Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global #------------------------------------------------------------------------------ _audit_creation_date '2002-08-16' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _journal_coden_Cambridge 182 loop_ _publ_author_name 'Michael Wolf' 'Olivier Clot' 'Carolyn Moorlag' 'Brian O. Patrick' _publ_contact_author_name 'Prof Michael Wolf' _publ_contact_author_address ; Chemistry University of British Columbia 2036 Main Mall Vancouver BC V6T 1Z1 CANADA ; _publ_contact_author_email 'MWOLF@CHEM.UBC.CA' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Switchable thiophene coordination in Ru(II) bipyridyl phosphinoterthiophene complexes ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1996-1998). d*TREK. Area Detector Software. Version 4.4. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Burla, M.C., Cammalli, G., Cascarano, M., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, A. (1998). SIR97: a new tool for crystal structure determination and refinement. Submitted. ; data_mw016/1b/CM35 _database_code_CSD 193871 _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 10.1989(3) _cell_length_b 14.9169(5) _cell_length_c 15.2939(3) _cell_angle_alpha 77.207(5) _cell_angle_beta 79.517(5) _cell_angle_gamma 88.763(6) _cell_volume 2230.7(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 13692 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.87 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'platelet' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1048.03 _chemical_formula_analytical ? _chemical_formula_sum 'C47 H38 F6 N4 O P2 S3 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1064.00 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.781 _exptl_special_details ; Data were collected in 0.50\% oscillations with 47.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -17.0 and 23.0\% at \c = -90.0\%. The crystal-to-detector distance was 38.00 mm. The detector swing angle was -5.6\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 20959 _reflns_number_total 9173 _reflns_number_gt 6582 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04517 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 94 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 76 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 6 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 2 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.89865(2) 0.17444(1) 0.72565(2) 0.00986(6) 1.000 . Uani d ? S(1) 0.77395(7) -0.02293(6) 1.01104(6) 0.0227(2) 1.000 . Uani d ? S(2) 0.54136(7) 0.11993(5) 1.03669(5) 0.0199(2) 1.000 . Uani d ? S(3) 0.33519(8) 0.37324(7) 1.06682(7) 0.0348(3) 1.000 . Uani d ? P(1) 0.79003(6) 0.28077(5) 0.79661(5) 0.0101(2) 1.000 . Uani d ? P(2) 0.52142(8) 0.20905(6) 0.45702(6) 0.0256(2) 1.000 . Uani d ? F(1) 0.6152(3) 0.2996(2) 0.4206(2) 0.0667(9) 1.000 . Uani d ? F(2) 0.4338(3) 0.1198(2) 0.4919(2) 0.073(1) 1.000 . Uani d ? F(3) 0.6293(2) 0.1641(2) 0.5158(2) 0.0527(8) 1.000 . Uani d ? F(4) 0.5993(3) 0.1709(2) 0.3736(2) 0.0639(9) 1.000 . Uani d ? F(5) 0.4190(3) 0.2545(2) 0.3957(2) 0.087(1) 1.000 . Uani d ? F(6) 0.4490(3) 0.2491(3) 0.5383(3) 0.107(1) 1.000 . Uani d ? O(1) 0.8600(2) 0.3107(2) 0.2368(2) 0.0424(8) 1.000 . Uani d ? N(1) 0.7331(2) 0.1063(2) 0.7071(2) 0.0137(6) 1.000 . Uani d ? N(2) 0.9875(2) 0.0713(2) 0.6610(2) 0.0142(6) 1.000 . Uani d ? N(3) 0.9620(2) 0.2640(2) 0.5944(2) 0.0136(6) 1.000 . Uani d ? N(4) 1.0786(2) 0.2278(2) 0.7376(2) 0.0127(6) 1.000 . Uani d ? C(1) 0.6037(3) 0.1243(2) 0.7332(2) 0.0189(8) 1.000 . Uani d ? C(2) 0.4993(3) 0.0688(2) 0.7296(2) 0.0270(9) 1.000 . Uani d ? C(3) 0.5269(3) -0.0092(3) 0.6965(3) 0.033(1) 1.000 . Uani d ? C(4) 0.6581(3) -0.0303(2) 0.6693(3) 0.0276(9) 1.000 . Uani d ? C(5) 0.7591(3) 0.0277(2) 0.6758(2) 0.0174(8) 1.000 . Uani d ? C(6) 0.9017(3) 0.0084(2) 0.6498(2) 0.0176(8) 1.000 . Uani d ? C(7) 0.9490(3) -0.0673(2) 0.6145(2) 0.0281(9) 1.000 . Uani d ? C(8) 1.0844(3) -0.0768(2) 0.5890(3) 0.031(1) 1.000 . Uani d ? C(9) 1.1716(3) -0.0098(2) 0.5961(2) 0.0250(9) 1.000 . Uani d ? C(10) 1.1198(3) 0.0630(2) 0.6329(2) 0.0196(8) 1.000 . Uani d ? C(11) 0.9026(3) 0.2736(2) 0.5211(2) 0.0181(8) 1.000 . Uani d ? C(12) 0.9594(3) 0.3236(3) 0.4352(2) 0.031(1) 1.000 . Uani d ? C(13) 1.0812(4) 0.3662(3) 0.4242(3) 0.041(1) 1.000 . Uani d ? C(14) 1.1455(3) 0.3562(3) 0.4979(2) 0.033(1) 1.000 . Uani d ? C(15) 1.0835(3) 0.3053(2) 0.5824(2) 0.0168(7) 1.000 . Uani d ? C(16) 1.1452(3) 0.2885(2) 0.6646(2) 0.0151(7) 1.000 . Uani d ? C(17) 1.2635(3) 0.3311(2) 0.6690(2) 0.0223(8) 1.000 . Uani d ? C(18) 1.3141(3) 0.3111(2) 0.7488(2) 0.0254(9) 1.000 . Uani d ? C(19) 1.2481(3) 0.2483(2) 0.8222(2) 0.0235(9) 1.000 . Uani d ? C(20) 1.1306(3) 0.2077(2) 0.8140(2) 0.0169(8) 1.000 . Uani d ? C(21) 0.8961(2) 0.3476(2) 0.8442(2) 0.0146(7) 1.000 . Uani d ? C(22) 0.9078(3) 0.3230(2) 0.9353(2) 0.0263(9) 1.000 . Uani d ? C(23) 0.9980(4) 0.3699(3) 0.9688(3) 0.041(1) 1.000 . Uani d ? C(24) 1.0762(3) 0.4410(3) 0.9108(3) 0.039(1) 1.000 . Uani d ? C(25) 1.0662(3) 0.4659(2) 0.8200(3) 0.030(1) 1.000 . Uani d ? C(26) 0.9768(3) 0.4189(2) 0.7865(2) 0.0193(8) 1.000 . Uani d ? C(27) 0.7014(2) 0.3735(2) 0.7312(2) 0.0143(7) 1.000 . Uani d ? C(28) 0.6623(3) 0.3616(2) 0.6518(2) 0.0172(7) 1.000 . Uani d ? C(29) 0.5940(3) 0.4306(2) 0.6015(2) 0.0243(8) 1.000 . Uani d ? C(30) 0.5628(3) 0.5102(2) 0.6308(3) 0.0284(9) 1.000 . Uani d ? C(31) 0.6005(3) 0.5231(2) 0.7100(2) 0.0256(9) 1.000 . Uani d ? C(32) 0.6700(3) 0.4554(2) 0.7598(2) 0.0186(8) 1.000 . Uani d ? C(33) 0.9111(3) -0.0605(2) 0.9464(2) 0.0248(9) 1.000 . Uani d ? C(34) 0.9486(3) -0.0006(2) 0.8657(2) 0.0180(8) 1.000 . Uani d ? C(35) 0.8698(2) 0.0799(2) 0.8498(2) 0.0132(7) 1.000 . Uani d ? C(36) 0.7691(3) 0.0760(2) 0.9256(2) 0.0149(7) 1.000 . Uani d ? C(37) 0.6701(2) 0.1438(2) 0.9426(2) 0.0134(7) 1.000 . Uani d ? C(38) 0.6637(2) 0.2334(2) 0.8945(2) 0.0137(7) 1.000 . Uani d ? C(39) 0.5550(3) 0.2821(2) 0.9347(2) 0.0164(7) 1.000 . Uani d ? C(40) 0.4803(3) 0.2307(2) 1.0123(2) 0.0175(8) 1.000 . Uani d ? C(41) 0.3660(3) 0.2581(2) 1.0719(2) 0.0212(8) 1.000 . Uani d ? C(42) 0.2732(3) 0.2046(3) 1.1368(2) 0.0296(9) 1.000 . Uani d ? C(43) 0.1764(3) 0.2574(3) 1.1815(3) 0.037(1) 1.000 . Uani d ? C(44) 0.1969(3) 0.3484(3) 1.1507(3) 0.036(1) 1.000 . Uani d ? C(45) 0.7812(3) 0.2772(2) 0.2015(2) 0.0278(9) 1.000 . Uani d ? C(46) 0.6630(4) 0.3287(3) 0.1733(3) 0.048(1) 1.000 . Uani d ? C(47) 0.8004(4) 0.1834(3) 0.1831(3) 0.041(1) 1.000 . Uani d ? H(1) 0.5822 0.1802 0.7564 0.022 1.000 . Uiso c ? H(2) 0.4071 0.0852 0.7500 0.032 1.000 . Uiso c ? H(3) 0.4543 -0.0494 0.6923 0.040 1.000 . Uiso c ? H(4) 0.6802 -0.0855 0.6451 0.033 1.000 . Uiso c ? H(5) 0.8866 -0.1131 0.6079 0.034 1.000 . Uiso c ? H(6) 1.1188 -0.1307 0.5660 0.036 1.000 . Uiso c ? H(7) 1.2679 -0.0143 0.5757 0.030 1.000 . Uiso c ? H(8) 1.1811 0.1102 0.6387 0.024 1.000 . Uiso c ? H(9) 0.8151 0.2438 0.5286 0.021 1.000 . Uiso c ? H(10) 0.9133 0.3289 0.3835 0.037 1.000 . Uiso c ? H(11) 1.1225 0.4030 0.3645 0.049 1.000 . Uiso c ? H(12) 1.2332 0.3851 0.4908 0.040 1.000 . Uiso c ? H(13) 1.3106 0.3753 0.6157 0.026 1.000 . Uiso c ? H(14) 1.3967 0.3412 0.7528 0.030 1.000 . Uiso c ? H(15) 1.2826 0.2326 0.8793 0.028 1.000 . Uiso c ? H(16) 1.0840 0.1624 0.8667 0.020 1.000 . Uiso c ? H(17) 0.8525 0.2726 0.9765 0.032 1.000 . Uiso c ? H(18) 1.0055 0.3524 1.0332 0.048 1.000 . Uiso c ? H(19) 1.1392 0.4739 0.9344 0.047 1.000 . Uiso c ? H(20) 1.1215 0.5165 0.7792 0.035 1.000 . Uiso c ? H(21) 0.9703 0.4361 0.7219 0.023 1.000 . Uiso c ? H(22) 0.6825 0.3043 0.6313 0.020 1.000 . Uiso c ? H(23) 0.5690 0.4222 0.5450 0.029 1.000 . Uiso c ? H(24) 0.5137 0.5580 0.5958 0.034 1.000 . Uiso c ? H(25) 0.5781 0.5802 0.7305 0.031 1.000 . Uiso c ? H(26) 0.6970 0.4650 0.8154 0.022 1.000 . Uiso c ? H(27) 0.9562 -0.1183 0.9655 0.030 1.000 . Uiso c ? H(28) 1.0253 -0.0116 0.8210 0.022 1.000 . Uiso c ? H(29) 0.5359 0.3463 