Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email han.vos@dcu.ie _publ_contact_author_name 'Prof Johannes Vos' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; School of Chemical Sciences Dublin City University Dublin 9 REPUBLIC OF IRELAND ; _publ_contact_author_phone '+353-1-7005307 ' _publ_contact_author_fax '+353-1-7005503 ' _publ_section_title ; Synthesis and Charakterisation of Ruthenium Complexes Containing a Pendent Catechol Ring ; loop_ _publ_author_name V.Johannes D.Marco G.Helmar 'G.Adrian L' K.Tia 'O.Noel M' O.Luke ; R.Sven ; S.Andreas data_FO893 _database_code_CSD 213441 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H29 F6 N8 O2 P Ru' _chemical_formula_weight 887.74 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 11.6379(9) _cell_length_b 19.473(2) _cell_length_c 16.8790(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.944(7) _cell_angle_gamma 90.00 _cell_volume 3728.0(5) _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 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8206 _exptl_absorpt_correction_T_max 0.8631 _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-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7896 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7631 _reflns_number_gt 4848 _reflns_threshold_expression >2sigma(I) _computing_data_collection DENZO _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^)+(0.0926P)^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 7631 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.029 _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 Ru Ru 0.90760(3) 0.76889(2) 0.03265(2) 0.03410(13) Uani 1 1 d . . . N1A N 1.0076(3) 0.6856(2) 0.0157(2) 0.0420(10) Uani 1 1 d . . . N2A N 0.8022(3) 0.7280(2) -0.0720(2) 0.0393(9) Uani 1 1 d . . . C1A C 1.1103(5) 0.6650(3) 0.0612(4) 0.0610(15) Uani 1 1 d . . . H1AA H 1.1442 0.6893 0.1096 0.073 Uiso 1 1 calc R . . C2A C 1.1687(6) 0.6085(4) 0.0391(5) 0.089(2) Uani 1 1 d . . . H2AA H 1.2403 0.5933 0.0737 0.107 Uiso 1 1 calc R . . C3A C 1.1248(7) 0.5748(4) -0.0310(5) 0.100(3) Uani 1 1 d . . . H3AA H 1.1683 0.5383 -0.0474 0.120 Uiso 1 1 calc R . . C4A C 1.0172(6) 0.5931(3) -0.0788(4) 0.0729(19) Uani 1 1 d . . . C5A C 0.9594(8) 0.5595(4) -0.1537(5) 0.099(3) Uani 1 1 d . . . H5AA H 0.9983 0.5226 -0.1736 0.119 Uiso 1 1 calc R . . C6A C 0.8538(7) 0.5788(4) -0.1952(5) 0.090(2) Uani 1 1 d . . . H6AA H 0.8166 0.5540 -0.2425 0.108 Uiso 1 1 calc R . . C7A C 0.7955(6) 0.6363(3) -0.1699(3) 0.0594(15) Uani 1 1 d . . . C8A C 0.6810(6) 0.6587(4) -0.2097(4) 0.0674(18) Uani 1 1 d . . . H8AA H 0.6384 0.6346 -0.2560 0.081 Uiso 1 1 calc R . . C9A C 0.6332(5) 0.7136(3) -0.1820(3) 0.0585(16) Uani 1 1 d . . . H9AA H 0.5569 0.7288 -0.2089 0.070 Uiso 1 1 calc R . . C10A C 0.6961(5) 0.7484(3) -0.1134(3) 0.0487(13) Uani 1 1 d . . . H10A H 0.6619 0.7881 -0.0955 0.058 Uiso 1 1 calc R . . C11A C 0.8501(4) 0.6724(3) -0.1003(3) 0.0454(12) Uani 1 1 d . . . C12A C 0.9610(5) 0.6497(3) -0.0535(3) 0.0480(13) Uani 1 1 d . . . N1B N 0.9861(3) 0.8348(2) -0.0345(2) 0.0413(10) Uani 1 1 d . . . N2B N 0.8049(4) 0.8547(2) 0.0328(2) 0.0424(10) Uani 1 1 d . . . C1B C 1.0790(5) 0.8243(3) -0.0665(3) 0.0501(13) Uani 1 1 d . . . H1BA H 1.1187 0.7814 -0.0575 0.060 Uiso 1 1 calc R . . C2B C 1.1199(6) 0.8734(4) -0.1121(4) 0.0665(17) Uani 1 1 d . . . H2BA H 1.1873 0.8637 -0.1332 0.080 Uiso 1 1 calc R . . C3B C 1.0666(6) 0.9345(4) -0.1273(4) 0.0670(17) Uani 1 1 d . . . H3BA H 1.0955 0.9678 -0.1591 0.080 Uiso 1 1 calc R . . C4B C 0.9675(6) 0.9485(3) -0.0954(3) 0.0586(16) Uani 1 1 d . . . C5B C 0.9033(7) 1.0112(3) -0.1062(4) 0.0712(19) Uani 1 1 d . . . H5BA H 0.9272 1.0470 -0.1373 0.085 Uiso 1 1 calc R . . C6B C 0.8108(8) 1.0209(3) -0.0740(4) 0.079(2) Uani 1 1 d . . . H6BA H 0.7690 1.0631 -0.0833 0.094 Uiso 1 1 calc R . . C7B C 0.7721(5) 0.9692(3) -0.0253(3) 0.0592(15) Uani 1 1 d . . . C8B C 0.6760(7) 0.9761(4) 0.0131(4) 0.083(2) Uani 1 1 d . . . H8BA H 0.6294 1.0166 0.0063 0.099 Uiso 1 1 calc R . . C9B C 0.6519(6) 0.9237(4) 0.0595(4) 0.080(2) Uani 1 1 d . . . H9BA H 0.5883 0.9280 0.0859 0.096 Uiso 1 1 calc R . . C10B C 0.7177(5) 0.8641(3) 0.0691(3) 0.0603(15) Uani 1 1 d . . . H10B H 0.6993 0.8289 0.1032 0.072 Uiso 1 1 calc R . . C11B C 0.8333(5) 0.9073(3) -0.0140(3) 0.0439(12) Uani 1 1 d . . . C12B C 0.9295(4) 0.8972(2) -0.0480(3) 0.0421(12) Uani 1 1 d . . . N3 N 0.8306(3) 0.7114(2) 0.1116(2) 0.0406(10) Uani 1 1 d . . . N4 N 1.0125(3) 0.7928(2) 0.1428(2) 0.0390(9) Uani 1 1 d . . . N5 N 1.1142(3) 0.8290(2) 0.1703(2) 0.0434(10) Uani 1 1 d . . . N6 N 1.0682(4) 0.7719(2) 0.2757(2) 0.0469(10) Uani 1 1 d . . . C13 C 0.7350(4) 0.6718(3) 0.0909(3) 0.0491(13) Uani 1 1 d . . . H13A H 0.6951 0.6691 0.0354 0.059 Uiso 1 1 calc R . . C14 C 0.6930(5) 0.6353(3) 0.1464(3) 0.0596(16) Uani 1 1 d . . . H14A H 0.6240 0.6082 0.1296 0.071 Uiso 1 1 calc R . . C15 C 0.7497(5) 0.6373(3) 0.2272(3) 0.0639(17) Uani 1 1 d . . . H15A H 0.7211 0.6114 0.2664 0.077 Uiso 1 1 calc R . . C16 C 0.8487(4) 0.6776(3) 0.2498(3) 0.0521(14) Uani 1 1 d . . . H16A H 0.8897 0.6799 0.3051 0.062 Uiso 1 1 calc R . . C17 C 0.8877(4) 0.7147(3) 0.1914(3) 0.0394(11) Uani 1 1 d . . . C18 C 0.9894(4) 0.7596(3) 0.2063(3) 0.0401(11) Uani 1 1 d . . . C19 C 1.1434(4) 0.8153(3) 0.2506(3) 0.0446(12) Uani 1 1 d . . . C20 C 1.2487(4) 0.8440(3) 0.3041(3) 0.0473(13) Uani 1 1 d . . . C21 C 1.3017(4) 0.8078(3) 0.3741(3) 0.0502(13) Uani 1 1 d . . . H21A H 1.2682 0.7657 0.3865 0.060 Uiso 1 1 calc R . . C22 C 1.4026(4) 0.8328(3) 0.4254(3) 0.0530(14) Uani 1 1 d . . . C23 C 1.4524(5) 0.8946(3) 0.4056(3) 0.0506(13) Uani 1 1 d . . . C24 C 1.4000(5) 0.9296(3) 0.3366(4) 0.0625(17) Uani 1 1 d . . . H24A H 1.4338 0.9711 0.3227 0.075 Uiso 1 1 calc R . . C25 C 1.2977(5) 0.9043(3) 0.2874(3) 0.0631(17) Uani 1 1 d . . . H25A H 1.2604 0.9297 0.2406 0.076 Uiso 1 1 calc R . . O1 O 1.4620(4) 0.8012(3) 0.4944(3) 0.0871(16) Uani 1 1 d . . . C26 C 1.4171(7) 0.7414(4) 0.5186(5) 0.111(4) Uani 1 1 d . . . H26A H 1.4691 0.7249 0.5688 0.167 Uiso 1 1 calc R . . H26B H 1.4117 0.7067 0.4760 0.167 Uiso 1 1 calc R . . H26C H 1.3384 0.7502 0.5282 0.167 Uiso 1 1 calc R . . O2 O 1.5539(4) 0.9139(2) 0.4596(3) 0.0748(14) Uani 1 1 d . . . C27 C 1.6109(6) 0.9735(4) 0.4409(5) 0.088(2) Uani 1 1 d . . . H27A H 1.6819 0.9817 0.4836 0.132 Uiso 1 1 calc R . . H27B H 1.5575 1.0128 0.4376 0.132 Uiso 1 1 calc R . . H27C H 1.6330 0.9674 0.3887 0.132 Uiso 1 1 calc R . . P P 0.41869(17) 0.90904(11) -0.21117(12) 0.0743(5) Uani 1 1 d . . . F1 F 0.4027(12) 0.9220(8) -0.1212(8) 0.113(5) Uiso 0.50 1 d P A 1 F2 F 0.4385(13) 0.9905(6) -0.2070(7) 0.130(4) Uiso 0.50 1 d P A 1 F3 F 0.2836(10) 0.9173(7) -0.2520(7) 0.123(4) Uiso 0.50 1 d P A 1 F4 F 0.4367(13) 0.8974(8) -0.3014(9) 0.126(5) Uiso 0.50 1 d P A 1 F5 F 0.4027(13) 0.8313(6) -0.2117(7) 0.131(4) Uiso 0.50 1 d P A 1 F6 F 0.5549(9) 0.8964(6) -0.1700(6) 0.104(3) Uiso 0.50 1 d P A 1 F1A F 0.3929(14) 0.8936(8) -0.1225(10) 0.140(6) Uiso 0.50 1 d P A 2 F2A F 0.5240(15) 0.9634(9) -0.1855(9) 0.174(6) Uiso 0.50 1 d P A 2 F3A F 0.3167(15) 0.9606(9) -0.2208(10) 0.172(6) Uiso 0.50 1 d P A 2 F4A F 0.4415(12) 0.9257(8) -0.2958(8) 0.116(5) Uiso 0.50 1 d P A 2 F5A F 0.3170(13) 0.8526(8) -0.2401(8) 0.149(4) Uiso 0.50 1 d P A 2 F6A F 0.5114(14) 0.8523(8) -0.1906(8) 0.153(5) Uiso 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0324(2) 0.0397(2) 0.02670(18) 0.00212(18) -0.00080(13) -0.00104(19) N1A 0.038(2) 0.045(2) 0.039(2) 0.0040(18) -0.0004(17) 0.0069(18) N2A 0.039(2) 0.045(2) 0.0290(18) 0.0025(18) -0.0011(16) -0.004(2) C1A 0.056(3) 0.061(4) 0.059(3) 0.005(3) -0.003(3) 0.016(3) C2A 0.074(5) 0.086(5) 0.093(5) 0.003(4) -0.010(4) 0.040(4) C3A 0.096(6) 0.077(5) 0.111(6) -0.023(5) -0.009(5) 0.046(4) C4A 0.073(4) 0.066(4) 0.072(4) -0.017(3) 0.001(3) 0.021(3) C5A 0.115(7) 0.068(5) 0.105(6) -0.040(5) 0.003(5) 0.023(5) C6A 0.092(5) 0.088(5) 0.078(5) -0.043(4) -0.004(4) 0.008(4) C7A 0.070(4) 0.062(4) 0.041(3) -0.009(3) 0.001(3) -0.002(3) C8A 0.068(4) 0.083(5) 