Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'J. Vos' 'S. Brooker' 'Helmar Gorls' 'Declan Mulhern' 'Sven Rau' _publ_contact_author_name 'Johannes Vos' _publ_contact_author_address ; School of Chemical Sciences Dublin City University Dublin 9 REPUBLIC OF IRELAND ; _publ_contact_author_email HAN.VOS@DCU.IE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis of mononuclear and dinuclear ruthenium(II) tris(heteroleptic) complexes via photosubstitution in bis(carbonyl) precursors. ; data_2vosrr _database_code_depnum_ccdc_archive 'CCDC 272204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 F6 N9 O0.50 P Ru' _chemical_formula_weight 845.75 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 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 13.95240(10) _cell_length_b 12.24230(10) _cell_length_c 23.4412(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.9090(10) _cell_angle_gamma 90.00 _cell_volume 3982.70(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22545 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.38 _reflns_number_total 8079 _reflns_number_gt 4996 _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^)+(0.1062P)^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 8079 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Ru Ru 0.39023(3) 0.00075(3) 0.318726(15) 0.03340(15) Uani 1 1 d . . . N7 N 0.5106(3) 0.0950(3) 0.33747(15) 0.0347(9) Uani 1 1 d . . . N8 N 0.5496(3) 0.1540(3) 0.38328(16) 0.0364(9) Uani 1 1 d . . . C2 C 0.6350(4) 0.1861(4) 0.3672(2) 0.0368(11) Uani 1 1 d . . . N9 N 0.6545(3) 0.1516(3) 0.31490(16) 0.0399(10) Uani 1 1 d . . . C5 C 0.5736(4) 0.0945(4) 0.29840(19) 0.0356(11) Uani 1 1 d . . . C6 C 0.5477(4) 0.0354(4) 0.2454(2) 0.0352(11) Uani 1 1 d . . . C7 C 0.6040(4) 0.0321(4) 0.2006(2) 0.0411(12) Uani 1 1 d . . . H7 H 0.6649 0.0677 0.2034 0.049 Uiso 1 1 calc R . . C8 C 0.5703(4) -0.0242(4) 0.1509(2) 0.0466(13) Uani 1 1 d . . . H8 H 0.6066 -0.0257 0.1187 0.056 Uiso 1 1 calc R . . C9 C 0.4836(4) -0.0775(4) 0.1493(2) 0.0481(13) Uani 1 1 d . . . H9 H 0.4594 -0.1171 0.1161 0.058 Uiso 1 1 calc R . . C10 C 0.4315(4) -0.0732(4) 0.1965(2) 0.0436(12) Uani 1 1 d . . . H10 H 0.3716 -0.1106 0.1948 0.052 Uiso 1 1 calc R . . N5 N 0.4623(3) -0.0185(3) 0.24478(17) 0.0361(9) Uani 1 1 d . . . C16 C 0.7027(4) 0.2564(4) 0.4038(2) 0.0411(12) Uani 1 1 d . . . C17 C 0.7901(4) 0.2869(6) 0.3855(3) 0.0647(17) Uani 1 1 d . . . H17 H 0.8092 0.2590 0.3506 0.078 Uiso 1 1 calc R . . C18 C 0.8495(5) 0.3587(7) 0.4186(3) 0.090(2) Uani 1 1 d . . . H18 H 0.9096 0.3814 0.4069 0.108 Uiso 1 1 calc R . . C19 C 0.8185(5) 0.3958(6) 0.4689(3) 0.080(2) Uani 1 1 d . . . H19 H 0.8563 0.4461 0.4925 0.096 Uiso 1 1 calc R . . C20 C 0.7321(5) 0.3592(5) 0.4846(3) 0.0655(18) Uani 1 1 d . . . H20 H 0.7130 0.3831 0.5203 0.079 Uiso 1 1 calc R . . N71 N 0.6732(3) 0.2920(4) 0.45283(18) 0.0532(12) Uani 1 1 d . . . N3 N 0.2692(3) -0.0902(3) 0.29218(17) 0.0390(9) Uani 1 1 d . . . C26 C 0.1988(4) -0.0370(4) 0.2587(2) 0.0417(12) Uani 1 1 d . . . C27 C 0.1125(4) -0.0893(5) 0.2404(3) 0.0609(16) Uani 1 1 d . . . H27 H 0.0643 -0.0513 0.2166 0.073 Uiso 1 1 calc R . . C28 C 0.0964(5) -0.1946(5) 0.2562(3) 0.0650(17) Uani 1 1 d . . . H28 H 0.0373 -0.2300 0.2440 0.078 Uiso 1 1 calc R . . C29 C 0.1661(5) -0.2470(5) 0.2894(3) 0.0661(17) Uani 1 1 d . . . H29 H 0.1566 -0.3203 0.3007 0.079 Uiso 1 1 calc R . . C30 C 0.2522(4) -0.1938(4) 0.3071(3) 0.0547(15) Uani 1 1 d . . . H30 H 0.3006 -0.2322 0.3305 0.066 Uiso 1 1 calc R . . N4 N 0.3054(3) 0.1152(3) 0.27271(16) 0.0361(9) Uani 1 1 d . . . C36 C 0.2202(4) 0.0772(4) 0.2462(2) 0.0399(11) Uani 1 1 d . . . C37 C 0.1607(4) 0.1435(5) 0.2099(3) 0.0596(16) Uani 1 1 d . . . H37 H 0.1035 0.1147 0.1900 0.072 Uiso 1 1 calc R . . C38 C 0.1853(4) 0.2519(5) 0.2030(3) 0.0611(16) Uani 1 1 d . . . H38 H 0.1443 0.2990 0.1793 0.073 Uiso 1 1 calc R . . C39 C 0.2699(4) 0.2904(5) 0.2310(2) 0.0548(15) Uani 1 1 d . . . H39 H 0.2881 0.3644 0.2265 0.066 Uiso 1 1 calc R . . C40 C 0.3283(4) 0.2218(4) 0.2654(2) 0.0445(12) Uani 1 1 d . . . H40 H 0.3864 0.2497 0.2847 0.053 Uiso 1 1 calc R . . N1 N 0.4601(3) -0.1216(3) 0.36682(17) 0.0377(9) Uani 1 1 d . . . C46 C 0.4445(4) -0.1246(4) 0.4231(2) 0.0395(11) Uani 1 1 d . . . C47 C 0.4871(4) -0.2014(4) 0.4603(2) 0.0493(13) Uani 1 1 d . . . H47 H 0.4760 -0.2000 0.4996 0.059 Uiso 1 1 calc R . . C48 C 0.5466(4) -0.2815(4) 0.4402(3) 0.0531(14) Uani 1 1 d . . . C49 C 0.5612(4) -0.2777(5) 0.3832(3) 0.0560(15) Uani 1 1 d . . . H49 H 0.6014 -0.3304 0.3678 0.067 Uiso 1 1 calc R . . C50 C 0.5178(4) -0.1974(4) 0.3481(2) 0.0486(13) Uani 1 1 d . . . H50 H 0.5296 -0.1962 0.3089 0.058 Uiso 1 1 calc R . . C51 C 0.5949(5) -0.3646(6) 0.4814(3) 0.083(2) Uani 1 1 d . . . H51A H 0.5758 -0.4384 0.4685 0.100 Uiso 1 1 calc R . . H51B H 0.5751 -0.3522 0.5198 0.100 Uiso 1 1 calc R . . H51C H 0.6650 -0.3572 0.4826 0.100 Uiso 1 1 calc R . . N2 N 0.3403(3) 0.0269(3) 0.39701(17) 0.0356(9) Uani 1 1 d . . . C56 C 0.3776(4) -0.0392(4) 0.4404(2) 0.0372(11) Uani 1 1 d . . . C57 C 0.3533(4) -0.0264(4) 0.4950(2) 0.0468(13) Uani 1 1 d . . . H57 H 0.3809 -0.0736 0.5244 0.056 Uiso 1 1 calc R . . C58 C 0.2889(4) 0.0541(5) 0.5085(2) 0.0483(13) Uani 1 1 d . . . C59 C 0.2536(4) 0.1202(4) 0.4639(2) 0.0496(13) Uani 1 1 d . . . H59 H 0.2098 0.1770 0.4707 0.060 Uiso 1 1 calc R . . C60 C 0.2804(4) 0.1057(4) 0.4095(2) 0.0466(13) Uani 1 1 d . . . H60 H 0.2551 0.1536 0.3798 0.056 Uiso 1 1 calc R . . C61 C 0.2600(5) 0.0675(6) 0.5680(3) 0.075(2) Uani 1 1 d . . . H61A H 0.2398 0.1431 0.5735 0.090 Uiso 1 1 calc R . . H61B H 0.3149 0.0501 0.5961 0.090 Uiso 1 1 calc R . . H61C H 0.2064 0.0180 0.5734 0.090 Uiso 1 1 calc R . . P1 P 0.85779(12) 0.57283(14) 0.62981(7) 0.0563(4) Uani 1 1 d . . . F11 F 0.8521(5) 0.5425(5) 0.6943(2) 0.130(2) Uani 1 1 d . . . F12 F 