A H -0.0118 0.2388 0.2854 0.176 Uiso 0.60 1 calc PR B 1 H14B H 0.0001 0.1555 0.3256 0.176 Uiso 0.60 1 calc PR B 1 H14C H 0.0500 0.1753 0.2904 0.176 Uiso 0.60 1 calc PR B 1 C13A C 0.0634(13) 0.2486(17) 0.3453(10) 0.061(9) Uiso 0.40 1 d PD B 2 H13C H 0.0661 0.2567 0.3827 0.074 Uiso 0.40 1 calc PR B 2 H13D H 0.0897 0.1952 0.3401 0.074 Uiso 0.40 1 calc PR B 2 C14A C -0.0047(15) 0.238(3) 0.3160(16) 0.19(2) Uiso 0.40 1 d PD B 2 H14D H -0.0055 0.2172 0.2808 0.285 Uiso 0.40 1 calc PR B 2 H14E H -0.0269 0.2965 0.3149 0.285 Uiso 0.40 1 calc PR B 2 H14F H -0.0260 0.1920 0.3333 0.285 Uiso 0.40 1 calc PR B 2 C15 C 0.1951(4) 0.2018(7) 0.4777(3) 0.089(3) Uani 1 1 d D B . H15A H 0.2331 0.2123 0.5061 0.107 Uiso 0.50 1 calc PR C 1 H15B H 0.2041 0.1484 0.4575 0.107 Uiso 0.50 1 calc PR C 1 H15C H 0.2077 0.2209 0.5144 0.107 Uiso 0.50 1 calc PR C 2 H15D H 0.2299 0.1640 0.4698 0.107 Uiso 0.50 1 calc PR C 2 C16 C 0.1404(8) 0.1811(13) 0.4997(8) 0.090(6) Uiso 0.50 1 d PD B 1 H16A H 0.1359 0.2289 0.5245 0.135 Uiso 0.50 1 calc PR B 1 H16B H 0.1470 0.1216 0.5173 0.135 Uiso 0.50 1 calc PR B 1 H16C H 0.1017 0.1787 0.4721 0.135 Uiso 0.50 1 calc PR B 1 C16A C 0.1342(8) 0.1471(13) 0.4687(8) 0.094(6) Uiso 0.50 1 d PD B 2 H16D H 0.1009 0.1835 0.4790 0.141 Uiso 0.50 1 calc PR B 2 H16E H 0.1414 0.0906 0.4891 0.141 Uiso 0.50 1 calc PR B 2 H16F H 0.1207 0.1316 0.4320 0.141 Uiso 0.50 1 calc PR B 2 C17 C 0.3498(6) 0.3705(7) 0.5000(4) 0.104(4) Uani 1 1 d D B . H17A H 0.3584 0.4136 0.5295 0.125 Uiso 0.35 1 calc PR D 1 H17B H 0.3617 0.4037 0.4712 0.125 Uiso 0.35 1 calc PR D 1 H17C H 0.3633 0.4242 0.5226 0.125 Uiso 0.65 1 calc PR D 2 H17D H 0.3679 0.3760 0.4691 0.125 Uiso 0.65 1 calc PR D 2 C18 C 0.3999(19) 0.299(3) 0.5146(19) 0.17(2) Uiso 0.35 1 d PD B 1 H18A H 0.3836 0.2486 0.5327 0.259 Uiso 0.35 1 calc PR B 1 H18B H 0.4379 0.3252 0.5372 0.259 Uiso 0.35 1 calc PR B 1 H18C H 0.4110 0.2745 0.4833 0.259 Uiso 0.35 1 calc PR B 1 C18A C 0.3723(9) 0.2804(11) 0.5293(7) 0.109(6) Uiso 0.65 1 d PD B 2 H18D H 0.3536 0.2757 0.5596 0.163 Uiso 0.65 1 calc PR B 2 H18E H 0.4190 0.2806 0.5405 0.163 Uiso 0.65 1 calc PR B 2 H18F H 0.3586 0.2280 0.5065 0.163 Uiso 0.65 1 calc PR B 2 C19 C 0.4094(5) 0.4887(7) 0.3792(4) 0.094(3) Uani 1 1 d D . . H19A H 0.4303 0.4280 0.3803 0.113 Uiso 0.50 1 calc PR E 1 H19B H 0.4051 0.5138 0.3439 0.113 Uiso 0.50 1 calc PR E 1 H19C H 0.4098 0.5439 0.3576 0.113 Uiso 0.50 1 calc PR E 2 H19D H 0.4202 0.4350 0.3600 0.113 Uiso 0.50 1 calc PR E 2 C20 C 0.4497(8) 0.5485(12) 0.4152(6) 0.070(5) Uiso 0.50 1 d PD F 1 H20A H 0.4235 0.5954 0.4269 0.105 Uiso 0.50 1 calc PR F 1 H20B H 0.4806 0.5783 0.3985 0.105 Uiso 0.50 1 calc PR F 1 H20C H 0.4725 0.5129 0.4449 0.105 Uiso 0.50 1 calc PR F 1 C20A C 0.4584(9) 0.4990(16) 0.4288(7) 0.100(7) Uiso 0.50 1 d PD F 2 H20D H 0.4444 0.5459 0.4502 0.150 Uiso 0.50 1 calc PR F 2 H20E H 0.4993 0.5174 0.4214 0.150 Uiso 0.50 1 calc PR F 2 H20F H 0.4637 0.4404 0.4473 0.150 Uiso 0.50 1 calc PR F 2 C21 C 0.2761(7) 0.5032(8) 0.2493(4) 0.128(5) Uani 1 1 d D . . H21A H 0.2463 0.5484 0.2290 0.153 Uiso 0.60 1 calc PR G 1 H21B H 0.2586 0.4408 0.2408 0.153 Uiso 0.60 1 calc PR G 1 H21C H 0.2575 0.4411 0.2420 0.153 Uiso 0.40 1 calc PR G 2 H21D H 0.3185 0.5026 0.2407 0.153 Uiso 0.40 1 calc PR G 2 C22 C 0.3410(12) 0.512(2) 0.2376(12) 0.224(14) Uiso 0.60 1 d PD H 1 H22A H 0.3606 0.5696 0.2516 0.335 Uiso 0.60 1 calc PR H 1 H22B H 0.3369 0.5103 0.2002 0.335 Uiso 0.60 1 calc PR H 1 H22C H 0.3679 0.4604 0.2535 0.335 Uiso 0.60 1 calc PR H 1 C22A C 0.235(2) 0.569(3) 0.2146(16) 0.25(2) Uiso 0.40 1 d PD H 2 H22D H 0.2514 0.5784 0.1835 0.380 Uiso 0.40 1 calc PR H 2 H22E H 0.2346 0.6279 0.2324 0.380 Uiso 0.40 1 calc PR H 2 H22F H 0.1912 0.5450 0.2048 0.380 Uiso 0.40 1 calc PR H 2 C31 C 0.1388(5) -0.1715(7) 0.0633(4) 0.104(3) Uani 1 1 d D . . H31A H 0.1379 -0.1622 0.1000 0.125 Uiso 0.50 1 calc PR I 1 H31B H 0.1126 -0.1226 0.0431 0.125 Uiso 0.50 1 calc PR I 1 H31C H 0.1180 -0.1107 0.0620 0.125 Uiso 0.50 1 calc PR I 2 H31D H 0.1381 -0.2008 0.0967 0.125 Uiso 0.50 1 calc PR I 2 C32 C 0.1104(9) -0.2579(11) 0.0470(8) 0.087(6) Uiso 0.50 1 d PD J 1 H32A H 0.1226 -0.2769 0.0152 0.130 Uiso 0.50 1 calc PR J 1 H32B H 0.0639 -0.2525 0.0405 0.130 Uiso 0.50 1 calc PR J 1 H32C H 0.1253 -0.3037 0.0740 0.130 Uiso 0.50 1 calc PR J 1 C32A C 0.1050(9) -0.2294(12) 0.0201(7) 0.079(5) Uiso 0.50 1 d PD J 2 H32D H 0.0892 -0.1910 -0.0103 0.119 Uiso 0.50 1 calc PR J 2 H32E H 0.0690 -0.2601 0.0299 0.119 Uiso 0.50 1 calc PR J 2 H32F H 0.1344 -0.2756 0.0120 0.119 Uiso 0.50 1 calc PR J 2 C33 C 0.2453(4) 0.0075(5) 0.0063(3) 0.066(2) Uani 1 1 d . . . H33A H 0.2254 0.0578 0.0222 0.079 Uiso 1 1 calc R . . H33B H 0.2108 -0.0300 -0.0149 0.079 Uiso 1 1 calc R . . C34 C 0.2849(5) 0.0463(6) -0.0267(3) 0.102(3) Uani 1 1 d . . . H34A H 0.2582 0.0836 -0.0539 0.152 Uiso 1 1 calc R . . H34B H 0.3045 -0.0036 -0.0424 0.152 Uiso 1 1 calc R . . H34C H 0.3184 0.0847 -0.0058 0.152 Uiso 1 1 calc R . . C35 C 0.4247(4) 0.0382(5) 0.0941(2) 0.059(2) Uani 1 1 d . . . H35A H 0.3888 0.0824 0.0888 0.070 Uiso 1 1 calc R . . H35B H 0.4150 -0.0084 0.0664 0.070 Uiso 1 1 calc R . . C36 C 0.4856(4) 0.0872(6) 0.0926(3) 0.083(3) Uani 1 1 d . . . H36A H 0.4814 0.1166 0.0588 0.124 Uiso 1 1 calc R . . H36B H 0.5209 0.0430 0.0981 0.124 Uiso 1 1 calc R . . H36C H 0.4944 0.1339 0.1197 0.124 Uiso 1 1 calc R . . C37 C 0.4330(4) 0.0464(6) 0.2603(3) 0.075(2) Uani 1 1 d . . . H37A H 0.4028 0.0976 0.2488 0.090 Uiso 1 1 calc R . . H37B H 0.4327 0.0325 0.2967 0.090 Uiso 1 1 calc R . . C38 C 0.4937(6) 0.0736(9) 0.2574(4) 0.133(4) Uani 1 1 d . . . H38A H 0.5061 0.1278 0.2792 0.199 Uiso 1 1 calc R . . H38B H 0.4940 0.0887 0.2216 0.199 Uiso 1 1 calc R . . H38C H 0.5239 0.0237 0.2694 0.199 Uiso 1 1 calc R . . C39 C 0.3338(5) -0.1528(6) 0.3035(3) 0.088(3) Uani 1 1 d D . . H39A H 0.3030 -0.1177 0.3185 0.106 Uiso 0.45 1 calc PR K 1 H39B H 0.3655 -0.1087 0.2958 0.106 Uiso 0.45 1 calc PR K 1 H39C H 0.3115 -0.0972 0.3116 0.106 Uiso 0.55 1 calc PR K 2 H39D H 0.3778 -0.1358 0.3015 0.106 Uiso 0.55 1 calc PR K 2 C40 C 0.3683(13) -0.2202(16) 0.3436(9) 0.113(10) Uiso 0.45 1 d PD L 1 H40A H 0.3399 -0.2718 0.3461 0.169 Uiso 0.45 1 calc PR L 1 H40B H 0.3806 -0.1895 0.3771 0.169 Uiso 0.45 1 calc PR L 1 H40C H 0.4066 -0.2429 0.3334 0.169 Uiso 0.45 1 calc PR L 1 C40A C 0.3350(9) -0.2264(9) 0.3443(6) 0.067(4) Uiso 0.55 1 d PD L 2 H40D H 0.2912 -0.2447 0.3445 0.100 Uiso 0.55 1 calc PR L 2 H40E H 0.3558 -0.2021 0.3783 0.100 Uiso 0.55 1 calc PR L 2 H40F H 0.3588 -0.2799 0.3364 0.100 Uiso 0.55 1 calc PR L 2 C41 C 0.1568(7) -0.2021(8) 0.2123(5) 0.047(3) Uiso 0.60 1 d PD M 1 H41A H 0.1218 -0.1613 0.1947 0.057 Uiso 0.60 1 calc PR M 1 H41B H 0.1718 -0.1808 0.2483 0.057 Uiso 0.60 1 calc PR M 1 C42 C 0.1331(9) -0.2996(10) 0.2117(6) 0.089(5) Uiso 0.60 1 d PD M 1 H42A H 0.1122 -0.3169 0.1763 0.134 Uiso 0.60 1 calc PR M 1 H42B H 0.1023 -0.3044 0.2337 0.134 Uiso 0.60 1 calc PR M 1 H42C H 0.1692 -0.3407 0.2246 0.134 Uiso 0.60 1 calc PR M 1 C41A C 0.1766(10) -0.2249(17) 0.2284(9) 0.074(8) Uiso 0.40 1 d PD M 2 H41C H 0.1725 -0.1715 0.2504 0.088 Uiso 0.40 1 calc PR M 2 H41D H 0.1991 -0.2752 0.2501 0.088 Uiso 0.40 1 calc PR M 2 C42A C 0.1111(11) -0.256(2) 0.1957(10) 0.105(9) Uiso 0.40 1 d PD M 2 H42D H 0.1169 -0.3105 0.1757 0.158 Uiso 0.40 1 calc PR M 2 H42E H 0.0924 -0.2066 0.1722 0.158 Uiso 0.40 1 