0.042(3) -0.014(3) -0.008(3) -0.014(4) C9A 0.054(3) 0.079(4) 0.034(3) 0.003(3) -0.007(2) 0.000(3) C10A 0.041(3) 0.062(4) 0.038(3) 0.000(2) -0.001(2) 0.006(2) C11A 0.047(3) 0.049(3) 0.040(3) -0.001(2) 0.007(2) -0.003(2) C12A 0.052(3) 0.043(3) 0.046(3) -0.003(2) 0.006(2) 0.002(2) N1B 0.043(2) 0.051(3) 0.0259(18) 0.0020(17) -0.0004(17) -0.0045(19) N2B 0.043(2) 0.044(2) 0.036(2) -0.0040(18) -0.0018(18) 0.0039(19) C1B 0.047(3) 0.059(3) 0.043(3) 0.003(3) 0.007(2) -0.004(3) C2B 0.060(4) 0.089(5) 0.052(3) 0.000(3) 0.016(3) -0.017(4) C3B 0.071(4) 0.077(5) 0.051(3) 0.011(3) 0.010(3) -0.024(4) C4B 0.075(4) 0.053(3) 0.037(3) 0.010(2) -0.011(3) -0.018(3) C5B 0.107(6) 0.046(4) 0.050(3) 0.009(3) -0.007(4) -0.004(4) C6B 0.113(6) 0.041(3) 0.060(4) 0.002(3) -0.028(4) 0.017(4) C7B 0.064(4) 0.056(4) 0.047(3) -0.005(3) -0.009(3) 0.015(3) C8B 0.091(5) 0.071(5) 0.070(4) -0.013(4) -0.016(4) 0.031(4) C9B 0.073(5) 0.101(6) 0.068(4) -0.009(4) 0.022(4) 0.030(4) C10B 0.055(3) 0.080(4) 0.047(3) 0.004(3) 0.013(3) 0.015(3) C11B 0.052(3) 0.044(3) 0.028(2) -0.001(2) -0.008(2) 0.004(2) C12B 0.048(3) 0.037(3) 0.033(2) 0.002(2) -0.007(2) -0.003(2) N3 0.038(2) 0.048(2) 0.0311(19) 0.0026(17) -0.0025(17) -0.0022(17) N4 0.034(2) 0.043(2) 0.036(2) 0.0051(17) -0.0020(17) -0.0069(17) N5 0.038(2) 0.045(2) 0.042(2) 0.0052(18) -0.0040(17) -0.0101(18) N6 0.040(2) 0.060(3) 0.033(2) 0.006(2) -0.0075(17) -0.011(2) C13 0.043(3) 0.059(3) 0.038(3) 0.003(2) -0.009(2) -0.015(3) C14 0.044(3) 0.079(4) 0.051(3) 0.006(3) -0.001(2) -0.029(3) C15 0.056(3) 0.086(5) 0.047(3) 0.017(3) 0.007(3) -0.021(3) C16 0.042(3) 0.073(4) 0.038(3) 0.006(3) 0.001(2) -0.012(3) C17 0.029(2) 0.054(3) 0.032(2) 0.004(2) -0.0013(18) -0.004(2) C18 0.037(2) 0.051(3) 0.029(2) 0.005(2) -0.0003(18) -0.007(2) C19 0.042(3) 0.047(3) 0.039(3) 0.007(2) -0.003(2) -0.005(2) C20 0.043(3) 0.055(3) 0.037(3) 0.002(2) -0.007(2) -0.013(2) C21 0.044(3) 0.056(3) 0.045(3) 0.010(3) -0.004(2) -0.011(3) C22 0.040(3) 0.062(4) 0.048(3) 0.012(3) -0.008(2) -0.008(3) C23 0.042(3) 0.047(3) 0.053(3) 0.001(2) -0.010(2) -0.007(2) C24 0.053(3) 0.055(3) 0.066(4) 0.014(3) -0.015(3) -0.024(3) C25 0.066(4) 0.061(4) 0.048(3) 0.014(3) -0.017(3) -0.015(3) O1 0.064(3) 0.100(3) 0.073(3) 0.043(3) -0.037(2) -0.026(3) C26 0.087(5) 0.116(6) 0.101(6) 0.076(5) -0.041(5) -0.031(5) O2 0.054(2) 0.074(3) 0.074(3) 0.013(2) -0.034(2) -0.024(2) C27 0.070(4) 0.081(5) 0.093(5) 0.010(4) -0.024(4) -0.040(4) P 0.0657(11) 0.0858(14) 0.0796(12) 0.0162(10) 0.0336(9) 0.0227(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N4 2.036(4) . ? Ru N1A 2.054(4) . ? Ru N2B 2.054(4) . ? Ru N1B 2.057(4) . ? Ru N2A 2.071(4) . ? Ru N3 2.089(4) . ? N1A C1A 1.330(6) . ? N1A C12A 1.365(6) . ? N2A C10A 1.336(6) . ? N2A C11A 1.353(6) . ? C1A C2A 1.388(9) . ? C2A C3A 1.349(10) . ? C3A C4A 1.377(9) . ? C4A C12A 1.395(8) . ? C4A C5A 1.448(9) . ? C5A C6A 1.326(10) . ? C6A C7A 1.423(9) . ? C7A C11A 1.394(7) . ? C7A C8A 1.420(8) . ? C8A C9A 1.337(9) . ? C9A C10A 1.400(7) . ? C11A C12A 1.425(7) . ? N1B C1B 1.327(6) . ? N1B C12B 1.378(6) . ? N2B C10B 1.312(7) . ? N2B C11B 1.378(6) . ? C1B C2B 1.377(8) . ? C2B C3B 1.339(9) . ? C3B C4B 1.404(9) . ? C4B C12B 1.411(7) . ? C4B C5B 1.423(9) . ? C5B C6B 1.324(11) . ? C6B C7B 1.435(10) . ? C7B C11B 1.391(7) . ? C7B C8B 1.418(10) . ? C8B C9B 1.353(11) . ? C9B C10B 1.379(9) . ? C11B C12B 1.382(7) . ? N3 C13 1.335(6) . ? N3 C17 1.363(5) . ? N4 C18 1.328(6) . ? N4 N5 1.367(5) . ? N5 C19 1.347(6) . ? N6 C18 1.339(5) . ? N6 C19 1.350(6) . ? C13 C14 1.351(7) . ? C14 C15 1.375(7) . ? C15 C16 1.376(7) . ? C16 C17 1.379(7) . ? C17 C18 1.447(6) . ? C19 C20 1.462(6) . ? C20 C25 1.361(8) . ? C20 C21 1.396(7) . ? C21 C22 1.382(7) . ? C22 O1 1.362(6) . ? C22 C23 1.408(7) . ? C23 C24 1.369(7) . ? C23 O2 1.373(6) . ? C24 C25 1.382(7) . ? O1 C26 1.375(8) . ? O2 C27 1.406(7) . ? P F5 1.524(13) . ? P F6A 1.530(14) . ? P F3A 1.536(16) . ? P F4A 1.545(14) . ? P F3 1.577(12) . ? P F1 1.591(14) . ? P F4 1.600(15) . ? P F6 1.601(10) . ? P F2 1.603(12) . ? P