0.7658(3) 0.6460(4) 0.6339(3) 0.1159(17) Uani 1 1 d . . . F13 F 0.7916(3) 0.4690(4) 0.6124(2) 0.0907(13) Uani 1 1 d . . . F14 F 0.9245(4) 0.6728(4) 0.6484(3) 0.1265(19) Uani 1 1 d . . . F15 F 0.8605(6) 0.6011(5) 0.5663(2) 0.160(3) Uani 1 1 d . . . F16 F 0.9499(4) 0.4988(4) 0.6289(4) 0.153(3) Uani 1 1 d . . . C80 C 0.0419(11) 0.2097(14) 0.0500(6) 0.090(5) Uani 0.50 1 d P . . H80A H 0.0318 0.1913 0.0092 0.108 Uiso 0.50 1 calc PR . . H80B H 0.0239 0.1472 0.0728 0.108 Uiso 0.50 1 calc PR . . H80C H 0.1100 0.2274 0.0605 0.108 Uiso 0.50 1 calc PR . . C81 C -0.0160(11) 0.3014(19) 0.0612(8) 0.102(6) Uani 0.50 1 d P . . H81A H -0.0356 0.3380 0.0242 0.122 Uiso 0.50 1 calc PR . . H81B H -0.0755 0.2738 0.0759 0.122 Uiso 0.50 1 calc PR . . O82 O 0.0228(6) 0.3785(8) 0.0986(4) 0.060(2) Uani 0.50 1 d P . . C83 C -0.0195(14) 0.469(2) 0.1084(9) 0.129(9) Uani 0.50 1 d P . . H83A H -0.0811 0.4499 0.1234 0.155 Uiso 0.50 1 calc PR . . H83B H -0.0363 0.5047 0.0708 0.155 Uiso 0.50 1 calc PR . . C84 C 0.0236(14) 0.5466(12) 0.1442(10) 0.118(8) Uani 0.50 1 d P . . H84A H 0.0413 0.5146 0.1821 0.142 Uiso 0.50 1 calc PR . . H84B H -0.0212 0.6074 0.1475 0.142 Uiso 0.50 1 calc PR . . H84C H 0.0816 0.5736 0.1285 0.142 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 Ru 0.0385(2) 0.0304(2) 0.0311(2) 0.00101(16) 0.00330(15) -0.00180(18) N7 0.041(2) 0.036(2) 0.026(2) 0.0007(16) 0.0019(17) -0.0028(18) N8 0.041(2) 0.034(2) 0.032(2) 0.0016(17) -0.0053(17) -0.0012(19) C2 0.046(3) 0.033(2) 0.030(3) 0.004(2) -0.004(2) 0.001(2) N9 0.043(2) 0.043(2) 0.034(2) -0.0020(18) 0.0022(18) -0.002(2) C5 0.045(3) 0.033(3) 0.029(2) -0.0013(19) 0.002(2) -0.006(2) C6 0.042(3) 0.034(2) 0.029(3) 0.0021(19) -0.001(2) -0.001(2) C7 0.044(3) 0.042(3) 0.038(3) -0.001(2) 0.004(2) -0.002(2) C8 0.060(3) 0.044(3) 0.038(3) -0.001(2) 0.015(3) 0.001(3) C9 0.060(3) 0.045(3) 0.039(3) -0.008(2) 0.001(2) -0.010(3) C10 0.050(3) 0.039(3) 0.041(3) -0.006(2) 0.001(2) -0.011(2) N5 0.042(2) 0.034(2) 0.031(2) 0.0003(16) 0.0013(17) -0.0014(18) C16 0.045(3) 0.041(3) 0.035(3) 0.000(2) -0.005(2) -0.002(2) C17 0.055(4) 0.083(5) 0.056(4) -0.018(3) 0.006(3) -0.020(3) C18 0.072(5) 0.114(7) 0.084(5) -0.022(5) 0.002(4) -0.043(5) C19 0.074(5) 0.086(5) 0.076(5) -0.025(4) -0.014(4) -0.027(4) C20 0.078(5) 0.069(4) 0.046(3) -0.018(3) -0.012(3) -0.004(4) N71 0.061(3) 0.059(3) 0.038(3) -0.008(2) -0.006(2) -0.007(3) N3 0.045(2) 0.032(2) 0.040(2) -0.0025(18) 0.0065(19) -0.0032(19) C26 0.045(3) 0.038(3) 0.042(3) -0.003(2) 0.005(2) -0.002(2) C27 0.051(3) 0.056(4) 0.073(4) 0.004(3) -0.011(3) -0.007(3) C28 0.056(4) 0.061(4) 0.075(4) 0.004(3) -0.007(3) -0.023(3) C29 0.069(4) 0.043(3) 0.088(5) 0.002(3) 0.012(4) -0.021(3) C30 0.055(4) 0.035(3) 0.073(4) 0.003(3) 0.004(3) -0.004(3) N4 0.046(2) 0.032(2) 0.031(2) 0.0013(16) 0.0030(18) 0.0000(19) C36 0.042(3) 0.039(3) 0.038(3) -0.001(2) -0.001(2) -0.001(2) C37 0.055(4) 0.060(4) 0.060(4) 0.009(3) -0.016(3) -0.003(3) C38 0.063(4) 0.058(4) 0.059(4) 0.016(3) -0.009(3) 0.015(3) C39 0.069(4) 0.040(3) 0.055(4) 0.008(3) 0.006(3) 0.000(3) C40 0.054(3) 0.041(3) 0.038(3) 0.003(2) 0.002(2) -0.003(3) N1 0.042(2) 0.031(2) 0.040(2) 0.0009(17) 0.0049(18) -0.0015(19) C46 0.040(3) 0.038(3) 0.041(3) 0.004(2) 0.005(2) -0.002(2) C47 0.054(3) 0.046(3) 0.046(3) 0.015(2) 0.002(3) 0.007(3) C48 0.054(3) 0.036(3) 0.069(4) 0.013(3) 0.001(3) 0.005(3) C49 0.060(4) 0.044(3) 0.066(4) 0.003(3) 0.016(3) 0.013(3) C50 0.052(3) 0.046(3) 0.048(3) 0.003(3) 0.007(3) 0.007(3) C51 0.092(5) 0.067(5) 0.089(5) 0.026(4) 0.003(4) 0.034(4) N2 0.036(2) 0.037(2) 0.034(2) 0.0017(16) 0.0066(17) 0.0020(17) C56 0.042(3) 0.035(2) 0.035(3) 0.005(2) 0.005(2) -0.001(2) C57 0.051(3) 0.051(3) 0.039(3) 0.008(2) 0.004(2) 0.004(3) C58 0.056(3) 0.049(3) 0.041(3) -0.001(3) 0.010(3) 0.004(3) C59 0.056(3) 0.046(3) 0.048(3) 0.003(2) 0.010(3) 0.010(3) C60 0.055(3) 0.041(3) 0.044(3) 0.005(2) 0.005(3) 0.009(3) C61 0.090(5) 0.085(5) 0.052(4) 0.007(4) 0.019(4) 0.018(4) P1 0.0534(9) 0.0558(9) 0.0587(10) -0.0052(8) 0.0016(7) -0.0045(8) F11 0.215(6) 0.111(4) 0.065(3) 0.000(3) 0.015(3) -0.004(4) F12 0.081(3) 0.078(3) 0.189(5) -0.003(3) 0.012(3) 0.014(3) F13 0.089(3) 0.073(3) 0.106(3) -0.014(2) -0.012(3) -0.021(2) F14 0.111(4) 0.079(3) 0.183(5) -0.026(3) -0.017(4) -0.039(3) F15 0.276(8) 0.140(5) 0.066(3) 0.005(3) 0.027(4) -0.042(5) F16 0.063(3) 0.116(5) 0.281(9) -0.046(4) 0.018(4) 0.018(3) C80 0.090(11) 0.114(13) 0.067(9) -0.023(9) 0.009(8) -0.064(11) C81 0.057(9) 0.157(18) 0.090(12) -0.002(12) -0.003(8) 0.018(11) O82 0.034(4) 0.062(5) 0.083(6) 0.020(5) -0.001(4) 0.006(4) C83 0.071(12) 0.20(3) 0.118(17) 0.087(17) 0.017(11) 0.032(15) C84 0.109(15) 0.038(8) 0.22(2) 0.016(11) 0.099(16) 0.018(9) _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 Ru N7 2.048(4) . y Ru N2 2.054(4) . y Ru N1 2.059(4) . y Ru N3 2.064(4) . y Ru N4 2.065(4) . y Ru N5 2.105(4) . y N7 C5 1.333(6) . ? N7 N8 1.360(5) . ? N8 C2 1.345(6) . ? C2 N9 1.352(6) . ? C2 C16 1.484(7) . ? N9 C5 1.350(6) . ? C5 C6 1.450(6) . ? C6 N5 1.361(6) . ? C6 C7 1.377(7) . ? C7 C8 1.393(8) . ? C8 C9 1.371(7) . ? C9 C10 1.386(7) . ? C10 N5 1.346(6) . ? C16 N71 1.332(6) . ? C16 C17 1.385(8) . ? C17 C18 1.390(9) . ? C18 C19 1.374(10) . ? C19 C20 1.371(9) . ? C20 N71 1.335(7) . ? N3 C30 1.343(6) . ? N3 C26 1.359(7) . ? C26 C27 1.392(7) . ? C26 C36 1.465(7) . ? C27 C28 1.366(8) . ? C28 C29 1.344(9) . ? C29 C30 1.390(8) . ? N4 C40 1.359(6) . ? N4 C36 1.365(6) . ? C36 C37 1.387(7) . ? C37 C38 1.385(8) . ? C38 C39 1.373(8) . ? C39 C40 1.373(7) . ? N1 C50 1.332(6) . ? N1 C46 1.361(6) . ? C46 C47 1.374(7) . ? C46 C56 1.485(7) . ? C47 C48 1.398(8) . ? C48 C49 1.373(8) . ? C48 C51 1.513(8) . ? C49 C50 1.380(8) . ? N2 C60 1.328(6) . ? N2 C56 1.361(6) . ? C56 C57 1.365(7) . ? C57 C58 1.391(8) . ? C58 C59 1.373(7) . ? C58 C61 1.502(7) . ? C59 C60 1.376(7) . ? P1 F15 1.533(5) . ? P1 F11 1.567(5) . ? P1 F14 1.572(5) . ? P1 F16 1.574(5) . ? P1 F12 1.576(5) . ? P1 F13 1.599(4) . ? C80 C81 1.42(2) . ? C81 O82 1.36(2) . ? O82 C83 1.29(2) . ? C83 C84 1.36(3) . ? 