Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;4,5-Di(2-pyridyl)-1,2,3-triazolate: the elusive member of a family of bridging ligands that facilitate strong metal-metal interactions ; _publ_contact_author_name 'Prof. Peter Steel' _publ_contact_author_email P.STEEL@CHEM.CANTERBURY.AC.NZ loop_ _publ_author_name P.J.Steel 'Christopher M. Fitchett' 'F. Keene' 'Chris Richardson' # Attachment '8.cif' data_cr14 _database_code_depnum_ccdc_archive 'CCDC 673126' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H9 N5, 2(H2 O)' _chemical_formula_sum 'C12 H13 N5 O2' _chemical_formula_weight 259.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4884(3) _cell_length_b 9.1666(3) _cell_length_c 9.8501(3) _cell_angle_alpha 66.450(2) _cell_angle_beta 84.740(2) _cell_angle_gamma 76.235(2) _cell_volume 602.02(4) _cell_formula_units_Z 2 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used 6650 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 34.26 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8593 _exptl_absorpt_correction_T_max 0.9798 _exptl_absorpt_process_details SADABS2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 148(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17597 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3468 _reflns_number_gt 3163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.0986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3468 _refine_ls_number_parameters 191 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 N1 N 0.74741(11) 0.86140(9) -0.19293(8) 0.02221(17) Uani 1 1 d . . . N2 N 0.68884(12) 0.72378(10) -0.11989(9) 0.02497(18) Uani 1 1 d . . . N3 N 0.65392(11) 0.70202(9) 0.02144(8) 0.02177(17) Uani 1 1 d . . . C4 C 0.69092(11) 0.82934(10) 0.04181(9) 0.01707(17) Uani 1 1 d . . . C5 C 0.74986(11) 0.93162(10) -0.09546(9) 0.01712(17) Uani 1 1 d . . . N6 N 0.79770(10) 1.16079(9) -0.05167(8) 0.01968(17) Uani 1 1 d D . . H6A H 0.768(3) 1.103(3) 0.047(2) 0.030 Uiso 0.54(3) 1 d PD A 2 C7 C 0.80091(11) 1.08949(10) -0.14816(9) 0.01739(17) Uani 1 1 d . . . C8 C 0.84762(12) 1.16933(11) -0.29603(10) 0.02107(18) Uani 1 1 d . . . H8A H 0.8507 1.1201 -0.3650 0.025 Uiso 1 1 calc R . . C9 C 0.88931(12) 1.32080(11) -0.34054(10) 0.02370(19) Uani 1 1 d . . . H9A H 0.9218 1.3759 -0.4406 0.028 Uiso 1 1 calc R . . C10 C 0.88379(13) 1.39278(11) -0.23932(11) 0.0251(2) Uani 1 1 d . . . H10A H 0.9114 1.4971 -0.2689 0.030 Uiso 1 1 calc R . . C11 C 0.83716(13) 1.30846(11) -0.09482(11) 0.02385(19) Uani 1 1 d . . . H11A H 0.8328 1.3558 -0.0242 0.029 Uiso 1 1 calc R . . N12 N 0.70665(10) 0.96201(9) 0.20693(8) 0.01955(16) Uani 1 1 d D . . H12A H 0.743(4) 1.047(3) 0.130(3) 0.029 Uiso 0.46(3) 1 d PD A 1 C13 C 0.67146(11) 0.83298(10) 0.18947(9) 0.01719(17) Uani 1 1 d . . . C14 C 0.62089(13) 0.70586(11) 0.31142(10) 0.02230(18) Uani 1 1 d . . . H14A H 0.5944 0.6152 0.2996 0.027 Uiso 1 1 calc R . . C15 C 0.60974(13) 0.71333(12) 0.44974(10) 0.02463(19) Uani 1 1 d . . . H15A H 0.5736 0.6285 0.5332 0.030 Uiso 1 1 calc R . . C16 C 0.65159(13) 0.84528(12) 0.46598(10) 0.0250(2) Uani 1 1 d . . . H16A H 0.6480 0.8508 0.5605 0.030 Uiso 1 1 calc R . . C17 C 0.69853(13) 0.96823(12) 0.34122(10) 0.02416(19) Uani 1 1 d . . . H17A H 0.7258 1.0598 0.3507 0.029 Uiso 1 1 calc R . . O1 O 0.93453(12) 0.25509(11) 0.36022(9) 0.0370(2) Uani 1 1 d . . . H1A H 1.022(2) 0.212(2) 0.311(2) 0.055 Uiso 1 1 d . . . H1B H 0.833(3) 0.291(2) 0.300(2) 0.055 Uiso 1 1 d . . . O2 O 0.59862(11) 0.38845(9) 0.20329(9) 0.03206(19) Uani 1 1 d . . . H2A H 0.507(2) 0.362(2) 0.1793(18) 0.048 Uiso 1 1 d . . . H2B H 0.601(2) 0.494(2) 0.1362(19) 0.048 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0281(4) 0.0234(4) 0.0193(3) -0.0108(3) 0.0030(3) -0.0101(3) N2 0.0341(4) 0.0255(4) 0.0209(4) -0.0118(3) 0.0043(3) -0.0135(3) N3 0.0273(4) 0.0218(3) 0.0195(4) -0.0094(3) 0.0020(3) -0.0098(3) C4 0.0178(4) 0.0178(4) 0.0162(4) -0.0065(3) 0.0004(3) -0.0052(3) C5 0.0177(4) 0.0184(4) 0.0162(3) -0.0072(3) 0.0007(3) -0.0051(3) N6 0.0219(4) 0.0186(3) 0.0196(3) -0.0077(3) 0.0012(3) -0.0064(3) C7 0.0157(3) 0.0181(4) 0.0176(4) -0.0063(3) -0.0001(3) -0.0034(3) C8 0.0220(4) 0.0218(4) 0.0184(4) -0.0067(3) 0.0022(3) -0.0061(3) C9 0.0234(4) 0.0222(4) 0.0213(4) -0.0038(3) 0.0032(3) -0.0070(3) C10 0.0262(4) 0.0185(4) 0.0285(5) -0.0061(3) 0.0017(3) -0.0075(3) C11 0.0277(4) 0.0197(4) 0.0260(4) -0.0097(3) 0.0012(3) -0.0076(3) N12 0.0230(4) 0.0200(3) 0.0168(3) -0.0080(3) 0.0005(3) -0.0057(3) C13 0.0167(4) 0.0184(4) 0.0163(4) -0.0066(3) -0.0002(3) -0.0039(3) C14 0.0272(4) 0.0216(4) 0.0181(4) -0.0066(3) 0.0024(3) -0.0084(3) C15 0.0292(4) 0.0250(4) 0.0161(4) -0.0049(3) 0.0021(3) -0.0058(3) C16 0.0286(4) 0.0288(4) 0.0171(4) -0.0101(3) -0.0002(3) -0.0031(3) C17 0.0292(4) 0.0265(4) 0.0203(4) -0.0126(3) 0.0002(3) -0.0066(3) O1 0.0360(4) 0.0485(5) 0.0291(4) -0.0192(4) 0.0019(3) -0.0075(4) O2 0.0392(4) 0.0249(4) 0.0312(4) -0.0043(3) -0.0082(3) -0.0140(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 N1 N2 1.3347(11) . ? N1 C5 1.3561(10) . ? N2 N3 1.3350(10) . ? N3 C4 1.3529(10) . ? C4 C5 1.4059(11) . ? C4 C13 1.4613(11) . ? C5 C7 1.4617(11) . ? N6 C11 1.3446(11) . ? N6 C7 1.3475(10) . ? N6 H6A 0.94(2) . ? C7 C8 1.3986(12) . ? C8 C9 1.3828(12) . ? C8 H8A 0.9500 . ? C9 C10 1.3915(13) . ? C9 H9A 0.9500 . ? C10 C11 1.3797(13) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? N12 C17 1.3419(10) . ? N12 C13 1.3480(10) . ? N12 H12A 0.92(2) . ? C13 C14 1.3973(12) . ? C14 C15 1.3852(12) . ? C14 H14A 0.9500 . ? C15 C16 1.3896(13) . ? C15 H15A 0.9500 . ? C16 C17 1.3807(13) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? O1 H1A 0.887(18) . ? O1 H1B 0.919(19) . ? O2 H2A 0.863(18) . ? O2 H2B 0.932(18) . ? 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 N2 N1 C5 107.30(7) . . ? N1 N2 N3 110.88(7) . . ? N2 N3 C4 107.80(7) . . ? N3 C4 C5 106.74(7) . . ? N3 C4 C13 119.30(7) . . ? C5 C4 C13 133.91(7) . . ? N1 C5 C4 107.28(7) . . ? N1 C5 C7 118.95(7) . . ? C4 C5 C7 133.71(7) . . ? C11 N6 C7 121.31(8) . . ? C11 N6 H6A 120.8(16) . . ? C7 N6 H6A 117.9(16) . . ? N6 C7 C8 119.68(8) . . ? N6 C7 C5 118.60(7) . . ? C8 C7 C5 121.70(8) . . ? C9 C8 C7 119.14(8) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 120.25(8) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 118.17(8) . . ? C11 C10 H10A 120.9 . . ? C9 C10 H10A 120.9 . . ? N6 C11 C10 121.45(8) . . ? N6 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C17 N12 C13 120.77(8) . . ? C17 N12 H12A 116(2) . . ? C13 N12 H12A 123(2) . . ? N12 C13 C14 119.95(8) . . ? N12 C13 C4 118.33(7) . . ? C14 C13 C4 121.71(7) . . ? C15 C14 C13 119.31(8) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 119.79(8) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 118.31(8) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? N12 C17 C16 121.82(8) . . ? N12 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? H1A O1 H1B 103.5(16) . . ? H2A O2 H2B 107.1(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 N3 -0.23(10) . . . . ? N1 N2 N3 C4 -0.05(10) . . . . ? N2 