F2A 1.603(16) . ? P F5A 1.609(14) . ? P F1A 1.619(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru N1A 93.73(16) . . ? N4 Ru N2B 92.47(15) . . ? N1A Ru N2B 172.10(15) . . ? N4 Ru N1B 96.42(15) . . ? N1A Ru N1B 94.58(17) . . ? N2B Ru N1B 79.86(17) . . ? N4 Ru N2A 170.42(15) . . ? N1A Ru N2A 79.83(15) . . ? N2B Ru N2A 94.59(16) . . ? N1B Ru N2A 91.19(15) . . ? N4 Ru N3 78.16(15) . . ? N1A Ru N3 90.17(16) . . ? N2B Ru N3 95.88(17) . . ? N1B Ru N3 173.03(15) . . ? N2A Ru N3 94.66(15) . . ? C1A N1A C12A 118.2(5) . . ? C1A N1A Ru 128.5(4) . . ? C12A N1A Ru 113.3(3) . . ? C10A N2A C11A 117.3(4) . . ? C10A N2A Ru 129.3(4) . . ? C11A N2A Ru 113.4(3) . . ? N1A C1A C2A 121.0(6) . . ? C3A C2A C1A 120.6(6) . . ? C2A C3A C4A 120.3(7) . . ? C3A C4A C12A 116.9(6) . . ? C3A C4A C5A 125.3(7) . . ? C12A C4A C5A 117.8(6) . . ? C6A C5A C4A 121.8(7) . . ? C5A C6A C7A 120.8(6) . . ? C11A C7A C8A 116.6(5) . . ? C11A C7A C6A 119.5(6) . . ? C8A C7A C6A 124.0(6) . . ? C9A C8A C7A 120.0(5) . . ? C8A C9A C10A 119.7(5) . . ? N2A C10A C9A 122.6(5) . . ? N2A C11A C7A 123.7(5) . . ? N2A C11A C12A 116.5(4) . . ? C7A C11A C12A 119.7(5) . . ? N1A C12A C4A 122.9(5) . . ? N1A C12A C11A 116.9(5) . . ? C4A C12A C11A 120.2(5) . . ? C1B N1B C12B 118.1(5) . . ? C1B N1B Ru 129.1(4) . . ? C12B N1B Ru 112.7(3) . . ? C10B N2B C11B 118.2(5) . . ? C10B N2B Ru 128.8(4) . . ? C11B N2B Ru 113.0(3) . . ? N1B C1B C2B 122.3(6) . . ? C3B C2B C1B 121.4(6) . . ? C2B C3B C4B 119.0(6) . . ? C3B C4B C12B 117.9(6) . . ? C3B C4B C5B 124.9(6) . . ? C12B C4B C5B 117.2(6) . . ? C6B C5B C4B 121.5(6) . . ? C5B C6B C7B 121.6(6) . . ? C11B C7B C8B 116.8(6) . . ? C11B C7B C6B 118.0(6) . . ? C8B C7B C6B 125.2(6) . . ? C9B C8B C7B 118.7(6) . . ? C8B C9B C10B 121.4(7) . . ? N2B C10B C9B 122.0(6) . . ? N2B C11B C12B 116.9(4) . . ? N2B C11B C7B 122.8(5) . . ? C12B C11B C7B 120.3(5) . . ? N1B C12B C11B 117.3(5) . . ? N1B C12B C4B 121.3(5) . . ? C11B C12B C4B 121.4(5) . . ? C13 N3 C17 118.6(4) . . ? C13 N3 Ru 126.5(3) . . ? C17 N3 Ru 114.9(3) . . ? C18 N4 N5 107.1(4) . . ? C18 N4 Ru 115.9(3) . . ? N5 N4 Ru 136.4(3) . . ? C19 N5 N4 104.1(4) . . ? C18 N6 C19 101.7(4) . . ? N3 C13 C14 122.2(5) . . ? C13 C14 C15 120.3(5) . . ? C14 C15 C16 118.5(5) . . ? C15 C16 C17 119.3(5) . . ? N3 C17 C16 121.1(4) . . ? N3 C17 C18 113.5(4) . . ? C16 C17 C18 125.4(4) . . ? N4 C18 N6 113.3(4) . . ? N4 C18 C17 117.3(4) . . ? N6 C18 C17 129.3(4) . . ? N5 C19 N6 113.9(4) . . ? N5 C19 C20 122.2(5) . . ? N6 C19 C20 123.9(4) . . ? C25 C20 C21 119.0(5) . . ? C25 C20 C19 122.3(5) . . ? C21 C20 C19 118.6(5) . . ? C22 C21 C20 120.2(5) . . ? O1 C22 C21 125.0(5) . . ? O1 C22 C23 115.6(4) . . ? C21 C22 C23 119.4(5) . . ? C24 C23 O2 125.6(5) . . ? C24 C23 C22 119.9(5) . . ? O2 C23 C22 114.5(5) . . ? C23 C24 C25 119.6(5) . . ? C20 C25 C24 121.9(5) . . ? C22 O1 C26 118.8(5) . . ? C23 O2 C27 117.1(5) . . ? F5 P F6A 50.4(6) . . ? F5 P F3A 123.9(8) . . ? F6A P F3A 170.5(8) . . ? F5 P F4A 104.5(7) . . ? F6A P F4A 95.9(7) . . ? F3A P F4A 93.1(8) . . ? F5 P F3 89.5(7) . . ? F6A P F3 139.2(8) . . ? F3A P F3 38.3(6) . . ? F4A P F3 86.3(7) . . ? F5 P F1 97.0(7) . . ? F6A P F1 97.2(7) . . ? F3A P F1 75.2(8) . . ? F4A P F1 158.5(8) . . ? F3 P F1 94.7(7) . . ? F5 P F4 84.1(7) . . ? F6A P F4 83.0(7) . . ? F3A P F4 104.8(8) . . ? F4A P F4 20.4(7) . . ? F3 P F4 85.9(7) . . ? F1 P F4 178.7(8) . . ? F5 P F6 87.6(6) . . ? F6A P F6 37.9(6) . . ? F3A P F6 144.4(8) . . ? F4A P F6 94.3(6) . . ? F3 P F6 177.0(7) . . ? F1 P F6 85.8(6) . . ? F4 P F6 93.6(6) . . ? F5 P F2 177.7(7) . . ? F6A P F2 128.2(8) . . ? F3A P F2 57.1(7) . . ? F4A P F2 77.3(7) . . ? F3 P F2 92.1(7) . . ? F1 P F2 81.2(7) . . ? F4 P F2 97.7(7) . . ? F6 P F2 90.8(6) . . ? F5 P F2A 137.8(9) . . ? F6A P F2A 87.6(8) . . ? F3A P F2A 97.1(9) . . ? F4A P F2A 80.3(7) . . ? F3 P F2A 132.6(9) . . ? F1 P F2A 83.3(7) . . ? F4 P F2A 95.4(8) . . ? F6 P F2A 50.3(6) . . ? F2 P F2A 40.7(6) . . ? F5 P F5A 40.5(6) . . ? F6A P F5A 90.5(8) . . ? F3A P F5A 85.2(8) . . ? F4A