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 N7 Ru N2 93.81(15) . . y N7 Ru N1 87.73(15) . . y N2 Ru N1 79.01(15) . . y N7 Ru N3 174.82(14) . . y N2 Ru N3 90.66(16) . . y N1 Ru N3 95.69(16) . . y N7 Ru N4 98.24(16) . . y N2 Ru N4 97.59(15) . . y N1 Ru N4 173.35(15) . . y N3 Ru N4 78.56(16) . . y N7 Ru N5 77.82(15) . . y N2 Ru N5 171.10(15) . . y N1 Ru N5 97.46(15) . . y N3 Ru N5 97.85(15) . . y N4 Ru N5 86.71(15) . . y C5 N7 N8 107.8(4) . . ? C5 N7 Ru 115.7(3) . . ? N8 N7 Ru 136.1(3) . . ? C2 N8 N7 103.2(4) . . ? N8 C2 N9 115.5(4) . . ? N8 C2 C16 122.5(4) . . ? N9 C2 C16 122.0(4) . . ? C5 N9 C2 100.4(4) . . ? N7 C5 N9 113.1(4) . . ? N7 C5 C6 117.8(4) . . ? N9 C5 C6 129.1(4) . . ? N5 C6 C7 123.0(4) . . ? N5 C6 C5 113.1(4) . . ? C7 C6 C5 123.9(5) . . ? C6 C7 C8 118.9(5) . . ? C9 C8 C7 118.6(5) . . ? C8 C9 C10 119.6(5) . . ? N5 C10 C9 122.8(5) . . ? C10 N5 C6 117.0(4) . . ? C10 N5 Ru 127.5(3) . . ? C6 N5 Ru 115.4(3) . . ? N71 C16 C17 122.7(5) . . ? N71 C16 C2 116.9(5) . . ? C17 C16 C2 120.3(5) . . ? C16 C17 C18 119.3(6) . . ? C19 C18 C17 117.8(7) . . ? C20 C19 C18 119.1(6) . . ? N71 C20 C19 124.0(6) . . ? C16 N71 C20 117.1(5) . . ? C30 N3 C26 117.8(5) . . ? C30 N3 Ru 126.3(4) . . ? C26 N3 Ru 115.8(3) . . ? N3 C26 C27 120.5(5) . . ? N3 C26 C36 115.0(4) . . ? C27 C26 C36 124.4(5) . . ? C28 C27 C26 120.8(6) . . ? C29 C28 C27 118.6(6) . . ? C28 C29 C30 120.0(6) . . ? N3 C30 C29 122.3(6) . . ? C40 N4 C36 118.4(4) . . ? C40 N4 Ru 126.0(4) . . ? C36 N4 Ru 115.6(3) . . ? N4 C36 C37 121.2(5) . . ? N4 C36 C26 114.8(4) . . ? C37 C36 C26 124.0(5) . . ? C38 C37 C36 119.5(6) . . ? C39 C38 C37 118.9(5) . . ? C38 C39 C40 120.0(5) . . ? N4 C40 C39 121.8(5) . . ? C50 N1 C46 117.6(4) . . ? C50 N1 Ru 126.5(3) . . ? C46 N1 Ru 115.9(3) . . ? N1 C46 C47 122.1(5) . . ? N1 C46 C56 114.4(4) . . ? C47 C46 C56 123.5(5) . . ? C46 C47 C48 120.0(5) . . ? C49 C48 C47 117.2(5) . . ? C49 C48 C51 122.9(6) . . ? C47 C48 C51 119.9(5) . . ? C48 C49 C50 120.2(5) . . ? N1 C50 C49 122.9(5) . . ? C60 N2 C56 117.9(4) . . ? C60 N2 Ru 126.1(3) . . ? C56 N2 Ru 115.9(3) . . ? N2 C56 C57 121.3(5) . . ? N2 C56 C46 114.7(4) . . ? C57 C56 C46 124.1(5) . . ? C56 C57 C58 121.5(5) . . ? C59 C58 C57 115.7(5) . . ? C59 C58 C61 122.3(5) . . ? C57 C58 C61 122.0(5) . . ? C58 C59 C60 121.2(5) . . ? N2 C60 C59 122.3(5) . . ? F15 P1 F11 178.4(4) . . ? F15 P1 F14 91.2(3) . . ? F11 P1 F14 90.2(3) . . ? F15 P1 F16 90.8(4) . . ? F11 P1 F16 90.0(4) . . ? F14 P1 F16 89.5(3) . . ? F15 P1 F12 91.8(4) . . ? F11 P1 F12 87.4(3) . . ? F14 P1 F12 90.1(3) . . ? F16 P1 F12 177.3(4) . . ? F15 P1 F13 90.2(3) . . ? F11 P1 F13 88.4(3) . . ? F14 P1 F13 178.3(3) . . ? F16 P1 F13 89.4(3) . . ? F12 P1 F13 90.8(3) . . ? O82 C81 C80 118.0(13) . . ? C83 O82 C81 123.5(15) . . ? O82 C83 C84 121.9(17) . . ? 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 N2 Ru N7 C5 174.0(3) . . . . ? N1 Ru N7 C5 95.2(3) . . . . ? N3 Ru N7 C5 -36.3(18) . . . . ? N4 Ru N7 C5 -87.7(3) . . . . ? N5 Ru N7 C5 -2.9(3) . . . . ? N2 Ru N7 N8 1.0(4) . . . . ? N1 Ru N7 N8 -77.8(4) . . . . ? N3 Ru N7 N8 150.7(15) . . . . ? N4 Ru N7 N8 99.2(4) . . . . ? N5 Ru N7 N8 -176.0(4) . . . . ? C5 N7 N8 C2 0.7(5) . . . . ? Ru N7 N8 C2 174.1(3) . . . . ? N7 N8 C2 N9 -0.6(5) . . . . ? N7 N8 C2 C16 178.3(4) . . . . ? N8 C2 N9 C5 0.3(5) . . . . ? C16 C2 N9 C5 -178.6(4) . . . . ? N8 N7 C5 N9 -0.6(5) . . . . ? Ru N7 C5 N9 -175.5(3) . . . . ? N8 N7 C5 C6 179.6(4) . . . . ? Ru N7 C5 C6 4.7(5) . . . . ? C2 N9 C5 N7 0.2(5) . . . . ? C2 N9 C5 C6 180.0(5) . . . . ? N7 C5 C6 N5 -3.9(6) . . . . ? N9 C5 C6 N5 176.3(5) . . . . ? N7 C5 C6 C7 177.1(5) . . . . ? N9 C5 C6 C7 -2.7(8) . . . . ? N5 C6 C7 C8 3.4(8) . . . . ? C5 C6 C7 C8 -177.8(5) . . . . ? C6 C7 C8 C9 -2.2(8) . . . . ? C7 C8 C9 C10 0.6(8) . . . . ? C8 C9 C10 N5 0.0(8) . . . . ? C9 C10 N5 C6 1.0(7) . . . . ? C9 C10 N5 Ru 177.6(4) . . . . ? C7 C6 N5 C10 -2.7(7) . . . . ? C5 C6 N5 C10 178.3(4) . . . . ? C7 C6 N5 Ru -179.7(4) . . . . ? C5 C6 N5 Ru 1.3(5) . . . . ? N7 Ru N5 C10 -175.9(4) . . . . ? N2 Ru N5 C10 164.1(8) . . . . ? N1 Ru N5 C10 98.1(4) . . . . ? N3 Ru N5 C10 1.3(4) . . . . ? N4 Ru N5 C10 -76.7(4) . . . . ? N7 Ru N5 C6 0.8(3) . . . . ? N2 Ru N5 C6 -19.3(11) . . . . ? N1 Ru N5 C6 -85.3(3) . . . . ? N3 Ru N5 C6 177.9(3) . . . . ? N4 Ru N5 C6 99.9(3) . . . . ? N8 C2 C16 N71 -3.5(7) . . . . ? N9 C2 C16 N71 175.4(5) . . . . ? N8 C2 C16 C17 179.7(5) . . . . ? N9 C2 C16 C17 -1.5(8) . . . . ? N71 C16 C17 C18 -1.0(10) . . . . ? C2 C16 C17 C18 175.7(6) . . . . ? C16 C17 C18 C19 0.5(11) . . . . ? C17 C18 C19 C20 1.2(12) . . . . ? C18 C19 C20 N71 -2.7(12) . . . . ? C17 C16 N71 C20 -0.3(8) . . . . ? C2 C16 N71 C20 -177.1(5) . . . . ? C19 C20 N71 C16 2.2(9) . . . . ? N7 Ru N3 C30 132.9(16) . . . . ? N2 Ru N3 C30 -77.3(4) . . . . ? N1 Ru N3 C30 1.7(4) . . . . ? N4 Ru N3 C30 -174.9(5) . . . . ? N5 Ru N3 C30 100.1(4) . . . . ? N7 Ru N3 C26 -50.5(18) . . . . ? N2 Ru N3 C26 99.3(4) . . . . ? N1 Ru N3 C26 178.3(3) . . . . ? N4 Ru N3 C26 1.7(3) . . . . ? N5 Ru N3 C26 -83.3(4) . . . . ? C30 N3 C26 C27 -0.4(7) . . . . ? Ru N3 C26 C27 -177.3(4) . . . . ? C30 N3 C26 C36 177.4(4) . . . . ? Ru N3 C26 C36 0.5(5) . . . . ? N3 C26 C27 C28 0.7(9) . . . . ? C36 C26 C27 C28 -176.9(6) . . . . ? C26 C27 C28 C29 -0.6(10) . . . . ? C27 C28 C29 C30 0.3(10) . . . . ? C26 N3 C30 C29 0.1(8) . . . . ? Ru N3 C30 C29 176.6(4) . . . . ? C28 C29 C30 N3 0.0(10) . . . . ? N7 Ru N4 C40 -5.7(4) . . . . ? N2 Ru N4 C40 89.3(4) . . . . ? N1 Ru N4 C40 148.1(12) . . . . ? N3 Ru N4 C40 178.5(4) . . . . ? N5 Ru N4 C40 -82.9(4) . . . . ? N7 Ru N4 