Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2001 data_ncf79m _database_code_CSD 166368 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Fletcher, Nicholas' 'Nieuwenhuyzen, Mark' 'Rainey, Sharon' _publ_contact_author_name 'Dr Nicholas Fletcher' _publ_contact_author_address ; School of Chemistry Queen's University of Belfast David Keir Building Belfast BT9 5AG NORTHERN IRELAND ; _publ_contact_author_email 'N.FLETCHER@QUB.AC.UK' _publ_section_title ; The Isolation and Purification of Tris-2,2'-Bipyridine Complexes of Ruthenium(II) Containing Unsymmetrical Ligands ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H30 F12 N6 P2 Ru' _chemical_formula_weight 901.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5990(15) _cell_length_b 13.5789(18) _cell_length_c 13.3087(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.815(3) _cell_angle_gamma 90.00 _cell_volume 1842.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14232 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.48 _reflns_number_total 8088 _reflns_number_gt 6728 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 8088 _refine_ls_number_parameters 501 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 0.10199(3) 0.85010(3) 0.22925(2) 0.02853(10) Uani 1 1 d . . . N1A N -0.0021(4) 0.8329(4) 0.0756(3) 0.0361(12) Uani 1 1 d . E . C2A C 0.0339(6) 0.7793(4) 0.0029(4) 0.0405(12) Uani 1 1 d . . . H2A H 0.1120 0.7414 0.0242 0.049 Uiso 1 1 calc R A 1 C4A C -0.1528(6) 0.8295(5) -0.1297(5) 0.060(2) Uani 1 1 d . . . H4A H -0.2040 0.8293 -0.2004 0.072 Uiso 1 1 calc R B 1 C5A C -0.1935(6) 0.8817(4) -0.0577(5) 0.0499(16) Uani 1 1 d . E . H5A H -0.2742 0.9165 -0.0778 0.060 Uiso 1 1 calc R . . C6A C -0.1181(5) 0.8846(4) 0.0453(5) 0.0406(13) Uani 1 1 d . . . C7A C -0.1512(5) 0.9402(4) 0.1290(5) 0.0434(13) Uani 1 1 d . E . C8A C -0.2609(6) 0.9999(5) 0.1150(6) 0.0573(17) Uani 1 1 d . . . H8A H -0.3200 1.0076 0.0476 0.069 Uiso 1 1 calc R E . C9A C -0.2834(7) 1.0483(6) 0.2000(8) 0.073(2) Uani 1 1 d . E . H9A H -0.3600 1.0874 0.1910 0.088 Uiso 1 1 calc R C 1 C11A C -0.0883(7) 0.9812(6) 0.3048(7) 0.0493(17) Uani 1 1 d . . . H11A H -0.0269 0.9756 0.3715 0.059 Uiso 1 1 calc R D 1 N12A N -0.0639(4) 0.9314(3) 0.2248(4) 0.0380(10) Uani 1 1 d . E . C13A C -0.2230(15) 1.0916(9) 0.3813(11) 0.080(4) Uani 0.636(11) 1 d P E 2 H13A H -0.2450 1.1603 0.3615 0.120 Uiso 0.636(11) 1 calc PR E 2 H13B H -0.1449 1.0894 0.4412 0.120 Uiso 0.636(11) 1 calc PR E 2 H13C H -0.2967 1.0604 