P F5A 97.5(7) . . ? F3 P F5A 49.0(6) . . ? F1 P F5A 99.4(7) . . ? F4 P F5A 81.9(7) . . ? F6 P F5A 128.1(7) . . ? F2 P F5A 141.1(8) . . ? F2A P F5A 176.9(8) . . ? F5 P F1A 76.9(7) . . ? F6A P F1A 85.6(8) . . ? F3A P F1A 85.5(8) . . ? F4A P F1A 178.4(8) . . ? F3 P F1A 92.9(7) . . ? F1 P F1A 20.2(7) . . ? F4 P F1A 160.9(8) . . ? F6 P F1A 86.6(7) . . ? F2 P F1A 101.4(7) . . ? F2A P F1A 99.3(8) . . ? F5A P F1A 83.0(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.996 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.098 #=== END data_FO895 _database_code_CSD 213442 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H29 F6 N8 O2 P Ru * H2 O' _chemical_formula_weight 857.72 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1165(9) _cell_length_b 18.068(1) _cell_length_c 21.424(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.599(6) _cell_angle_gamma 90.00 _cell_volume 3505.5(4) _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 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8375 _exptl_absorpt_correction_T_max 0.8938 _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 7295 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.31 _reflns_number_total 7105 _reflns_number_gt 4810 _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^)+(0.0871P)^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/difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7105 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.191 _refine_ls_shift/su_mean 0.004 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 0.85097(3) 0.183930(18) 0.812679(16) 0.03629(12) Uani 1 1 d . . . N1A N 0.8967(4) 0.25132(19) 0.88999(17) 0.0402(8) Uani 1 1 d . . . N2A N 0.7407(4) 0.27840(19) 0.78293(17) 0.0412(8) Uani 1 1 d . . . C1A C 0.9883(5) 0.2373(3) 0.9413(2) 0.0467(11) Uani 1 1 d . . . H1AA H 1.0497 0.1947 0.9420 0.056 Uiso 1 1 calc R . . C2A C 0.9978(6) 0.2826(3) 0.9939(3) 0.0639(14) Uani 1 1 d . . . H2AA H 1.0652 0.2715 1.0299 0.077 Uiso 1 1 calc R . . C3A C 0.9082(7) 0.3436(3) 0.9930(3) 0.0675(15) Uani 1 1 d . . . H3AA H 0.9111 0.3746 1.0290 0.081 Uiso 1 1 calc R . . C4A C 0.8153(6) 0.3594(3) 0.9405(3) 0.0597(13) Uani 1 1 d . . . H4AA H 0.7534 0.4018 0.9394 0.072 Uiso 1 1 calc R . . C5A C 0.8111(5) 0.3142(2) 0.8890(2) 0.0460(10) Uani 1 1 d . . . C6A C 0.7256(5) 0.3295(2) 0.8272(2) 0.0455(11) Uani 1 1 d . . . C7A C 0.6398(5) 0.3922(3) 0.8143(3) 0.0553(13) Uani 1 1 d . . . H7AA H 0.6251 0.4262 0.8468 0.066 Uiso 1 1 calc R . . C8A C 0.5765(5) 0.4047(3) 0.7539(3) 0.0629(15) Uani 1 1 d . . . H8AA H 0.5180 0.4475 0.7443 0.075 Uiso 1 1 calc R . . C9A C 0.5980(6) 0.3552(3) 0.7081(3) 0.0607(14) Uani 1 1 d . . . H9AA H 0.5578 0.3639 0.6658 0.073 Uiso 1 1 calc R . . C10A C 0.6787(5) 0.2923(3) 0.7237(2) 0.0508(12) Uani 1 1 d . . . H10A H 0.6915 0.2573 0.6917 0.061 Uiso 1 1 calc R . . N1B N 1.0297(4) 0.2085(2) 0.76661(18) 0.0425(8) Uani 1 1 d . . . N2B N 0.8008(4) 0.12713(19) 0.73056(17) 0.0458(9) Uani 1 1 d . . . C1B C 1.1398(5) 0.2549(3) 0.7874(2) 0.0499(11) Uani 1 1 d . . . H1BA H 1.1343 0.2818 0.8251 0.060 Uiso 1 1 calc R . . C2B C 1.2592(6) 0.2639(3) 0.7552(3) 0.0660(15) Uani 1 1 d . . . H2BA H 1.3339 0.2985 0.7698 0.079 Uiso 1 1 calc R . . C3B C 1.2721(6) 0.2250(4) 0.7038(3) 0.0802(18) Uani 1 1 d . . . H3BA H 1.3581 0.2300 0.6829 0.096 Uiso 1 1 calc R . . C4B C 1.1596(7) 0.1764(4) 0.6799(3) 0.0750(18) Uani 1 1 d . . . H4BA H 1.1668 0.1484 0.6428 0.090 Uiso 1 1 calc R . . C5B C 1.0373(6) 0.1707(3) 0.7126(2) 0.0517(12) Uani 1 1 d . . . C6B C 0.9047(6) 0.1282(2) 0.6912(2) 0.0518(12) Uani 1 1 d . . . C7B C 0.8751(8) 0.0957(3) 0.6316(3) 0.0741(17) Uani 1 1 d . . . H7BA H 0.9485 0.0966 0.6035 0.089 Uiso 1 1 calc R . . C8B C 0.7436(9) 0.0632(3) 0.6137(3) 0.085(2) Uani 1 1 d . . . H8BA H 0.7241 0.0415 0.5732 0.102 Uiso 1 1 calc R . . C9B C 0.6403(8) 0.0620(3) 0.6540(3) 0.0800(19) Uani 1 1 d . . . H9BA H 0.5469 0.0397 0.6421 0.096 Uiso 1 1 calc R . . C10B C 0.6716(6) 0.0931(3) 0.7118(3) 0.0643(15) Uani 1 1 d . . . H10B H 0.5992 0.0906 0.7402 0.077 Uiso 1 1 calc R . . C11 C 0.5419(5) 0.1692(3) 0.8583(3) 0.0548(13) Uani 1 1 d . . . H11A H 0.5185 0.2136 0.8356 0.066 Uiso 1 1 calc R . . N3 N 0.6780(4) 0.1407(2) 0.85878(17) 0.0416(8) Uani 1 1 d . . . N4 N 0.9437(4) 0.09063(18) 0.85362(15) 0.0363(7) Uani 1 1 d . . . N5 N 1.0751(4) 0.05401(18) 0.85354(16) 0.0385(8) Uani 1 1 d . . . N6 N 0.9247(4) -0.01143(18) 0.91017(16) 0.0380(8) Uani 1 1 d . . . C12 C 0.4349(5) 0.1365(3) 0.8896(3) 0.0601(13) Uani 1 1 d . . . H12A H 0.3390 0.1576 0.8876 0.072 Uiso 1 1 calc R . . C13 C 0.4681(5) 0.0738(3) 0.9233(2) 0.0521(12) Uani 1 1 d . . . H13A H 0.3962 0.0512 0.9458 0.063 Uiso 1 1 calc R . . C14 C 0.6065(5) 0.0432(3) 0.9245(2) 0.0486(11) Uani 1 1 d . . . H14A H 0.6314 -0.0007 0.9478 0.058 Uiso 1 1 calc R . . C15 C 0.7093(4) 0.0776(2) 0.89109(19) 0.0367(9) Uani 1 1 d . . . C16 C 0.8582(4) 0.0503(2) 0.88699(19) 0.0357(9) Uani 1 1 d . . . C17 C 1.0579(4) -0.0063(2) 0.88861(19) 0.0358(9) Uani 1 1 d . . . C18 C 1.1739(4) -0.0633(2) 0.89914(19) 0.0377(9) Uani 1 1 d . . . C19 C 1.1718(5) -0.1138(2) 0.9470(2) 0.0444(10) Uani 1 1 d . . . H19A H 1.0947 -0.1127 0.9733 0.053 Uiso 1 1 calc R . . C20 C 1.2837(5) -0.1670(2) 0.9569(2) 0.0482(11) Uani 1 1 d . . . H20A H 1.2815 -0.2021 0.9898 0.058 Uiso 1 1 calc R . . C21 C 1.3962(5) -0.1691(2) 0.9198(2) 0.0467(11) Uani 1 1 d . . . C22 C 1.3961(5) -0.1186(2) 0.8700(2) 0.0451(10) Uani 1 1 d . . . C23 C 1.2859(4) -0.0669(2) 0.8598(2) 0.0416(10) Uani 1 1 d . . . H23A H 1.2855 -0.0333 0.8257 0.050 Uiso 1 1 calc R . . O1 O 1.5110(4) -0.1257(2) 0.83495(18) 0.0642(10) Uani 1 1 d . . . C24 C 1.5128(6) -0.0762(3) 0.7830(3) 0.0680(15) Uani 1 1 d . . . H24A H 1.5990 -0.0869 0.7610 0.102 Uiso 1 1 calc R . . H24B H 1.5183 -0.0251 0.7983 0.102 Uiso 1 1 calc R . . H24C H 1.4225 -0.0828 0.7540 0.102 Uiso 1 1 calc R . . O2 O 1.5111(4) -0.2183(2) 0.92640(17) 0.0617(9) Uani 1 1 d . . . C25 C 1.5196(7) -0.2683(3) 0.9775(3) 0.0792(18) Uani 1 1 d . . . H25A H 1.6061 -0.3003 0.9766 0.119 Uiso 1 1 calc R . . H25B H 1.4300 -0.2987 0.9743 0.119 Uiso 1 1 calc R . . H25C H 1.5285 -0.2405 1.0171 0.119 Uiso 1 1 calc R . . P P 1.2792(2) 0.44461(10) 0.90464(8) 0.0753(5) Uani 1 1 d . . . F1 F 1.212(2) 0.5224(11) 0.8666(11) 0.127(7) Uiso 0.259(8) 1 d P A 1 F2 F 1.161(2) 0.4764(11) 0.9547(10) 0.127(7) Uiso 0.259(8) 1 d P A 1 F3 F 1.312(2) 0.4263(14) 0.8335(10) 0.125(7) Uiso 0.259(8) 1 d P A 1 F4 F 1.257(3) 0.3662(15) 0.9344(12) 0.158(9) Uiso 0.259(8) 1 d P A 1 F5 F 1.346(4) 0.5226(18) 0.9463(16) 0.206(13) Uiso 0.259(8) 1 d P A 1 F6 F 1.113(3) 0.4474(18) 0.8799(15) 0.152(12) Uiso 0.259(8) 1 d P A 1 F1A F 1.2357(10) 0.5237(5) 0.9177(4) 0.138(3) Uiso 0.741(8) 1 d P A 2 F2A F 1.2590(7) 0.4171(4) 0.9711(3) 0.115(2) Uiso 0.741(8) 1 d P A 2 F3A F 1.3220(9) 0.4711(5) 0.8392(4) 0.130(3) Uiso 0.741(8) 1 d P A 2 F4A F 1.3322(7) 0.3617(4) 0.8873(3) 0.113(2) Uiso 0.741(8) 1 d P A 2 F5A F 1.4471(6) 0.4584(3) 0.9273(3) 0.104(2) Uiso 0.741(8) 1 d P A 2 F6A F 1.1177(8) 0.4176(5) 0.8745(4) 0.104(2) Uiso 0.741(8) 1 d P A 2 O3 O 0.7846(5) -0.1337(3) 0.9651(3) 0.125(2) Uani 1 1 d . . . H1O3 H 0.8202 -0.1741 0.9307 0.188 Uiso 1 1 d . . . H2O3 H 0.8413 -0.0958 0.9442 0.188 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 Ru 0.03148(18) 0.03290(18) 0.0441(2) 0.00630(16) 0.00249(13) 0.00083(14) N1A 0.0357(18) 0.0398(19) 0.046(2) 0.0051(16) 0.0067(15) -0.0029(15) N2A 0.0338(18) 0.0393(19) 0.050(2) 0.0106(17) 0.0028(16) 0.0011(15) C1A 0.044(2) 0.049(3) 0.047(3) 0.008(2) 0.003(2) -0.002(2) C2A 0.065(3) 0.065(3) 0.059(3) 0.003(3) -0.005(3) -0.008(3) C3A 0.091(4) 0.058(3) 0.055(3) -0.010(3) 0.012(3) -0.005(3) C4A 0.070(3) 0.046(3) 0.066(3) -0.003(3) 0.024(3) 0.005(3) C5A 0.044(2) 0.040(2) 0.056(3) 0.005(2) 0.012(2) -0.002(2) C6A 0.039(2) 0.040(2) 0.058(3) 0.009(2) 0.012(2) -0.0009(18) C7A 0.045(3) 0.043(3) 0.080(4) 0.007(2) 0.017(3) 0.008(2) C8A 0.044(3) 0.050(3) 0.095(4) 0.024(3) 0.006(3) 0.012(2) C9A 0.050(3) 0.056(3) 0.074(4) 0.025(3) -0.002(3) 