C36 172.2(3) . . . . ? N2 Ru N4 C36 -92.8(3) . . . . ? N1 Ru N4 C36 -34.1(14) . . . . ? N3 Ru N4 C36 -3.7(3) . . . . ? N5 Ru N4 C36 95.0(3) . . . . ? C40 N4 C36 C37 3.7(7) . . . . ? Ru N4 C36 C37 -174.3(4) . . . . ? C40 N4 C36 C26 -176.9(4) . . . . ? Ru N4 C36 C26 5.1(5) . . . . ? N3 C26 C36 N4 -3.6(6) . . . . ? C27 C26 C36 N4 174.0(5) . . . . ? N3 C26 C36 C37 175.7(5) . . . . ? C27 C26 C36 C37 -6.6(8) . . . . ? N4 C36 C37 C38 -3.7(9) . . . . ? C26 C36 C37 C38 177.0(5) . . . . ? C36 C37 C38 C39 2.0(9) . . . . ? C37 C38 C39 C40 -0.5(9) . . . . ? C36 N4 C40 C39 -2.1(7) . . . . ? Ru N4 C40 C39 175.7(4) . . . . ? C38 C39 C40 N4 0.5(8) . . . . ? N7 Ru N1 C50 -88.3(4) . . . . ? N2 Ru N1 C50 177.4(5) . . . . ? N3 Ru N1 C50 87.8(4) . . . . ? N4 Ru N1 C50 117.7(12) . . . . ? N5 Ru N1 C50 -10.9(4) . . . . ? N7 Ru N1 C46 92.2(3) . . . . ? N2 Ru N1 C46 -2.2(3) . . . . ? N3 Ru N1 C46 -91.7(3) . . . . ? N4 Ru N1 C46 -61.8(14) . . . . ? N5 Ru N1 C46 169.5(3) . . . . ? C50 N1 C46 C47 0.9(7) . . . . ? Ru N1 C46 C47 -179.6(4) . . . . ? C50 N1 C46 C56 -178.6(4) . . . . ? Ru N1 C46 C56 1.0(5) . . . . ? N1 C46 C47 C48 -1.7(8) . . . . ? C56 C46 C47 C48 177.7(5) . . . . ? C46 C47 C48 C49 1.3(8) . . . . ? C46 C47 C48 C51 178.8(6) . . . . ? C47 C48 C49 C50 -0.2(9) . . . . ? C51 C48 C49 C50 -177.6(6) . . . . ? C46 N1 C50 C49 0.3(8) . . . . ? Ru N1 C50 C49 -179.2(4) . . . . ? C48 C49 C50 N1 -0.6(9) . . . . ? N7 Ru N2 C60 91.8(4) . . . . ? N1 Ru N2 C60 178.8(4) . . . . ? N3 Ru N2 C60 -85.5(4) . . . . ? N4 Ru N2 C60 -7.0(4) . . . . ? N5 Ru N2 C60 111.5(10) . . . . ? N7 Ru N2 C56 -83.8(4) . . . . ? N1 Ru N2 C56 3.1(3) . . . . ? N3 Ru N2 C56 98.8(4) . . . . ? N4 Ru N2 C56 177.3(3) . . . . ? N5 Ru N2 C56 -64.2(10) . . . . ? C60 N2 C56 C57 1.0(7) . . . . ? Ru N2 C56 C57 177.0(4) . . . . ? C60 N2 C56 C46 -179.5(4) . . . . ? Ru N2 C56 C46 -3.5(5) . . . . ? N1 C46 C56 N2 1.6(6) . . . . ? C47 C46 C56 N2 -177.8(5) . . . . ? N1 C46 C56 C57 -178.9(5) . . . . ? C47 C46 C56 C57 1.7(8) . . . . ? N2 C56 C57 C58 0.4(8) . . . . ? C46 C56 C57 C58 -179.0(5) . . . . ? C56 C57 C58 C59 -1.2(9) . . . . ? C56 C57 C58 C61 178.7(6) . . . . ? C57 C58 C59 C60 0.6(9) . . . . ? C61 C58 C59 C60 -179.3(6) . . . . ? C56 N2 C60 C59 -1.6(8) . . . . ? Ru N2 C60 C59 -177.2(4) . . . . ? C58 C59 C60 N2 0.8(9) . . . . ? C80 C81 O82 C83 174.0(16) . . . . ? C81 O82 C83 C84 -176.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.248 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.225 data_FO1746 _database_code_depnum_ccdc_archive 'CCDC 273899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 F6 N11 O P Ru' _chemical_formula_weight 828.69 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 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 16.2156(4) _cell_length_b 13.8572(4) _cell_length_c 14.8161(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.117(2) _cell_angle_gamma 90.00 _cell_volume 3326.95(16) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min 0.9480 _exptl_absorpt_correction_T_max 0.9649 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13029 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7514 _reflns_number_gt 6106 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0659P)^2^+5.8376P] 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 7514 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ru Ru 0.262211(15) 0.096146(19) 0.116999(17) 0.03374(10) Uani 1 1 d . . . N1 N 0.29055(17) -0.0356(2) 0.06150(19) 0.0375(6) Uani 1 1 d . . . N2 N 0.33862(17) 0.1370(2) 0.01662(18) 0.0338(6) Uani 1 1 d . . . N3 N 0.15828(18) 0.1251(3) 0.0362(2) 0.0429(7) Uani 1 1 d . . . N4 N 0.23121(17) 0.2315(2) 0.1612(2) 0.0381(6) Uani 1 1 d . . . N5 N 0.20072(17) 0.0494(2) 0.2288(2) 0.0390(6) Uani 1 1 d . . . N6 N 0.1338(2) 0.0094(3) 0.3968(2) 0.0612(10) Uani 1 1 d . . . N7 N 0.35759(17) 0.0709(2) 0.20814(19) 0.0356(6) Uani 1 1 d . . . N8 N 0.44107(17) 0.0765(2) 0.20693(19) 0.0360(6) Uani 1 1 d . . . N9 N 0.40258(18) 0.0143(2) 0.34200(19) 0.0383(6) Uani 1 1 d . . . N10 N 0.6544(2) -0.0234(3) 0.4249(2) 0.0586(9) Uani 1 1 d . . . N11 N 0.6068(2) 0.0844(2) 0.2719(2) 0.0480(7) Uani 1 1 d . . . C1 C 0.2592(2) -0.1223(3) 0.0846(3) 0.0460(8) Uani 1 1 d . . . H1A H 0.2196 -0.1247 0.1302 0.055 Uiso 1 1 calc R . . C2 C 0.2825(3) -0.2070(3) 0.0446(3) 0.0512(9) Uani 1 1 d . . . H2A H 0.2584 -0.2662 0.0620 0.061 Uiso 1 1 calc R . . C3 C 0.3418(3) -0.2063(3) -0.0219(3) 0.0483(9) Uani 1 1 d . . . C4 C 0.3743(2) -0.1167(3) -0.0446(3) 0.0432(8) Uani 1 1 d . . . H4A H 0.4151 -0.1128 -0.0887 0.052 Uiso 1 1 calc R . . C5 C 0.3475(2) -0.0337(2) -0.0034(2) 0.0351(7) Uani 1 1 d . . . C6 C 0.3763(2) 0.0636(2) -0.0268(2) 0.0335(6) Uani 1 1 d . . . C7 C 0.4349(2) 0.0815(3) -0.0906(2) 0.0384(7) Uani 1 1 d . . . H7A H 0.4608 0.0289 -0.1194 0.046 Uiso 1 1 calc R . . C8 C 0.4560(2) 0.1750(3) -0.1127(2) 0.0418(8) Uani 1 1 d . . . C9 C 0.4166(2) 0.2492(3) -0.0682(2) 0.0412(8) Uani 1 1 d . . . H9A H 0.4290 0.3145 -0.0818 0.049 Uiso 1 1 calc R . . C10 C 0.3594(2) 0.2282(2) -0.0043(2) 0.0395(7) Uani 1 1 d . . . H10A H 0.3338 0.2800 0.0260 0.047 Uiso 1 1 calc R . . C11 C 0.3692(3) -0.2956(3) -0.0667(4) 0.0689(13) Uani 1 1 d . . . H11A H 0.4107 -0.2796 -0.1107 0.103 Uiso 1 1 calc R . . H11B H 0.3217 -0.3265 -0.0977 0.103 Uiso 1 1 calc R . . H11C H 0.3932 -0.3398 -0.0213 0.103 Uiso 1 1 calc R . . C12 C 0.5176(3) 0.1954(3) -0.1841(3) 0.0575(11) Uani 1 1 d . . . H12A H 0.5386 0.1344 -0.2075 0.086 Uiso 1 1 calc R . . H12B H 0.5636 0.2332 -0.1576 0.086 Uiso 1 1 calc R . . H12C H 0.4907 0.2320 -0.2335 0.086 Uiso 1 1 calc R . . C13 C 0.1239(3) 0.0647(4) -0.0265(3) 0.0553(10) Uani 1 1 d . . . H13A H 0.1465 0.0021 -0.0338 0.066 Uiso 1 1 calc R . . C14 C 0.0568(3) 0.0925(5) -0.0797(3) 0.0739(16) Uani 1 1 d . . . H14A H 0.0326 0.0483 -0.1219 0.089 Uiso 1 1 calc R . . C15 C 0.0246(3) 0.1835(5) -0.0723(4) 0.0846(18) Uani 1 1 d . . . H15A H -0.0205 0.2038 -0.1105 0.102 Uiso 1 1 calc R . . C16 C 0.0593(3) 0.2451(4) -0.0083(3) 0.0690(13) Uani 1 1 d . . . H16A H 0.0379 0.3084 -0.0018 0.083 Uiso 1 1 calc R . . C17 C 0.1251(2) 0.2145(3) 0.0466(3) 0.0465(8) Uani 1 1 d . . . C18 C 0.1626(2) 0.2712(3) 0.1212(3) 0.0439(8) Uani 1 1 d . . . C19 C 0.1290(3) 0.3565(3) 0.1524(3) 0.0575(10) Uani 1 1 d . . . H19A H 0.0809 0.3833 0.1237 0.069 Uiso 1 1 calc R . . C20 C 0.1667(3) 0.4018(3) 0.2260(3) 0.0590(11) Uani 1 1 d . . . H20A H 0.1447 0.4602 0.2485 0.071 Uiso 1 1 calc R . . C21 C 0.2363(3) 0.3618(3) 0.2664(3) 0.0571(10) Uani 1 1 d . . . H21A H 0.2627 0.3920 0.3172 0.069 Uiso 1 1 calc R . . C22 C 0.2670(3) 0.2775(3) 0.2321(3) 0.0490(9) Uani 1 1 d . . . H22A H 0.3156 0.2508 0.2597 0.059 Uiso 1 1 calc R . . C23 C 0.1184(2) 0.0513(3) 0.2413(3) 0.0468(8) Uani 1 1 d . . . H23A H 0.0817 0.0662 0.1918 0.056 Uiso 1 1 calc R . . C24 C 0.0868(3) 0.0321(4) 0.3240(3) 0.0596(11) Uani 1 1 d . . . H24A H 0.0287 0.0351 0.3297 0.072 Uiso 1 1 calc R . . C25 C 0.2155(3) 0.0074(3) 0.3850(3) 0.0521(10) Uani 1 1 d . . . H25A H 0.2514 -0.0082 0.4349 0.063 Uiso 1 1 calc R . . C26 C 0.2492(2) 0.0274(3) 0.3027(2) 0.0399(7) Uani 1 1 d . . . C27 C 0.3372(2) 0.0342(2) 0.2880(2) 0.0360(7) Uani 1 1 d . . . C28 C 0.4649(2) 0.0415(2) 0.2888(2) 0.0345(7) Uani 1 1 d . . . C29 C 0.5516(2) 0.0353(3) 0.3190(2) 0.0382(7) Uani 1 1 d . . . C30 C 0.5765(2) -0.0191(3) 0.3948(3) 0.0494(9) Uani 1 1 d . . . H30A H 0.5360 -0.0542 0.4259 0.059 Uiso 1 1 calc R . . C31 C 0.7081(2) 0.0292(4) 0.3794(3) 0.0566(11) Uani 1 1 d . . . H31A H 0.7642 0.0309 0.4000 0.068 Uiso 1 1 calc R . . C32 C 0.6844(2) 0.0813(3) 0.3033(3) 0.0568(10) Uani 1 1 d . . . H32A H 0.7251 0.1161 0.2724 0.068 Uiso 1 1 calc R . . P1 P 0.11689(8) -0.28163(11) 0.31253(11) 0.0721(4) Uani 1 1 d . . . F1 F 0.0428(3) -0.3464(5) 0.3331(6) 0.238(5) Uani 1 1 d . . . F2 F 0.0566(4) -0.2008(5) 0.2823(4) 0.209(4) Uani 1 1 d . . . F3 F 0.1205(3) -0.3225(4) 0.2130(3) 0.161(2) Uani 1 1 d . . . F4 F 0.1936(3) -0.2200(4) 0.2949(4) 0.1383(17) Uani 1 1 d . . . F5 F 0.1164(2) -0.2391(3) 0.4107(3) 0.1124(13) Uani 1 1 d . . . F6 F 0.1777(2) -0.3664(3) 0.3460(3) 0.0975(10) Uani 1 1 d . . . O1W O 0.0727(3) -0.0666(4) 0.5573(4) 0.1136(16) 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 Ru 0.03183(15) 0.03731(16) 0.03187(15) 0.00186(10) -0.00143(10) -0.00190(10) N1 0.0377(15) 0.0385(15) 0.0360(14) 0.0029(12) -0.0022(11) -0.0040(12) N2 0.0367(14) 0.0334(14) 0.0308(13) 0.0017(11) -0.0040(11) -0.0019(11) N3 0.0351(15) 0.0593(19) 0.0340(15) 0.0035(13) -0.0022(12) -0.0051(13) N4 0.0348(14) 0.0420(16) 0.0375(14) 0.0031(12) 0.0021(11) 0.0011(11) N5 0.0343(14) 0.0419(16) 0.0405(15) 0.0003(13) -0.0011(12) -0.0046(12) N6 0.0435(18) 0.091(3) 0.0496(19) 0.0104(19) 0.0092(15) -0.0063(18) N7 0.0320(14) 0.0376(14) 0.0370(14) 0.0018(12) -0.0007(11) -0.0011(11) N8 0.0328(14) 0.0386(15) 0.0365(14) 0.0000(11) 0.0002(11) 0.0002(11) N9 0.0379(15) 0.0413(15) 0.0358(14) 0.0035(12) 0.0010(12) 0.0006(12) N10 0.0474(19) 0.082(3) 0.0453(18) -0.0027(18) -0.0083(15) 0.0148(18) N11 0.0388(16) 0.0542(19) 0.0511(19) 0.0011(15) 0.0032(14) 0.0013(13) C1 0.046(2) 0.0428(19) 0.049(2) 0.0067(17) 0.0043(16) -0.0086(16) C2 0.058(2) 0.038(2) 0.058(2) 0.0097(17) 0.0007(19) -0.0079(17) C3 0.055(2) 0.0366(19) 0.053(2) 0.0033(16) -0.0069(18) -0.0017(16) C4 0.048(2) 0.0403(19) 0.0413(19) 0.0008(15) 0.0002(16) 0.0006(15) C5 0.0349(16) 0.0343(16) 0.0357(16) 0.0024(13) -0.0043(13) -0.0020(13) C6 0.0360(16) 0.0342(16) 0.0299(15) 0.0045(13) -0.0042(12) -0.0021(13) C7 0.0390(17) 0.0395(18) 0.0369(17) -0.0037(14) 0.0017(14) 0.0004(14) C8 0.0389(18) 0.0454(19) 0.0413(18) 0.0049(15) 0.0023(14) -0.0064(15) C9 0.048(2) 0.0323(17) 0.0433(19) 0.0041(14) 0.0017(15) -0.0062(14) C10 0.0466(19) 0.0340(17) 0.0377(17) 0.0006(14) -0.0011(14) 0.0002(14) C11 0.087(3) 0.040(2) 0.081(3) -0.008(2) 0.016(3) 0.003(2) C12 0.062(3) 0.047(2) 0.065(3) 0.0054(19) 0.021(2) -0.0072(19) C13 0.045(2) 0.078(3) 0.043(2) -0.007(2) -0.0034(17) -0.011(2) C14 0.048(2) 0.121(5) 0.052(3) -0.014(3) -0.014(2) -0.011(3) C15 0.049(3) 0.136(5) 0.067(3) 0.002(3) -0.022(2) 0.018(3) C16 0.049(2) 0.092(4) 0.065(3) 0.004(3) -0.014(2) 0.017(2) C17 0.0357(18) 0.058(2) 0.046(2) 0.0077(17) 0.0002(15) 0.0056(16) C18 0.0371(18) 0.049(2) 0.046(2) 0.0076(16) 0.0035(15) 0.0031(15) C19 0.048(2) 0.056(2) 0.069(3) 0.005(2) 0.009(2) 0.0125(18) C20 0.061(3) 0.053(2) 0.063(3) -0.006(2) 0.017(2) 0.007(2) C21 0.067(3) 0.052(2) 0.052(2) -0.0117(19) 0.004(2) 0.000(2) C22 0.050(2) 0.051(2) 0.046(2) -0.0038(17) -0.0027(16) -0.0009(17) C23 0.0329(17) 0.060(2) 0.047(2) 0.0015(18) 0.0017(15) -0.0066(16) C24 0.038(2) 0.086(3) 0.056(2) 0.006(2) 0.0065(18) -0.007(2) C25 0.045(2) 0.074(3) 0.0376(19) 0.0079(18) 0.0036(16) -0.0017(19) C26 0.0369(17) 0.0441(19) 0.0387(18) 0.0017(14) 0.0020(14) -0.0020(14) C27 0.0353(16) 0.0364(17) 0.0362(17) 0.0009(13) -0.0006(13) -0.0002(13) C28 0.0379(17) 0.0317(16) 0.0338(16) -0.0010(13) 0.0005(13) 0.0015(13) C29 0.0362(17) 0.0429(18) 0.0355(17) -0.0041(14) 0.0011(13) 0.0030(14) C30 0.0396(19) 0.063(2) 0.045(2) 0.0013(18) -0.0021(16) 0.0045(17) C31 0.0330(18) 0.084(3) 0.052(2) -0.018(2) -0.0038(16) 0.0064(19) C32 0.0364(19) 0.073(3) 0.061(3) -0.006(2) 0.0044(18) -0.0016(18) P1 0.0483(6) 0.0833(9) 0.0841(9) -0.0198(7) -0.0069(6) 0.0101(6) F1 0.076(3) 0.226(7) 0.419(12) -0.171(8) 0.073(5) -0.073(4) F2 0.219(6) 0.224(7) 0.176(5) -0.082(5) -0.095(5) 0.166(5) F3 0.145(4) 0.220(6) 0.113(3) -0.082(3) -0.064(3) 0.101(4) F4 0.136(4) 0.130(4) 0.152(4) 0.007(3) 0.050(3) -0.036(3) F5 0.107(3) 0.139(3) 0.092(3) -0.033(2) 0.020(2) 0.008(2) F6 0.096(2) 0.100(2) 0.097(2) 0.007(2) 0.009(2) 0.025(2) O1W 