0.4003 0.120 Uiso 0.636(11) 1 calc PR E 2 C3A C -0.0364(7) 0.7764(5) -0.1007(5) 0.0518(18) Uani 0.636(11) 1 d P E 2 H3A H -0.0065 0.7396 -0.1503 0.062 Uiso 0.636(11) 1 calc PR E 2 C10A C -0.1975(8) 1.0404(5) 0.2959(7) 0.067(2) Uani 0.636(11) 1 d P E 2 C3' C -0.0364(7) 0.7764(5) -0.1007(5) 0.0518(18) Uani 0.36 1 d P E 1 C13' C 0.0011(13) 0.7177(11) -0.1758(10) 0.035(4) Uani 0.364(11) 1 d P E 1 H13D' H 0.0966 0.7201 -0.1630 0.053 Uiso 0.364(11) 1 calc PR E 1 H13E' H -0.0409 0.7430 -0.2460 0.053 Uiso 0.364(11) 1 calc PR E 1 H13F' H -0.0264 0.6495 -0.1704 0.053 Uiso 0.364(11) 1 calc PR E 1 C10' C -0.1975(8) 1.0404(5) 0.2959(7) 0.067(2) Uani 0.36 1 d P E 1 H10' H -0.2115 1.0740 0.3545 0.081 Uiso 0.364(11) 1 calc PR E 1 N1B N 0.2027(4) 0.8873(3) 0.3787(3) 0.0332(9) Uani 1 1 d . . . C2B C 0.2003(6) 0.8384(6) 0.4653(4) 0.0457(14) Uani 1 1 d . . . H2B H 0.1476 0.7809 0.4588 0.055 Uiso 1 1 calc R . . C3B C 0.2718(7) 0.8682(6) 0.5646(4) 0.062(2) Uani 1 1 d . . . H3B H 0.2670 0.8323 0.6247 0.074 Uiso 1 1 calc R . . C4B C 0.3489(8) 0.9499(5) 0.5737(5) 0.0609(18) Uani 1 1 d . . . H4B H 0.3989 0.9718 0.6405 0.073 Uiso 1 1 calc R . . C5B C 0.3534(6) 1.0011(5) 0.4838(5) 0.0538(15) Uani 1 1 d . . . H5B H 0.4070 1.0580 0.4890 0.065 Uiso 1 1 calc R . . C6B C 0.2809(5) 0.9693(4) 0.3888(4) 0.0371(11) Uani 1 1 d . . . C7B C 0.2783(5) 1.0164(4) 0.2889(4) 0.0331(11) Uani 1 1 d . . . C8B C 0.3552(6) 1.0974(5) 0.2808(5) 0.0437(16) Uani 1 1 d . . . H8B H 0.4090 1.1280 0.3418 0.052 Uiso 1 1 calc R . . C9B C 0.3523(6) 1.1328(4) 0.1828(6) 0.0480(15) Uani 1 1 d . . . H9B H 0.4078 1.1861 0.1765 0.058 Uiso 1 1 calc R . . C10B C 0.2696(6) 1.0919(4) 0.0935(5) 0.0409(13) Uani 1 1 d . . . C11B C 0.1923(5) 1.0127(4) 0.1082(4) 0.0364(11) Uani 1 1 d . . . H11B H 0.1342 0.9834 0.0485 0.044 Uiso 1 1 calc R . . N12B N 0.1963(4) 0.9762(3) 0.2032(3) 0.0299(9) Uani 1 1 d . . . C13B C 0.2626(7) 1.1280(5) -0.0138(5) 0.0541(16) Uani 1 1 d . . . H13D H 0.3031 1.1933 -0.0094 0.081 Uiso 1 1 calc R . . H13E H 0.1707 1.1322 -0.0547 0.081 Uiso 1 1 calc R . . H13F H 0.3095 1.0821 -0.0477 0.081 Uiso 1 1 calc R . . N1C N 0.0360(4) 0.7161(3) 0.2701(3) 0.0365(10) Uani 1 1 d . . . C2C C -0.0728(7) 0.7018(5) 0.3010(6) 0.0441(16) Uani 1 1 d . . . H2C H -0.1266 0.7569 0.3048 0.053 Uiso 1 1 calc R . . C3C C -0.1097(7) 0.6098(5) 0.3275(6) 0.0529(16) Uani 1 1 d . . . H3C H -0.1888 0.6018 0.3471 0.063 Uiso 1 1 calc R . . C4C C -0.0313(7) 0.5307(5) 0.3251(6) 0.0586(17) Uani 1 1 d . . . H4C