calc PR M 2 H42F H 0.0826 -0.2708 0.2186 0.158 Uiso 0.40 1 calc PR M 2 C51 C 0.4260(3) 0.2271(5) 0.3598(3) 0.0520(17) Uani 1 1 d . B . H51 H 0.4206 0.2792 0.3378 0.062 Uiso 1 1 calc R . . C52 C 0.4861(4) 0.2023(6) 0.3843(3) 0.067(2) Uani 1 1 d . . . H52 H 0.5219 0.2352 0.3785 0.080 Uiso 1 1 calc R B . C53 C 0.4944(4) 0.1284(6) 0.4179(4) 0.073(2) Uani 1 1 d . B . H53 H 0.5356 0.1116 0.4371 0.087 Uiso 1 1 calc R . . C54 C 0.4404(4) 0.0795(6) 0.4225(3) 0.064(2) Uani 1 1 d . . . H54 H 0.4448 0.0273 0.4444 0.077 Uiso 1 1 calc R B . C55 C 0.3815(4) 0.1055(5) 0.3961(3) 0.0489(18) Uani 1 1 d . B . C56 C 0.3219(4) 0.0557(5) 0.3947(2) 0.0459(18) Uani 1 1 d . B . C57 C 0.3179(4) -0.0257(5) 0.4206(3) 0.060(2) Uani 1 1 d . . . H57 H 0.3546 -0.0516 0.4427 0.072 Uiso 1 1 calc R B . C58 C 0.2600(5) -0.0676(6) 0.4137(3) 0.068(2) Uani 1 1 d . B . H58 H 0.2565 -0.1227 0.4319 0.081 Uiso 1 1 calc R . . C59 C 0.2072(5) -0.0330(5) 0.3815(3) 0.070(3) Uani 1 1 d . . . H59 H 0.1674 -0.0640 0.3761 0.084 Uiso 1 1 calc R B . C60 C 0.2133(4) 0.0499(5) 0.3568(3) 0.0542(19) Uani 1 1 d . B . H60 H 0.1769 0.0758 0.3343 0.065 Uiso 1 1 calc R . . C61 C 0.2594(4) 0.2155(5) 0.0957(3) 0.0564(19) Uani 1 1 d . M . H61 H 0.3038 0.2030 0.1070 0.068 Uiso 1 1 calc R . . C62 C 0.2384(5) 0.2763(5) 0.0554(3) 0.069(2) Uani 1 1 d . . . H62 H 0.2682 0.3025 0.0381 0.083 Uiso 1 1 calc R M . C63 C 0.1758(5) 0.2988(5) 0.0403(3) 0.064(2) Uani 1 1 d . M . H63 H 0.1613 0.3430 0.0141 0.076 Uiso 1 1 calc R . . C64 C 0.1342(4) 0.2549(5) 0.0646(3) 0.062(2) Uani 1 1 d . . . H64 H 0.0898 0.2677 0.0540 0.074 Uiso 1 1 calc R M . C65 C 0.1546(4) 0.1941(4) 0.1032(2) 0.0420(17) Uani 1 1 d . M . C66 C 0.1132(3) 0.1455(4) 0.1314(2) 0.0441(17) Uani 1 1 d . M . C67 C 0.0487(4) 0.1588(5) 0.1243(3) 0.062(2) Uani 1 1 d . . . H67 H 0.0268 0.2001 0.0987 0.074 Uiso 1 1 calc R M . C68 C 0.0166(4) 0.1112(5) 0.1549(3) 0.069(2) Uani 1 1 d . M . H68 H -0.0283 0.1178 0.1498 0.083 Uiso 1 1 calc R . . C69 C 0.0490(4) 0.0537(5) 0.1933(3) 0.066(2) Uani 1 1 d . . . H69 H 0.0272 0.0212 0.2150 0.079 Uiso 1 1 calc R M . C70 C 0.1132(4) 0.0452(4) 0.1987(3) 0.056(2) Uani 1 1 d . M . H70 H 0.1358 0.0071 0.2257 0.068 Uiso 1 1 calc R . . C1S C 0.9534(12) 1.0549(17) 0.0070(10) 0.155(10) Uiso 0.50 1 d PD . . H1SA H 0.9821 1.0755 -0.0146 0.232 Uiso 0.50 1 calc PR . . H1SB H 0.9459 1.1054 0.0292 0.232 Uiso 0.50 1 calc PR . . H1SC H 0.9126 1.0354 -0.0151 0.232 Uiso 0.50 1 calc PR . . C2S C 0.9833(10) 0.9759(15) 0.0398(8) 0.116(7) Uiso 0.50 1 d PD . . H2SA H 0.9897 0.9236 0.0178 0.139 Uiso 0.50 1 calc PR . . H2SB H 1.0253 0.9941 0.0613 0.139 Uiso 0.50 1 calc PR . . O3S O 0.9414(9) 0.9505(13) 0.0715(7) 0.157(6) Uiso 0.50 1 d PD . . C4S C 0.9669(12) 0.8698(17) 0.1004(10) 0.152(10) Uiso 0.50 1 d PD . . H4SA H 1.0069 0.8824 0.1263 0.183 Uiso 0.50 1 calc PR . . H4SB H 0.9732 0.8182 0.0780 0.183 Uiso 0.50 1 calc PR . . C5S C 0.9126(11) 0.8560(17) 0.1238(9) 0.124(8) Uiso 0.50 1 d PD . . H5SA H 0.9203 0.8023 0.1465 0.187 Uiso 0.50 1 calc PR . . H5SB H 0.8740 0.8461 0.0966 0.187 Uiso 0.50 1 calc PR . . H5SC H 0.9069 0.9103 0.1439 0.187 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0505(4) 0.0388(3) 0.0327(3) -0.0049(2) 0.0149(3) 0.0012(3) Ru2 0.0503(3) 0.0335(3) 0.0324(3) -0.0027(2) 0.0188(3) 0.0026(3) Co1 0.0632(7) 0.0517(6) 0.0402(5) -0.0069(5) 0.0133(5) 0.0155(5) Co2 0.0413(5) 0.0371(5) 0.0410(5) -0.0044(4) 0.0118(4) 0.0033(4) P1 0.0553(13) 0.0617(12) 0.0443(10) -0.0058(10) 0.0091(9) 0.0123(11) P2 0.0651(13) 0.0566(11) 0.0347(9) -0.0030(10) 0.0178(9) 0.0132(11) P3 0.0696(14) 0.0403(10) 0.0444(11) -0.0036(9) 0.0187(11) 0.0029(10) P4 0.0388(11) 0.0406(9) 0.0365(9) -0.0097(8) 0.0111(8) 0.0017(8) P5 0.0407(11) 0.0467(10) 0.0363(9) -0.0036(8) 0.0110(9) -0.0043(8) P6 0.0530(12) 0.0374(9) 0.0423(10) -0.0010(8) 0.0179(9) 0.0000(8) O1 0.093(4) 0.065(3) 0.042(3) -0.002(3) -0.002(3) 0.008(3) O2 0.055(4) 0.093(4) 0.100(4) -0.014(4) 0.012(3) 0.015(3) O3 0.073(4) 0.080(4) 0.080(4) 0.027(3) 0.039(3) 0.020(3) O4 0.096(5) 0.087(4) 0.032(3) -0.017(3) -0.001(3) 0.028(4) O5 0.067(4) 0.075(4) 0.063(3) -0.024(3) 0.021(3) -0.007(3) O6 0.129(6) 0.045(3) 0.071(4) 0.008(3) 0.039(4) 0.010(3) O7 0.050(3) 0.053(3) 0.046(3) -0.007(2) 0.012(2) -0.003(2) O8 0.052(3) 0.047(3) 0.034(2) -0.009(2) 0.014(2) 0.009(2) O9 0.059(3) 0.044(3) 0.041(2) -0.004(2) 0.018(2) 0.005(2) N10 0.051(4) 0.037(3) 0.034(3) -0.004(3) 0.019(3) -0.001(3) N20 0.047(4) 0.038(3) 0.042(3) 0.004(3) 0.016(3) -0.001(3) O11 0.045(3) 0.061(3) 0.058(3) -0.027(3) 0.008(2) 0.001(3) O12 0.046(3) 0.053(3) 0.036(2) 0.004(2) 0.011(2) 0.011(2) O13 0.044(3) 0.057(3) 0.056(3) 0.002(2) 0.010(2) -0.004(2) O14 0.055(3) 0.067(3) 0.044(3) 0.000(2) -0.003(2) -0.010(3) O15 0.118(5) 0.047(3) 0.046(3) 0.003(2) 0.028(3) 0.021(3) O16 0.063(4) 0.054(3) 0.079(4) -0.013(3) 0.043(3) -0.017(3) O17 0.043(3) 0.043(2) 0.033(2) -0.006(2) 0.010(2) 0.007(2) O18 0.050(3) 0.034(2) 0.052(2) -0.012(2) 0.023(2) -0.004(2) O19 0.063(3) 0.034(2) 0.037(2) 0.0045(19) 0.024(2) 0.006(2) N1 0.059(4) 0.041(3) 0.039(3) -0.001(3) 0.020(3) 0.006(3) N2 0.058(4) 0.042(3) 0.036(3) -0.004(2) 0.020(3) -0.005(3) N3 0.059(4) 0.039(3) 0.035(3) -0.005(2) 0.020(3) 0.006(3) N4 0.051(3) 0.038(3) 0.040(3) 0.001(3) 0.027(3) 0.008(3) B1 0.042(8) 0.107(11) 0.043(7) 0.000 0.013(6) 0.000 F1 0.085(4) 0.130(4) 0.121(4) 0.054(4) 0.067(3) 0.011(3) F2 0.067(3) 0.100(4) 0.089(3) -0.003(3) 0.010(3) -0.022(3) B2 0.016(6) 0.036(6) 0.098(10) 0.000 -0.022(6) 0.000 F3 0.133(5) 0.112(4) 0.174(6) -0.056(4) 0.091(5) -0.032(4) F4 0.184(9) 0.313(13) 0.261(10) -0.135(9) 0.046(8) -0.127(9) B3 0.167(19) 0.160(18) 0.159(19) 0.033(14) -0.110(16) -0.067(15) C6 0.062(5) 0.047(4) 0.063(5) -0.007(4) -0.001(4) 0.017(4) C7 0.060(5) 0.033(4) 0.073(5) 0.002(4) 0.024(5) 0.011(3) C8 0.069(6) 0.041(4) 0.054(4) -0.009(3) 0.023(4) 0.015(4) C9 0.072(6) 0.060(5) 0.084(6) 0.016(4) 0.053(5) 0.033(5) C10 0.051(5) 0.055(5) 0.096(7) -0.022(5) 0.003(5) 0.023(4) C11 0.141(9) 0.093(7) 0.063(6) -0.027(6) -0.010(6) -0.001(7) C12 0.140(10) 0.092(7) 0.052(5) -0.009(5) -0.003(6) 0.022(7) C15 0.085(7) 0.110(8) 0.076(6) 0.037(6) 0.027(5) 0.012(6) C17 0.119(10) 0.124(9) 0.063(6) -0.037(6) 0.008(6) -0.032(7) C19 0.084(7) 0.112(8) 0.094(7) -0.029(6) 0.033(6) -0.025(6) C21 0.177(14) 0.110(9) 0.097(9) 0.041(7) 0.034(9) 0.026(9) C31 0.080(7) 0.128(9) 0.101(7) -0.048(7) 0.014(6) -0.059(7) C33 0.086(6) 0.070(5) 0.045(4) 0.001(4) 0.022(5) 0.006(5) C34 0.129(9) 0.099(7) 0.085(6) 0.043(6) 0.042(7) 0.023(6) C35 0.071(6) 0.074(5) 0.040(4) 0.003(4) 0.034(4) -0.002(4) C36 0.087(6) 0.079(6) 0.086(6) 0.010(5) 0.029(5) -0.027(5) C37 0.053(6) 0.088(6) 0.079(6) -0.011(5) 0.004(5) -0.017(5) C38 0.116(10) 0.162(11) 0.109(8) -0.051(9) 0.002(7) -0.020(9) C39 0.143(9) 0.058(5) 0.058(5) 0.020(5) 0.013(6) 0.010(6) C51 0.050(5) 0.051(4) 0.059(4) 0.000(4) 0.019(4) 0.002(4) C52 0.053(6) 0.070(6) 0.081(6) 0.000(5) 0.026(5) -0.003(4) C53 0.043(5) 0.084(6) 0.092(7) -0.003(5) 0.016(5) 0.023(5) C54 0.069(6) 0.058(5) 0.066(5) 0.017(4) 0.019(4) 0.028(5) C55 0.064(5) 0.047(4) 0.041(4) -0.008(3) 0.023(4) 0.008(4) C56 0.059(5) 0.054(5) 0.028(3) -0.003(3) 0.017(3) 0.013(4) C57 0.084(6) 0.056(5) 0.045(4) 0.008(4) 0.021(4) 0.009(4) C58 0.091(7) 0.065(5) 0.055(5) 0.014(4) 0.034(5) -0.014(5) C59 0.085(7) 0.067(6) 0.066(5) 0.001(4) 0.032(5) -0.031(5) C60 0.054(5) 0.061(5) 