N3 C4 C5 0.31(10) . . . . ? N2 N3 C4 C13 -177.52(7) . . . . ? N2 N1 C5 C4 0.41(10) . . . . ? N2 N1 C5 C7 -177.16(7) . . . . ? N3 C4 C5 N1 -0.44(9) . . . . ? C13 C4 C5 N1 176.93(9) . . . . ? N3 C4 C5 C7 176.62(9) . . . . ? C13 C4 C5 C7 -6.01(16) . . . . ? C11 N6 C7 C8 0.55(13) . . . . ? C11 N6 C7 C5 -177.71(8) . . . . ? N1 C5 C7 N6 178.04(7) . . . . ? C4 C5 C7 N6 1.25(14) . . . . ? N1 C5 C7 C8 -0.19(12) . . . . ? C4 C5 C7 C8 -176.98(8) . . . . ? N6 C7 C8 C9 -0.17(13) . . . . ? C5 C7 C8 C9 178.04(7) . . . . ? C7 C8 C9 C10 -0.32(13) . . . . ? C8 C9 C10 C11 0.43(14) . . . . ? C7 N6 C11 C10 -0.44(14) . . . . ? C9 C10 C11 N6 -0.06(14) . . . . ? C17 N12 C13 C14 1.79(13) . . . . ? C17 N12 C13 C4 -177.14(7) . . . . ? N3 C4 C13 N12 -179.13(7) . . . . ? C5 C4 C13 N12 3.75(14) . . . . ? N3 C4 C13 C14 1.95(12) . . . . ? C5 C4 C13 C14 -175.16(9) . . . . ? N12 C13 C14 C15 -0.79(13) . . . . ? C4 C13 C14 C15 178.11(8) . . . . ? C13 C14 C15 C16 -1.01(14) . . . . ? C14 C15 C16 C17 1.79(14) . . . . ? C13 N12 C17 C16 -0.98(14) . . . . ? C15 C16 C17 N12 -0.83(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O2 0.919(19) 1.91(2) 2.8197(12) 167.9(16) . O1 H1A N1 0.887(18) 2.122(18) 3.0008(11) 170.7(16) 2_765 O2 H2B N3 0.932(18) 1.905(18) 2.8210(11) 167.3(15) . O2 H2A N2 0.863(18) 2.043(18) 2.9018(11) 173.3(15) 2_665 N6 H6A N12 0.94(2) 1.70(2) 2.6148(10) 164(2) . N12 H12A N6 0.92(2) 1.74(2) 2.6148(10) 157(3) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.386 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.089 # Attachment '9rac.cif' data_3cf3a _database_code_depnum_ccdc_archive 'CCDC 673127' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C52H40N13Ru2), C4H10O, 6(F6P), 2(C2H3N), 0.75(C2H3N), 0.25(O)' _chemical_formula_sum 'C113.50 H98.25 F36 N28.75 O1.25 P6 Ru4' _chemical_formula_weight 3159.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4722(5) _cell_length_b 13.6208(5) _cell_length_c 19.1473(7) _cell_angle_alpha 73.191(2) _cell_angle_beta 87.006(2) _cell_angle_gamma 70.094(2) _cell_volume 3158.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 101(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.78 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1581 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7907 _exptl_absorpt_correction_T_max 0.9075 _exptl_absorpt_process_details SADABS2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 101(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30687 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11120 _reflns_number_gt 7920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+26.2780P] 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 11120 _refine_ls_number_parameters 882 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2473 _refine_ls_wR_factor_gt 0.2035 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.30938(5) 1.05994(5) 0.19536(4) 0.0275(2) Uani 1 1 d . . . Ru2 Ru 0.73084(5) 0.69522(5) 0.29393(4) 0.0277(2) Uani 1 1 d . . . N1 N 0.6134(5) 0.8421(5) 0.2578(4) 0.0283(15) Uani 1 1 d . . . N2 N 0.5179(5) 0.8669(5) 0.2257(4) 0.0264(15) Uani 1 1 d . . . N3 N 0.4607(5) 0.9658(5) 0.2302(4) 0.0261(15) Uani 1 1 d . . . C4 C 0.5167(6) 1.0049(6) 0.2650(5) 0.0268(17) Uani 1 1 d . . . C5 C 0.6168(6) 0.9250(7) 0.2826(5) 0.0290(18) Uani 1 1 d . . . N6 N 0.7848(6) 0.7970(6) 0.3324(5) 0.0421(19) Uani 1 1 d U . . C7 C 0.7193(7) 0.9031(7) 0.3174(7) 0.048(2) Uani 1 1 d U . . C8 C 0.7518(9) 0.9800(9) 0.3318(9) 0.072(3) Uani 1 1 d U . . H8A H 0.7070 1.0542 0.3185 0.087 Uiso 1 1 calc R . . C9 C 0.8517(10) 0.9494(10) 0.3664(10) 0.085(3) Uani 1 1 d U . . H9A H 0.8743 1.0020 0.3781 0.102 Uiso 1 1 calc R . . C10 C 0.9160(10) 0.8421(10) 0.3829(10) 0.083(3) Uani 1 1 d U . . H10A H 0.9836 0.8187 0.4068 0.099 Uiso 1 1 calc R . . C11 C 0.8799(8) 0.7686(8) 0.3640(8) 0.060(3) Uani 1 1 d U . . H11A H 0.9253 0.6949 0.3741 0.072 Uiso 1 1 calc R . . N12 N 0.3604(5) 1.1593(5) 0.2397(4) 0.0239(14) Uani 1 1 d . . . C13 C 0.4594(6) 1.1143(6) 0.2728(4) 0.0251(17) Uani 1 1 d . . . C14 C 0.4957(7) 1.1697(7) 0.3086(5) 0.034(2) Uani 1 1 d . . . H14A H 0.5642 1.1371 0.3322 0.041 Uiso 1 1 calc R . . C15 C 0.4327(7) 1.2735(7) 0.3107(5) 0.036(2) Uani 1 1 d . . . H15A H 0.4575 1.3117 0.3363 0.043 Uiso 1 1 calc R . . C16 C 0.3346(7) 1.3202(7) 0.2756(5) 0.034(2) Uani 1 1 d . . . H16A H 0.2910 1.3921 0.2747 0.041 Uiso 1 1 calc R . . C17 C 0.3010(6) 1.2600(7) 0.2417(5) 0.0288(18) Uani 1 1 d . . . H17A H 0.2322 1.2912 0.2185 0.035 Uiso 1 1 calc R . . N18 N 0.6331(5) 0.6672(5) 0.3769(4) 0.0305(16) Uani 1 1 d . . . C19 C 0.5560(7) 0.6315(7) 0.3591(6) 0.038(2) Uani 1 1 d . . . C20 C 0.4762(8) 0.6195(9) 0.4071(7) 0.051(3) Uani 1 1 d . . . H20A H 0.4230 0.5953 0.3947 0.061 Uiso 1 1 calc R . . C21 C 0.4752(9) 0.6426(9) 0.4714(7) 0.057(3) Uani 1 1 d . . . H21A H 0.4210 0.6347 0.5040 0.068 Uiso 1 1 calc R . . C22 C 0.5512(10) 0.6771(11) 0.4896(7) 0.064(3) Uani 1 1 d . . . H22A H 0.5508 0.6935 0.5346 0.077 Uiso 1 1 calc R . . C23 C 0.6298(9) 0.6879(9) 0.4405(6) 0.050(3) Uani 1 1 d . . . H23A H 0.6834 0.7111 0.4534 0.060 Uiso 1 1 calc R . . N24 N 0.6515(6) 0.6181(5) 0.2523(4) 0.0314(16) Uani 1 1 d . . . C25 C 0.5643(8) 0.6068(7) 0.2878(6) 0.040(2) Uani 1 1 d . . . C26 C 0.4901(9) 0.5790(9) 0.2583(7) 0.057(3) Uani 1 1 d . . . H26A H 0.4272 0.5773 0.2828 0.069 Uiso 1 1 calc R . . C27 C 0.5076(11) 0.5537(9) 0.1931(8) 0.068(4) Uani 1 1 d . . . H27A H 0.4577 0.5333 0.1725 0.081 Uiso 1 1 calc R . . C28 C 0.5999(12) 0.5585(8) 0.1577(7) 0.061(3) Uani 1 1 d . . . H28A H 0.6147 0.5396 0.1133 0.074 Uiso 1 1 calc R . . C29 C 0.6705(8) 0.5916(7) 0.1887(5) 0.042(2) Uani 1 1 d . . . H29A H 0.7330 0.5956 0.1646 0.051 Uiso 1 1 calc R . . N30 N 0.8581(6) 0.5537(6) 0.3325(4) 0.0380(18) Uani 1 1 d . . . C31 C 0.9364(8) 0.5340(9) 0.2844(7) 0.051(3) Uani 1 1 d . . . C32 C 1.0241(8) 0.4393(10) 0.3003(9) 0.068(4) Uani 1 1 d . . . H32A H 1.0768 0.4275 0.2658 0.081 Uiso 1 1 calc R . . C33 C 1.0334(10) 0.3642(10) 0.3659(9) 0.073(4) Uani 1 1 d . . . H33A H 1.0918 0.2979 0.3769 0.087 Uiso 1 1 calc R . . C34 C 0.9593(9) 0.3830(8) 0.4167(8) 0.060(3) Uani 1 1 d . . . H34A H 0.9674 0.3326 0.4640 0.072 Uiso 1 1 calc R . . C35 C 0.8711(9) 0.4789(8) 0.3967(7) 0.049(3) Uani 1 1 d . . . H35A H 0.8179 0.4909 0.4309 0.059 Uiso 1 1 calc R . . N36 N 0.8327(6) 0.7132(8) 0.2109(5) 0.053(2) Uani 1 1 d U . . C37 C 0.9238(8) 0.6262(11) 0.2155(7) 0.058(3) Uani 1 1 d U . . C38 C 0.9963(9) 0.6287(13) 0.1605(7) 0.074(3) Uani 1 1 d U . . H38A H 1.0583 0.5674 0.1630 0.089 Uiso 1 1 calc R . . C39 C 0.9758(10) 0.7222(14) 0.1026(8) 0.084(4) Uani 1 1 d U . . H39A H 1.0228 0.7246 0.0639 0.101 Uiso 1 1 calc R . . C40 C 0.8875(10) 0.8121(13) 0.1004(7) 0.078(3) Uani 1 1 d U . . H40A H 0.8751 0.8785 0.0624 0.094 Uiso 1 1 calc R . . C41 C 0.8189(9) 0.8023(11) 0.1545(6) 0.065(3) Uani 1 1 d U . . H41A H 0.7566 0.8633 0.1519 0.078 Uiso 1 1 calc R . . N42 N 0.2443(6) 1.0089(6) 0.2938(4) 0.0354(18) Uani 1 1 d . . . C43 C 0.1420(7) 1.0711(8) 0.2992(6) 0.042(2) Uani 1 1 d . . . C44 C 