0.123(4) 0.121(4) 0.099(3) 0.013(3) 0.020(3) -0.017(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 Ru N7 2.046(3) . ? Ru N2 2.050(3) . ? Ru N4 2.055(3) . ? Ru N1 2.061(3) . ? Ru N5 2.069(3) . ? Ru N3 2.070(3) . ? N1 C1 1.353(5) . ? N1 C5 1.359(4) . ? N2 C10 1.348(4) . ? N2 C6 1.360(4) . ? N3 C13 1.355(5) . ? N3 C17 1.362(5) . ? N4 C22 1.342(5) . ? N4 C18 1.358(4) . ? N5 C23 1.355(4) . ? N5 C26 1.357(4) . ? N6 C24 1.336(6) . ? N6 C25 1.342(5) . ? N7 C27 1.340(4) . ? N7 N8 1.357(4) . ? N8 C28 1.349(4) . ? N9 C27 1.334(4) . ? N9 C28 1.357(4) . ? N10 C30 1.326(5) . ? N10 C31 1.337(6) . ? N11 C32 1.326(5) . ? N11 C29 1.340(5) . ? C1 C2 1.374(6) . ? C2 C3 1.401(6) . ? C3 C4 1.394(5) . ? C3 C11 1.480(6) . ? C4 C5 1.379(5) . ? C5 C6 1.473(5) . ? C6 C7 1.386(5) . ? C7 C8 1.382(5) . ? C8 C9 1.390(5) . ? C8 C12 1.508(5) . ? C9 C10 1.380(5) . ? C13 C14 1.374(6) . ? C14 C15 1.371(8) . ? C15 C16 1.380(8) . ? C16 C17 1.385(6) . ? C17 C18 1.469(6) . ? C18 C19 1.389(6) . ? C19 C20 1.380(7) . ? C20 C21 1.375(7) . ? C21 C22 1.374(6) . ? C23 C24 1.371(6) . ? C25 C26 1.382(5) . ? C26 C27 1.455(5) . ? C28 C29 1.464(5) . ? C29 C30 1.399(5) . ? C31 C32 1.380(7) . ? P1 F1 1.539(5) . ? P1 F4 1.539(4) . ? P1 F2 1.543(5) . ? P1 F5 1.570(4) . ? P1 F3 1.582(4) . ? P1 F6 1.601(4) . ? 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 N7 Ru N2 93.65(11) . . ? N7 Ru N4 97.68(11) . . ? N2 Ru N4 98.11(11) . . ? N7 Ru N1 86.40(11) . . ? N2 Ru N1 78.78(11) . . ? N4 Ru N1 175.05(11) . . ? N7 Ru N5 78.03(11) . . ? N2 Ru N5 171.61(11) . . ? N4 Ru N5 84.23(12) . . ? N1 Ru N5 99.39(12) . . ? N7 Ru N3 173.99(12) . . ? N2 Ru N3 91.61(11) . . ? N4 Ru N3 78.69(12) . . ? N1 Ru N3 97.46(12) . . ? N5 Ru N3 96.75(11) . . ? C1 N1 C5 117.9(3) . . ? C1 N1 Ru 126.5(3) . . ? C5 N1 Ru 115.6(2) . . ? C10 N2 C6 118.1(3) . . ? C10 N2 Ru 126.1(2) . . ? C6 N2 Ru 115.6(2) . . ? C13 N3 C17 119.0(3) . . ? C13 N3 Ru 125.6(3) . . ? C17 N3 Ru 115.3(2) . . ? C22 N4 C18 118.2(3) . . ? C22 N4 Ru 125.4(3) . . ? C18 N4 Ru 115.9(2) . . ? C23 N5 C26 116.0(3) . . ? C23 N5 Ru 127.6(3) . . ? C26 N5 Ru 115.7(2) . . ? C24 N6 C25 115.8(3) . . ? C27 N7 N8 108.2(3) . . ? C27 N7 Ru 116.2(2) . . ? N8 N7 Ru 135.4(2) . . ? C28 N8 N7 102.7(3) . . ? C27 N9 C28 100.7(3) . . ? C30 N10 C31 115.8(4) . . ? C32 N11 C29 116.3(4) . . ? N1 C1 C2 122.5(4) . . ? C1 C2 C3 120.3(4) . . ? C4 C3 C2 116.8(4) . . ? C4 C3 C11 121.0(4) . . ? C2 C3 C11 122.3(4) . . ? C5 C4 C3 120.6(4) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 123.5(3) . . ? N2 C6 C7 121.4(3) . . ? N2 C6 C5 114.9(3) . . ? C7 C6 C5 123.7(3) . . ? C8 C7 C6 120.7(3) . . ? C7 C8 C9 117.3(3) . . ? C7 C8 C12 121.3(3) . . ? C9 C8 C12 121.4(3) . . ? C10 C9 C8 120.1(3) . . ? N2 C10 C9 122.4(3) . . ? N3 C13 C14 121.2(5) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 118.5(4) . . ? C15 C16 C17 120.1(5) . . ? N3 C17 C16 120.7(4) . . ? N3 C17 C18 114.7(3) . . ? C16 C17 C18 124.6(4) . . ? N4 C18 C19 121.6(4) . . ? N4 C18 C17 114.9(3) . . ? C19 C18 C17 123.3(4) . . ? C20 C19 C18 118.9(4) . . ? C21 C20 C19 119.5(4) . . ? C22 C21 C20 119.0(4) . . ? N4 C22 C21 122.7(4) . . ? N5 C23 C24 121.4(4) . . ? N6 C24 C23 123.1(4) . . ? N6 C25 C26 122.4(4) . . ? N5 C26 C25 121.3(3) . . ? N5 C26 C27 114.0(3) . . ? C25 C26 C27 124.5(3) . . ? N9 C27 N7 113.0(3) . . ? N9 C27 C26 131.3(3) . . ? N7 C27 C26 115.6(3) . . ? N8 C28 N9 115.3(3) . . ? N8 C28 C29 122.4(3) . . ? N9 C28 C29 122.2(3) . . ? N11 C29 C30 120.9(3) . . ? N11 C29 C28 117.6(3) . . ? C30 C29 C28 121.5(3) . . ? N10 C30 C29 122.5(4) . . ? N10 C31 C32 122.1(4) . . ? N11 C32 C31 122.3(4) . . ? F1 P1 F4 177.2(4) . . ? F1 P1 F2 89.4(5) . . ? F4 P1 F2 93.2(4) . . ? F1 P1 F5 90.3(3) . . ? F4 P1 F5 88.9(3) . . ? F2 P1 F5 88.4(3) . . ? F1 P1 F3 91.9(4) . . ? F4 P1 F3 89.0(3) . . ? F2 P1 F3 92.0(3) . . ? F5 P1 F3 177.9(3) . . ? F1 P1 F6 89.2(4) . . ? F4 P1 F6 88.1(3) . . ? F2 P1 F6 178.4(4) . . ? F5 P1 F6 90.7(2) . . ? F3 P1 F6 89.0(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.872 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.083 data_FO1962 _database_code_depnum_ccdc_archive 'CCDC 273900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 F12 N6 O P2 Ru' _chemical_formula_weight 887.66 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' 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 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 11.1155(3) _cell_length_b 18.1355(5) _cell_length_c 18.3079(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.932(1) _cell_angle_gamma 90.00 _cell_volume 3670.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14401 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1591 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8418 _reflns_number_gt 4583 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0448P)^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_number_reflns 8418 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Ru Ru 0.34377(3) 0.770283(18) 0.52491(2) 0.02248(11) Uani 1 1 d . . . N1 N 0.2519(3) 0.75618(18) 0.42181(19) 0.0228(8) Uani 1 1 d . . . N2 N 0.4353(3) 0.68315(18) 0.48614(19) 0.0246(8) Uani 1 1 d . . . N3 N 0.2354(3) 0.69943(18) 0.57509(19) 0.0232(8) Uani 1 1 d . . . N4 N 0.4309(3) 0.76720(18) 0.63023(18) 0.0244(8) Uani 1 1 d . . . N5 N 0.4590(3) 0.84120(19) 0.4817(2) 0.0248(8) Uani 1 1 d . . . N6 N 0.2435(3) 0.85672(19) 0.55580(19) 0.0263(9) Uani 1 1 d . . . C1 C 0.1591(4) 0.7978(2) 0.3918(2) 0.0276(11) Uani 1 1 d . . . H1A H 0.1385 0.8414 0.4165 0.033 Uiso 1 1 calc R . . C2 C 0.0930(4) 0.7792(2) 0.3265(2) 0.0309(11) Uani 1 1 d . . . H2A H 0.0275 0.8095 0.3074 0.037 Uiso 1 1 calc R . . C3 C 0.1214(4) 0.7171(2) 0.2888(2) 0.0291(11) Uani 1 1 d . . . C4 C 0.2181(4) 0.6750(3) 0.3196(2) 0.0317(11) Uani 1 1 d . . . H4A H 0.2401 0.6315 0.2953 