0.051(4) -0.006(4) 0.020(4) -0.010(4) C61 0.073(5) 0.049(4) 0.055(4) 0.005(4) 0.031(4) 0.007(4) C62 0.111(8) 0.052(5) 0.057(5) 0.010(4) 0.047(5) -0.005(5) C63 0.081(7) 0.057(5) 0.059(5) 0.016(4) 0.027(5) 0.010(4) C64 0.077(6) 0.069(5) 0.041(4) 0.004(4) 0.014(4) 0.020(4) C65 0.058(5) 0.032(3) 0.040(4) -0.001(3) 0.018(4) 0.014(3) C66 0.055(5) 0.045(4) 0.036(4) -0.002(3) 0.019(4) 0.006(3) C67 0.043(5) 0.072(5) 0.070(5) 0.014(4) 0.014(4) 0.011(4) C68 0.058(6) 0.066(5) 0.091(6) 0.003(5) 0.033(5) 0.014(4) C69 0.055(5) 0.065(5) 0.091(6) 0.016(5) 0.046(5) -0.001(4) C70 0.077(6) 0.044(4) 0.056(4) 0.008(3) 0.031(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O7 2.092(5) . ? Ru1 O8 2.054(4) . ? Ru1 O9 2.108(4) . ? Ru1 N10 1.890(5) . ? Ru1 N1 2.004(6) . ? Ru1 N2 2.023(5) . ? Ru2 N20 1.916(6) . ? Ru2 O17 2.073(4) . ? Ru2 O18 2.089(4) . ? Ru2 O19 2.117(4) . ? Ru2 N3 2.010(5) . ? Ru2 N4 2.005(5) . ? Co1 P1 2.163(2) . ? Co1 P2 2.158(2) . ? Co1 C1 2.013(15) . ? Co1 C2 1.980(19) . ? Co1 C3 2.014(17) . ? Co1 C4 2.045(13) . ? Co1 C5 2.00(2) . ? Co1 C1A 2.109(10) . ? Co1 C2A 2.120(12) . ? Co1 C3A 2.158(14) . ? Co1 C4A 2.131(17) . ? Co1 C5A 2.160(13) . ? Co2 P4 2.156(2) . ? Co2 P5 2.1616(19) . ? Co2 P6 2.1649(18) . ? Co2 C6 2.080(7) . ? Co2 C7 2.087(7) . ? Co2 C8 2.105(6) . ? Co2 C9 2.063(7) . ? Co2 C10 2.066(7) . ? P1 O1 1.605(5) . ? P1 O2 1.591(6) . ? P1 O7 1.500(5) . ? P2 O3 1.602(5) . ? P2 O4 1.580(5) . ? P2 O8 1.512(4) . ? P3 O5 1.585(6) . ? P3 O6 1.565(5) . ? P3 O9 1.507(4) . ? P4 O11 1.604(5) . ? P4 O12 1.605(4) . ? P4 O17 1.509(4) . ? P5 O13 1.576(4) . ? P5 O14 1.581(5) . ? P5 O18 1.512(4) . ? P6 O15 1.579(5) . ? P6 O16 1.570(5) . ? P6 O19 1.510(4) . ? O1 C11 1.461(9) . ? O2 C13 1.42(3) . ? O2 C13A 1.488(17) . ? O3 C15 1.445(9) . ? O4 C17 1.444(11) . ? O5 C19 1.456(9) . ? O6 C21 1.454(11) . ? N10 N20 1.130(6) . ? O11 C31 1.433(9) . ? O12 C33 1.435(8) . ? O13 C35 1.453(7) . ? O14 C37 1.495(9) . ? O15 C39 1.419(9) . ? O16 C41 1.465(12) . ? O16 C41A 1.51(2) . ? N1 C51 1.342(8) . ? N1 C55 1.360(8) . ? N2 C56 1.356(8) . ? N2 C60 1.330(8) . ? N3 C61 1.343(8) . ? N3 C65 1.359(8) . ? N4 C66 1.379(8) . ? N4 C70 1.330(8) . ? B1 F1 1.375(7) 2_655 ? B1 F1 1.375(7) . ? B1 F2 1.356(7) . ? B1 F2 1.356(7) 2_655 ? B2 F3 1.351(7) . ? B2 F3 1.351(7) 2_656 ? B2 F4 1.326(8) . ? B2 F4 1.326(8) 2_656 ? B3 F5 1.353(13) . ? B3 F6 1.322(13) . ? B3 F7 1.436(14) . ? B3 F8 1.322(14) . ? B3 F5A 1.398(15) . ? B3 F6A 1.421(15) . ? B3 F7A 1.343(16) . ? B3 F8A 1.276(14) . ? C1 C2 1.234(15) . ? C1 C3 2.018(18) . ? C1 C4 2.017(17) . ? C1 C5 1.258(15) . ? C2 C3 1.258(14) . ? C2 C4 2.022(18) . ? C2 C5 2.03(2) . ? C3 C4 1.252(15) . ? C4 C5 1.262(14) . ? C1A C2A 1.510(12) . ? C1A C5A 1.548(13) . ? C2A C3A 1.537(14) . ? C3A C4A 1.550(14) . ? C4A C5A 1.519(14) . ? C6 C7 1.387(10) . ? C6 C10 1.388(11) . ? C7 C8 1.414(9) . ? C8 C9 1.400(11) . ? C9 C10 1.401(11) . ? C11 C12 1.440(12) . ? C13 C14 1.516(17) . ? C13A C14A 1.504(19) . ? C15 C16 1.458(14) . ? C15 C16A 1.506(15) . ? C17 C18 1.490(19) . ? C17 C18A 1.548(14) . ? C19 C20 1.433(14) . ? C19 C20A 1.500(15) . ? C21 C22 1.502(17) . ? C21 C22A 1.482(19) . ? C31 C32 1.424(14) . ? C31 C32A 1.479(14) . ? C33 C34 1.466(10) . ? C35 C36 1.502(10) . ? C37 C38 1.383(12) . ? C39 C40 1.515(16) . ? C39 C40A 1.523(12) . ? C41 C42 1.509(14) . ? C41A C42A 1.546(18) . ? C51 C52 1.358(10) . ? C52 C53 1.384(11) . ? C53 C54 1.392(11) . ? C54 C55 1.355(10) . ? C55 C56 1.467(10) . ? C56 C57 1.384(9) . ? C57 C58 1.361(11) . ? C58 C59 1.355(11) . ? C59 C60 1.397(10) . ? C61 C62 1.387(10) . ? C62 C63 1.355(11) . ? C63 C64 1.373(10) . ? C64 C65 1.353(9) . ? C65 C66 1.471(9) . ? C66 C67 1.369(9) . ? C67 C68 1.371(10) . ? C68 C69 1.380(10) . ? C69 C70 1.361(10) . ? C1S C2S 1.501(17) . ? C2S O3S 1.414(15) . ? O3S C4S 1.444(17) . ? C4S C5S 1.456(17) . ? 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 O7 Ru1 O9 89.37(17) . . ? O8 Ru1 O7 89.53(17) . . ? O8 Ru1 O9 88.65(16) . . ? N10 Ru1 O7 88.3(2) . . ? N10 Ru1 O8 176.4(2) . . ? N10 Ru1 O9 94.23(18) . . ? N10 Ru1 N1 96.5(2) . . ? N10 Ru1 N2 91.4(2) . . ? N1 Ru1 O7 172.80(19) . . ? N1 Ru1 O8 85.40(18) . . ? N1 Ru1 O9 95.6(2) . . ? N1 Ru1 N2 79.8(2) . . ? N2 Ru1 O7 94.7(2) . . ? N2 Ru1 O8 85.87(18) . . ? N2 Ru1 O9 173.1(2) . . ? N20 Ru2 O17 175.95(19) . . ? N20 Ru2 O18 91.67(19) . . ? N20 Ru2 O19 87.22(19) . . ? N20 Ru2 N3 97.4(2) . . ? N20 Ru2 N4 92.0(2) . . ? O17 Ru2 O18 89.72(15) . . ? O17 Ru2 O19 88.98(16) . . ? O18 Ru2 O19 90.17(16) . . ? N3 Ru2 O17 86.30(18) . . ? N3 Ru2 O18 93.6(2) . . ? N3 Ru2 O19 174.0(2) . . ? N4 Ru2 O17 87.04(18) . . ? N4 Ru2 O18 172.86(18) . . ? N4 Ru2 O19 96.14(19) . . ? N4 Ru2 N3 79.9(2) . . ? P2 Co1 P1 90.87(8) . . ? P2 Co1 C3A 159.8(4) . . ? P2 Co1 C5A 93.5(3) . . ? C1 Co1 P1 126.0(6) . . ? C1 Co1 P2 94.2(4) . . ? C1 Co1 C3 60.2(5) . . ? C1 Co1 C4 59.6(5) . . ? C1 Co1 C1A 26.2(5) . . ? C1 Co1 C2A 58.0(5) . . ? C1 Co1 C3A 67.2(5) . . ? C1 Co1 C4A 49.6(6) . . ? C1 Co1 C5A 16.5(5) . . ? C2 Co1 P1 156.3(5) . . ? C2 Co1 P2 103.9(6) . . ? C2 Co1 C1 36.0(4) . . ? C2 Co1 C3 36.7(4) . . ? C2 Co1 C4 60.3(6) . . ? C2 Co1 C5 61.3(7) . . ? C2 Co1 C1A 16.6(6) . . ? C2 Co1 C2A 25.3(5) . . ? C2 Co1 C3A 56.6(6) . . ? C2 Co1 C4A 68.2(6) . . ? C2 Co1 C5A 52.0(6) . . ? C3 Co1 P1 129.6(6) . . ? C3 Co1 P2 139.2(6) . . ? C3 Co1 C4 35.9(4) . . ? C3 Co1 C1A 52.5(5) . . ? C3 Co1 C2A 18.2(5) . . ? C3 Co1 C3A 24.0(5) . . ? C3 Co1 C4A 57.9(5) . . ? C3 Co1 C5A 70.4(5) . . ? C4 Co1 P1 98.5(4) . . ? C4 Co1 P2 152.7(4) . . ? C4 Co1 C1A 69.9(4) . . ? C4 Co1 C2A 53.0(5) . . ? C4 Co1 C3A 16.3(4) . . ? C4 Co1 C4A 26.2(4) . . ? C4 Co1 C5A 59.2(5) . . ? C5 Co1 P1 95.6(6) . . ? C5 Co1 P2 117.5(6) . . ? C5 Co1 C1 36.5(5) . . ? C5 Co1 C3 61.1(6) . . ? C5 Co1 C4 36.3(4) . . ? C5 Co1 C1A 59.7(6) . . ? C5 Co1 C2A 71.1(6) . . ? C5 Co1 C3A 51.3(5) . . ? C5 Co1 C4A 14.4(6) . . ? C5 Co1 C5A 27.0(6) . . ? C1A Co1 P1 152.0(3) . . ? C1A Co1 P2 90.0(3) . . ? C1A Co1 C2A 41.8(3) . . ? C1A Co1 C3A 69.9(5) . . ? C1A Co1 C4A 70.3(5) . . ? C1A Co1 C5A 42.5(4) . . ? C2A Co1 P1 147.2(4) . . ? C2A Co1 P2 121.9(4) . . ? C2A Co1 C3A 42.1(4) . . ? C2A Co1 C4A 71.7(5) . . ? C2A Co1 C5A 72.1(5) . . ? C3A Co1 P1 106.1(4) . . ? C3A Co1 C5A 70.9(5) . . ? C4A Co1 P1 88.1(4) . . ? C4A Co1 P2 130.2(4) . . ? C4A Co1 C3A 42.4(4) . . ? C4A Co1 C5A 41.4(4) . . ? C5A Co1 P1 109.6(4) . . ? P4 Co2 P5 92.19(7) . . ? P4 Co2 P6 90.07(7) . . ? P5 Co2 P6 91.09(7) . . ? C6 Co2 P4 150.1(2) . . ? C6 Co2 P5 117.6(2) . . ? C6 Co2 P6 92.6(2) . . ? C6 Co2 C7 38.9(3) . . ? C6 Co2 C8 66.0(3) . . ? C7 Co2 P4 111.2(2) . . ? C7 Co2 P5 155.1(2) . . ? C7 Co2 P6 97.16(19) . . ? C7 Co2 C8 39.4(3) . . ? C8 Co2 P4 90.5(2) . . ? C8 Co2 P5 136.8(2) . . ? C8 Co2 P6 132.1(2) . . ? C9 Co2 P4 108.5(3) . . ? C9 Co2 P5 100.0(3) . . ? C9 Co2 P6 157.8(2) . . ? C9 Co2 C6 65.2(3) . . ? C9 Co2 C7 65.2(3) . . ? C9 Co2 C8 39.2(3) . . ? C9 Co2 C10 39.7(3) . . ? C10 Co2 P4 147.7(3) . . ? C10 Co2 P5 89.7(2) . . ? C10 Co2 P6 122.2(3) . . ? C10 Co2 C6 39.1(3) . . ? C10 Co2 C7 66.0(3) . . ? C10 Co2 C8 67.0(3) . . ? O1 P1 Co1 106.6(2) . . ? O2 P1 Co1 113.1(2) . . ? O2 P1 O1 98.0(3) . . ? O7 P1 Co1 118.5(2) . . ? O7 P1 O1 110.5(3) . . ? O7 P1 O2 108.1(3) . . ? O3 P2 Co1 106.6(2) . . ? O4 P2 Co1 113.9(2) . . ? O4 P2 O3 99.8(3) . . ? O8 P2 Co1 119.32(18) . . ? O8 P2 O3 109.7(3) . . ? O8 P2 O4 105.7(3) . . ? O5 