0.0901(8) 1.0472(11) 0.3639(7) 0.058(3) Uani 1 1 d . . . H44A H 0.0205 1.0930 0.3685 0.070 Uiso 1 1 calc R . . C45 C 0.1414(10) 0.9556(11) 0.4217(7) 0.063(3) Uani 1 1 d . . . H45A H 0.1064 0.9373 0.4654 0.076 Uiso 1 1 calc R . . C46 C 0.2419(9) 0.8934(10) 0.4144(7) 0.057(3) Uani 1 1 d . . . H46A H 0.2778 0.8304 0.4530 0.068 Uiso 1 1 calc R . . C47 C 0.2921(8) 0.9224(8) 0.3500(5) 0.041(2) Uani 1 1 d . . . H47A H 0.3631 0.8790 0.3460 0.049 Uiso 1 1 calc R . . N48 N 0.1554(6) 1.1665(6) 0.1739(5) 0.0368(18) Uani 1 1 d . . . C49 C 0.0935(7) 1.1598(9) 0.2336(7) 0.047(3) Uani 1 1 d . . . C50 C -0.0080(8) 1.2327(9) 0.2280(8) 0.056(3) Uani 1 1 d . . . H50A H -0.0509 1.2280 0.2690 0.067 Uiso 1 1 calc R . . C51 C -0.0474(9) 1.3128(10) 0.1630(9) 0.067(4) Uani 1 1 d . . . H51A H -0.1167 1.3643 0.1599 0.081 Uiso 1 1 calc R . . C52 C 0.0134(9) 1.3185(9) 0.1023(8) 0.060(3) Uani 1 1 d . . . H52A H -0.0137 1.3712 0.0567 0.072 Uiso 1 1 calc R . . C53 C 0.1162(8) 1.2438(8) 0.1109(7) 0.047(3) Uani 1 1 d . . . H53A H 0.1601 1.2478 0.0705 0.057 Uiso 1 1 calc R . . N54 N 0.2797(5) 0.9526(6) 0.1499(5) 0.0366(18) Uani 1 1 d . . . C55 C 0.3028(7) 0.9641(8) 0.0789(6) 0.041(2) Uani 1 1 d . . . C56 C 0.2858(9) 0.8961(10) 0.0421(7) 0.056(3) Uani 1 1 d . . . H56A H 0.2990 0.9072 -0.0084 0.068 Uiso 1 1 calc R . . C57 C 0.2498(10) 0.8131(10) 0.0790(8) 0.064(3) Uani 1 1 d . . . H57A H 0.2398 0.7656 0.0544 0.076 Uiso 1 1 calc R . . C58 C 0.2281(9) 0.7986(9) 0.1521(7) 0.055(3) Uani 1 1 d . . . H58A H 0.2038 0.7412 0.1783 0.066 Uiso 1 1 calc R . . C59 C 0.2428(7) 0.8701(8) 0.1861(7) 0.046(3) Uani 1 1 d . . . H59A H 0.2269 0.8618 0.2359 0.056 Uiso 1 1 calc R . . N60 N 0.3593(6) 1.1070(6) 0.0916(4) 0.0315(16) Uani 1 1 d . . . C61 C 0.3470(7) 1.0499(8) 0.0457(5) 0.040(2) Uani 1 1 d . . . C62 C 0.3778(9) 1.0749(9) -0.0252(6) 0.049(3) Uani 1 1 d . . . H62A H 0.3692 1.0353 -0.0566 0.058 Uiso 1 1 calc R . . C63 C 0.4206(9) 1.1557(8) -0.0514(5) 0.048(3) Uani 1 1 d . . . H63A H 0.4410 1.1731 -0.1004 0.058 Uiso 1 1 calc R . . C64 C 0.4333(8) 1.2113(8) -0.0043(5) 0.046(2) Uani 1 1 d . . . H64A H 0.4623 1.2681 -0.0206 0.055 Uiso 1 1 calc R . . C65 C 0.4033(7) 1.1832(8) 0.0665(5) 0.039(2) Uani 1 1 d . . . H65A H 0.4145 1.2201 0.0989 0.047 Uiso 1 1 calc R . . P10 P 0.2730(3) 0.5154(2) 0.05495(19) 0.0628(9) Uani 1 1 d . . . F11 F 0.1925(10) 0.4568(10) 0.0820(7) 0.140(5) Uani 1 1 d . . . F12 F 0.1875(7) 0.6244(7) 0.0121(5) 0.091(3) Uani 1 1 d . . . F13 F 0.2585(6) 0.5550(6) 0.1250(4) 0.0692(19) Uani 1 1 d . . . F14 F 0.3594(7) 0.5761(8) 0.0325(5) 0.106(3) Uani 1 1 d . . . F15 F 0.3693(8) 0.4095(7) 0.1003(6) 0.120(4) Uani 1 1 d . . . F16 F 0.2871(17) 0.4756(10) -0.0145(7) 0.218(9) Uani 1 1 d . . . P20 P 0.74106(19) 0.27230(18) 0.36120(14) 0.0358(6) Uani 1 1 d D . . F21 F 0.6906(4) 0.1848(4) 0.4111(3) 0.0472(14) Uani 1 1 d D . . F22 F 0.6305(5) 0.3438(6) 0.3222(5) 0.098(3) Uani 1 1 d D . . F23 F 0.7222(6) 0.3301(6) 0.4219(4) 0.086(3) Uani 1 1 d D . . F24 F 0.7919(4) 0.3558(4) 0.3105(3) 0.0503(15) Uani 1 1 d D . . F25 F 0.8533(4) 0.1950(5) 0.3972(4) 0.070(2) Uani 1 1 d D . . F26 F 0.7629(7) 0.2094(5) 0.3017(3) 0.079(2) Uani 1 1 d D . . P30 P 0.1971(3) 0.5817(5) 0.3777(3) 0.1045(16) Uani 1 1 d DU . . F31 F 0.1919(9) 0.4550(7) 0.4154(6) 0.170(5) Uani 1 1 d DU . . F32 F 0.1401(10) 0.5858(9) 0.3081(5) 0.173(5) Uani 1 1 d DU . . F33 F 0.0978(6) 0.6216(10) 0.4160(6) 0.197(7) Uani 1 1 d DU . . F34 F 0.2164(8) 0.6888(6) 0.3423(5) 0.148(5) Uani 1 1 d DU . . F35 F 0.2690(6) 0.5559(7) 0.4479(4) 0.111(3) Uani 1 1 d DU . . F36 F 0.3051(7) 0.5190(8) 0.3455(6) 0.138(4) Uani 1 1 d DU . . N80 N 0.6676(9) 0.0999(9) 0.1355(6) 0.065(3) Uani 1 1 d D . . C81 C 0.6516(10) 0.1855(10) 0.1379(6) 0.052(3) Uani 1 1 d D . . C82 C 0.6309(13) 0.2947(11) 0.1399(7) 0.077(4) Uani 1 1 d D . . H82A H 0.6467 0.3379 0.0929 0.115 Uiso 1 1 calc R . . H82B H 0.6754 0.2941 0.1790 0.115 Uiso 1 1 calc R . . H82C H 0.5563 0.3269 0.1492 0.115 Uiso 1 1 calc R . . O99 O 1.0000 1.0000 0.0000 0.017(6) Uani 0.25 2 d SPU A 1 N83 N 0.9872(17) 1.0743(18) 0.0664(15) 0.050(6) Uani 0.375 1 d PDU B 2 C84 C 0.9664(19) 1.043(2) 0.1221(15) 0.038(6) Uani 0.375 1 d PDU B 2 C85 C 0.955(3) 0.986(3) 0.1958(19) 0.12(2) Uani 0.375 1 d PDU B 2 H85A H 0.9941 0.9078 0.2047 0.178 Uiso 0.375 1 calc PR B 2 H85B H 0.8797 0.9968 0.2037 0.178 Uiso 0.375 1 calc PR B 2 H85C H 0.9824 1.0137 0.2294 0.178 Uiso 0.375 1 calc PR B 2 C90 C 0.277(5) 1.147(4) 0.478(3) 0.17(2) Uani 0.50 1 d P C 3 H90A H 0.2119 1.1459 0.4575 0.252 Uiso 0.50 1 calc PR C 3 H90B H 0.2924 1.2116 0.4487 0.252 Uiso 0.50 1 calc PR C 3 H90C H 0.2678 1.1484 0.5283 0.252 Uiso 0.50 1 calc PR C 3 C91 C 0.364(3) 1.049(2) 0.4747(13) 0.150(11) Uani 0.50 1 d P C 3 H91A H 0.3493 0.9833 0.5043 0.180 Uiso 0.50 1 calc PR C 3 H91B H 0.3721 1.0457 0.4236 0.180 Uiso 0.50 1 calc PR C 3 O92 O 0.4562(19) 1.0499(13) 0.5009(10) 0.137(7) Uani 0.50 1 d P . 3 C93 C 0.364(3) 1.049(2) 0.4747(13) 0.150(11) Uani 0.50 1 d P D 4 H93A H 0.3056 1.1122 0.4802 0.226 Uiso 0.50 1 calc PR D 4 H93B H 0.3518 0.9818 0.5022 0.226 Uiso 0.50 1 calc PR D 4 H93C H 0.3700 1.0520 0.4229 0.226 Uiso 0.50 1 calc PR D 4 C94 C 0.4562(19) 1.0499(13) 0.5009(10) 0.137(7) Uani 0.50 1 d P . 4 H94A H 0.4483 1.0544 0.5517 0.164 Uiso 0.50 1 calc PR . 4 H94B H 0.4721 1.1147 0.4707 0.164 Uiso 0.50 1 calc PR . 4 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 0.0193(3) 0.0262(4) 0.0385(4) -0.0178(3) -0.0005(3) -0.0022(3) Ru2 0.0229(4) 0.0198(4) 0.0361(4) -0.0093(3) 0.0047(3) -0.0013(3) N1 0.020(3) 0.025(4) 0.037(4) -0.009(3) 0.006(3) -0.005(3) N2 0.022(3) 0.022(3) 0.034(4) -0.013(3) 0.004(3) -0.002(3) N3 0.025(3) 0.026(4) 0.028(4) -0.013(3) 0.008(3) -0.006(3) C4 0.024(4) 0.021(4) 0.036(5) -0.009(4) 0.005(3) -0.007(3) C5 0.020(4) 0.023(4) 0.044(5) -0.008(4) 0.006(4) -0.009(3) N6 0.024(3) 0.019(3) 0.078(5) -0.007(3) -0.005(3) -0.005(3) C7 0.028(4) 0.023(4) 0.092(6) -0.011(4) -0.013(4) -0.007(3) C8 0.039(5) 0.029(4) 0.142(8) -0.018(5) -0.028(5) -0.005(4) C9 0.045(5) 0.037(5) 0.167(8) -0.018(6) -0.041(6) -0.008(4) C10 0.042(5) 0.041(5) 0.155(8) -0.014(6) -0.039(6) -0.007(4) C11 0.032(4) 0.027(4) 0.114(7) -0.011(5) -0.020(5) -0.006(4) N12 0.024(3) 0.024(3) 0.023(3) -0.009(3) 0.002(3) -0.006(3) C13 0.021(4) 0.023(4) 0.028(4) -0.007(3) 0.003(3) -0.005(3) C14 0.025(4) 0.037(5) 0.040(5) -0.018(4) -0.006(4) -0.004(4) C15 0.039(5) 0.035(5) 0.044(5) -0.028(4) 0.004(4) -0.011(4) C16 0.031(5) 0.029(5) 0.041(5) -0.019(4) 0.006(4) -0.001(4) C17 0.021(4) 0.023(4) 0.040(5) -0.016(4) 0.001(3) 0.001(3) N18 0.029(4) 0.019(3) 0.039(4) -0.006(3) 0.005(3) -0.004(3) C19 0.031(5) 0.022(4) 0.053(6) -0.006(4) -0.002(4) -0.002(4) C20 0.032(5) 0.043(6) 0.068(8) -0.004(5) 0.010(5) -0.012(5) C21 0.040(6) 0.050(7) 0.059(7) -0.001(6) 0.020(5) -0.001(5) C22 0.066(8) 0.078(9) 0.050(7) -0.027(6) 0.022(6) -0.023(7) C23 0.044(6) 0.061(7) 0.051(6) -0.027(6) 0.011(5) -0.017(5) N24 0.035(4) 0.015(3) 0.036(4) -0.007(3) -0.004(3) 0.002(3) C25 0.040(5) 0.019(4) 0.055(6) -0.011(4) -0.006(5) -0.005(4) C26 0.041(6) 