0.005(2) C10A 0.043(3) 0.049(3) 0.060(3) 0.014(2) 0.001(2) 0.002(2) N1B 0.0377(19) 0.0366(18) 0.053(2) 0.0133(17) 0.0068(16) 0.0058(15) N2B 0.053(2) 0.0368(19) 0.045(2) 0.0046(16) -0.0046(17) -0.0025(17) C1B 0.036(2) 0.048(3) 0.065(3) 0.010(2) 0.003(2) -0.002(2) C2B 0.041(3) 0.072(4) 0.085(4) 0.014(3) 0.009(3) -0.005(2) C3B 0.050(3) 0.102(5) 0.095(5) 0.011(4) 0.036(3) 0.002(3) C4B 0.071(4) 0.089(5) 0.071(4) 0.008(3) 0.031(3) 0.019(3) C5B 0.055(3) 0.049(3) 0.052(3) 0.003(2) 0.012(2) 0.006(2) C6B 0.067(3) 0.036(2) 0.053(3) 0.005(2) 0.010(2) 0.009(2) C7B 0.111(5) 0.056(3) 0.057(3) -0.006(3) 0.017(3) -0.002(3) C8B 0.137(6) 0.058(4) 0.055(4) -0.008(3) -0.007(4) -0.010(4) C9B 0.101(5) 0.059(4) 0.074(4) 0.004(3) -0.019(4) -0.023(3) C10B 0.072(3) 0.047(3) 0.068(3) 0.006(3) -0.014(3) -0.013(3) C11 0.033(2) 0.056(3) 0.075(3) 0.011(2) 0.007(2) 0.005(2) N3 0.0334(18) 0.042(2) 0.048(2) 0.0021(17) 0.0013(15) -0.0005(15) N4 0.0325(17) 0.0358(18) 0.0403(19) -0.0012(15) 0.0032(14) 0.0015(14) N5 0.0321(17) 0.0358(18) 0.047(2) 0.0019(16) 0.0028(15) 0.0005(14) N6 0.0376(18) 0.0358(18) 0.0405(19) 0.0038(15) 0.0043(15) 0.0005(14) C12 0.034(2) 0.067(3) 0.081(4) 0.009(3) 0.012(2) 0.002(2) C13 0.038(2) 0.062(3) 0.059(3) -0.004(2) 0.014(2) -0.011(2) C14 0.047(3) 0.047(3) 0.053(3) -0.001(2) 0.011(2) -0.005(2) C15 0.035(2) 0.038(2) 0.037(2) -0.0012(18) 0.0035(17) 0.0003(17) C16 0.034(2) 0.034(2) 0.039(2) -0.0002(17) 0.0067(17) -0.0029(17) C17 0.036(2) 0.032(2) 0.039(2) -0.0016(17) 0.0006(17) -0.0047(16) C18 0.033(2) 0.035(2) 0.043(2) -0.0023(18) -0.0012(17) 0.0022(16) C19 0.039(2) 0.046(2) 0.048(3) 0.006(2) 0.0052(19) 0.0022(19) C20 0.051(3) 0.042(2) 0.051(3) 0.009(2) 0.003(2) 0.008(2) C21 0.040(2) 0.040(2) 0.058(3) -0.004(2) -0.003(2) 0.0056(18) C22 0.043(2) 0.042(2) 0.051(3) -0.002(2) 0.008(2) -0.0009(19) C23 0.039(2) 0.037(2) 0.048(3) 0.0044(19) 0.0024(19) -0.0022(18) O1 0.050(2) 0.069(2) 0.078(2) 0.007(2) 0.0288(18) 0.0139(17) C24 0.065(3) 0.075(4) 0.070(4) 0.005(3) 0.033(3) 0.004(3) O2 0.053(2) 0.057(2) 0.074(2) 0.0106(18) 0.0034(17) 0.0196(17) C25 0.090(4) 0.061(4) 0.085(4) 0.012(3) -0.001(3) 0.033(3) P 0.0781(11) 0.0811(11) 0.0671(10) 0.0070(8) 0.0099(8) -0.0086(9) O3 0.078(3) 0.117(4) 0.177(5) 0.086(4) -0.003(3) -0.015(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 N4 2.038(3) . ? Ru N2B 2.043(4) . ? Ru N2A 2.045(3) . ? Ru N1B 2.048(4) . ? Ru N1A 2.059(4) . ? Ru N3 2.105(4) . ? N1A C1A 1.326(5) . ? N1A C5A 1.377(5) . ? N2A C6A 1.342(6) . ? N2A C10A 1.352(6) . ? C1A C2A 1.389(7) . ? C2A C3A 1.371(8) . ? C3A C4A 1.360(8) . ? C4A C5A 1.369(7) . ? C5A C6A 1.484(7) . ? C6A C7A 1.387(6) . ? C7A C8A 1.372(7) . ? C8A C9A 1.359(8) . ? C9A C10A 1.373(7) . ? N1B C1B 1.344(6) . ? N1B C5B 1.352(6) . ? N2B C6B 1.339(6) . ? N2B C10B 1.349(6) . ? C1B C2B 1.365(7) . ? C2B C3B 1.323(9) . ? C3B C4B 1.402(9) . ? C4B C5B 1.386(7) . ? C5B C6B 1.461(7) . ? C6B C7B 1.402(7) . ? C7B C8B 1.350(9) . ? C8B C9B 1.348(9) . ? C9B C10B 1.360(8) . ? C11 N3 1.342(5) . ? C11 C12 1.378(7) . ? N3 C15 1.348(5) . ? N4 C16 1.334(5) . ? N4 N5 1.368(4) . ? N5 C17 1.344(5) . ? N6 C16 1.337(5) . ? N6 C17 1.351(5) . ? C12 C13 1.360(7) . ? C13 C14 1.375(6) . ? C14 C15 1.390(6) . ? C15 C16 1.456(5) . ? C17 C18 1.473(5) . ? C18 C19 1.376(6) . ? C18 C23 1.398(6) . ? C19 C20 1.399(6) . ? C20 C21 1.368(7) . ? C21 O2 1.368(5) . ? C21 C22 1.404(6) . ? C22 O1 1.363(5) . ? C22 C23 1.371(6) . ? O1 C24 1.429(6) . ? O2 C25 1.415(6) . ? P F1A 1.517(8) . ? P F6 1.54(3) . ? P F2A 1.540(7) . ? P F3A 1.572(8) . ? P F5A 1.572(6) . ? P F4 1.58(3) . ? P F6A 1.614(8) . ? P F3 1.62(2) . ? P F4A 1.630(7) . ? P F2 1.70(2) . ? P F1 1.70(2) . ? P F5 1.74(3) . ? F1 F6 1.67(3) . ? F2 F6 1.69(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 N4 Ru N2B 89.76(13) . . ? N4 Ru N2A 171.46(14) . . ? N2B Ru N2A 95.60(14) . . ? N4 Ru N1B 94.18(13) . . ? N2B Ru N1B 78.79(16) . . ? N2A Ru N1B 93.38(14) . . ? N4 Ru N1A 96.15(13) . . ? N2B Ru N1A 173.90(14) . . ? N2A Ru N1A 