0.038 Uiso 1 1 calc R . . C5 C 0.2826(4) 0.6954(2) 0.3848(2) 0.0243(10) Uani 1 1 d . . . C6 C 0.3897(4) 0.6556(2) 0.4198(2) 0.0267(10) Uani 1 1 d . . . C7 C 0.4435(4) 0.5965(2) 0.3882(3) 0.0311(11) Uani 1 1 d . . . H7A H 0.4099 0.5781 0.3420 0.037 Uiso 1 1 calc R . . C8 C 0.5464(4) 0.5640(2) 0.4237(3) 0.0320(12) Uani 1 1 d . . . C9 C 0.5923(4) 0.5927(2) 0.4903(3) 0.0331(11) Uani 1 1 d . . . H9A H 0.6632 0.5721 0.5158 0.040 Uiso 1 1 calc R . . C10 C 0.5353(4) 0.6513(2) 0.5200(3) 0.0311(11) Uani 1 1 d . . . H10A H 0.5680 0.6701 0.5663 0.037 Uiso 1 1 calc R . . C11 C 0.0499(4) 0.6948(3) 0.2179(3) 0.0424(13) Uani 1 1 d . . . H11A H -0.0142 0.7310 0.2050 0.064 Uiso 1 1 calc R . . H11B H 0.0137 0.6462 0.2238 0.064 Uiso 1 1 calc R . . H11C H 0.1036 0.6927 0.1788 0.064 Uiso 1 1 calc R . . C12 C 0.6075(4) 0.5001(2) 0.3892(3) 0.0426(13) Uani 1 1 d . . . H12A H 0.5623 0.4876 0.3420 0.064 Uiso 1 1 calc R . . H12B H 0.6094 0.4573 0.4220 0.064 Uiso 1 1 calc R . . H12C H 0.6904 0.5140 0.3813 0.064 Uiso 1 1 calc R . . C13 C 0.1299(4) 0.6707(2) 0.5445(3) 0.0309(11) Uani 1 1 d . . . H13A H 0.1026 0.6831 0.4951 0.037 Uiso 1 1 calc R . . C14 C 0.0600(4) 0.6238(2) 0.5826(3) 0.0319(11) Uani 1 1 d . . . H14A H -0.0151 0.6058 0.5600 0.038 Uiso 1 1 calc R . . C15 C 0.1004(4) 0.6038(2) 0.6531(2) 0.0280(11) Uani 1 1 d . . . H15A H 0.0549 0.5708 0.6797 0.034 Uiso 1 1 calc R . . C16 C 0.2084(4) 0.6326(2) 0.6845(3) 0.0297(11) Uani 1 1 d . . . H16A H 0.2383 0.6188 0.7331 0.036 Uiso 1 1 calc R . . C17 C 0.2735(4) 0.6814(2) 0.6458(2) 0.0218(10) Uani 1 1 d . . . C18 C 0.3841(4) 0.7194(2) 0.6767(2) 0.0240(10) Uani 1 1 d . . . C19 C 0.4349(4) 0.7104(2) 0.7479(3) 0.0316(11) Uani 1 1 d . . . H19A H 0.4003 0.6770 0.7798 0.038 Uiso 1 1 calc R . . C20 C 0.5361(4) 0.7504(3) 0.7724(3) 0.0391(13) Uani 1 1 d . . . H20A H 0.5728 0.7441 0.8212 0.047 Uiso 1 1 calc R . . C21 C 0.5844(4) 0.7997(3) 0.7258(3) 0.0386(12) Uani 1 1 d . . . H21A H 0.6535 0.8284 0.7421 0.046 Uiso 1 1 calc R . . C22 C 0.5294(4) 0.8061(3) 0.6549(3) 0.0369(12) Uani 1 1 d . . . H22A H 0.5627 0.8394 0.6223 0.044 Uiso 1 1 calc R . . C23 C 0.5198(4) 0.8816(2) 0.4556(3) 0.0295(11) Uani 1 1 d . . . C24 C 0.5954(4) 0.9350(3) 0.4211(3) 0.0414(13) Uani 1 1 d . . . H24A H 0.6393 0.9098 0.3846 0.062 Uiso 1 1 calc R . . H24B H 0.6534 0.9572 0.4587 0.062 Uiso 1 1 calc R . . H24C H 0.5440 0.9736 0.3969 0.062 Uiso 1 1 calc R . . C25 C 0.1846(4) 0.9050(2) 0.5711(2) 0.0278(11) Uani 1 1 d . . . C26 C 0.1096(4) 0.9657(3) 0.5913(3) 0.0420(13) Uani 1 1 d . . . H26A H 0.0288 0.9472 0.5985 0.063 Uiso 1 1 calc R . . H26B H 0.1030 1.0026 0.5520 0.063 Uiso 1 1 calc R . . H26C H 0.1463 0.9882 0.6369 0.063 Uiso 1 1 calc R . . P1 P -0.24703(11) 0.98860(7) 0.64392(7) 0.0319(3) Uani 1 1 d . . . F11 F -0.1883(3) 1.00721(17) 0.57016(16) 0.0599(9) Uani 1 1 d . . . F12 F -0.1879(3) 0.90918(16) 0.64573(19) 0.0709(10) Uani 1 1 d . . . F13 F -0.3069(3) 0.97053(17) 0.71704(17) 0.0671(10) Uani 1 1 d . . . F14 F -0.3077(2) 1.06844(14) 0.64243(16) 0.0478(8) Uani 1 1 d . . . F15 F -0.3638(3) 0.95718(15) 0.59564(17) 0.0547(8) Uani 1 1 d . . . F16 F -0.1308(2) 1.02097(17) 0.69065(17) 0.0586(9) Uani 1 1 d . . . P2 P 0.23837(12) 1.07870(8) 0.78299(8) 0.0436(4) Uani 1 1 d . . . F21 F 0.1099(3) 1.0536(3) 0.7484(2) 0.1134(17) Uani 1 1 d . . . F22 F 0.2225(4) 1.0337(2) 0.8547(2) 0.1042(14) Uani 1 1 d . . . F23 F 0.2570(4) 1.12339(19) 0.71106(19) 0.0855(12) Uani 1 1 d . . . F24 F 0.3677(3) 1.1035(2) 0.8175(2) 0.0868(12) Uani 1 1 d . . . F25 F 0.2959(3) 1.00809(17) 0.74739(18) 0.0657(9) Uani 1 1 d . . . F26 F 0.1806(3) 1.1479(2) 0.8179(2) 0.0897(12) Uani 1 1 d . . . O1E O -0.1220(3) 0.69307(19) 0.44189(19) 0.0507(10) Uani 1 1 d . . . C1E C -0.1445(7) 0.7920(4) 0.5220(4) 0.119(3) Uani 1 1 d . . . H1EA H -0.1879 0.8382 0.5287 0.179 Uiso 1 1 calc R . . H1EB H -0.0576 0.8021 0.5236 0.179 Uiso 1 1 calc R . . H1EC H -0.1590 0.7575 0.5613 0.179 Uiso 1 1 calc R . . C2E C -0.1882(5) 0.7593(3) 0.4500(3) 0.0640(17) Uani 1 1 d . . . H2EA H -0.2757 0.7485 0.4480 0.077 Uiso 1 1 calc R . . H2EB H -0.1752 0.7942 0.4100 0.077 Uiso 1 1 calc R . . C3E C -0.1554(4) 0.6585(3) 0.3741(3) 0.0452(14) Uani 1 1 d . . . H3EA H -0.1405 0.6922 0.3334 0.054 Uiso 1 1 calc R . . H3EB H -0.2426 0.6463 0.3696 0.054 Uiso 1 1 calc R . . C4E C -0.0826(5) 0.5894(3) 0.3692(3) 0.0575(16) Uani 1 1 d . . . H4EA H -0.1058 0.5651 0.3221 0.086 Uiso 1 1 calc R . . H4EB H -0.0980 0.5561 0.4094 0.086 Uiso 1 1 calc R . . H4EC H 0.0037 0.6018 0.3731 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02704(19) 0.02384(19) 0.01652(19) 0.00075(18) 0.00200(14) -0.00178(17) N1 0.0255(19) 0.0242(19) 0.019(2) 0.0058(16) 0.0028(16) -0.0028(16) N2 0.027(2) 0.026(2) 0.021(2) 0.0050(17) 0.0025(17) -0.0012(17) N3 0.028(2) 0.0262(19) 0.016(2) 0.0029(16) 0.0054(17) -0.0035(16) N4 0.0285(19) 0.0249(19) 0.018(2) 0.0007(18) -0.0040(16) -0.0001(18) N5 0.0230(19) 0.028(2) 0.023(2) -0.0013(18) 0.0000(17) -0.0007(17) N6 0.033(2) 0.030(2) 0.015(2) 0.0004(17) -0.0012(17) -0.0057(19) C1 0.033(3) 0.025(2) 0.026(3) 0.001(2) 0.009(2) 0.001(2) C2 0.027(2) 0.040(3) 0.025(3) 0.004(2) -0.001(2) -0.004(2) C3 0.036(3) 0.032(3) 0.020(3) -0.002(2) 0.002(2) -0.007(2) C4 0.039(3) 0.037(3) 0.020(3) -0.006(2) 0.007(2) -0.002(2) C5 0.032(2) 0.022(2) 0.019(3) 0.001(2) 0.004(2) -0.004(2) C6 0.029(2) 0.033(3) 0.019(3) 0.004(2) 0.009(2) -0.003(2) C7 0.035(3) 0.034(3) 0.026(3) -0.006(2) 0.008(2) -0.006(2) C8 0.038(3) 0.025(2) 0.035(3) 0.005(2) 0.014(2) -0.003(2) C9 0.030(3) 0.036(3) 0.033(3) 0.006(2) 0.002(2) 0.006(2) C10 0.032(3) 0.039(3) 0.023(3) 0.006(2) 0.004(2) 0.004(2) C11 0.043(3) 0.055(3) 0.028(3) -0.011(3) -0.004(2) -0.001(3) C12 0.042(3) 0.038(3) 0.050(4) -0.003(3) 0.015(3) 0.002(2) C13 0.030(3) 0.038(3) 0.024(3) 0.002(2) 0.004(2) 0.001(2) C14 0.027(2) 