0.035(6) 0.088(9) -0.011(6) -0.016(6) -0.007(5) C27 0.078(9) 0.034(6) 0.092(10) -0.015(6) -0.039(8) -0.016(6) C28 0.094(10) 0.029(5) 0.057(7) -0.014(5) -0.028(7) -0.011(6) C29 0.053(6) 0.021(4) 0.045(6) -0.012(4) -0.004(5) 0.000(4) N30 0.043(5) 0.023(4) 0.044(5) -0.011(4) -0.011(4) -0.004(3) C31 0.027(5) 0.049(6) 0.072(8) -0.032(6) -0.009(5) 0.007(4) C32 0.025(5) 0.058(8) 0.131(13) -0.057(9) 0.004(6) -0.002(5) C33 0.048(7) 0.037(7) 0.121(12) -0.017(8) -0.022(8) -0.001(6) C34 0.051(7) 0.023(5) 0.094(9) -0.007(6) -0.023(7) -0.003(5) C35 0.049(6) 0.031(5) 0.066(7) -0.014(5) -0.013(5) -0.009(5) N36 0.030(4) 0.065(5) 0.050(4) -0.015(4) 0.010(3) -0.003(4) C37 0.026(4) 0.078(6) 0.062(5) -0.026(5) 0.005(4) -0.003(4) C38 0.038(5) 0.098(7) 0.068(6) -0.028(5) 0.012(5) 0.002(5) C39 0.049(5) 0.115(8) 0.061(6) -0.011(6) 0.015(5) -0.007(6) C40 0.045(5) 0.106(7) 0.059(6) 0.001(6) 0.009(5) -0.017(5) C41 0.037(5) 0.085(6) 0.049(5) 0.002(5) 0.007(4) -0.011(5) N42 0.030(4) 0.036(4) 0.053(5) -0.029(4) 0.009(3) -0.013(3) C43 0.028(5) 0.045(6) 0.065(7) -0.036(5) 0.008(5) -0.011(4) C44 0.029(5) 0.079(9) 0.092(9) -0.054(8) 0.027(6) -0.028(6) C45 0.059(8) 0.068(8) 0.067(8) -0.023(7) 0.020(6) -0.028(7) C46 0.055(7) 0.064(7) 0.056(7) -0.021(6) 0.017(6) -0.025(6) C47 0.042(5) 0.037(5) 0.041(6) -0.006(4) 0.006(4) -0.014(4) N48 0.030(4) 0.032(4) 0.053(5) -0.025(4) -0.007(4) -0.005(3) C49 0.023(5) 0.050(6) 0.086(8) -0.045(6) 0.005(5) -0.014(4) C50 0.030(5) 0.052(7) 0.088(9) -0.035(7) 0.000(6) -0.006(5) C51 0.029(5) 0.057(8) 0.124(12) -0.049(8) -0.001(7) -0.004(5) C52 0.045(6) 0.043(6) 0.088(9) -0.027(6) -0.028(6) 0.001(5) C53 0.033(5) 0.039(6) 0.070(7) -0.023(5) -0.016(5) -0.004(4) N54 0.022(4) 0.030(4) 0.056(5) -0.020(4) -0.006(3) 0.000(3) C55 0.035(5) 0.036(5) 0.052(6) -0.024(5) -0.010(4) -0.001(4) C56 0.054(7) 0.063(7) 0.059(7) -0.036(6) -0.004(5) -0.014(6) C57 0.062(7) 0.055(7) 0.090(10) -0.037(7) -0.010(7) -0.024(6) C58 0.047(6) 0.045(6) 0.085(9) -0.027(6) -0.002(6) -0.020(5) C59 0.030(5) 0.038(6) 0.072(7) -0.020(5) -0.007(5) -0.008(4) N60 0.033(4) 0.024(4) 0.033(4) -0.014(3) -0.004(3) 0.000(3) C61 0.032(5) 0.038(5) 0.037(5) -0.018(4) -0.011(4) 0.011(4) C62 0.056(6) 0.041(6) 0.038(6) -0.021(5) -0.015(5) 0.007(5) C63 0.055(6) 0.043(6) 0.022(5) -0.010(4) -0.005(4) 0.016(5) C64 0.052(6) 0.032(5) 0.038(6) -0.008(4) 0.004(5) 0.002(5) C65 0.040(5) 0.033(5) 0.033(5) -0.013(4) -0.004(4) 0.004(4) P10 0.079(2) 0.0363(15) 0.063(2) -0.0188(14) 0.0294(17) -0.0075(15) F11 0.189(12) 0.154(10) 0.156(10) -0.068(8) 0.038(9) -0.142(10) F12 0.083(6) 0.072(5) 0.104(6) -0.031(5) -0.040(5) 0.000(4) F13 0.072(5) 0.066(4) 0.068(5) -0.023(4) 0.008(4) -0.018(4) F14 0.069(5) 0.108(7) 0.106(7) 0.008(6) 0.027(5) -0.021(5) F15 0.112(8) 0.054(5) 0.142(9) -0.003(5) 0.029(7) 0.013(5) F16 0.42(3) 0.104(9) 0.119(9) -0.081(8) 0.125(13) -0.049(12) P20 0.0345(12) 0.0241(11) 0.0511(15) -0.0138(11) 0.0004(11) -0.0101(10) F21 0.055(3) 0.044(3) 0.049(3) -0.012(3) 0.003(3) -0.028(3) F22 0.046(4) 0.060(5) 0.159(9) 0.024(5) -0.035(5) -0.021(4) F23 0.097(6) 0.103(6) 0.119(7) -0.089(5) 0.070(5) -0.073(5) F24 0.055(4) 0.034(3) 0.069(4) -0.015(3) 0.006(3) -0.025(3) F25 0.036(3) 0.061(4) 0.081(5) 0.008(4) 0.004(3) -0.002(3) F26 0.163(8) 0.065(4) 0.047(4) -0.025(3) 0.027(4) -0.081(5) P30 0.064(2) 0.181(5) 0.120(3) -0.097(3) 0.025(2) -0.064(3) F31 0.165(10) 0.175(11) 0.208(12) -0.039(10) -0.019(9) -0.113(9) F32 0.228(12) 0.160(10) 0.149(10) -0.040(8) -0.077(9) -0.078(9) F33 0.053(5) 0.265(14) 0.143(9) 0.035(10) 0.002(6) 0.027(8) F34 0.189(11) 0.081(7) 0.151(9) -0.014(6) -0.080(8) -0.022(7) F35 0.058(5) 0.111(7) 0.151(8) -0.004(6) -0.011(5) -0.039(5) F36 0.126(8) 0.154(9) 0.195(10) -0.117(8) 0.044(8) -0.072(7) N80 0.086(8) 0.058(7) 0.062(7) -0.023(5) 0.010(6) -0.032(6) C81 0.070(8) 0.054(7) 0.041(6) -0.017(5) 0.007(5) -0.031(6) C82 0.122(13) 0.068(9) 0.058(8) -0.020(7) 0.005(8) -0.052(9) O99 0.016(7) 0.015(7) 0.022(7) -0.010(5) -0.005(5) -0.004(5) N83 0.028(11) 0.038(13) 0.09(2) -0.007(13) -0.009(12) -0.021(10) C84 0.034(13) 0.043(15) 0.063(18) -0.046(15) 0.016(13) -0.021(12) C85 0.06(2) 0.12(3) 0.24(6) -0.13(4) 0.03(3) -0.06(2) C90 0.23(6) 0.08(3) 0.15(4) 0.02(3) -0.01(4) -0.03(4) C91 0.23(3) 0.16(2) 0.112(17) -0.023(16) 0.019(19) -0.15(3) O92 0.23(2) 0.112(13) 0.105(12) -0.037(12) 0.038(14) -0.101(16) C93 0.23(3) 0.16(2) 0.112(17) -0.023(16) 0.019(19) -0.15(3) C94 0.23(2) 0.112(13) 0.105(12) -0.037(12) 0.038(14) -0.101(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.028(7) . ? Ru1 N54 2.056(7) . ? Ru1 N60 2.057(8) . ? Ru1 N48 2.066(7) . ? Ru1 N42 2.071(8) . ? Ru1 N12 2.094(7) . ? Ru2 N1 2.035(7) . ? Ru2 N18 2.045(7) . ? Ru2 N24 2.055(7) . ? Ru2 N36 2.061(9) . ? Ru2 N30 2.064(7) . ? Ru2 N6 2.079(8) . ? N1 N2 1.347(9) . ? N1 C5 1.362(11) . ? N2 N3 1.330(9) . ? N3 C4 1.353(11) . ? C4 C5 1.398(11) . ? C4 C13 1.473(11) . ? C5 C7 1.462(12) . ? N6 C11 1.329(12) . ? N6 C7 1.366(12) . ? C7 C8 1.363(15) . ? C8 C9 1.405(16) . ? C8 H8A 0.9500 . ? C9 C10 1.373(16) . ? C9 H9A 0.9500 . ? C10 C11 1.389(16) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? N12 C17 1.342(10) . ? N12 C13 1.365(10) . ? C13 C14 1.365(12) . ? C14 C15 1.391(12) . ? C14 H14A 0.9500 . ? C15 C16 1.370(13) . ? C15 H15A 0.9500 . ? C16 C17 1.375(12) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? N18 C23 1.321(13) . ? N18 C19 1.381(12) . ? C19 C20 1.399(14) . ? C19 C25 1.487(14) . ? C20 C21 1.354(17) . ? C20 H20A 0.9500 . ? C21 C22 1.360(18) . ? C21 H21A 0.9500 . ? C22 C23 1.395(15) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? N24 C29 1.355(12) . ? N24 C25 1.359(12) . ? C25 C26 1.379(14) . ? C26 C27 1.376(18) . ? C26 H26A 0.9500 . ? C27 C28 1.398(19) . ? C27 H27A 0.9500 . ? C28 C29 1.401(15) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? N30 C35 1.325(13) . ? N30 C31 1.372(14) . ? C31 C32 1.387(15) . ? C31 C37 1.505(17) . ? C32 C33 1.35(2) . ? C32 H32A 0.9500 . ? C33 C34 1.37(2) . ? C33 H33A 0.9500 . ? C34 C35 1.402(14) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? N36 C41 1.336(15) . ? N36 C37 1.371(14) . ? C37 C38 1.399(16) . ? C38 C39 1.38(2) . ? C38 H38A 0.9500 . ? C39 C40 1.378(19) . ? C39 H39A 0.9500 . ? C40 C41 1.360(16) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? N42 C47 1.336(12) . ? N42 C43 1.366(12) . ? C43 C44 1.401(16) . ? C43 C49 1.461(16) . ? C44 C45 1.397(18) . ? C44 H44A 0.9500 . ? C45 C46 1.355(17) . ? C45 H45A 0.9500 . ? C46 C47 1.396(15) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? N48 C53 1.341(13) . ? N48 C49 1.379(14) . ? C49 C50 1.377(14) . ? C50 C51 1.382(19) . ? C50 H50A 0.9500 . ? C51 C52 1.386(19) . ? C51 H51A 0.9500 . ? C52 C53 1.395(14) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? N54 C55 1.355(13) . ? N54 C59 1.371(13) . ? C55 C56 1.395(14) . ? C55 C61 1.459(15) . ? C56 C57 1.374(17) . ? C56 H56A 0.9500 . ? C57 C58 1.386(18) . ? C57 H57A 0.9500 . ? C58 C59 1.386(15) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? N60 C65 1.326(13) . ? N60 C61 1.379(11) . ? C61 C62 