H -0.0554 0.4668 0.3424 0.070 Uiso 1 1 calc R . . C5C C 0.0844(7) 0.5450(4) 0.2969(6) 0.0553(16) Uani 1 1 d . . . H5C H 0.1412 0.4911 0.2962 0.066 Uiso 1 1 calc R . . C6C C 0.1161(5) 0.6380(4) 0.2699(4) 0.0394(12) Uani 1 1 d . . . C7C C 0.2396(6) 0.6619(4) 0.2440(4) 0.0375(12) Uani 1 1 d . . . C8C C 0.3362(7) 0.5952(5) 0.2405(5) 0.0473(17) Uani 1 1 d . . . H8C H 0.3246 0.5274 0.2529 0.057 Uiso 1 1 calc R . . C9C C 0.4496(7) 0.6268(5) 0.2190(5) 0.0539(16) Uani 1 1 d . . . H9C H 0.5153 0.5804 0.2154 0.065 Uiso 1 1 calc R . . C10C C 0.4683(5) 0.7236(5) 0.2029(4) 0.0405(13) Uani 1 1 d . . . C11C C 0.3660(5) 0.7880(4) 0.2040(4) 0.0371(12) Uani 1 1 d . . . H11C H 0.3762 0.8558 0.1901 0.044 Uiso 1 1 calc R . . N12C N 0.2546(4) 0.7593(3) 0.2236(3) 0.0298(9) Uani 1 1 d . . . C13C C 0.5925(6) 0.7647(6) 0.1854(5) 0.0553(17) Uani 1 1 d . . . H13G H 0.6517 0.7104 0.1807 0.083 Uiso 1 1 calc R . . H13H H 0.6352 0.8078 0.2438 0.083 Uiso 1 1 calc R . . H13I H 0.5714 0.8025 0.1202 0.083 Uiso 1 1 calc R . . P1 P 0.37454(14) 0.85668(16) 0.88273(10) 0.0463(3) Uani 1 1 d . . . F11 F 0.4661(7) 0.9257(5) 0.9640(5) 0.128(3) Uani 1 1 d . . . F12 F 0.4731(6) 0.8477(8) 0.8116(5) 0.149(3) Uani 1 1 d . . . F13 F 0.3182(5) 0.9511(4) 0.8141(4) 0.0779(13) Uani 1 1 d . . . F14 F 0.2807(9) 0.7923(4) 0.7972(4) 0.135(3) Uani 1 1 d . . . F15 F 0.2766(7) 0.8700(6) 0.9466(5) 0.130(3) Uani 1 1 d . . . F16 F 0.4361(14) 0.7659(5) 0.9399(5) 0.223(7) Uani 1 1 d . . . P2 P 0.6886(2) 0.81965(14) 0.51238(14) 0.0611(5) Uani 1 1 d . . . F21 F 0.5616(6) 0.7630(4) 0.5187(5) 0.1078(18) Uani 1 1 d . . . F22 F 0.7069(6) 0.7392(5) 0.4312(5) 0.114(2) Uani 1 1 d . . . F23 F 0.6006(6) 0.8842(4) 0.4220(4) 0.111(2) Uani 1 1 d . . . F24 F 0.6682(6) 0.8952(6) 0.5957(5) 0.135(3) Uani 1 1 d . . . F25 F 0.8168(6) 0.8696(6) 0.5042(6) 0.135(3) Uani 1 1 d . . . F26 F 0.7720(6) 0.7523(6) 0.6028(5) 0.130(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03085(17) 0.02584(16) 0.02816(17) 0.0022(2) 0.00679(11) 0.0017(2) N1A 0.036(2) 0.039(3) 0.0309(19) 0.0072(19) 0.0049(16) -0.0100(19) C2A 0.045(3) 0.034(3) 0.039(3) 0.002(2) 0.005(2) -0.005(2) C4A 0.060(3) 0.062(5) 0.039(3) 0.020(3) -0.017(3) -0.027(3) C5A 0.038(3) 0.043(3) 0.057(4) 0.015(3) -0.007(3) -0.009(2) C6A 0.036(3) 0.031(2) 0.049(3) 0.016(2) 0.002(2) -0.004(2) C7A 0.034(3) 0.040(3) 0.057(4) 0.017(3) 0.014(2) 0.002(2) C8A 0.042(3) 0.053(4) 0.073(5) 0.021(3) 0.008(3) 0.008(3) C9A 0.049(4) 0.062(5) 0.114(7) 0.019(5) 0.033(5) 0.021(3) C11A 