0.041(3) 0.029(3) 0.000(2) 0.008(2) -0.005(2) C15 0.033(3) 0.024(2) 0.028(3) 0.004(2) 0.010(2) 0.003(2) C16 0.034(3) 0.031(3) 0.025(3) 0.004(2) 0.006(2) 0.006(2) C17 0.030(2) 0.019(2) 0.017(3) 0.0007(19) 0.006(2) 0.0036(19) C18 0.026(2) 0.026(2) 0.019(2) -0.001(2) 0.0019(19) 0.007(2) C19 0.040(3) 0.031(3) 0.024(3) 0.005(2) 0.002(2) 0.007(2) C20 0.048(3) 0.046(3) 0.020(3) -0.003(2) -0.012(2) 0.002(2) C21 0.047(3) 0.044(3) 0.023(3) 0.000(2) -0.009(2) -0.004(2) C22 0.044(3) 0.033(3) 0.032(3) 0.006(2) -0.004(2) -0.002(2) C23 0.031(3) 0.032(3) 0.026(3) 0.000(2) 0.000(2) 0.004(2) C24 0.033(3) 0.046(3) 0.046(4) 0.008(3) 0.010(2) -0.011(2) C25 0.027(2) 0.031(3) 0.026(3) 0.003(2) 0.004(2) -0.001(2) C26 0.050(3) 0.037(3) 0.041(3) -0.006(2) 0.016(3) 0.010(2) P1 0.0378(7) 0.0332(7) 0.0244(8) -0.0018(6) 0.0015(6) 0.0007(6) F11 0.068(2) 0.080(2) 0.0347(19) -0.0023(17) 0.0181(16) -0.0107(18) F12 0.095(3) 0.0452(18) 0.069(3) -0.0111(17) -0.009(2) 0.0322(18) F13 0.096(3) 0.069(2) 0.042(2) 0.0058(17) 0.0317(19) -0.0060(19) F14 0.0505(18) 0.0330(15) 0.057(2) -0.0050(14) -0.0084(15) 0.0065(13) F15 0.0548(19) 0.0505(18) 0.056(2) -0.0160(16) -0.0099(16) -0.0140(15) F16 0.0375(16) 0.081(2) 0.053(2) -0.0268(18) -0.0152(15) 0.0011(16) P2 0.0357(8) 0.0652(10) 0.0300(8) -0.0056(7) 0.0041(6) -0.0052(7) F21 0.0360(19) 0.203(5) 0.103(3) -0.094(3) 0.012(2) -0.019(2) F22 0.158(4) 0.111(3) 0.048(3) 0.009(2) 0.035(3) -0.043(3) F23 0.128(3) 0.082(3) 0.048(2) 0.017(2) 0.019(2) 0.025(2) F24 0.049(2) 0.133(3) 0.075(3) -0.022(2) -0.0113(19) -0.022(2) F25 0.074(2) 0.066(2) 0.058(2) -0.0062(18) 0.0106(18) 0.0195(18) F26 0.091(3) 0.096(3) 0.084(3) -0.046(2) 0.015(2) 0.020(2) O1E 0.057(2) 0.053(2) 0.039(2) -0.0153(19) -0.0107(19) 0.0120(19) C1E 0.156(8) 0.098(6) 0.092(6) -0.059(5) -0.039(6) 0.058(6) C2E 0.064(4) 0.061(4) 0.064(5) -0.008(3) -0.005(3) 0.020(3) C3E 0.039(3) 0.060(4) 0.035(3) 0.005(3) -0.004(2) -0.014(3) C4E 0.073(4) 0.051(3) 0.048(4) -0.012(3) 0.000(3) -0.016(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 Ru N5 2.032(4) . ? Ru N6 2.037(4) . ? Ru N3 2.043(3) . ? Ru N2 2.046(3) . ? Ru N1 2.067(3) . ? Ru N4 2.067(3) . ? N1 C5 1.356(5) . ? N1 C1 1.348(5) . ? N2 C10 1.346(5) . ? N2 C6 1.361(5) . ? N3 C13 1.350(5) . ? N3 C17 1.360(5) . ? N4 C22 1.341(5) . ? N4 C18 1.356(5) . ? N5 C23 1.134(5) . ? N6 C25 1.145(5) . ? C1 C2 1.379(6) . ? C2 C3 1.374(6) . ? C3 C4 1.390(6) . ? C3 C11 1.506(6) . ? C4 C5 1.379(6) . ? C5 C6 1.479(6) . ? C6 C7 1.384(6) . ? C7 C8 1.387(6) . ? C8 C9 1.374(6) . ? C8 C12 1.514(6) . ? C9 C10 1.378(6) . ? C13 C14 1.388(6) . ? C14 C15 1.371(6) . ? C15 C16 1.379(6) . ? C16 C17 1.384(6) . ? C17 C18 1.471(6) . ? C18 C19 1.375(6) . ? C19 C20 1.374(6) . ? C20 C21 1.382(6) . ? C21 C22 1.381(6) . ? C23 C24 1.468(6) . ? C25 C26 1.451(6) . ? P1 F12 1.582(3) . ? P1 F16 1.587(3) . ? P1 F13 1.589(3) . ? P1 F15 1.598(3) . ? P1 F14 1.596(3) . ? P1 F11 1.596(3) . ? P2 F21 1.568(3) . ? P2 F22 1.572(4) . ? P2 F26 1.575(3) . ? P2 F24 1.575(3) . ? P2 F23 1.578(4) . ? P2 F25 1.600(3) . ? O1E C3E 1.406(6) . ? O1E C2E 1.425(6) . ? C1E C2E 1.480(8) . ? C3E C4E 1.499(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 N5 Ru N6 90.35(13) . . ? N5 Ru N3 176.04(14) . . ? N6 Ru N3 89.66(13) . . ? N5 Ru N2 89.88(13) . . ? N6 Ru N2 175.34(14) . . ? N3 Ru N2 90.43(13) . . ? N5 Ru N1 89.67(13) . . ? N6 Ru N1 96.65(14) . . ? N3 Ru N1 94.26(13) . . ? N2 Ru N1 78.70(14) . . ? N5 Ru N4 97.30(14) . . ? N6 Ru N4 88.80(13) . . ? N3 Ru N4 78.74(14) . . ? N2 Ru N4 95.79(14) . . ? N1 Ru N4 171.14(13) . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Ru 115.5(3) . . ? C1 N1 Ru 126.0(3) . . ? C10 N2 C6 117.9(4) . . ? C10 N2 Ru 126.0(3) . . ? C6 N2 Ru 116.1(3) . . ? C13 N3 C17 118.3(4) . . ? C13 N3 Ru 125.6(3) . . ? C17 N3 Ru 116.1(3) . . ? C22 N4 C18 118.5(4) . . ? C22 N4 Ru 126.0(3) . . ? C18 N4 Ru 115.4(3) . . ? C23 N5 Ru 177.4(4) . . ? C25 N6 Ru 177.8(4) . . ? N1 C1 C2 122.1(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 117.0(4) . . ? C2 C3 C11 121.7(4) . . ? C4 C3 C11 121.3(4) . . ? C5 C4 C3 121.0(4) . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 114.4(4) . . ? C4 C5 C6 124.6(4) . . ? N2 C6 C7 121.3(4) . . ? N2 C6 C5 114.6(4) . . ? C7 C6 C5 124.1(4) . . ? C6 C7 C8 120.3(4) . . ? C9 C8 C7 117.8(4) . . ? C9 C8 C12 121.2(4) . . ? C7 C8 C12 120.9(4) . . ? C8 C9 C10 119.9(4) . . ? N2 C10 C9 122.7(4) . . ? N3 C13 C14 122.4(4) . . ? C15 C14 C13 119.3(4) . . ? C14 C15 C16 118.6(4) . . ? C15 C16 C17 120.4(4) . . ? N3 C17 C16 120.9(4) . . ? N3 C17 C18 114.8(4) . . ? C16 C17 C18 124.3(4) . . ? N4 C18 C19 121.6(4) . . ? N4 C18 C17 114.7(4) . . ? C19 C18 C17 123.7(4) . . ? C20 C19 C18 119.3(4) . . ? C19 C20 C21 119.8(4) . . ? C22 C21 C20 118.2(4) . . ? N4 C22 C21 122.6(4) . . ? N5 C23 C24 178.4(5) . . ? N6 C25 C26 179.3(5) . . ? F12 P1 F16 90.69(18) . . ? F12 P1 F13 90.21(19) . . ? F16 P1 F13 90.61(18) . . ? F12 P1 F15 89.93(17) . . ? F16 P1 F15 178.87(19) . . ? F13 P1 F15 90.33(18) . . ? F12 P1 F14 179.5(2) . . ? F16 P1 F14 89.58(16) . . ? F13 P1 F14 89.35(17) . . ? F15 P1 F14 89.80(15) . . ? F12 P1 F11 90.27(19) . . ? F16 P1 F11 89.78(17) . . ? F13 P1 F11 179.4(2) . . ? F15 P1 F11 89.27(17) . . ? F14 P1 F11 90.17(17) . . ? F21 P2 F22 90.6(2) . . ? F21 P2 F26 90.2(2) . . ? F22 P2 F26 89.4(2) . . ? F21 P2 F24 179.6(2) . . ? F22 P2 F24 89.4(2) . . ? F26 P2 F24 90.2(2) . . ? F21 P2 F23 90.3(3) . . ? F22 P2 F23 178.9(3) . . ? F26 P2 F23 91.3(2) . . ? F24 P2 F23 89.7(2) . . ? F21 P2 F25 89.35(19) . . ? F22 P2 F25 90.5(2) . . ? F26 P2 F25 179.5(2) . . ? F24 P2 F25 90.3(2) . . ? F23 P2 F25 88.77(19) . . ? C3E O1E C2E 112.1(4) . . ? O1E C2E C1E 107.8(5) . . ? O1E C3E C4E 109.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.451 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.105