1.380(15) . ? C62 C63 1.371(16) . ? C62 H62A 0.9500 . ? C63 C64 1.382(15) . ? C63 H63A 0.9500 . ? C64 C65 1.378(14) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? P10 F11 1.542(10) . ? P10 F16 1.556(11) . ? P10 F12 1.560(8) . ? P10 F13 1.564(8) . ? P10 F14 1.618(10) . ? P10 F15 1.624(10) . ? P20 F23 1.548(6) . ? P20 F22 1.560(6) . ? P20 F25 1.574(6) . ? P20 F26 1.574(6) . ? P20 F24 1.589(6) . ? P20 F21 1.618(5) . ? P30 F33 1.502(8) . ? P30 F34 1.524(8) . ? P30 F32 1.550(8) . ? P30 F35 1.582(7) . ? P30 F36 1.609(8) . ? P30 F31 1.691(8) . ? N80 C81 1.125(13) . ? C81 C82 1.428(16) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N83 C84 1.09(2) . ? C84 C85 1.43(2) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C90 C91 1.46(5) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 O92 1.36(3) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? O92 O92 1.47(4) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 N54 95.9(3) . . ? N3 Ru1 N60 89.3(3) . . ? N54 Ru1 N60 79.2(3) . . ? N3 Ru1 N48 170.5(3) . . ? N54 Ru1 N48 92.6(3) . . ? N60 Ru1 N48 96.5(3) . . ? N3 Ru1 N42 95.5(3) . . ? N54 Ru1 N42 94.9(3) . . ? N60 Ru1 N42 172.8(3) . . ? N48 Ru1 N42 79.5(3) . . ? N3 Ru1 N12 77.3(3) . . ? N54 Ru1 N12 172.5(3) . . ? N60 Ru1 N12 97.4(3) . . ? N48 Ru1 N12 94.5(3) . . ? N42 Ru1 N12 88.9(3) . . ? N1 Ru2 N18 83.9(3) . . ? N1 Ru2 N24 92.3(3) . . ? N18 Ru2 N24 80.1(3) . . ? N1 Ru2 N36 99.1(3) . . ? N18 Ru2 N36 176.4(3) . . ? N24 Ru2 N36 97.8(4) . . ? N1 Ru2 N30 174.9(3) . . ? N18 Ru2 N30 97.9(3) . . ? N24 Ru2 N30 92.7(3) . . ? N36 Ru2 N30 79.2(3) . . ? N1 Ru2 N6 77.4(3) . . ? N18 Ru2 N6 96.3(3) . . ? N24 Ru2 N6 169.4(3) . . ? N36 Ru2 N6 86.3(4) . . ? N30 Ru2 N6 97.7(3) . . ? N2 N1 C5 110.7(6) . . ? N2 N1 Ru2 129.8(5) . . ? C5 N1 Ru2 117.7(5) . . ? N3 N2 N1 106.3(6) . . ? N2 N3 C4 111.2(7) . . ? N2 N3 Ru1 130.7(5) . . ? C4 N3 Ru1 118.1(5) . . ? N3 C4 C5 106.3(7) . . ? N3 C4 C13 115.0(7) . . ? C5 C4 C13 138.8(8) . . ? N1 C5 C4 105.6(7) . . ? N1 C5 C7 113.1(7) . . ? C4 C5 C7 141.3(8) . . ? C11 N6 C7 118.9(8) . . ? C11 N6 Ru2 125.0(7) . . ? C7 N6 Ru2 115.9(6) . . ? C8 C7 N6 120.9(9) . . ? C8 C7 C5 124.8(9) . . ? N6 C7 C5 114.2(8) . . ? C7 C8 C9 120.0(10) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 118.6(11) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 118.6(11) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? N6 C11 C10 122.9(10) . . ? N6 C11 H11A 118.5 . . ? C10 C11 H11A 118.5 . . ? C17 N12 C13 118.4(7) . . ? C17 N12 Ru1 124.9(5) . . ? C13 N12 Ru1 116.5(5) . . ? N12 C13 C14 120.5(7) . . ? N12 C13 C4 112.8(7) . . ? C14 C13 C4 126.7(7) . . ? C13 C14 C15 120.3(8) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.3(8) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C17 118.0(8) . . ? C15 C16 H16A 121.0 . . ? C17 C16 H16A 121.0 . . ? N12 C17 C16 123.5(8) . . ? N12 C17 H17A 118.3 . . ? C16 C17 H17A 118.3 . . ? C23 N18 C19 118.2(8) . . ? C23 N18 Ru2 128.2(7) . . ? C19 N18 Ru2 113.3(6) . . ? N18 C19 C20 120.3(10) . . ? N18 C19 C25 116.4(8) . . ? C20 C19 C25 123.4(9) . . ? C21 C20 C19 119.5(11) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 120.6(10) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C23 118.4(11) . . ? C21 C22 H22A 120.8 . . ? C23 C22 H22A 120.8 . . ? N18 C23 C22 123.0(11) . . ? N18 C23 H23A 118.5 . . ? C22 C23 H23A 118.5 . . ? C29 N24 C25 118.4(8) . . ? C29 N24 Ru2 125.8(7) . . ? C25 N24 Ru2 115.2(6) . . ? N24 C25 C26 122.3(10) . . ? N24 C25 C19 113.2(8) . . ? C26 C25 C19 124.4(10) . . ? C27 C26 C25 119.6(12) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 118.9(11) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C27 C28 C29 119.0(11) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N24 C29 C28 121.5(11) . . ? N24 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C35 N30 C31 116.8(9) . . ? C35 N30 Ru2 127.8(7) . . ? C31 N30 Ru2 115.3(7) . . ? N30 C31 C32 122.4(12) . . ? N30 C31 C37 114.9(8) . . ? C32 C31 C37 122.6(11) . . ? C33 C32 C31 118.9(13) . . ? C33 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C32 C33 C34 120.5(11) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C33 C34 C35 117.9(12) . . ? C33 C34 H34A 121.0 . . ? C35 C34 H34A 121.0 . . ? N30 C35 C34 123.4(12) . . ? N30 C35 H35A 118.3 . . ? C34 C35 H35A 118.3 . . ? C41 N36 C37 117.6(10) . . ? C41 N36 Ru2 125.9(7) . . ? C37 N36 Ru2 116.4(8) . . ? N36 C37 C38 120.9(12) . . ? N36 C37 C31 113.4(9) . . ? C38 C37 C31 125.6(11) . . ? C39 C38 C37 118.5(12) . . ? C39 C38 H38A 120.8 . . ? C37 C38 H38A 120.8 . . ? C40 C39 C38 120.6(12) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C41 C40 C39 117.5(14) . . ? C41 C40 H40A 121.2 . . ? C39 C40 H40A 121.2 . . ? N36 C41 C40 124.8(12) . . ? N36 C41 H41A 117.6 . . ? C40 C41 H41A 117.6 . . ? C47 N42 C43 118.9(9) . . ? C47 N42 Ru1 126.3(6) . . ? C43 N42 Ru1 114.8(7) . . ? N42 C43 C44 120.4(10) . . ? N42 C43 C49 115.3(9) . . ? C44 C43 C49 124.3(9) . . ? C45 C44 C43 119.6(10) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C46 C45 C44 119.0(12) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C45 C46 C47 119.6(12) . . ? C45 C46 H46A 120.2 . . ? C47 C46 H46A 120.2 . . ? N42 C47 C46 122.5(10) . . ? N42 C47 H47A 118.8 . . ? C46 C47 H47A 118.8 . . ? C53 N48 C49 119.7(9) . . ? C53 N48 Ru1 125.9(7) . . ? C49 N48 Ru1 114.2(7) . . ? C50 C49 N48 119.8(11) . . ? C50 C49 C43 124.5(11) . . ? N48 C49 C43 115.7(8) . . ? C49 C50 C51 120.1(12) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C50 C51 C52 120.5(11) . . ? C50 C51 H51A 119.8 . . ? C52 C51 H51A 119.8 . . ? C51 C52 C53 117.3(12) . . ? C51 C52 H52A 121.4 . . ? C53 C52 H52A 121.4 . . ? N48 C53 C52 122.7(12) . . ? N48 C53 H53A 118.7 . . ? C52 C53 H53A 118.7 . . ? C55 N54 C59 118.9(8) . . ? C55 N54 Ru1 115.6(6) . . ? C59 N54 Ru1 125.5(7) . . ? N54 C55 C56 120.8(10) . . ? N54 C55 C61 115.4(8) . . ? C56 C55 C61 123.8(10) . . ? C57 C56 C55 119.7(11) . . ? C57 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? C56 C57 C58 120.2(11) . . ? C56 C57 H57A 119.9 . . ? C58 C57 H57A 119.9 . . ? C59 C58 C57 118.3(11) . . ? C59 C58 H58A 120.8 . . ? C57 C58 H58A 120.8 . . ? N54 C59 C58 122.0(11) . . ? N54 C59 H59A 119.0 . . ? C58 C59 H59A 119.0 . . ? C65 N60 C61 118.7(8) . . ? C65 N60 Ru1 126.4(6) . . ? C61 N60 Ru1 114.8(6) . . ? N60 C61 C62 119.6(10) . . ? N60 C61 C55 115.0(8) . . ? C62 C61 C55 125.4(9) . . ? C63 C62 C61 121.3(9) . . ? C63 C62 H62A 119.3 . . ? C61 C62 H62A 119.3 . . ? C62 C63 C64 118.1(9) . . ? C62 C63 H63A 121.0 . . ? C64 C63 H63A 121.0 . . ? C65 C64 C63 119.2(11) . . ? C65 C64 H64A 120.4 . . ? C63 C64 H64A 120.4 . . ? N60 C65 C64 123.0(9) . . ? N60 C65 H65A 118.5 . . ? C64 C65 H65A 118.5 . . ? F11 P10 F16 90.2(9) . . ? F11 P10 F12 94.0(7) . . ? F16 P10 F12 89.8(7) . . ? F11 P10 F13 89.5(5) . . ? F16 P10 F13 179.7(8) . . ? F12 P10 F13 90.2(4) . . ? F11 P10 F14 176.0(6) . . ? F16 P10 F14 93.4(8) . . ? F12 P10 F14 87.8(5) . . ? F13 P10 F14 86.9(5) . . ? F11 P10 F15 91.2(7) . . ? F16 P10 F15 92.8(8) . . ? F12 P10 F15 174.1(6) . . ? F13 P10 F15 87.2(5) . . ? F14 P10 F15 86.8(5) . . ? F23 P20 F22 93.1(5) . . ? F23 P20 F25 90.7(4) . . ? F22 P20 F25 176.1(5) . . ? F23 P20 F26 177.8(5) . . ? F22 P20 F26 88.8(5) . . ? F25 P20 F26 87.4(4) . . ? F23 P20 F24 92.5(3) . . ? F22 P20 F24 90.2(3) . . ? F25 P20 F24 90.5(3) . . ? F26 P20 F24 88.7(3) . . ? F23 P20 F21 89.4(3) . . ? F22 P20 F21 90.1(3) . . ? F25 P20 F21 89.2(3) . . ? F26 P20 F21 89.5(3) . . ? F24 P20 F21 178.1(3) . . ? F33 P30 F34 100.2(6) . . ? F33 P30 F32 95.4(6) . . ? F34 P30 F32 93.8(5) . . ? F33 P30 F35 91.9(5) . . ? F34 P30 F35 92.4(4) . . ? F32 P30 F35 169.4(6) . . ? F33 P30 F36 170.4(6) . . ? F34 P30 F36 89.0(5) . . ? F32 P30 F36 86.5(6) . . ? F35 P30 F36 84.9(5) . . ? F33 P30 F31 86.5(5) . . ? F34 P30 F31 172.8(6) . . ? F32 P30 F31 87.9(5) . . ? F35 P30 F31 84.9(5) . . ? F36 P30 F31 84.1(5) . . ? N80 C81 C82 179.2(14) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N83 C84 C85 170(3) . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C91 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O92 C91 C90 110(3) . . ? O92 C91 H91A 109.6 . . ? C90 C91 H91A 109.6 . . ? O92 C91 H91B 109.6 . . ? C90 C91 H91B 109.6 . . ? H91A C91 H91B 108.1 . . ? C91 O92 O92 110(2) . 2_676 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.889 _refine_diff_density_min -2.023 _refine_diff_density_rms 0.238 # Attachment '12.cif' data_cr10 _database_code_depnum_ccdc_archive 'CCDC 673128' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C34 H28 N8 Ru), C3 H6 O2, C3 H6 O, 4(F6 P)' _chemical_formula_sum 'C37 H34 F12 N8 O1.50 P2 Ru' _chemical_formula_weight 1005.73 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' 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' 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 _symmetry_space_group_name_Hall -P2ybc 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 11.6741(3) _cell_length_b 14.0245(4) _cell_length_c 26.2735(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.946(2) _cell_angle_gamma 90.00 _cell_volume 4249.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7179 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.99 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7484 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details SADABS2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60555 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7693 _reflns_number_gt 6515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+8.2957P] 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 7693 _refine_ls_number_parameters 596 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.114 _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 0.76135(3) 0.97007(2) 0.138975(12) 0.02612(13) Uani 1 1 d . . . N1 N 0.6531(3) 0.7039(3) 0.08107(14) 0.0391(9) Uani 1 1 d . . . N2 N 0.6206(3) 0.7907(3) 0.09629(15) 0.0407(9) Uani 1 1 d . . . N3 N 0.7195(3) 0.8382(2) 0.10912(13) 0.0313(8) Uani 1 1 d . . . C4 C 0.8111(4) 0.7823(3) 0.10207(14) 0.0296(9) Uani 1 1 d . . . C5 C 0.7676(4) 0.6957(3) 0.08389(16) 0.0350(10) Uani 1 1 d . . . H5A H 0.8099 0.6418 0.0752 0.042 Uiso 1 1 calc R . . N6 N 0.9245(3) 0.9146(2) 0.13314(11) 0.0266(7) Uani 1 1 d . . . C7 C 0.9257(4) 0.8228(3) 0.11634(14) 0.0286(8) Uani 1 1 d . . . C8 C 1.0287(4) 0.7746(3) 0.11389(15) 0.0353(10) Uani 1 1 d . . . H8A H 1.0274 0.7111 0.1012 0.042 Uiso 1 1 calc R . . C9 C 1.1328(4) 0.8199(3) 0.12999(16) 0.0386(10) Uani 1 1 d . . . H9A H 1.2042 0.7878 0.1291 0.046 Uiso 1 1 calc R . . C10 C 1.1316(4) 0.9126(4) 0.14749(16) 0.0373(10) Uani 1 1 d . . . H10A H 1.2023 0.9451 0.1588 0.045 Uiso 1 1 calc R . . C11 C 1.0274(4) 0.9577(3) 0.14841(16) 0.0319(9) Uani 1 1 d . . . H11A H 1.0279 1.0218 0.1603 0.038 Uiso 1 1 calc R . . C12 C 0.5631(5) 0.6318(4) 0.0647(2) 0.0530(13) Uani 1 1 d . . . H12A H 0.4997 0.6391 0.0855 0.064 Uiso 1 1 calc R . . H12B H 0.5968 0.5674 0.0714 0.064 Uiso 1 1 calc R . . C13 C 0.5124(5) 0.6406(3) 0.0070(2) 0.0566(15) Uani 1 1 d . . . C14 C 0.3960(6) 0.6394(5) -0.0073(3) 0.0732(19) Uani 1 1 d . . . H14A H 0.3471 0.6358 0.0184 0.088 Uiso 1 1 calc R . . C15 C 0.3480(7) 0.6433(5) -0.0579(3) 0.087(3) Uani 1 1 d . . . H15A H 0.2660 0.6435 -0.0671 0.104 Uiso 1 1 calc R . . C16 C 0.4163(7) 0.6471(5) -0.0957(3) 0.084(2) Uani 1 1 d . . . H16A H 0.3825 0.6467 -0.1310 0.100 Uiso 1 1 calc R . . C17 C 0.5333(7) 0.6514(6) -0.0819(3) 0.085(2) Uani 1 1 d . . . H17A H 0.5815 0.6576 -0.1077 0.103 Uiso 1 1 calc R . . C18 C 0.5833(6) 0.6468(5) -0.0298(2) 0.0708(18) Uani 1 1 d . . . H18A H 0.6652 0.6480 -0.0202 0.085 Uiso 1 1 calc R . . N19 N 0.7926(3) 0.9282(3) 0.21510(14) 0.0328(8) Uani 1 1 d . . . C20 C 0.8277(4) 0.9988(3) 0.24946(16) 0.0337(9) Uani 1 1 d . . . C21 C 0.8533(5) 0.9807(4) 0.3012(2) 0.0521(13) Uani 1 1 d . . . H21A H 0.8782 1.0311 0.3244 0.063 Uiso 1 1 calc R . . C22 C 0.8430(6) 0.8894(4) 0.3197(2) 0.0619(16) Uani 1 1 d . . . H22A H 0.8604 0.8763 0.3556 0.074 Uiso 1 1 calc R . . C23 C 0.8070(5) 0.8176(4) 0.2850(2) 0.0519(13) Uani 1 1 d . . . H23A H 0.7985 0.7541 0.2965 0.062 Uiso 1 1 calc R . . C24 C 0.7836(4) 0.8398(3) 0.23365(18) 0.0389(10) Uani 1 1 d . . . H24A H 0.7597 0.7899 0.2099 0.047 Uiso 1 1 calc R . . N25 N 0.8204(3) 1.0955(2) 0.17395(12) 0.0268(7) Uani 1 1 d . . . C26 C 0.8415(4) 1.0933(3) 0.22633(15) 0.0301(9) Uani 1 1 d . . . C27 C 0.8750(4) 1.1740(3) 0.25480(17) 0.0404(11) Uani 1 1 d . . . H27A H 0.8883 1.1711 0.2914 0.048 Uiso 1 1 calc R . . C28 C 0.8890(4) 1.2584(3) 0.23023(18) 0.0436(11) Uani 1 1 d . . . H28A H 0.9121 1.3144 0.2495 0.052 Uiso 1 1 calc R . . C29 C 0.8691(4) 1.2611(3) 0.17682(18) 0.0393(10) Uani 1 1 d . . . H29A H 0.8786 1.3186 0.1588 0.047 Uiso 1 1 calc R . . C30 C 0.8351(4) 1.1779(3) 0.15029(16) 0.0344(9) Uani 1 1 d . . . H30A H 0.8216 1.1794 0.1137 0.041 Uiso 1 1 calc R . . N31 N 0.7212(3) 1.0273(2) 0.06637(14) 0.0330(8) Uani 1 1 d . . . C32 C 0.7892(5) 1.0272(3) 0.03027(17) 0.0399(11) Uani 1 1 d . . . H32A H 0.8630 0.9974 0.0377 0.048 Uiso 1 1 calc R . . C33 C 0.7570(5) 1.0688(4) -0.01791(18) 0.0524(13) Uani 1 1 d . . . H33A H 0.8080 1.0692 -0.0428 0.063 Uiso 1 1 calc R . . C34 C 0.6474(5) 1.1100(4) -0.0284(2) 0.0546(14) Uani 1 1 d . . . H34A H 0.6221 1.1383 -0.0611 0.066 Uiso 1 1 calc R . . C35 C 0.5767(5) 1.1098(3) 0.00808(19) 0.0469(12) Uani 1 1 d . . . H35A H 0.5021 1.1383 0.0010 0.056 Uiso 1 1 calc R . . C36 C 0.6135(4) 1.0677(3) 0.05565(18) 0.0371(10) Uani 1 1 d . . . N37 N 0.5960(3) 1.0172(2) 0.13994(15) 0.0348(8) Uani 1 1 d . . . C38 C 0.5444(4) 1.0637(3) 0.09723(19) 0.0378(10) Uani 1 1 d . . . C39 C 0.4329(4) 1.1021(4) 0.0955(2) 0.0552(14) Uani 1 1 d . . . H39A H 0.3972 1.1352 0.0657 0.066 Uiso 1 1 calc R . . C40 C 0.3752(5) 1.0921(4) 0.1370(3) 0.0654(17) Uani 1 1 d . . . H40A H 0.2992 1.1172 0.1357 0.078 Uiso 1 1 calc R . . C41 C 0.4277(5) 1.0459(4) 0.1803(3) 0.0614(16) Uani 1 1 d . . . H41A H 0.3898 1.0396 0.2096 0.074 Uiso 1 1 calc R . . C42 C 0.5376(4) 1.0085(4) 0.1803(2) 0.0461(12) Uani 1 1 d . . . H42A H 0.5736 0.9752 0.2100 0.055 Uiso 1 1 calc R . . P10 P 0.79649(11) 0.54749(8) 0.20651(4) 0.0360(3) Uani 1 1 d . . . F11 F 0.9063(3) 0.4818(2) 0.22575(13) 0.0560(8) Uani 1 1 d . . . F12 F 0.8030(3) 0.5896(2) 0.26374(11) 0.0593(8) Uani 1 1 d . . . F13 F 0.8792(2) 0.6303(2) 0.19256(11) 0.0470(7) Uani 1 1 d . . . F14 F 0.6872(3) 0.6146(2) 0.18802(13) 0.0621(9) Uani 1 1 d . . . F15 F 0.7883(3) 0.5056(2) 0.14981(11) 0.0590(8) Uani 1 1 d . . . F16 F 0.7125(3) 0.4648(2) 0.22080(14) 0.0605(9) Uani 1 1 d . . . P20 P 0.09064(15) 0.21264(12) 0.04366(5) 0.0608(4) Uani 1 1 d . . . F21 F -0.0139(5) 0.2557(5) 0.0664(2) 0.133(2) Uani 1 1 d . . . F22 F 0.1832(5) 0.2673(4) 0.08338(18) 0.1179(18) Uani 1 1 d . . . F23 F 0.0849(4) 0.2960(3) 0.00299(17) 0.0995(16) Uani 1 1 d . . . F24 F 0.1997(3) 0.1714(3) 0.02026(14) 0.0744(10) Uani 1 1 d . . . F25 F 0.0095(4) 0.1531(5) 0.00122(19) 0.1263(19) Uani 1 1 d . . . F26 F 0.0976(5) 0.1254(4) 0.08129(19) 0.1246(19) Uani 1 1 d . . . C70 C -0.0202(15) 0.4979(14) 0.0492(8) 0.122(5) Uani 0.50 1 d PDU . 