0.047(4) 0.045(4) 0.062(4) 0.007(3) 0.025(3) 0.009(3) N12A 0.038(2) 0.031(2) 0.047(3) 0.004(2) 0.015(2) 0.0022(19) C13A 0.115(11) 0.053(7) 0.090(10) 0.016(6) 0.056(9) 0.033(7) C3A 0.066(4) 0.046(4) 0.040(3) 0.004(3) 0.009(3) -0.020(3) C10A 0.070(5) 0.052(4) 0.095(6) 0.012(4) 0.049(5) 0.021(4) C3' 0.066(4) 0.046(4) 0.040(3) 0.004(3) 0.009(3) -0.020(3) C13' 0.030(7) 0.045(9) 0.026(7) -0.003(6) -0.001(5) -0.017(6) C10' 0.070(5) 0.052(4) 0.095(6) 0.012(4) 0.049(5) 0.021(4) N1B 0.034(2) 0.034(2) 0.031(2) -0.0053(17) 0.0084(17) 0.0034(16) C2B 0.067(3) 0.041(4) 0.028(2) 0.001(3) 0.011(2) -0.005(3) C3B 0.085(4) 0.066(6) 0.027(3) 0.004(3) 0.003(3) 0.007(4) C4B 0.083(5) 0.053(4) 0.037(3) -0.010(3) 0.000(3) 0.003(4) C5B 0.055(4) 0.058(4) 0.043(3) -0.005(3) 0.006(3) -0.011(3) C6B 0.039(3) 0.036(3) 0.037(3) -0.002(2) 0.011(2) 0.005(2) C7B 0.033(3) 0.031(3) 0.036(3) -0.006(2) 0.011(2) 0.002(2) C8B 0.040(3) 0.040(3) 0.054(4) -0.013(3) 0.016(3) -0.004(3) C9B 0.044(3) 0.027(3) 0.081(5) 0.000(3) 0.030(3) -0.006(2) C10B 0.046(3) 0.027(3) 0.057(4) 0.006(2) 0.026(3) 0.003(2) C11B 0.048(3) 0.029(3) 0.036(3) 0.003(2) 0.016(2) 0.006(2) N12B 0.034(2) 0.025(2) 0.033(2) 0.0035(18) 0.0132(18) 0.0067(17) C13B 0.076(4) 0.039(3) 0.059(4) 0.004(3) 0.038(3) 0.002(3) N1C 0.038(2) 0.034(2) 0.032(2) 0.0017(19) 0.0011(18) -0.0023(18) C2C 0.043(3) 0.043(4) 0.044(3) 0.009(3) 0.008(3) -0.003(3) C3C 0.052(4) 0.049(4) 0.062(4) 0.008(3) 0.023(3) -0.008(3) C4C 0.060(4) 0.048(4) 0.063(4) 0.015(3) 0.009(3) -0.014(3) C5C 0.062(4) 0.029(3) 0.068(4) 0.006(3) 0.008(3) 0.006(3) C6C 0.042(3) 0.033(3) 0.037(3) 0.003(2) 0.000(2) 0.000(2) C7C 0.049(3) 0.032(3) 0.028(3) 0.001(2) 0.004(2) 0.007(2) C8C 0.063(5) 0.032(3) 0.049(4) 0.006(3) 0.020(3) 0.015(3) C9C 0.058(4) 0.051(4) 0.053(4) 0.006(3) 0.017(3) 0.027(3) C10C 0.034(3) 0.055(4) 0.030(3) -0.002(2) 0.005(2) 0.013(2) C11C 0.035(3) 0.045(3) 0.030(3) -0.002(2) 0.007(2) 0.007(2) N12C 0.037(2) 0.027(2) 0.022(2) -0.0015(16) 0.0016(17) 0.0024(18) C13C 0.036(3) 0.091(5) 0.040(3) 0.001(3) 0.012(2) 0.015(3) P1 0.0563(7) 0.0410(8) 0.0392(6) -0.0051(9) 0.0093(5) 0.0049(10) F11 0.140(5) 0.111(5) 0.083(4) -0.011(4) -0.057(4) -0.033(4) F12 0.132(5) 0.223(8) 0.104(4) 0.007(6) 0.050(4) 0.108(6) F13 0.105(3) 0.067(3) 0.060(3) 0.019(2) 0.020(2) 0.011(3) F14 0.240(8) 0.071(4) 0.058(3) -0.001(3) -0.020(4) -0.057(4) F15 0.170(5) 0.131(6) 0.136(5) -0.023(4) 0.121(5) -0.028(5) F16 0.475(18) 0.093(5) 0.051(3) 0.002(3) -0.012(6) 0.139(8) P2 0.0787(12) 