0.9090 0.019 1.000 . Uiso c ? H(30) 0.2729 0.1373 1.1510 0.035 1.000 . Uiso c ? H(31) 0.1026 0.2300 1.2302 0.043 1.000 . Uiso c ? H(32) 0.1395 0.3951 1.1734 0.043 1.000 . Uiso c ? H(33) 0.6935 0.3856 0.1281 0.057 1.000 . Uiso c ? H(34) 0.6119 0.2908 0.1464 0.057 1.000 . Uiso c ? H(35) 0.6064 0.3446 0.2266 0.057 1.000 . Uiso c ? H(36) 0.7997 0.1383 0.2405 0.048 1.000 . Uiso c ? H(37) 0.7278 0.1686 0.1541 0.048 1.000 . Uiso c ? H(38) 0.8859 0.1815 0.1422 0.048 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0113(1) 0.0083(1) 0.0101(1) -0.00010(7) -0.00164(7) -0.00254(8) S(1) 0.0268(4) 0.0177(4) 0.0184(4) 0.0016(3) -0.0022(3) 0.0050(3) S(2) 0.0168(3) 0.0214(4) 0.0162(4) -0.0010(3) 0.0027(3) 0.0023(3) S(3) 0.0287(4) 0.0333(5) 0.0415(6) 0.0056(3) 0.0038(4) -0.0153(4) P(1) 0.0116(3) 0.0088(4) 0.0097(4) 0.0004(2) -0.0012(2) -0.0020(3) P(2) 0.0271(4) 0.0262(5) 0.0270(5) 0.0064(3) -0.0073(3) -0.0120(4) F(1) 0.077(2) 0.030(1) 0.090(2) -0.010(1) -0.018(2) -0.004(1) F(2) 0.069(2) 0.075(2) 0.066(2) -0.047(1) -0.022(1) 0.013(2) F(3) 0.040(1) 0.063(2) 0.052(2) -0.007(1) -0.023(1) 0.006(1) F(4) 0.089(2) 0.058(2) 0.045(2) 0.007(1) 0.005(1) -0.027(1) F(5) 0.066(2) 0.092(2) 0.101(3) 0.025(2) -0.051(2) 0.006(2) F(6) 0.090(2) 0.151(4) 0.099(3) 0.034(2) 0.011(2) -0.093(3) O(1) 0.032(1) 0.049(2) 0.050(2) -0.007(1) -0.005(1) -0.018(1) N(1) 0.020(1) 0.012(1) 0.010(1) -0.0033(9) -0.0037(9) -0.002(1) N(2) 0.022(1) 0.012(1) 0.008(1) 0.0009(9) -0.0012(9) -0.002(1) N(3) 0.014(1) 0.013(1) 0.013(1) 0.0005(8) 0.0002(8) -0.004(1) N(4) 0.014(1) 0.011(1) 0.013(1) 0.0026(8) -0.0006(8) -0.004(1) C(1) 0.020(1) 0.019(2) 0.019(2) -0.001(1) -0.005(1) -0.005(1) C(2) 0.021(2) 0.031(2) 0.029(2) -0.007(1) -0.006(1) -0.004(2) C(3) 0.032(2) 0.031(2) 0.038(2) -0.018(1) -0.011(1) -0.006(2) C(4) 0.039(2) 0.017(2) 0.032(2) -0.006(1) -0.014(1) -0.010(1) C(5) 0.024(1) 0.015(2) 0.014(2) -0.003(1) -0.007(1) -0.002(1) C(6) 0.031(2) 0.011(1) 0.011(2) 0.002(1) -0.004(1) -0.003(1) C(7) 0.043(2) 0.016(2) 0.028(2) 0.002(1) -0.007(1) -0.010(1) C(8) 0.045(2) 0.020(2) 0.028(2) 0.012(1) -0.004(1) -0.013(2) C(9) 0.030(2) 0.020(2) 0.023(2) 0.009(1) 0.000(1) -0.006(1) C(10) 0.023(1) 0.017(2) 0.018(2) 0.003(1) -0.001(1) -0.004(1) C(11) 0.019(1) 0.021(2) 0.015(2) 0.000(1) -0.004(1) -0.005(1) C(12) 0.039(2) 0.036(2) 0.016(2) -0.004(1) -0.007(1) 0.001(2) C(13) 0.048(2) 0.051(3) 0.016(2) -0.017(2) -0.002(2) 0.011(2) C(14) 0.029(2) 0.043(2) 0.022(2) -0.014(1) -0.001(1) 0.004(2) C(15) 0.018(1) 0.017(2) 0.014(2) -0.002(1) 0.000(1) -0.002(1) C(16) 0.013(1) 0.015(1) 0.018(2) 0.001(1) 0.000(1) -0.007(1) C(17) 0.013(1) 0.027(2) 0.027(2) -0.006(1) 