1 H70A H -0.0335 0.5002 0.0844 0.183 Uiso 0.50 1 d PR . 1 H70B H -0.0749 0.5386 0.0285 0.183 Uiso 0.50 1 d PR . 1 H70C H -0.0296 0.4336 0.0367 0.183 Uiso 0.50 1 d PR . 1 C71 C 0.0770(17) 0.5261(14) 0.0456(8) 0.117(4) Uani 0.50 1 d PDU A 1 C72 C 0.0988(14) 0.5212(11) -0.0026(7) 0.094(4) Uani 0.50 1 d PDU . 1 H72A H 0.1752 0.5419 -0.0067 0.141 Uiso 0.50 1 d PR . 1 H72B H 0.0875 0.4565 -0.0143 0.141 Uiso 0.50 1 d PR . 1 H72C H 0.0422 0.5615 -0.0226 0.141 Uiso 0.50 1 d PR . 1 O73 O 0.1561(14) 0.5514(11) 0.0786(6) 0.145(5) Uani 0.50 1 d PDU A 1 C80 C 0.4124(16) 0.6416(13) 0.1914(8) 0.126(5) Uani 0.50 1 d PDU B 2 H80A H 0.3605 0.6173 0.2133 0.190 Uiso 0.50 1 d PR B 2 H80B H 0.4827 0.6050 0.1965 0.190 Uiso 0.50 1 d PR B 2 H80C H 0.3764 0.6369 0.1561 0.190 Uiso 0.50 1 d PR B 2 C81 C 0.4348(16) 0.7250(14) 0.2023(8) 0.117(4) Uani 0.50 1 d PDU B 2 C82 C 0.4229(15) 0.7766(13) 0.1596(7) 0.115(5) Uani 0.50 1 d PDU B 2 H82A H 0.3859 0.8360 0.1652 0.173 Uiso 0.50 1 d PR B 2 H82B H 0.3762 0.7423 0.1323 0.173 Uiso 0.50 1 d PR B 2 H82C H 0.4978 0.7889 0.1502 0.173 Uiso 0.50 1 d PR B 2 O83 O 0.4418(15) 0.7672(11) 0.2432(7) 0.154(5) Uani 0.50 1 d PDU B 2 O100 O 0.3091(13) 0.6409(10) 0.1219(5) 0.141(6) Uani 0.50 1 d P C 3 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 0.0313(2) 0.0227(2) 0.0230(2) -0.00117(12) -0.00012(13) 0.00169(12) N1 0.049(2) 0.0285(19) 0.034(2) -0.0052(15) -0.0096(16) -0.0040(17) N2 0.041(2) 0.033(2) 0.043(2) -0.0032(16) -0.0092(17) -0.0033(17) N3 0.0345(18) 0.0286(18) 0.0272(17) -0.0006(14) -0.0058(14) 0.0011(15) C4 0.042(2) 0.025(2) 0.0199(18) 0.0018(15) -0.0014(16) 0.0040(17) C5 0.051(3) 0.026(2) 0.025(2) -0.0013(16) -0.0026(18) 0.0041(19) N6 0.0362(18) 0.0288(17) 0.0137(14) 0.0008(13) 0.0009(13) 0.0022(14) C7 0.041(2) 0.028(2) 0.0157(17) 0.0043(15) 0.0015(15) 0.0044(17) C8 0.049(3) 0.033(2) 0.024(2) 0.0032(17) 0.0028(18) 0.0128(19) C9 0.039(2) 0.048(3) 0.029(2) 0.010(2) 0.0044(18) 0.013(2) C10 0.034(2) 0.050(3) 0.026(2) 0.0043(19) 0.0004(17) 0.001(2) C11 0.035(2) 0.034(2) 0.026(2) 0.0005(17) 0.0033(17) -0.0010(18) C12 0.058(3) 0.040(3) 0.055(3) -0.007(2) -0.010(2) -0.012(2) C13 0.073(4) 0.026(2) 0.063(3) -0.001(2) -0.015(3) -0.006(2) C14 0.078(4) 0.058(4) 0.073(4) 0.002(3) -0.020(3) -0.017(3) C15 0.111(6) 0.061(4) 0.070(5) 0.021(3) -0.043(4) -0.028(4) C16 0.113(6) 0.068(4) 0.055(4) 0.013(3) -0.036(4) -0.036(4) C17 0.106(6) 0.093(5) 0.050(4) 0.004(4) -0.014(4) -0.025(4) C18 0.079(4) 0.078(5) 0.049(3) 0.001(3) -0.010(3) -0.008(4) N19 0.0384(19) 0.0280(18) 0.0331(19) 0.0041(15) 0.0091(15) 0.0058(15) C20 0.040(2) 0.034(2) 0.027(2) -0.0002(18) 0.0051(18) 0.0031(19) C21 0.080(4) 0.045(3) 0.031(3) 0.002(2) 0.009(2) -0.001(3) C22 0.101(5) 0.052(3) 0.033(3) 0.014(2) 0.009(3) 0.001(3) C23 0.079(4) 0.035(3) 0.043(3) 0.012(2) 0.017(3) 0.004(3) C24 0.050(3) 0.030(2) 0.037(2) 0.0017(19) 0.009(2) 0.004(2) N25 0.0290(17) 0.0274(17) 0.0233(16) -0.0014(13) 0.0019(13) 0.0023(14) C26 0.033(2) 0.033(2) 0.0243(19) -0.0018(17) 0.0031(16) 0.0045(17) C27 0.052(3) 0.040(3) 0.027(2) -0.0058(19) 0.0005(19) 0.003(2) C28 0.059(3) 0.031(2) 0.038(3) -0.0100(19) -0.003(2) -0.003(2) C29 0.046(3) 0.027(2) 0.043(3) 0.0014(19) -0.001(2) -0.0017(19) C30 0.043(2) 0.031(2) 0.027(2) 0.0031(17) 0.0006(17) -0.0016(18) N31 0.045(2) 0.0240(18) 0.0268(18) -0.0030(13) -0.0036(15) 0.0029(15) C32 0.054(3) 0.038(3) 0.025(2) -0.0027(18) -0.001(2) 0.008(2) C33 0.079(4) 0.054(3) 0.021(2) 0.002(2) -0.001(2) 0.010(3) C34 0.076(4) 0.045(3) 0.035(3) 0.005(2) -0.015(3) 0.007(3) C35 0.055(3) 0.035(3) 0.043(3) 0.000(2) -0.015(2) 0.004(2) C36 0.042(2) 0.023(2) 0.041(2) -0.0040(18) -0.0092(19) 0.0007(18) N37 0.0354(19) 0.0245(18) 0.043(2) -0.0035(15) 0.0015(16) -0.0025(15) C38 0.034(2) 0.025(2) 0.051(3) -0.0031(19) -0.004(2) 0.0006(18) C39 0.039(3) 0.040(3) 0.082(4) 0.002(3) -0.005(3) 0.010(2) C40 0.035(3) 0.059(4) 0.104(5) 0.002(3) 0.017(3) 0.008(3) C41 0.041(3) 0.062(4) 0.085(5) -0.004(3) 0.020(3) 0.000(3) C42 0.041(3) 0.043(3) 0.055(3) 0.001(2) 0.009(2) -0.003(2) P10 0.0454(7) 0.0292(6) 0.0318(6) 0.0013(5) 0.0012(5) -0.0034(5) F11 0.0618(19) 0.0426(17) 0.0605(19) 0.0129(14) 0.0004(15) 0.0095(14) F12 0.099(2) 0.0429(17) 0.0368(15) -0.0041(13) 0.0122(15) -0.0064(16) F13 0.0520(16) 0.0404(15) 0.0459(16) 0.0105(12) -0.0009(12) -0.0116(13) F14 0.0490(17) 0.058(2) 0.075(2) 0.0081(17) -0.0043(15) 0.0078(15) F15 0.090(2) 0.0488(17) 0.0355(15) -0.0067(14) 0.0020(15) -0.0095(17) F16 0.070(2) 0.0462(18) 0.067(2) 0.0032(15) 0.0156(17) -0.0204(15) P20 0.0826(11) 0.0624(10) 0.0369(7) 0.0140(7) 0.0073(7) 0.0106(8) F21 0.137(4) 0.183(6) 0.095(3) 0.061(4) 0.075(3) 0.073(4) F22 0.165(5) 0.114(4) 0.079(3) -0.053(3) 0.032(3) -0.020(3) F23 0.139(4) 0.087(3) 0.088(3) 0.046(2) 0.066(3) 0.062(3) F24 0.095(3) 0.065(2) 0.060(2) -0.0007(17) 0.0006(18) 0.031(2) F25 0.107(4) 0.170(5) 0.091(3) 0.013(4) -0.019(3) -0.027(4) F26 0.152(5) 0.124(4) 0.096(3) 0.069(3) 0.014(3) 0.004(4) C70 0.107(10) 0.083(9) 0.167(13) 0.010(10) -0.006(10) 0.033(9) C71 0.107(8) 0.084(7) 0.157(11) 0.025(8) 0.009(8) 0.008(7) C72 0.073(8) 0.061(7) 0.148(12) 0.023(8) 0.022(8) 0.012(6) O73 0.141(10) 0.127(9) 0.165(12) 0.038(9) 0.017(9) -0.014(8) C80 0.103(9) 0.125(11) 0.171(13) 0.019(11) 0.083(9) 0.013(9) C81 0.098(7) 0.110(9) 0.161(12) 0.016(8) 0.075(8) 0.037(7) C82 0.088(8) 0.113(11) 0.161(13) 0.021(10) 0.071(9) 0.025(8) O83 0.142(9) 0.117(10) 0.212(13) 0.014(9) 0.059(10) 0.034(8) O100 0.166(12) 0.151(12) 0.113(9) 0.032(9) 0.042(9) 0.137(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.038(3) . ? Ru1 N37 2.044(4) . ? Ru1 N25 2.054(3) . ? Ru1 N31 2.056(4) . ? Ru1 N19 2.062(4) . ? Ru1 N6 2.084(3) . ? N1 C5 1.333(6) . ? N1 N2 1.353(5) . ? N1 C12 1.473(6) . ? N2 N3 1.331(5) . ? N3 C4 1.361(5) . ? C4 C5 1.374(6) . ? C4 C7 1.448(6) . ? C5 H5A 0.9500 . ? N6 C11 1.349(5) . ? N6 C7 1.363(5) . ? C7 C8 1.389(6) . ? C8 C9 1.378(7) . ? C8 H8A 0.9500 . ? C9 C10 1.380(7) . ? C9 H9A 0.9500 . ? C10 C11 1.374(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.546(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.352(9) . ? C13 