P3 Co1 106.0(2) . . ? O6 P3 Co1 112.1(2) . . ? O6 P3 O5 100.7(3) . . ? O9 P3 Co1 119.2(2) . . ? O9 P3 O5 110.3(3) . . ? O9 P3 O6 106.9(3) . . ? O11 P4 Co2 112.5(2) . . ? O11 P4 O12 100.1(2) . . ? O12 P4 Co2 107.67(18) . . ? O17 P4 Co2 119.82(18) . . ? O17 P4 O11 105.5(2) . . ? O17 P4 O12 109.5(2) . . ? O13 P5 Co2 113.31(18) . . ? O13 P5 O14 99.8(3) . . ? O14 P5 Co2 106.01(19) . . ? O18 P5 Co2 118.00(19) . . ? O18 P5 O13 107.1(2) . . ? O18 P5 O14 111.1(2) . . ? O15 P6 Co2 113.3(2) . . ? O16 P6 Co2 106.70(19) . . ? O16 P6 O15 98.8(3) . . ? O19 P6 Co2 119.00(17) . . ? O19 P6 O15 107.0(2) . . ? O19 P6 O16 110.1(3) . . ? C11 O1 P1 118.2(5) . . ? C13 O2 P1 126.9(14) . . ? C13 O2 C13A 13(2) . . ? C13A O2 P1 119.6(12) . . ? C15 O3 P2 119.8(5) . . ? C17 O4 P2 122.5(5) . . ? C19 O5 P3 121.2(5) . . ? C21 O6 P3 122.9(6) . . ? P1 O7 Ru1 127.1(3) . . ? P2 O8 Ru1 126.6(3) . . ? P3 O9 Ru1 126.8(2) . . ? N20 N10 Ru1 170.7(5) . . ? N10 N20 Ru2 169.6(5) . . ? C31 O11 P4 123.0(4) . . ? C33 O12 P4 119.2(4) . . ? C35 O13 P5 122.1(4) . . ? C37 O14 P5 120.1(4) . . ? C39 O15 P6 126.6(4) . . ? C41 O16 P6 123.3(6) . . ? C41 O16 C41A 24.2(10) . . ? C41A O16 P6 113.5(8) . . ? P4 O17 Ru2 125.8(3) . . ? P5 O18 Ru2 125.8(2) . . ? P6 O19 Ru2 125.4(2) . . ? C51 N1 Ru1 125.9(5) . . ? C51 N1 C55 118.7(6) . . ? C55 N1 Ru1 115.1(5) . . ? C56 N2 Ru1 113.9(5) . . ? C60 N2 Ru1 125.9(5) . . ? C60 N2 C56 120.0(6) . . ? C61 N3 Ru2 124.9(5) . . ? C61 N3 C65 119.0(6) . . ? C65 N3 Ru2 115.6(4) . . ? C66 N4 Ru2 115.8(4) . . ? C70 N4 Ru2 127.0(5) . . ? C70 N4 C66 117.1(6) . . ? F1 B1 F1 109.7(10) 2_655 . ? F2 B1 F1 107.8(3) 2_655 . ? F2 B1 F1 109.7(3) . . ? F2 B1 F1 109.7(3) 2_655 2_655 ? F2 B1 F1 107.8(3) . 2_655 ? F2 B1 F2 112.2(10) . 2_655 ? F3 B2 F3 106.5(9) . 2_656 ? F4 B2 F3 108.1(5) 2_656 2_656 ? F4 B2 F3 111.0(5) . 2_656 ? F4 B2 F3 111.0(5) 2_656 . ? F4 B2 F3 108.1(5) . . ? F4 B2 F4 112.0(12) . 2_656 ? F5 B3 F7 102.8(11) . . ? F5 B3 F5A 30.0(9) . . ? F5 B3 F6A 98.7(12) . . ? F6 B3 F5 112.4(10) . . ? F6 B3 F7 104.2(11) . . ? F6 B3 F5A 137.9(13) . . ? F6 B3 F6A 78.7(11) . . ? F6 B3 F7A 61.0(16) . . ? F8 B3 F5 117.0(14) . . ? F8 B3 F6 115.5(13) . . ? F8 B3 F7 102.5(12) . . ? F8 B3 F5A 87.9(14) . . ? F8 B3 F6A 55.7(11) . . ? F8 B3 F7A 174.4(19) . . ? F5A B3 F7 104.0(12) . . ? F5A B3 F6A 88.5(13) . . ? F6A B3 F7 155.0(13) . . ? F7A B3 F5 68.5(14) . . ? F7A B3 F7 74.9(16) . . ? F7A B3 F5A 97.5(15) . . ? F7A B3 F6A 125.5(18) . . ? F8A B3 F5 133.6(14) . . ? F8A B3 F6 109.1(13) . . ? F8A B3 F7 46.4(9) . . ? F8A B3 F8 58.4(10) . . ? F8A B3 F5A 113.0(14) . . ? F8A B3 F6A 108.9(14) . . ? F8A B3 F7A 117.7(18) . . ? Co1 C1 C3 59.9(6) . . ? Co1 C1 C4 61.0(5) . . ? C2 C1 Co1 70.5(11) . . ? C2 C1 C3 36.3(6) . . ? C2 C1 C4 72.4(6) . . ? C2 C1 C5 109.2(10) . . ? C4 C1 C3 36.1(4) . . ? C5 C1 Co1 71.4(11) . . ? C5 C1 C3 73.0(6) . . ? C5 C1 C4 36.9(6) . . ? Co1 C2 C4 61.4(6) . . ? Co1 C2 C5 60.0(8) . . ? C1 C2 Co1 73.5(11) . . ? C1 C2 C3 108.2(10) . . ? C1 C2 C4 72.0(7) . . ? C1 C2 C5 35.8(6) . . ? C3 C2 Co1 73.1(11) . . ? C3 C2 C4 36.2(6) . . ? C3 C2 C5 72.5(7) . . ? C4 C2 C5 36.3(4) . . ? Co1 C3 C1 59.9(6) . . ? C2 C3 Co1 70.2(11) . . ? C2 C3 C1 35.5(6) . . ? C4 C3 Co1 73.4(9) . . ? C4 C3 C1 71.9(6) . . ? C4 C3 C2 107.4(9) . . ? C1 C4 Co1 59.4(6) . . ? C1 C4 C2 35.6(4) . . ? C2 C4 Co1 58.3(7) . . ? C3 C4 Co1 70.7(9) . . ? C3 C4 C1 72.0(6) . . ? C3 C4 C2 36.4(5) . . ? C3 C4 C5 108.6(9) . . ? C5 C4 Co1 70.1(11) . . ? C5 C4 C1 36.8(6) . . ? C5 C4 C2 72.2(8) . . ? Co1 C5 C2 58.8(8) . . ? C1 C5 Co1 72.1(11) . . ? C1 C5 C2 35.0(6) . . ? C1 C5 C4 106.3(10) . . ? C4 C5 Co1 73.6(10) . . ? C4 C5 C2 71.5(7) . . ? C2A C1A Co1 69.4(6) . . ? C2A C1A C5A 110.9(7) . . ? C5A C1A Co1 70.5(6) . . ? C1A C2A Co1 68.7(6) . . ? C1A C2A C3A 106.7(7) . . ? C3A C2A Co1 70.3(6) . . ? C2A C3A Co1 67.6(6) . . ? C2A C3A C4A 107.5(7) . . ? C4A C3A Co1 67.9(7) . . ? C3A C4A Co1 69.7(7) . . ? C5A C4A Co1 70.3(7) . . ? C5A C4A C3A 109.4(7) . . ? C1A C5A Co1 67.0(6) . . ? C4A C5A Co1 68.3(7) . . ? C4A C5A C1A 105.4(7) . . ? C7 C6 Co2 70.8(4) . . ? C7 C6 C10 109.2(7) . . ? C10 C6 Co2 69.9(4) . . ? C6 C7 Co2 70.3(4) . . ? C6 C7 C8 108.9(7) . . ? C8 C7 Co2 71.0(4) . . ? C7 C8 Co2 69.6(4) . . ? C9 C8 Co2 68.8(4) . . ? C9 C8 C7 105.3(7) . . ? C8 C9 Co2 72.0(4) . . ? C8 C9 C10 110.4(7) . . ? C10 C9 Co2 70.3(4) . . ? C6 C10 Co2 71.0(4) . . ? C6 C10 C9 106.2(8) . . ? C9 C10 Co2 70.1(4) . . ? C12 C11 O1 110.1(8) . . ? O2 C13 C14 103.5(17) . . ? O2 C13A C14A 102(2) . . ? O3 C15 C16 112.3(10) . . ? O3 C15 C16A 108.5(10) . . ? C16 C15 C16A 37.2(9) . . ? O4 C17 C18 132(2) . . ? O4 C17 C18A 105.9(10) . . ? C18 C17 C18A 31.4(19) . . ? O5 C19 C20A 110.7(10) . . ? C20 C19 O5 113.7(9) . . ? C20 C19 C20A 32.0(9) . . ? O6 C21 C22 106.0(16) . . ? O6 C21 C22A 116(2) . . ? C22A C21 C22 106(3) . . ? O11 C31 C32A 107.4(10) . . ? C32 C31 O11 114.7(11) . . ? C32 C31 C32A 32.4(9) . . ? O12 C33 C34 110.2(7) . . ? O13 C35 C36 108.4(6) . . ? C38 C37 O14 112.4(8) . . ? O15 C39 C40 115.3(12) . . ? O15 C39 C40A 105.5(8) . . ? C40 C39 C40A 27.6(11) . . ? O16 C41 C42 108.5(10) . . ? O16 C41A C42A 99.8(17) . . ? N1 C51 C52 122.8(7) . . ? C51 C52 C53 119.1(7) . . ? C52 C53 C54 117.8(7) . . ? C55 C54 C53 120.8(7) . . ? N1 C55 C56 113.6(7) . . ? C54 C55 N1 120.7(7) . . ? C54 C55 C56 125.7(7) . . ? N2 C56 C55 115.0(6) . . ? N2 C56 C57 120.6(7) . . ? C57 C56 C55 124.4(7) . . ? C58 C57 C56 118.4(8) . . ? C59 C58 C57 121.8(8) . . ? C58 C59 C60 117.8(8) . . ? N2 C60 C59 121.4(8) . . ? N3 C61 C62 120.6(7) . . ? C63 C62 C61 120.8(7) . . ? C62 C63 C64 117.3(7) . . ? C65 C64 C63 121.8(8) . . ? N3 C65 C66 114.6(6) . . ? C64 C65 N3 120.4(6) . . ? C64 C65 C66 125.0(7) . . ? N4 C66 C65 113.1(6) . . ? C67 C66 N4 122.0(6) . . ? C67 C66 C65 124.8(7) . . ? C66 C67 C68 118.4(7) . . ? C67 C68 C69 120.6(8) . . ? C70 C69 C68 117.6(7) . . ? N4 C70 C69 124.2(7) . . ? O3S C2S C1S 107.6(19) . . ? C2S O3S C4S 108.4(18) . . ? O3S C4S C5S 95.5(19) . . ? ### end data_ip16_Compound13 _database_code_depnum_ccdc_archive 'CCDC 838446' #TrackingRef '- cif-re3.cif' _audit_creation_date 2011-05-20 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H46 Co2 N6 O18 P6 Ru2, 2(B F4), 0.5(C4 H10 O)' _chemical_formula_sum 'C56 H91 B2 Co2 F8 N6 O18.50 P6 Ru2' _chemical_formula_weight 1823.79 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 C2 _space_group_IT_number 5 _space_group_name_Hall 'C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' _cell_length_a 21.501(3) _cell_length_b 14.5812(19) _cell_length_c 26.604(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.057(2) _cell_angle_gamma 90.00 _cell_volume 8124.9(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5309 _cell_measurement_temperature 175.0 _cell_measurement_theta_max 23.68 _cell_measurement_theta_min 2.21 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.846418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0396 before and 0.0282 after correction. The Ratio of minimum to maximum transmission is 0.846418. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3724 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_unetI/netI 0.0912 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 29502 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.78 _diffrn_ambient_temperature 175.0 _diffrn_detector_area_resol_mean 8 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_current 40.0 _diffrn_source_power 2.0 _diffrn_source_target MO _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 11008 _reflns_number_total 15493 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v7.34A (Bruker, 2001)' _computing_data_collection ? _computing_data_reduction 'SAINT v7.34A (Bruker, 2001)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(18) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 880 _refine_ls_number_reflns 15493 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0549 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1054 _refine_ls_wR_factor_ref 0.1144 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.28316(3) 0.22066(3) 0.33854(2) 0.03973(15) Uani 1 1 d . B . Ru2 Ru 0.23922(3) 0.07084(3) 0.170060(19) 0.03716(14) Uani 1 1 d . B . Co1 Co 0.20530(5) 0.44343(7) 0.37871(4) 0.0514(3) Uani 1 1 d . . . Co2 Co 0.32730(4) -0.15387(6) 0.14692(3) 0.0394(2) Uani 1 1 d . . . P1 P 0.15680(10) 0.34719(15) 0.32121(7) 0.0543(5) Uani 1 1 d . B . P2 P 0.24420(10) 0.33254(14) 0.43003(7) 0.0511(5) Uani 1 1 d . B . P3 P 0.28789(11) 0.44270(13) 0.34501(7) 0.0503(5) Uani 1 1 d . B . P4 P 0.25229(9) -0.08899(12) 0.09068(6) 0.0380(4) Uani 1 1 d . . . P5 P 0.37408(9) -0.02419(12) 0.16961(7) 0.0408(4) Uani 1 1 d . . . P6 P 0.27104(9) -0.13993(11) 0.20454(7) 0.0430(4) Uani 1 1 d . C . O1 O 0.1468(3) 0.3978(4) 0.26651(18) 0.0693(16) Uani 1 1 d . . . O2 O 0.0840(3) 0.3338(5) 0.3216(2) 0.0838(18) Uani 1 1 d . . . O3 O 0.1847(3) 0.2816(4) 0.4448(2) 0.0747(17) Uani 1 1 d . . . O4 O 0.2811(3) 0.3651(4) 0.48530(17) 0.0739(17) Uani 1 1 d . . . O5 O 0.3460(3) 0.4766(4) 0.3890(2) 0.0675(15) Uani 1 1 d . . . O6 O 0.2847(3) 0.5211(4) 0.3041(2) 0.0805(19) Uani 1 1 d . . . O7 O 0.1861(2) 0.2540(3) 0.31886(17) 0.0492(12) Uani 1 1 d . . . O8 O 0.2869(2) 0.2628(3) 0.41277(16) 0.0438(11) Uani 1 1 d . . . O9 O 0.3057(2) 0.3559(3) 0.32082(16) 0.0474(12) Uani 1 1 d . . . N10 N 0.2752(3) 0.1776(3) 0.2704(2) 0.0392(13) Uani 1 1 d . . . N20 N 0.2638(3) 0.1443(4) 0.2308(2) 0.0414(14) Uani 1 1 d . B . O11 O 0.2035(2) -0.1617(4) 0.05799(18) 0.0556(13) Uani 1 1 d . . . O12 O 0.2836(2) -0.0481(3) 0.04598(16) 0.0454(12) Uani 1 1 d . . . O13 O 0.4323(2) -0.0054(3) 0.14418(18) 0.0535(13) Uani 1 1 d . . . O14 O 0.4108(2) -0.0358(3) 0.22779(18) 0.0583(13) Uani 1 1 d . . . O15 O 0.3004(3) -0.1926(3) 0.25644(19) 0.0699(17) Uani 1 1 d . . . O16 O 0.2094(2) -0.1997(3) 0.1856(2) 0.0609(15) Uani 1 1 d . . . O17 O 0.2113(2) -0.0163(3) 0.10770(16) 0.0398(11) Uani 1 1 d . . . O18 O 0.3337(2) 0.0615(3) 0.16247(16) 0.0435(11) Uani 1 1 d . . . O19 O 0.2533(2) -0.0450(3) 0.21930(16) 0.0428(12) Uani 1 1 d . . . N1 N 0.3740(3) 0.1814(4) 0.3655(2) 0.0443(14) Uani 1 1 d . . . N2 N 0.2693(3) 0.0931(4) 0.3640(2) 0.0440(15) Uani 1 1 d . . . N3 N 0.2180(3) 0.1739(4) 0.1191(2) 0.0423(14) Uani 1 1 d . . . N4 N 0.1463(3) 0.0872(3) 0.1689(2) 0.0417(14) Uani 1 1 d . . . B1 B 0.5000 0.8917(9) 0.0000 0.064(4) Uani 1 2 d SD . . F1 F 0.4886(2) 0.8376(4) 0.0389(2) 0.1033(18) Uani 1 1 d D . . F2 F 0.5526(2) 0.9445(4) 0.01759(19) 0.0867(15) Uani 1 1 d D . . B2 B 0.5000 0.8550(7) 0.5000 0.056(4) Uani 1 2 d SD . . F3 F 0.5449(3) 0.9103(4) 0.4873(3) 0.129(2) Uani 1 1 d D . . F4 F 0.4751(5) 0.8036(8) 0.4593(3) 0.247(5) Uani 1 1 d D . . B3 B 0.0452(6) 0.8920(9) 0.3094(5) 0.054(4) Uiso 0.50 1 d PD . . F5 F 0.0904(4) 0.9364(7) 0.2923(4) 0.092(3) Uiso 0.65 1 d PD A 1 F6 F 0.0511(4) 0.8966(5) 0.3595(3) 0.081(2) Uiso 0.65 1 d PD A 1 F7 F -0.0122(5) 0.9349(10) 0.2887(4) 0.153(4) Uiso 0.65 1 d PD A 1 F8 F 0.0391(10) 0.8061(9) 0.2936(7) 0.221(7) Uiso 0.65 1 d PD A 1 F5A F 0.0822(8) 0.8968(13) 0.2737(7) 0.114(7) Uiso 0.35 1 d PD A 2 F6A F 0.0829(11) 0.8196(15) 0.3331(9) 0.189(10) Uiso 0.35 1 d PD A 2 F7A F 0.0495(15) 0.9793(13) 0.3245(12) 0.239(14) Uiso 0.35 1 d PD A 2 F8A F -0.0107(7) 0.8602(15) 0.2888(7) 0.125(6) Uiso 0.35 1 d PD A 2 C1 C 0.1636(10) 0.5052(13) 0.4314(6) 0.061(5) Uiso 0.52 1 d PD B 1 H1 H 0.1569 0.4760 0.4637 0.073 Uiso 0.52 1 calc PR B 1 C2 C 0.2138(8) 0.5506(15) 0.4273(8) 0.091(7) Uiso 0.52 1 d PD B 1 H2 H 0.2514 0.5650 0.4559 0.109 Uiso 0.52 1 calc PR B 1 C3 C 0.2032(9) 0.5816(11) 0.3808(7) 0.061(4) Uiso 0.52 1 d PD B 1 H3 H 0.2320 0.6235 0.3668 0.073 Uiso 0.52 1 calc PR B 1 C4 C 0.1475(8) 0.5551(11) 0.3564(5) 0.045(4) Uiso 0.52 1 d PD B 1 H4 H 0.1264 0.5716 0.3201 0.054 Uiso 0.52 1 calc PR B 1 C5 C 0.1228(9) 0.5037(14) 0.3869(8) 0.079(6) Uiso 0.52 1 d PD B 1 H5 H 0.0792 0.4757 0.3792 0.095 Uiso 0.52 1 calc PR B 1 C1A C 0.2081(6) 0.5293(8) 0.4429(4) 0.025(3) Uiso 0.48 1 d PD B 2 H1A H 0.2365 0.5194 0.4778 0.029 Uiso 0.48 1 calc PR B 2 C2A C 0.2268(6) 0.5817(9) 0.4002(5) 0.035(3) Uiso 0.48 1 d PD B 2 H2A H 0.2682 0.6140 0.4018 0.041 Uiso 0.48 1 calc PR B 2 C3A C 0.1698(8) 0.5783(11) 0.3543(6) 0.049(4) Uiso 0.48 1 d PD B 2 H3A H 0.1677 0.6062 0.3196 0.059 Uiso 0.48 1 calc PR B 2 C4A C 0.1187(8) 0.5183(14) 0.3692(6) 0.067(6) Uiso 0.48 1 d PD B 2 H4A H 0.0773 0.5007 0.3456 0.080 Uiso 0.48 1 calc PR B 2 C5A C 0.1408(7) 0.4878(11) 0.4247(6) 0.043(4) Uiso 0.48 1 d PD B 2 H5A H 0.1171 0.4488 0.4450 0.051 Uiso 0.48 1 calc PR B 2 C6 C 0.3721(4) -0.2718(5) 0.1810(3) 0.060(2) Uani 1 1 d . . . H6 H 0.3766 -0.2900 0.2179 0.072 Uiso 1 1 calc R . . C7 C 0.3215(4) -0.2965(5) 0.1401(3) 0.054(2) Uani 1 1 d . . . H7 H 0.2840 -0.3351 0.1427 0.065 Uiso 1 1 calc R . . C8 C 0.3337(4) -0.2589(5) 0.0943(3) 0.052(2) Uani 1 1 d . . . H8 H 0.3069 -0.2661 0.0585 0.063 Uiso 1 1 calc R . . C9 C 0.3907(4) -0.2118(6) 0.1086(4) 0.064(2) Uani 1 1 d . . . H9 H 0.4121 -0.1784 0.0843 0.077 Uiso 1 1 calc R . . C10 C 0.4147(4) -0.2185(6) 0.1621(4) 0.072(3) Uani 1 1 d . . . H10 H 0.4560 -0.1930 0.1823 0.086 Uiso 1 1 calc R . . C11 C 0.1209(6) 0.3455(8) 0.2200(3) 0.102(3) Uani 1 1 d . B . H11A H 0.1537 0.3025 0.2132 0.123 Uiso 1 1 calc R . . H11B H 0.0838 0.3091 0.2248 0.123 Uiso 1 1 calc R . . C12 C 0.1014(6) 0.4058(7) 0.1769(3) 0.102(4) Uani 1 1 d . . . H12A H 0.0840 0.3697 0.1458 0.154 Uiso 1 1 calc R B . H12B H 0.1383 0.4412 0.1718 0.154 Uiso 1 1 calc R . . H12C H 0.0685 0.4478 0.1834 0.154 Uiso 1 1 calc R . . C13 C 0.0580(9) 0.2676(15) 0.3492(7) 0.087(6) Uiso 0.60 1 d PD B 1 C14 C 0.0213(12) 0.2020(16) 0.3082(8) 0.123(8) Uiso 0.60 1 d PD B 1 C13A C 0.0668(13) 0.231(2) 0.3468(11) 0.082(9) Uiso 0.40 1 d P B 2 C14A C -0.0033(15) 0.235(3) 0.3137(15) 0.153(16) Uiso 0.40 1 d PD B 2 C15 C 0.1970(5) 0.2006(7) 0.4785(4) 0.090(3) Uani 1 1 d D B . C16 C 0.1390(9) 0.1810(15) 0.4986(8) 0.092(6) Uiso 0.50 1 d PD . . C16A C 0.1349(9) 0.1471(14) 0.4694(9) 0.097(7) Uiso 0.50 1 d PD B . C17 C 0.3512(6) 0.3713(8) 0.5000(4) 0.099(3) Uani 1 1 d D B . C18 C 0.398(2) 0.295(3) 0.5189(19) 0.148(19) Uiso 0.35 1 d PD . . C18A C 0.3725(11) 0.2792(12) 0.5291(8) 0.112(7) Uiso 0.65 1 d PD B . C19 C 0.4105(5) 0.4891(8) 0.3782(4) 0.096(3) Uani 1 1 d D . . C20 C 0.4499(9) 0.5484(13) 0.4164(7) 0.072(5) Uiso 0.50 1 d PD . . C20A C 0.4587(9) 0.5019(16) 0.4304(7) 0.091(7) Uiso 0.50 1 d PD . . C21 C 0.2756(8) 0.5016(9) 0.2485(4) 0.131(5) Uani 1 1 d D . . C22 C 0.3416(12) 0.503(2) 0.2386(13) 0.197(12) Uiso 0.60 1 d PD . . C22A C 0.2333(19) 0.568(3) 0.2150(16) 0.197(17) Uiso 0.40 1 d PD . . C31 C 0.1382(5) -0.1702(8) 0.0634(4) 0.110(4) Uani 1 1 d D . . C32 C 0.1092(10) -0.2597(12) 0.0483(9) 0.093(7) Uiso 