78.70(14) . . ? N1B Ru N1A 99.25(15) . . ? N4 Ru N3 77.73(13) . . ? N2B Ru N3 96.44(15) . . ? N2A Ru N3 95.03(13) . . ? N1B Ru N3 170.71(14) . . ? N1A Ru N3 86.29(13) . . ? C1A N1A C5A 118.2(4) . . ? C1A N1A Ru 127.1(3) . . ? C5A N1A Ru 114.4(3) . . ? C6A N2A C10A 118.0(4) . . ? C6A N2A Ru 116.1(3) . . ? C10A N2A Ru 125.8(3) . . ? N1A C1A C2A 122.3(4) . . ? C3A C2A C1A 118.8(5) . . ? C4A C3A C2A 119.6(5) . . ? C3A C4A C5A 119.9(5) . . ? C4A C5A N1A 121.1(4) . . ? C4A C5A C6A 124.8(4) . . ? N1A C5A C6A 113.9(4) . . ? N2A C6A C7A 121.5(4) . . ? N2A C6A C5A 114.7(4) . . ? C7A C6A C5A 123.8(5) . . ? C8A C7A C6A 119.2(5) . . ? C9A C8A C7A 119.5(5) . . ? C8A C9A C10A 119.1(5) . . ? N2A C10A C9A 122.5(5) . . ? C1B N1B C5B 119.3(4) . . ? C1B N1B Ru 125.5(3) . . ? C5B N1B Ru 115.2(3) . . ? C6B N2B C10B 118.4(4) . . ? C6B N2B Ru 115.5(3) . . ? C10B N2B Ru 126.0(4) . . ? N1B C1B C2B 121.1(5) . . ? C3B C2B C1B 120.6(6) . . ? C2B C3B C4B 120.4(5) . . ? C5B C4B C3B 117.3(6) . . ? N1B C5B C4B 121.2(5) . . ? N1B C5B C6B 114.3(4) . . ? C4B C5B C6B 124.4(5) . . ? N2B C6B C7B 119.4(5) . . ? N2B C6B C5B 115.4(4) . . ? C7B C6B C5B 124.8(5) . . ? C8B C7B C6B 120.8(6) . . ? C9B C8B C7B 119.2(6) . . ? C8B C9B C10B 119.1(6) . . ? N2B C10B C9B 123.0(6) . . ? N3 C11 C12 122.5(5) . . ? C11 N3 C15 118.0(4) . . ? C11 N3 Ru 126.6(3) . . ? C15 N3 Ru 115.4(3) . . ? C16 N4 N5 107.6(3) . . ? C16 N4 Ru 116.3(3) . . ? N5 N4 Ru 136.0(3) . . ? C17 N5 N4 103.5(3) . . ? C16 N6 C17 101.7(3) . . ? C13 C12 C11 119.3(4) . . ? C12 C13 C14 119.6(4) . . ? C13 C14 C15 118.8(4) . . ? N3 C15 C14 121.8(4) . . ? N3 C15 C16 113.6(4) . . ? C14 C15 C16 124.6(4) . . ? N4 C16 N6 112.8(3) . . ? N4 C16 C15 117.0(4) . . ? N6 C16 C15 130.2(4) . . ? N5 C17 N6 114.4(3) . . ? N5 C17 C18 121.6(4) . . ? N6 C17 C18 123.9(4) . . ? C19 C18 C23 119.5(4) . . ? C19 C18 C17 120.4(4) . . ? C23 C18 C17 120.1(4) . . ? C18 C19 C20 119.7(4) . . ? C21 C20 C19 121.0(4) . . ? C20 C21 O2 125.1(4) . . ? C20 C21 C22 119.2(4) . . ? O2 C21 C22 115.7(4) . . ? O1 C22 C23 124.9(4) . . ? O1 C22 C21 115.1(4) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C18 120.6(4) . . ? C22 O1 C24 116.6(4) . . ? C21 O2 C25 117.9(4) . . ? F1A P F6 76.5(13) . . ? F1A P F2A 94.1(5) . . ? F6 P F2A 96.4(12) . . ? F1A P F3A 88.6(5) . . ? F6 P F3A 91.0(12) . . ? F2A P F3A 172.5(4) . . ? F1A P F5A 93.4(4) . . ? F6 P F5A 168.9(13) . . ? F2A P F5A 88.9(3) . . ? F3A P F5A 84.0(4) . . ? F1A P F4 136.3(11) . . ? F6 P F4 90.1(15) . . ? F2A P F4 45.7(9) . . ? F3A P F4 133.7(11) . . ? F5A P F4 100.6(9) . . ? F1A P F6A 96.5(5) . . ? F6 P F6A 20.0(12) . . ? F2A P F6A 94.2(4) . . ? F3A P F6A 92.5(4) . . ? F5A P F6A 169.4(4) . . ? F4 P F6A 74.7(9) . . ? F1A P F3 116.5(9) . . ? F6 P F3 88.0(14) . . ? F2A P F3 149.2(9) . . ? F3A P F3 29.7(8) . . ? F5A P F3 92.4(8) . . ? F4 P F3 104.1(13) . . ? F6A P F3 79.8(8) . . ? F1A P F4A 176.4(4) . . ? F6 P F4A 104.8(13) . . ? F2A P F4A 89.1(4) . . ? F3A P F4A 88.1(4) . . ? F5A P F4A 85.0(3) . . ? F4 P F4A 47.2(9) . . ? F6A P F4A 84.9(4) . . ? F3 P F4A 60.4(9) . . ? F1A P F2 50.9(7) . . ? F6 P F2 62.7(13) . . ? F2A P F2 51.3(7) . . ? F3A P F2 134.3(8) . . ? F5A P F2 114.5(7) . . ? F4 P F2 85.9(12) . . ? F6A P F2 74.9(7) . . ? F3 P F2 149.3(10) . . ? F4A P F2 132.7(8) . . ? F1A P F1 39.1(7) . . ? F6 P F1 61.5(13) . . ? F2A P F1 129.3(8) . . ? F3A P F1 55.7(7) . . ? F5A P F1 107.6(7) . . ? F4 P F1 151.4(11) . . ? F6A P F1 78.1(8) . . ? F3 P F1 79.4(11) . . ? F4A P F1 138.6(8) . . ? F2 P F1 78.6(10) . . ? F1A P F5 39.2(11) . . ? F6 P F5 114.8(17) . . ? F2A P F5 81.9(11) . . ? F3A P F5 95.9(11) . . ? F5A P F5 56.2(12) . . ? F4 P F5 125.1(14) . . ? F6A P F5 134.3(13) . . ? F3 P F5 123.7(14) . . ? F4A P F5 140.1(13) . . ? F2 P F5 67.2(13) . . ? F1 P F5 70.3(13) . . ? F6 F1 P 54.5(12) . . ? F6 F2 P 54.1(12) . . ? P F6 F2 63.3(14) . . ? P F6 F1 64.0(14) . . ? F2 F6 F1 79.9(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.167 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.087