C18 1.370(9) . ? C14 C15 1.363(9) . ? C14 H14A 0.9500 . ? C15 C16 1.368(12) . ? C15 H15A 0.9500 . ? C16 C17 1.359(11) . ? C16 H16A 0.9500 . ? C17 C18 1.404(8) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? N19 C24 1.343(6) . ? N19 C20 1.359(6) . ? C20 C21 1.369(7) . ? C20 C26 1.477(6) . ? C21 C22 1.382(7) . ? C21 H21A 0.9500 . ? C22 C23 1.379(8) . ? C22 H22A 0.9500 . ? C23 C24 1.371(7) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? N25 C30 1.335(5) . ? N25 C26 1.360(5) . ? C26 C27 1.380(6) . ? C27 C28 1.370(7) . ? C27 H27A 0.9500 . ? C28 C29 1.387(7) . ? C28 H28A 0.9500 . ? C29 C30 1.386(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? N31 C32 1.329(6) . ? N31 C36 1.367(6) . ? C32 C33 1.392(6) . ? C32 H32A 0.9500 . ? C33 C34 1.391(8) . ? C33 H33A 0.9500 . ? C34 C35 1.359(8) . ? C34 H34A 0.9500 . ? C35 C36 1.388(7) . ? C35 H35A 0.9500 . ? C36 C38 1.457(7) . ? N37 C42 1.352(7) . ? N37 C38 1.356(6) . ? C38 C39 1.403(7) . ? C39 C40 1.375(9) . ? C39 H39A 0.9500 . ? C40 C41 1.368(9) . ? C40 H40A 0.9500 . ? C41 C42 1.386(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? P10 F13 1.589(3) . ? P10 F15 1.591(3) . ? P10 F11 1.596(3) . ? P10 F14 1.599(3) . ? P10 F16 1.601(3) . ? P10 F12 1.606(3) . ? P20 F21 1.562(5) . ? P20 F26 1.567(4) . ? P20 F23 1.578(4) . ? P20 F22 1.579(5) . ? P20 F25 1.584(5) . ? P20 F24 1.605(4) . ? C70 C71 1.22(2) . ? C70 C72 1.44(3) 3_565 ? C70 H70A 0.9601 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 O73 1.217(16) . ? C71 C72 1.33(2) . ? C72 C70 1.44(3) 3_565 ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C80 C81 1.22(2) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 O83 1.219(17) . ? C81 C82 1.32(2) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? O100 H80C 1.0979 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 N37 97.35(14) . . ? N3 Ru1 N25 173.27(13) . . ? N37 Ru1 N25 88.23(13) . . ? N3 Ru1 N31 89.48(13) . . ? N37 Ru1 N31 78.78(15) . . ? N25 Ru1 N31 95.32(13) . . ? N3 Ru1 N19 96.37(14) . . ? N37 Ru1 N19 96.01(15) . . ? N25 Ru1 N19 79.24(14) . . ? N31 Ru1 N19 172.66(14) . . ? N3 Ru1 N6 78.48(13) . . ? N37 Ru1 N6 175.36(13) . . ? N25 Ru1 N6 96.07(13) . . ? N31 Ru1 N6 99.02(14) . . ? N19 Ru1 N6 86.54(13) . . ? C5 N1 N2 112.7(4) . . ? C5 N1 C12 128.4(4) . . ? N2 N1 C12 118.9(4) . . ? N3 N2 N1 104.7(4) . . ? N2 N3 C4 110.3(3) . . ? N2 N3 Ru1 134.3(3) . . ? C4 N3 Ru1 115.4(3) . . ? N3 C4 C5 107.5(4) . . ? N3 C4 C7 116.9(4) . . ? C5 C4 C7 135.5(4) . . ? N1 C5 C4 104.9(4) . . ? N1 C5 H5A 127.6 . . ? C4 C5 H5A 127.6 . . ? C11 N6 C7 117.8(4) . . ? C11 N6 Ru1 126.3(3) . . ? C7 N6 Ru1 115.6(3) . . ? N6 C7 C8 121.8(4) . . ? N6 C7 C4 113.5(4) . . ? C8 C7 C4 124.7(4) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 118.8(4) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? N6 C11 C10 122.5(4) . . ? N6 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? N1 C12 C13 112.2(4) . . ? N1 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N1 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C18 119.8(6) . . ? C14 C13 C12 119.0(6) . . ? C18 C13 C12 121.1(5) . . ? C13 C14 C15 120.8(8) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C14 C15 C16 120.9(8) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C17 C16 C15 118.9(6) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C13 C18 C17 119.1(7) . . ? C13 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C24 N19 C20 117.6(4) . . ? C24 N19 Ru1 127.1(3) . . ? C20 N19 Ru1 115.3(3) . . ? N19 C20 C21 121.4(4) . . ? N19 C20 C26 114.9(4) . . ? C21 C20 C26 123.6(4) . . ? C20 C21 C22 120.2(5) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 118.6(5) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? N19 C24 C23 123.5(5) . . ? N19 C24 H24A 118.3 . . ? C23 C24 H24A 118.3 . . ? C30 N25 C26 118.4(4) . . ? C30 N25 Ru1 126.2(3) . . ? C26 N25 Ru1 115.4(3) . . ? N25 C26 C27 121.4(4) . . ? N25 C26 C20 115.0(4) . . ? C27 C26 C20 123.6(4) . . ? C28 C27 C26 119.9(4) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C30 C29 C28 118.4(4) . . ? C30 C29 H29A 120.8 . . ? C28 C29 H29A 120.8 . . ? N25 C30 C29 122.8(4) . . ? N25 C30 H30A 118.6 . . ? C29 C30 H30A 118.6 . . ? C32 N31 C36 119.1(4) . . ? C32 N31 Ru1 125.9(3) . . ? C36 N31 Ru1 115.0(3) . . ? N31 C32 C33 122.8(5) . . ? N31 C32 H32A 118.6 . . ? C33 C32 H32A 118.6 . . ? C34 C33 C32 117.7(5) . . ? C34 C33 H33A 121.2 . . ? C32 C33 H33A 121.2 . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 119.9(5) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? N31 C36 C35 120.5(5) . . ? N31 C36 C38 115.3(4) . . ? C35 C36 C38 124.2(4) . . ? C42 N37 C38 118.6(4) . . ? C42 N37 Ru1 124.9(3) . . ? C38 N37 Ru1 116.4(3) . . ? N37 C38 C39 120.2(5) . . ? N37 C38 C36 114.4(4) . . ? C39 C38 C36 125.5(5) . . ? C40 C39 C38 120.1(5) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C41 C40 C39 119.7(5) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C40 C41 C42 118.4(6) . . ? C40 C41 H41A 120.8 . . ? C42 C41 H41A 120.8 . . ? N37 C42 C41 123.0(5) . . ? N37 C42 H42A 118.5 . . ? C41 C42 H42A 118.5 . . ? F13 P10 F15 90.26(17) . . ? F13 P10 F11 90.47(17) . . ? F15 P10 F11 90.67(19) . . ? F13 P10 F14 89.12(17) . . ? F15 P10 F14 90.22(19) . . ? F11 P10 F14 179.0(2) . . ? F13 P10 F16 179.5(2) . . ? F15 P10 F16 90.11(19) . . ? F11 P10 F16 89.91(18) . . ? F14 P10 F16 90.50(19) . . ? F13 P10 F12 90.32(17) . . ? F15 P10 F12 179.2(2) . . ? F11 P10 F12 89.83(18) . . ? F14 P10 F12 89.28(19) . . ? F16 P10 F12 89.31(18) . . ? F21 P20 F26 91.6(3) . . ? F21 P20 F23 91.1(2) . . ? F26 P20 F23 176.4(3) . . ? F21 P20 F22 93.1(3) . . ? F26 P20 F22 89.9(3) . . ? F23 P20 F22 92.3(3) . . ? F21 P20 F25 93.2(4) . . ? F26 P20 F25 90.0(3) . . ? F23 P20 F25 87.5(3) . . ? F22 P20 F25 173.6(3) . . ? F21 P20 F24 178.3(3) . . ? F26 P20 F24 89.7(3) . . ? F23 P20 F24 87.7(2) . . ? F22 P20 F24 85.7(3) . . ? F25 P20 F24 87.9(3) . . ? C71 C70 C72 118(2) . 3_565 ? C71 C70 H70A 110.9 . . ? C72 C70 H70A 130.5 3_565 . ? C71 C70 H70B 108.0 . . ? C72 C70 H70B 49.2 3_565 . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.6 . . ? C72 C70 H70C 60.6 3_565 . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O73 C71 C70 130(2) . . ? O73 C71 C72 117.3(19) . . ? C70 C71 C72 112.1(18) . . ? C71 C72 C70 129.0(17) . 3_565 ? C71 C72 H72A 114.1 . . ? C70 C72 H72A 116.3 3_565 . ? C71 C72 H72B 108.4 . . ? C70 C72 H72B 60.9 3_565 . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 105.8 . . ? C70 C72 H72C 49.5 3_565 . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C81 C80 H80A 109.4 . . ? C81 C80 H80B 109.3 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.7 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O83 C81 C80 131(2) . . ? O83 C81 C82 117.8(18) . . ? C80 C81 C82 109.6(19) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.3 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.6 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.515 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.237