0.0632(12) 0.0433(9) -0.0035(7) 0.0198(8) -0.0096(8) F21 0.109(4) 0.097(4) 0.119(5) -0.001(3) 0.033(4) -0.031(3) F22 0.121(4) 0.110(5) 0.110(5) -0.038(4) 0.027(4) 0.018(4) F23 0.153(5) 0.095(4) 0.077(3) 0.017(3) 0.018(3) 0.033(4) F24 0.112(4) 0.171(7) 0.126(5) -0.100(5) 0.039(4) -0.035(4) F25 0.108(4) 0.109(6) 0.215(7) 0.019(5) 0.089(5) -0.020(4) F26 0.104(4) 0.197(7) 0.082(4) 0.062(4) 0.011(3) -0.004(5) _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 N1B 2.048(4) . ? Ru1 N12C 2.052(4) . ? Ru1 N1A 2.055(4) . ? Ru1 N12B 2.059(4) . ? Ru1 N12A 2.063(4) . ? Ru1 N1C 2.074(5) . ? N1A C2A 1.346(7) . ? N1A C6A 1.378(7) . ? C2A C3A 1.377(8) . ? C4A C5A 1.353(10) . ? C4A C3A 1.390(10) . ? C5A C6A 1.386(8) . ? C6A C7A 1.464(9) . ? C7A N12A 1.362(7) . ? C7A C8A 1.388(8) . ? C8A C9A 1.384(12) . ? C9A C10A 1.355(12) . ? C11A N12A 1.344(9) . ? C11A C10A 1.388(10) . ? C13A C10A 1.420(14) . ? N1B C2B 1.336(7) . ? N1B C6B 1.373(7) . ? C2B C3B 1.392(8) . ? C3B C4B 1.364(11) . ? C4B C5B 1.396(10) . ? C5B C6B 1.359(8) . ? C6B C7B 1.469(8) . ? C7B N12B 1.347(7) . ? C7B C8B 1.391(9) . ? C8B C9B 1.383(9) . ? C9B C10B 1.385(9) . ? C10B C11B 1.398(8) . ? C10B C13B 1.492(9) . ? C11B N12B 1.349(7) . ? N1C C2C 1.340(8) . ? N1C C6C 1.359(7) . ? C2C C3C 1.384(9) . ? C3C C4C 1.363(10) . ? C4C C5C 1.391(10) . ? C5C C6C 1.379(8) . ? C6C C7C 1.478(8) . ? C7C N12C 1.368(7) . ? C7C C8C 1.377(9) . ? C8C C9C 1.379(10) . ? C9C C10C 1.354(9) . ? C10C C11C 1.397(7) . ? C10C C13C 1.504(8) . ? C11C N12C 1.335(7) . ? P1 F16 1.501(6) . ? P1 F15 1.521(5) . ? P1 F11 1.555(5) . ? P1 F14 1.560(6) . ? P1 F13 1.593(5) . ? P1 F12 1.594(5) . ? P2 F25 1.548(6) . ? P2 F24 1.568(6) . ? P2 F21 1.572(6) . ? P2 F23 1.572(6) . ? P2 F26 1.576(6) . ? P2 F22 1.585(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1B Ru1 N12C 88.66(16) . . ? N1B Ru1 N1A 172.24(18) . . ? N12C Ru1 N1A 96.31(17) . . ? N1B Ru1 N12B 79.03(17) . . ? N12C Ru1 N12B 93.98(19) . . ? N1A Ru1 N12B 94.64(17) . . ? N1B Ru1 N12A 96.33(18) . . ? N12C Ru1 N12A 174.15(19) . . ? N1A Ru1 N12A 79.06(19) . . ? N12B Ru1 N12A 89.98(16) . . ? N1B Ru1 N1C 94.90(17) . . ? N12C Ru1 N1C 78.94(18) . . ? N1A Ru1 N1C 91.91(18) . . ? N12B Ru1 N1C 170.86(17) . . ? N12A Ru1 N1C 97.53(18) . . ? C2A N1A C6A 118.1(5) . . ? C2A N1A Ru1 126.6(4) . . ? C6A N1A Ru1 115.3(4) . . ? N1A C2A C3A 123.5(6) . . ? C5A C4A C3A 120.3(6) . . ? C4A C5A C6A 120.4(6) . . ? N1A C6A C5A 120.2(6) . . ? N1A C6A C7A 114.8(5) . . ? C5A C6A C7A 