0.50 1 d PD . . C32A C 0.1054(9) -0.2346(12) 0.0211(7) 0.073(5) Uiso 0.50 1 d PD . . C33 C 0.2458(4) 0.0067(6) 0.0062(3) 0.064(2) Uani 1 1 d . . . H33A H 0.2250 0.0563 0.0219 0.076 Uiso 1 1 calc R . . H33B H 0.2118 -0.0317 -0.0151 0.076 Uiso 1 1 calc R . . C34 C 0.2844(6) 0.0464(6) -0.0264(4) 0.099(4) Uani 1 1 d . . . H34A H 0.2574 0.0836 -0.0534 0.148 Uiso 1 1 calc R . . H34B H 0.3045 -0.0027 -0.0423 0.148 Uiso 1 1 calc R . . H34C H 0.3176 0.0853 -0.0054 0.148 Uiso 1 1 calc R . . C35 C 0.4242(4) 0.0384(5) 0.0941(3) 0.060(2) Uani 1 1 d . . . H35A H 0.3885 0.0829 0.0889 0.072 Uiso 1 1 calc R . . H35B H 0.4142 -0.0082 0.0663 0.072 Uiso 1 1 calc R . . C36 C 0.4858(4) 0.0872(6) 0.0924(3) 0.082(3) Uani 1 1 d . . . H36A H 0.4816 0.1167 0.0587 0.123 Uiso 1 1 calc R . . H36B H 0.5209 0.0427 0.0978 0.123 Uiso 1 1 calc R . . H36C H 0.4949 0.1339 0.1196 0.123 Uiso 1 1 calc R . . C37 C 0.4330(4) 0.0469(6) 0.2599(3) 0.072(2) Uani 1 1 d . . . H37A H 0.4033 0.0982 0.2477 0.087 Uiso 1 1 calc R . . H37B H 0.4314 0.0337 0.2961 0.087 Uiso 1 1 calc R . . C38 C 0.4946(6) 0.0741(9) 0.2585(4) 0.125(4) Uani 1 1 d . . . H38A H 0.5064 0.1282 0.2805 0.188 Uiso 1 1 calc R . . H38B H 0.4964 0.0891 0.2230 0.188 Uiso 1 1 calc R . . H38C H 0.5245 0.0241 0.2712 0.188 Uiso 1 1 calc R . . C39 C 0.3341(5) -0.1513(6) 0.3039(3) 0.090(3) Uani 1 1 d D . . C40 C 0.3648(13) -0.2208(15) 0.3453(8) 0.093(8) Uiso 0.45 1 d PD . . C40A C 0.3333(10) -0.2282(11) 0.3438(7) 0.076(6) Uiso 0.55 1 d PD . . C41 C 0.1568(7) -0.2024(7) 0.2129(5) 0.045(3) Uiso 0.60 1 d PD C 1 C42 C 0.1344(9) -0.3011(10) 0.2131(7) 0.093(6) Uiso 0.60 1 d PD C 1 C41A C 0.1803(11) -0.2237(15) 0.2322(10) 0.075(7) Uiso 0.40 1 d PD C 2 C42A C 0.1085(14) -0.264(2) 0.1957(11) 0.091(8) Uiso 0.40 1 d P C 2 C51 C 0.4262(4) 0.2276(5) 0.3600(3) 0.0527(18) Uani 1 1 d . B . H51 H 0.4209 0.2800 0.3382 0.063 Uiso 1 1 calc R . . C52 C 0.4867(4) 0.2021(6) 0.3847(3) 0.067(2) Uani 1 1 d . . . H52 H 0.5228 0.2349 0.3793 0.080 Uiso 1 1 calc R B . C53 C 0.4938(4) 0.1285(6) 0.4171(4) 0.072(2) Uani 1 1 d . B . H53 H 0.5350 0.1110 0.4360 0.086 Uiso 1 1 calc R . . C54 C 0.4399(4) 0.0790(6) 0.4224(3) 0.064(2) Uani 1 1 d . . . H54 H 0.4447 0.0270 0.4444 0.077 Uiso 1 1 calc R B . C55 C 0.3814(4) 0.1048(5) 0.3962(3) 0.0492(19) Uani 1 1 d . B . C56 C 0.3220(4) 0.0555(5) 0.3949(2) 0.0452(18) Uani 1 1 d . B . C57 C 0.3184(5) -0.0255(5) 0.4207(3) 0.061(2) Uani 1 1 d . . . H57 H 0.3553 -0.0510 0.4427 0.073 Uiso 1 1 calc R B . C58 C 0.2611(5) -0.0680(6) 0.4141(3) 0.067(2) Uani 1 1 d . B . H58 H 0.2579 -0.1230 0.4326 0.080 Uiso 1 1 calc R . . C59 C 0.2082(5) -0.0341(6) 0.3818(3) 0.072(3) Uani 1 1 d . . . H59 H 0.1687 -0.0660 0.3763 0.086 Uiso 1 1 calc R B . C60 C 0.2134(4) 0.0500(5) 0.3565(3) 0.054(2) Uani 1 1 d . B . H60 H 0.1768 0.0759 0.3342 0.065 Uiso 1 1 calc R . . C61 C 0.2599(4) 0.2153(5) 0.0962(3) 0.057(2) Uani 1 1 d . C . H61 H 0.3042 0.2027 0.1077 0.068 Uiso 1 1 calc R . . C62 C 0.2392(5) 0.2765(5) 0.0558(3) 0.071(3) Uani 1 1 d . . . H62 H 0.2692 0.3031 0.0388 0.085 Uiso 1 1 calc R C . C63 C 0.1755(5) 0.2988(5) 0.0403(3) 0.065(2) Uani 1 1 d . C . H63 H 0.1609 0.3426 0.0138 0.078 Uiso 1 1 calc R . . C64 C 0.1341(4) 0.2552(5) 0.0646(3) 0.061(2) Uani 1 1 d . . . H64 H 0.0897 0.2678 0.0541 0.074 Uiso 1 1 calc R C . C65 C 0.1551(4) 0.1944(4) 0.1033(3) 0.0427(17) Uani 1 1 d . C . C66 C 0.1132(4) 0.1458(5) 0.1315(3) 0.0433(17) Uani 1 1 d . C . C67 C 0.0490(4) 0.1591(6) 0.1247(3) 0.062(2) Uani 1 1 d . . . H67 H 0.0272 0.2009 0.0993 0.074 Uiso 1 1 calc R C . C68 C 0.0167(4) 0.1120(6) 0.1546(4) 0.071(2) Uani 1 1 d . C . H68 H -0.0282 0.1191 0.1492 0.086 Uiso 1 1 calc R . . C69 C 0.0491(4) 0.0528(5) 0.1935(3) 0.067(2) Uani 1 1 d . . . H69 H 0.0271 0.0199 0.2150 0.081 Uiso 1 1 calc R C . C70 C 0.1138(4) 0.0447(5) 0.1991(3) 0.056(2) Uani 1 1 d . C . H70 H 0.1367 0.0066 0.2259 0.068 Uiso 1 1 calc R . . C1S C 0.9498(13) 1.0532(19) 0.0076(10) 0.157(11) Uiso 0.50 1 d PD . . H1SA H 0.9767 1.0764 -0.0148 0.236 Uiso 0.50 1 calc PR . . H1SB H 0.9418 1.1026 0.0304 0.236 Uiso 0.50 1 calc PR . . H1SC H 0.9091 1.0316 -0.0136 0.236 Uiso 0.50 1 calc PR . . C2S C 0.9831(11) 0.9755(15) 0.0396(9) 0.112(7) Uiso 0.50 1 d PD . . H2SA H 0.9897 0.9235 0.0175 0.134 Uiso 0.50 1 calc PR . . H2SB H 1.0250 0.9953 0.0606 0.134 Uiso 0.50 1 calc PR . . O3S O 0.9415(10) 0.9513(14) 0.0709(8) 0.159(7) Uiso 0.50 1 d PD . . C4S C 0.9669(12) 0.8711(18) 0.1010(11) 0.147(10) Uiso 0.50 1 d PD . . H4SA H 1.0065 0.8845 0.1272 0.177 Uiso 0.50 1 calc PR . . H4SB H 0.9738 0.8188 0.0792 0.177 Uiso 0.50 1 calc PR . . C5S C 0.9116(11) 0.8580(18) 0.1238(9) 0.126(8) Uiso 0.50 1 d PD . . H5SA H 0.9187 0.8044 0.1466 0.189 Uiso 0.50 1 calc PR . . H5SB H 0.8733 0.8483 0.0963 0.189 Uiso 0.50 1 calc PR . . H5SC H 0.9058 0.9126 0.1437 0.189 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0504(4) 0.0388(3) 0.0326(3) -0.0049(3) 0.0148(3) 0.0011(3) Ru2 0.0502(4) 0.0335(3) 0.0323(3) -0.0026(2) 0.0187(3) 0.0026(3) Co1 0.0635(7) 0.0513(6) 0.0402(5) -0.0067(5) 0.0135(5) 0.0154(5) Co2 0.0413(5) 0.0371(5) 0.0412(5) -0.0044(4) 0.0121(4) 0.0036(4) P1 0.0548(13) 0.0623(13) 0.0445(10) -0.0060(10) 0.0087(10) 0.0118(11) P2 0.0648(14) 0.0569(11) 0.0345(9) -0.0026(10) 0.0175(9) 0.0131(11) P3 0.0690(15) 0.0406(10) 0.0439(11) -0.0029(9) 0.0184(11) 0.0034(10) P4 0.0381(11) 0.0408(10) 0.0364(9) -0.0098(8) 0.0111(8) 0.0014(8) P5 0.0407(11) 0.0461(10) 0.0366(9) -0.0037(8) 0.0109(9) -0.0042(8) P6 0.0528(12) 0.0372(10) 0.0423(10) -0.0011(8) 0.0176(9) -0.0004(9) O1 0.092(5) 0.064(3) 0.043(3) 0.000(3) -0.004(3) 0.008(3) O2 0.053(4) 0.100(4) 0.097(4) -0.015(4) 0.012(3) 0.019(4) O3 0.074(4) 0.084(4) 0.078(4) 0.026(3) 0.040(3) 0.020(3) O4 0.100(5) 0.085(4) 0.030(3) -0.017(3) 0.000(3) 0.028(4) O5 0.069(4) 0.073(4) 0.062(3) -0.025(3) 0.019(3) -0.006(3) O6 0.129(6) 0.043(3) 0.077(4) 0.009(3) 0.040(4) 0.009(3) O7 0.051(3) 0.052(3) 0.045(3) -0.009(2) 0.012(2) -0.003(2) O8 0.054(3) 0.047(3) 0.033(2) -0.007(2) 0.013(2) 0.008(2) O9 0.061(3) 0.044(3) 0.040(2) -0.003(2) 0.017(2) 0.005(2) N10 0.051(4) 0.038(3) 0.033(3) -0.004(3) 0.019(3) 0.000(3) N20 0.046(4) 0.039(3) 0.041(3) 0.005(3) 0.015(3) 0.002(3) O11 0.046(3) 0.061(3) 0.057(3) -0.029(3) 0.008(2) 0.002(3) O12 0.046(3) 0.055(3) 0.037(2) 0.006(2) 0.012(2) 0.010(2) O13 0.046(3) 0.058(3) 0.056(3) 0.002(3) 0.009(3) -0.004(3) O14 0.054(3) 0.069(3) 0.045(3) -0.001(3) -0.003(3) -0.011(3) O15 0.118(5) 0.048(3) 0.049(3) 0.004(2) 0.030(3) 0.022(3) O16 0.062(4) 0.054(3) 0.078(4) -0.016(3) 0.041(3) -0.018(3) O17 0.044(3) 0.044(2) 0.034(2) -0.006(2) 0.012(2) 0.006(2) O18 0.049(3) 0.036(2) 0.051(3) -0.014(2) 0.022(2) -0.004(2) O19 0.062(3) 0.036(2) 0.036(2) 0.004(2) 0.023(2) 0.006(2) N1 0.058(4) 0.040(3) 0.039(3) 0.000(3) 0.021(3) 0.008(3) N2 0.060(4) 0.041(3) 0.037(3) -0.004(3) 0.022(3) -0.006(3) N3 0.055(4) 0.040(3) 0.036(3) -0.004(3) 0.019(3) 0.006(3) N4 0.051(4) 0.038(3) 0.044(3) -0.002(3) 0.029(3) 0.007(3) B1 0.043(8) 0.109(12) 0.043(7) 0.000 0.013(7) 0.000 F1 0.081(4) 0.131(4) 0.116(4) 0.055(4) 0.060(3) 0.010(3) F2 0.066(3) 0.103(4) 0.088(4) -0.007(3) 0.011(3) -0.023(3) B2 0.020(6) 0.033(6) 0.099(10) 0.000 -0.020(7) 0.000 F3 0.130(5) 0.114(5) 0.171(6) -0.058(5) 0.089(5) -0.032(4) F4 0.175(9) 0.310(13) 0.254(11) -0.131(10) 0.046(8) -0.118(9) C6 0.060(5) 0.046(4) 0.067(5) -0.006(4) 0.000(5) 0.015(4) C7 0.061(5) 0.035(4) 0.071(5) 0.003(4) 0.022(5) 0.010(4) C8 0.066(6) 0.043(4) 0.050(4) -0.011(3) 0.020(4) 0.016(4) C9 0.067(6) 0.060(5) 0.080(6) 0.017(5) 0.048(5) 0.031(5) C10 0.049(6) 0.053(5) 0.106(8) -0.025(5) 0.004(5) 0.022(4) C11 0.140(10) 0.087(7) 0.063(6) -0.026(6) -0.013(6) 0.004(7) C12 0.146(11) 0.097(7) 0.052(5) -0.009(6) -0.004(6) 0.029(7) C15 0.092(7) 0.102(8) 0.084(6) 0.044(6) 0.034(6) 0.010(6) C17 0.100(9) 0.121(9) 0.067(6) -0.027(6) 0.000(6) -0.018(7) C19 0.068(7) 0.123(8) 0.105(8) -0.035(7) 0.034(6) -0.029(6) C21 0.191(15) 0.133(11) 0.076(8) 0.042(8) 0.043(9) 0.028(10) C31 0.075(7) 0.141(10) 0.114(8) -0.059(8) 0.023(6) -0.070(7) C33 0.086(6) 0.065(5) 0.043(4) 0.003(4) 0.021(5) 0.007(5) C34 0.127(9) 0.095(8) 0.084(7) 0.042(6) 0.044(7) 0.028(6) C35 0.068(6) 0.081(6) 0.041(4) 0.004(4) 0.031(4) -0.003(4) C36 0.081(6) 0.082(6) 0.087(6) 0.010(5) 0.027(5) -0.029(5) C37 0.056(6) 0.077(6) 0.078(6) -0.012(5) 0.005(5) -0.013(4) C38 0.115(10) 0.148(11) 0.103(8) -0.039(9) 0.005(7) -0.027(9) C39 0.153(10) 0.064(6) 0.046(5) 0.017(5) 0.007(6) 0.007(6) C51 0.052(5) 0.048(4) 0.062(5) 0.007(4) 0.021(4) 0.004(4) C52 0.053(6) 0.069(6) 0.083(6) 0.000(5) 0.023(5) -0.002(4) C53 0.043(5) 0.087(7) 0.085(6) -0.001(5) 0.011(5) 0.024(5) C54 0.068(6) 0.060(5) 0.066(5) 0.016(4) 0.018(5) 0.023(5) C55 0.063(5) 0.049(4) 0.042(4) -0.006(3) 0.026(4) 0.007(4) C56 0.060(5) 0.052(5) 0.027(3) -0.004(3) 0.017(3) 0.014(4) C57 0.082(7) 0.058(5) 0.044(4) 0.006(4) 0.021(4) 0.008(5) C58 0.091(8) 0.065(5) 0.052(5) 0.016(4) 0.032(5) -0.008(5) C59 0.088(8) 0.071(6) 0.066(6) -0.003(5) 0.037(6) -0.033(5) C60 0.055(5) 0.060(5) 0.052(4) -0.006(4) 0.021(4) -0.012(4) C61 0.076(6) 0.050(4) 0.053(4) 0.004(4) 0.032(4) 0.004(5) C62 0.113(8) 0.052(5) 0.063(5) 0.012(4) 0.051(6) -0.002(5) C63 0.081(7) 0.058(5) 0.061(5) 0.018(4) 0.027(5) 0.010(5) C64 0.074(6) 0.069(5) 0.042(4) 0.004(4) 0.015(4) 0.017(4) C65 0.061(5) 0.032(4) 0.038(4) -0.003(3) 0.017(4) 0.012(3) C66 0.053(5) 0.044(4) 0.037(4) -0.001(3) 0.017(4) 0.008(3) C67 0.047(5) 0.068(5) 0.072(5) 0.013(4) 0.017(4) 0.012(4) C68 0.062(6) 0.067(5) 0.092(7) 0.005(5) 0.033(5) 0.016(5) C69 0.057(5) 0.067(5) 0.093(6) 0.017(5) 0.047(5) 0.001(4) C70 0.074(6) 0.046(4) 0.058(5) 0.009(3) 0.034(5) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O7 2.092(5) . ? Ru1 O8 2.052(4) . ? Ru1 O9 2.109(4) . ? Ru1 N10 1.888(5) . ? Ru1 N1 2.005(6) . ? Ru1 N2 2.025(5) . ? Ru2 N20 1.911(6) . ? Ru2 O17 2.069(4) . ? Ru2 O18 2.091(4) . ? Ru2 O19 2.117(4) . ? Ru2 N3 2.006(6) . ? Ru2 N4 2.006(5) . ? Co1 P1 2.162(2) . ? Co1 P2 2.159(2) . ? Co1 C1 2.036(17) . ? Co1 C2 2.01(2) . ? Co1 C3 2.016(17) . ? Co1 C4 2.053(14) . ? Co1 C5 2.03(2) . ? Co1 C1A 2.106(12) . ? Co1 C2A 2.118(14) . ? Co1 C3A 2.156(16) . ? Co1 C4A 2.12(2) . ? Co1 C5A 2.146(15) . ? Co2 P4 2.155(2) . ? Co2 P5 2.163(2) . ? Co2 P6 2.1662(18) . ? Co2 C6 2.076(8) . ? Co2 C7 2.088(7) . ? Co2 C8 2.101(6) . ? Co2 C9 2.060(7) . ? Co2 C10 2.059(8) . ? P1 O1 1.602(5) . ? P1 O2 1.580(6) . ? P1 O7 1.505(5) . ? P2 O3 1.603(6) . ? P2 O4 1.578(5) . ? P2 O8 1.509(4) . ? P3 O5 1.586(6) . ? P3 O6 1.570(6) . ? P3 O9 1.508(5) . ? P4 O11 1.603(5) . ? P4 O12 1.608(4) . ? P4 O17 1.512(4) . ? P5 O13 1.575(5) . ? P5 O14 1.580(5) . ? P5 O18 1.509(5) . ? P6 O15 1.581(5) . ? P6 O16 1.571(5) . ? P6 O19 1.510(4) . ? O1 C11 1.454(9) . ? O2 C13 1.40(2) . ? O2 C13A 1.72(3) . ? O3 C15 1.469(10) . ? O4 C17 1.472(12) . ? O5 C19 1.489(10) . ? O6 C21 1.474(12) . ? N10 N20 1.136(6) . ? O11 C31 1.449(10) . ? O12 C33 1.425(9) . ? O13 C35 1.453(8) . ? O14 C37 1.493(9) . ? O15 C39 1.438(10) . ? O16 C41 1.477(12) . ? O16 C41A 1.55(2) . ? N1 C51 1.345(8) . ? N1 C55 1.373(8) . ? N2 C56 1.357(9) . ? N2 C60 1.330(9) . ? N3 C61 1.341(8) . ? N3 C65 1.357(9) . ? N4 C66 1.382(8) . ? N4 C70 1.330(8) . ? B1 F1 1.368(8) . ? B1 F1 1.368(8) 2_655 ? B1 F2 1.361(7) 2_655 ? B1 F2 1.361(7) . ? B2 F3 1.358(7) 2_656 ? B2 F3 1.358(7) . ? B2 F4 1.325(8) 2_656 ? B2 F4 1.325(8) . ? B3 F5 1.330(13) . ? B3 F6 1.312(12) . ? B3 F7 1.381(14) . ? B3 F8 1.318(14) . ? B3 F5A 1.373(14) . ? B3 F6A 1.392(15) . ? B3 F7A 1.331(15) . ? B3 F8A 1.289(14) . ? C1 C2 1.290(16) . ? C1 C5 1.303(16) . ? C2 C3 1.289(15) . ? C3 C4 1.286(16) . ? C4 C5 1.302(15) . ? C1A C2A 1.498(14) . ? C1A C5A 1.542(15) . ? C2A C3A 1.522(15) . ? C3A C4A 1.526(16) . ? C4A C5A 1.511(15) . ? C6 C7 1.399(10) . ? C6 C10 1.380(11) . ? C7 C8 1.414(10) . ? C8 C9 1.382(11) . ? C9 C10 1.405(12) . ? C11 C12 1.430(12) . ? C13 C14 1.529(18) . ? C13A C14A 1.56(4) . ? C15 C16 1.493(15) . ? C15 C16A 1.518(16) . ? C16 C16A 0.91(3) . ? C17 C18 1.504(19) . ? C17 C18A 1.566(15) . ? C18 C18A 0.70(5) . ? C19 C20 1.454(15) . ? C19 C20A 1.545(16) . ? C20 C20A 0.78(2) . ? C21 C22 1.502(18) . ? C21 C22A 1.478(19) . ? C31 C32 1.462(15) . ? C31 C32A 1.513(15) . ? C32 C32A 0.80(2) . ? C33 C34 1.451(11) . ? C35 C36 1.514(10) . ? C37 C38 1.393(12) . ? C39 C40 1.532(16) . ? C39 C40A 1.547(14) . ? C40 C40A 0.68(3) . ? C41 C42 1.518(15) . ? C41A C42A 1.73(3) . ? C51 C52 1.369(11) . ? C52 C53 1.365(11) . ? C53 C54 1.398(11) . ? C54 C55 1.347(10) . ? C55 C56 1.459(10) . ? C56 C57 1.377(10) . ? C57 C58 1.355(11) . ? C58 C59 1.354(12) . ? C59 C60 1.416(10) . ? C61 C62 1.390(10) . ? C62 C63 1.377(12) . ? C63 C64 1.369(11) . ? C64 C65 1.356(9) . ? C65 C66 1.477(9) . ? C66 C67 1.365(10) . ? C67 C68 1.356(10) . ? C68 C69 1.406(11) . ? C69 C70 1.370(11) . ? C1S C2S 1.498(18) . ? C2S O3S 1.398(16) . ? O3S C4S 1.452(17) . ? C4S C5S 1.465(17) . ? 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 O7 Ru1 O9 89.65(18) . . ? O8 Ru1 O7 89.49(17) . . ? O8 Ru1 O9 88.53(17) . . ? N10 Ru1 O7 88.2(2) . . ? N10 Ru1 O8 176.4(2) . . ? N10 Ru1 O9 94.15(19) . . ? N10 Ru1 N1 96.7(2) . . ? N10 Ru1 N2 91.5(2) . . ? N1 Ru1 O7 172.7(2) . . ? N1 Ru1 O8 85.34(19) . . ? N1 Ru1 O9 95.3(2) . . ? N1 Ru1 N2 79.8(2) . . ? N2 Ru1 O7 94.7(2) . . ? N2 Ru1 O8 85.97(19) . . ? N2 Ru1 O9 172.9(2) . . ? N20 Ru2 O17 175.85(19) . . ? N20 Ru2 O18 91.7(2) . . ? N20 Ru2 O19 87.2(2) . . ? N20 Ru2 N3 97.4(2) . . ? N20 Ru2 N4 91.7(2) . . ? O17 Ru2 O18 89.73(16) . . ? O17 Ru2 O19 88.90(17) . . ? O18 Ru2 O19 90.07(17) . . ? N3 Ru2 O17 86.45(19) . . ? N3 Ru2 O18 93.5(2) . . ? N3 Ru2 O19 174.1(2) . . ? N4 Ru2 O17 87.31(19) . . ? N4 Ru2 O18 173.0(2) . . ? N4 Ru2 O19 96.17(19) . . ? N4 Ru2 N3 80.0(2) . . ? P2 Co1 P1 91.00(8) . . ? C1 Co1 P1 123.9(6) . . ? C1 Co1 P2 93.7(4) . . ? C1 Co1 C4 61.0(6) . . ? C1 Co1 C1A 27.9(5) . . ? C1 Co1 C2A 59.7(6) . . ? C1 Co1 C3A 67.8(6) . . ? C1 Co1 C4A 49.0(6) . . ? C1 Co1 C5A 14.7(6) . . ? C2 Co1 P1 156.7(5) . . ? C2 Co1 P2 102.1(6) . . ? C2 Co1 C1 37.2(5) . . ? C2 Co1 C3 37.4(5) . . ? C2 Co1 C4 62.0(6) . . ? C2 Co1 C5 63.2(7) . . ? C2 Co1 C1A 15.2(6) . . ? C2 Co1 C2A 26.4(5) . . ? C2 Co1 C3A 57.3(6) . . ? C2 Co1 C4A 68.1(7) . . ? C2 Co1 C5A 51.3(6) . . ? C3 Co1 P1 131.1(6) . . ? C3 Co1 P2 137.6(6) . . ? C3 Co1 C1 61.5(6) . . ? C3 Co1 C4 36.8(4) . . ? C3 Co1 C5 62.6(6) . . ? C3 Co1 C1A 51.7(5) . . ? C3 Co1 C2A 17.5(5) . . ? C3 Co1 C3A 24.2(5) . . ? C3 Co1 C4A 57.7(6) . . ? C3 Co1 C5A 70.2(5) . . ? C4 Co1 P1 98.4(4) . . ? C4 Co1 P2 154.1(4) . . ? C4 Co1 C1A 70.6(5) . . ? C4 Co1 C2A 53.4(5) . . ? C4 Co1 C3A 16.2(4) . . ? C4 Co1 C4A 25.9(5) . . ? C4 Co1 C5A 59.9(5) . . ? C5 Co1 P1 93.7(6) . . ? C5 Co1 P2 118.6(5) . . ? C5 Co1 C1 37.3(5) . . ? C5 Co1 C4 