125.0(5) . . ? N12A C7A C8A 120.5(6) . . ? N12A C7A C6A 115.1(5) . . ? C8A C7A C6A 124.4(6) . . ? C9A C8A C7A 119.5(7) . . ? C10A C9A C8A 120.7(6) . . ? N12A C11A C10A 124.0(8) . . ? C11A N12A C7A 118.0(5) . . ? C11A N12A Ru1 126.3(5) . . ? C7A N12A Ru1 115.5(4) . . ? C2A C3A C4A 117.5(6) . . ? C9A C10A C11A 117.2(8) . . ? C9A C10A C13A 119.4(8) . . ? C11A C10A C13A 123.4(10) . . ? C2B N1B C6B 118.1(5) . . ? C2B N1B Ru1 126.0(4) . . ? C6B N1B Ru1 115.9(3) . . ? N1B C2B C3B 122.8(6) . . ? C4B C3B C2B 118.6(6) . . ? C3B C4B C5B 119.3(6) . . ? C6B C5B C4B 119.7(6) . . ? C5B C6B N1B 121.5(5) . . ? C5B C6B C7B 124.7(5) . . ? N1B C6B C7B 113.8(5) . . ? N12B C7B C8B 120.8(5) . . ? N12B C7B C6B 116.0(5) . . ? C8B C7B C6B 123.2(5) . . ? C9B C8B C7B 119.0(6) . . ? C8B C9B C10B 121.1(5) . . ? C9B C10B C11B 116.5(6) . . ? C9B C10B C13B 122.9(6) . . ? C11B C10B C13B 120.5(6) . . ? N12B C11B C10B 123.0(5) . . ? C7B N12B C11B 119.5(5) . . ? C7B N12B Ru1 115.2(4) . . ? C11B N12B Ru1 124.8(4) . . ? C2C N1C C6C 118.5(5) . . ? C2C N1C Ru1 126.0(4) . . ? C6C N1C Ru1 115.4(4) . . ? N1C C2C C3C 122.4(6) . . ? C4C C3C C2C 119.2(6) . . ? C3C C4C C5C 119.0(6) . . ? C6C C5C C4C 119.5(6) . . ? N1C C6C C5C 121.2(5) . . ? N1C C6C C7C 115.0(5) . . ? C5C C6C C7C 123.8(5) . . ? N12C C7C C8C 120.1(6) . . ? N12C C7C C6C 114.7(5) . . ? C8C C7C C6C 125.3(6) . . ? C7C C8C C9C 120.0(6) . . ? C10C C9C C8C 120.6(6) . . ? C9C C10C C11C 117.3(5) . . ? C9C C10C C13C 123.8(5) . . ? C11C C10C C13C 119.0(6) . . ? N12C C11C C10C 123.4(5) . . ? C11C N12C C7C 118.6(5) . . ? C11C N12C Ru1 125.4(4) . . ? C7C N12C Ru1 116.0(4) . . ? F16 P1 F15 94.8(6) . . ? F16 P1 F11 92.3(5) . . ? F15 P1 F11 86.0(4) . . ? F16 P1 F14 90.7(5) . . ? F15 P1 F14 94.5(5) . . ? F11 P1 F14 176.9(4) . . ? F16 P1 F13 174.1(5) . . ? F15 P1 F13 91.1(4) . . ? F11 P1 F13 88.8(3) . . ? F14 P1 F13 88.1(3) . . ? F16 P1 F12 88.5(6) . . ? F15 P1 F12 176.7(4) . . ? F11 P1 F12 94.2(5) . . ? F14 P1 F12 85.1(5) . . ? F13 P1 F12 85.7(4) . . ? F25 P2 F24 93.2(4) . . ? F25 P2 F21 176.6(4) . . ? F24 P2 F21 89.8(3) . . ? F25 P2 F23 92.9(4) . . ? F24 P2 F23 90.5(4) . . ? F21 P2 F23 88.6(4) . . ? F25 P2 F26 89.3(4) . . ? F24 P2 F26 89.8(4) . . ? F21 P2 F26 89.2(3) . . ? F23 P2 F26 177.8(4) . . ? F25 P2 F22 89.0(4) . . ? F24 P2 F22 177.2(4) . . ? F21 P2 F22 88.0(4) . . ? F23 P2 F22 91.1(3) . . ? F26 P2 F22 88.5(4) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.993 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.100