37.2(4) . . ? C5 Co1 C1A 61.5(6) . . ? C5 Co1 C2A 72.7(6) . . ? C5 Co1 C3A 51.8(5) . . ? C5 Co1 C4A 13.8(5) . . ? C5 Co1 C5A 28.0(5) . . ? C1A Co1 P1 151.6(3) . . ? C1A Co1 P2 89.8(3) . . ? C1A Co1 C2A 41.5(4) . . ? C1A Co1 C3A 69.2(5) . . ? C1A Co1 C4A 69.8(6) . . ? C1A Co1 C5A 42.5(4) . . ? C2A Co1 P1 148.1(4) . . ? C2A Co1 P2 120.9(4) . . ? C2A Co1 C3A 41.7(4) . . ? C2A Co1 C4A 71.0(6) . . ? C2A Co1 C5A 71.9(5) . . ? C3A Co1 P1 107.3(5) . . ? C3A Co1 P2 159.0(4) . . ? C4A Co1 P1 88.8(5) . . ? C4A Co1 P2 131.6(5) . . ? C4A Co1 C3A 41.8(4) . . ? C4A Co1 C5A 41.5(4) . . ? C5A Co1 P1 109.2(4) . . ? C5A Co1 P2 94.2(4) . . ? C5A Co1 C3A 70.5(5) . . ? P4 Co2 P5 92.17(8) . . ? P4 Co2 P6 90.01(7) . . ? P5 Co2 P6 91.11(7) . . ? C6 Co2 P4 150.1(2) . . ? C6 Co2 P5 117.5(2) . . ? C6 Co2 P6 92.7(2) . . ? C6 Co2 C7 39.3(3) . . ? C6 Co2 C8 66.0(3) . . ? C7 Co2 P4 110.9(2) . . ? C7 Co2 P5 155.4(2) . . ? C7 Co2 P6 97.1(2) . . ? C7 Co2 C8 39.5(3) . . ? C8 Co2 P4 90.5(2) . . ? C8 Co2 P5 136.6(2) . . ? C8 Co2 P6 132.2(2) . . ? C9 Co2 P4 108.1(3) . . ? C9 Co2 P5 100.3(3) . . ? C9 Co2 P6 158.0(2) . . ? C9 Co2 C6 65.4(3) . . ? C9 Co2 C7 65.3(3) . . ? C9 Co2 C8 38.8(3) . . ? C10 Co2 P4 147.6(3) . . ? C10 Co2 P5 89.9(3) . . ? C10 Co2 P6 122.3(3) . . ? C10 Co2 C6 39.0(3) . . ? C10 Co2 C7 66.1(3) . . ? C10 Co2 C8 66.6(3) . . ? C10 Co2 C9 39.9(3) . . ? O1 P1 Co1 106.7(2) . . ? O2 P1 Co1 113.3(2) . . ? O2 P1 O1 97.7(3) . . ? O7 P1 Co1 118.4(2) . . ? O7 P1 O1 110.5(3) . . ? O7 P1 O2 108.2(3) . . ? O3 P2 Co1 106.6(2) . . ? O4 P2 Co1 113.9(2) . . ? O4 P2 O3 99.9(3) . . ? O8 P2 Co1 119.19(19) . . ? O8 P2 O3 109.6(3) . . ? O8 P2 O4 105.9(3) . . ? O5 P3 Co1 106.1(2) . . ? O6 P3 Co1 111.9(3) . . ? O6 P3 O5 100.9(3) . . ? O9 P3 Co1 119.5(2) . . ? O9 P3 O5 110.0(3) . . ? O9 P3 O6 106.9(3) . . ? O11 P4 Co2 112.4(2) . . ? O11 P4 O12 100.2(3) . . ? O12 P4 Co2 107.65(19) . . ? O17 P4 Co2 119.70(19) . . ? O17 P4 O11 105.7(3) . . ? O17 P4 O12 109.4(2) . . ? O13 P5 Co2 113.37(19) . . ? O13 P5 O14 99.8(3) . . ? O14 P5 Co2 106.1(2) . . ? O18 P5 Co2 118.1(2) . . ? O18 P5 O13 107.0(3) . . ? O18 P5 O14 111.0(3) . . ? O15 P6 Co2 113.3(2) . . ? O16 P6 Co2 106.61(19) . . ? O16 P6 O15 98.8(3) . . ? O19 P6 Co2 118.92(18) . . ? O19 P6 O15 107.0(3) . . ? O19 P6 O16 110.4(3) . . ? C11 O1 P1 118.6(6) . . ? P1 O2 C13A 114.3(10) . . ? C13 O2 P1 127.0(10) . . ? C13 O2 C13A 18.0(13) . . ? C15 O3 P2 118.6(5) . . ? C17 O4 P2 122.3(5) . . ? C19 O5 P3 120.5(5) . . ? C21 O6 P3 122.0(6) . . ? P1 O7 Ru1 127.0(3) . . ? P2 O8 Ru1 126.9(3) . . ? P3 O9 Ru1 126.6(2) . . ? N20 N10 Ru1 170.6(5) . . ? N10 N20 Ru2 169.9(5) . . ? C31 O11 P4 122.2(5) . . ? C33 O12 P4 119.5(4) . . ? C35 O13 P5 121.9(5) . . ? C37 O14 P5 119.9(5) . . ? C39 O15 P6 125.9(5) . . ? C41 O16 P6 122.8(6) . . ? C41 O16 C41A 26.8(9) . . ? C41A O16 P6 109.4(8) . . ? P4 O17 Ru2 126.0(3) . . ? P5 O18 Ru2 125.9(3) . . ? P6 O19 Ru2 125.4(2) . . ? C51 N1 Ru1 126.0(5) . . ? C51 N1 C55 119.0(6) . . ? C55 N1 Ru1 114.7(5) . . ? C56 N2 Ru1 114.0(5) . . ? C60 N2 Ru1 125.5(5) . . ? C60 N2 C56 120.2(6) . . ? C61 N3 Ru2 124.8(5) . . ? C61 N3 C65 119.0(6) . . ? C65 N3 Ru2 115.7(4) . . ? C66 N4 Ru2 115.7(4) . . ? C70 N4 Ru2 126.3(5) . . ? C70 N4 C66 117.9(6) . . ? F1 B1 F1 109.6(10) 2_655 . ? F2 B1 F1 110.1(3) 2_655 2_655 ? F2 B1 F1 108.0(3) . 2_655 ? F2 B1 F1 110.1(3) . . ? F2 B1 F1 108.0(3) 2_655 . ? F2 B1 F2 111.1(10) . 2_655 ? F3 B2 F3 107.2(9) . 2_656 ? F4 B2 F3 111.1(6) 2_656 . ? F4 B2 F3 108.1(5) . . ? F4 B2 F3 111.1(5) . 2_656 ? F4 B2 F3 108.1(5) 2_656 2_656 ? F4 B2 F4 111.1(12) . 2_656 ? F5 B3 F7 107.4(11) . . ? F5 B3 F5A 32.4(9) . . ? F5 B3 F6A 97.4(13) . . ? F5 B3 F7A 68.3(13) . . ? F6 B3 F5 114.3(11) . . ? F6 B3 F7 104.8(10) . . ? F6 B3 F8 110.6(12) . . ? F6 B3 F5A 139.7(14) . . ? F6 B3 F6A 70.5(12) . . ? F6 B3 F7A 70.2(15) . . ? F7 B3 F6A 154.1(14) . . ? F8 B3 F5 112.4(12) . . ? F8 B3 F7 106.7(13) . . ? F8 B3 F5A 81.9(12) . . ? F8 B3 F6A 55.2(12) . . ? F8 B3 F7A 178.2(19) . . ? F5A B3 F7 107.8(12) . . ? F5A B3 F6A 89.0(13) . . ? F7A B3 F7 71.5(14) . . ? F7A B3 F5A 98.5(14) . . ? F7A B3 F6A 126.5(18) . . ? F8A B3 F5 135.4(14) . . ? F8A B3 F6 108.5(12) . . ? F8A B3 F7 48.0(10) . . ? F8A B3 F8 60.4(11) . . ? F8A B3 F5A 110.7(14) . . ? F8A B3 F6A 108.1(15) . . ? F8A B3 F7A 117.9(16) . . ? C2 C1 Co1 70.3(11) . . ? C2 C1 C5 109.7(9) . . ? C5 C1 Co1 71.3(11) . . ? C1 C2 Co1 72.5(11) . . ? C3 C2 Co1 71.6(11) . . ? C3 C2 C1 106.8(10) . . ? C2 C3 Co1 71.1(11) . . ? C4 C3 Co1 73.2(9) . . ? C4 C3 C2 108.8(9) . . ? C3 C4 Co1 70.0(9) . . ? C3 C4 C5 108.8(9) . . ? C5 C4 Co1 70.6(10) . . ? C1 C5 Co1 71.4(11) . . ? C4 C5 Co1 72.2(9) . . ? C4 C5 C1 105.7(10) . . ? C2A C1A Co1 69.7(6) . . ? C2A C1A C5A 110.8(7) . . ? C5A C1A Co1 70.1(7) . . ? C1A C2A Co1 68.8(6) . . ? C1A C2A C3A 106.7(7) . . ? C3A C2A Co1 70.5(7) . . ? C2A C3A Co1 67.8(7) . . ? C2A C3A C4A 107.8(7) . . ? C4A C3A Co1 67.9(8) . . ? C3A C4A Co1 70.3(8) . . ? C5A C4A Co1 70.1(8) . . ? C5A C4A C3A 109.7(8) . . ? C1A C5A Co1 67.4(6) . . ? C4A C5A Co1 68.4(9) . . ? C4A C5A C1A 104.8(8) . . ? C7 C6 Co2 70.8(4) . . ? C10 C6 Co2 69.8(5) . . ? C10 C6 C7 109.0(8) . . ? C6 C7 Co2 69.9(4) . . ? C6 C7 C8 107.9(7) . . ? C8 C7 Co2 70.8(4) . . ? C7 C8 Co2 69.8(4) . . ? C9 C8 Co2 69.0(4) . . ? C9 C8 C7 106.3(7) . . ? C8 C9 Co2 72.2(4) . . ? C8 C9 C10 110.1(8) . . ? C10 C9 Co2 70.0(4) . . ? C6 C10 Co2 71.2(5) . . ? C6 C10 C9 106.6(8) . . ? C9 C10 Co2 70.1(4) . . ? C12 C11 O1 110.3(8) . . ? O2 C13 C14 105.1(15) . . ? C14A C13A O2 91(2) . . ? O3 C15 C16 108.9(10) . . ? O3 C15 C16A 106.6(11) . . ? C16 C15 C16A 35.1(10) . . ? C16A C16 C15 74.0(15) . . ? C16 C16A C15 70.9(15) . . ? O4 C17 C18 127(2) . . ? O4 C17 C18A 104.3(11) . . ? C18 C17 C18A 26(2) . . ? C18A C18 C17 82(3) . . ? C18 C18A C17 72(2) . . ? O5 C19 C20A 107.8(10) . . ? C20 C19 O5 111.0(9) . . ? C20 C19 C20A 29.8(9) . . ? C20A C20 C19 81.6(17) . . ? C20 C20A C19 68.6(16) . . ? O6 C21 C22 104.8(17) . . ? O6 C21 C22A 114(2) . . ? C22A C21 C22 111(2) . . ? O11 C31 C32 114.2(12) . . ? O11 C31 C32A 106.1(10) . . ? C32 C31 C32A 31.1(9) . . ? C32A C32 C31 77.9(16) . . ? C32 C32A C31 70.9(16) . . ? O12 C33 C34 111.0(7) . . ? O13 C35 C36 108.1(7) . . ? C38 C37 O14 113.4(8) . . ? O15 C39 C40 113.8(12) . . ? O15 C39 C40A 102.6(9) . . ? C40 C39 C40A 25.4(11) . . ? C40A C40 C39 79(2) . . ? C40 C40A C39 76(2) . . ? O16 C41 C42 107.8(10) . . ? O16 C41A C42A 95.6(16) . . ? N1 C51 C52 122.5(7) . . ? C53 C52 C51 118.4(8) . . ? C52 C53 C54 119.5(8) . . ? C55 C54 C53 120.2(8) . . ? N1 C55 C56 113.7(7) . . ? C54 C55 N1 120.3(7) . . ? C54 C55 C56 125.9(7) . . ? N2 C56 C55 115.0(6) . . ? N2 C56 C57 121.0(7) . . ? C57 C56 C55 123.9(7) . . ? C58 C57 C56 118.7(8) . . ? C57 C58 C59 121.5(8) . . ? C58 C59 C60 118.2(8) . . ? N2 C60 C59 120.2(8) . . ? N3 C61 C62 120.7(8) . . ? C63 C62 C61 120.4(7) . . ? C64 C63 C62 117.2(8) . . ? C65 C64 C63 121.5(8) . . ? N3 C65 C66 114.6(6) . . ? C64 C65 N3 121.1(7) . . ? C64 C65 C66 124.3(7) . . ? N4 C66 C65 112.9(6) . . ? C67 C66 N4 121.6(6) . . ? C67 C66 C65 125.3(7) . . ? C68 C67 C66 119.1(8) . . ? C67 C68 C69 120.6(8) . . ? C70 C69 C68 117.0(7) . . ? N4 C70 C69 123.6(7) . . ? O3S C2S C1S 104(2) . . ? C2S O3S C4S 108.7(19) . . ? O3S C4S C5S 95(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.906 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.096