0.001(1) -0.008(1) C(18) 0.015(1) 0.030(2) 0.034(2) -0.003(1) -0.007(1) -0.012(2) C(19) 0.020(1) 0.029(2) 0.026(2) 0.000(1) -0.011(1) -0.008(1) C(20) 0.019(1) 0.017(2) 0.016(2) 0.001(1) -0.007(1) -0.005(1) C(21) 0.012(1) 0.015(1) 0.018(2) 0.002(1) -0.001(1) -0.008(1) C(22) 0.025(2) 0.037(2) 0.020(2) -0.005(1) -0.003(1) -0.013(2) C(23) 0.039(2) 0.066(3) 0.026(2) -0.004(2) -0.011(2) -0.027(2) C(24) 0.029(2) 0.045(2) 0.055(3) -0.007(2) -0.010(2) -0.034(2) C(25) 0.020(2) 0.020(2) 0.052(3) -0.006(1) -0.004(1) -0.015(2) C(26) 0.018(1) 0.012(2) 0.029(2) 0.002(1) -0.005(1) -0.009(1) C(27) 0.011(1) 0.013(1) 0.016(2) 0.001(1) 0.000(1) 0.000(1) C(28) 0.015(1) 0.017(2) 0.018(2) 0.001(1) -0.002(1) -0.002(1) C(29) 0.021(1) 0.030(2) 0.020(2) 0.000(1) -0.008(1) 0.003(1) C(30) 0.021(2) 0.024(2) 0.034(2) 0.005(1) -0.008(1) 0.009(2) C(31) 0.025(2) 0.014(2) 0.035(2) 0.007(1) -0.001(1) -0.002(1) C(32) 0.019(1) 0.014(2) 0.021(2) 0.002(1) -0.002(1) -0.002(1) C(33) 0.032(2) 0.016(2) 0.025(2) 0.009(1) -0.007(1) -0.002(1) C(34) 0.023(1) 0.013(2) 0.018(2) 0.005(1) -0.004(1) -0.002(1) C(35) 0.015(1) 0.007(1) 0.019(2) -0.0009(9) -0.006(1) -0.003(1) C(36) 0.018(1) 0.009(1) 0.017(2) -0.001(1) -0.006(1) 0.001(1) C(37) 0.011(1) 0.017(2) 0.011(1) -0.002(1) -0.0012(9) -0.003(1) C(38) 0.014(1) 0.016(1) 0.011(1) -0.001(1) -0.002(1) -0.003(1) C(39) 0.016(1) 0.016(2) 0.017(2) 0.002(1) -0.002(1) -0.003(1) C(40) 0.015(1) 0.021(2) 0.017(2) 0.001(1) -0.003(1) -0.006(1) C(41) 0.018(1) 0.032(2) 0.014(2) 0.001(1) -0.003(1) -0.006(1) C(42) 0.025(2) 0.040(2) 0.019(2) 0.003(1) 0.005(1) -0.004(2) C(43) 0.019(2) 0.061(3) 0.028(2) 0.003(2) 0.005(1) -0.012(2) C(44) 0.023(2) 0.060(3) 0.028(2) 0.012(2) 0.000(1) -0.022(2) C(45) 0.027(2) 0.032(2) 0.021(2) -0.001(1) 0.003(1) -0.003(2) C(46) 0.038(2) 0.054(3) 0.052(3) 0.014(2) -0.011(2) -0.008(2) C(47) 0.052(2) 0.037(2) 0.034(2) 0.004(2) -0.007(2) -0.010(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.00024|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 9173 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_all 0.0899 _refine_ls_wR_factor_ref 0.0899 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_shift/su_max 0.0030 _refine_ls_shift/su_mean 0.1170 _refine_diff_density_min -0.73 _refine_diff_density_max 0.91 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) P(1) 2.2737(7) . . yes Ru(1) N(1) 2.083(2) . . yes Ru(1) N(2) 2.110(2) . . yes Ru(1) N(3) 2.147(2) . . yes Ru(1) N(4) 2.069(2) . . yes Ru(1) C(35) 2.076(3) . . yes S(1) C(33) 1.719(3) . . yes S(1) C(36) 1.747(3) . . yes S(2) C(37) 1.739(3) . . yes S(2) C(40) 1.739(3) . . yes S(3) C(41) 1.727(3) . . yes S(3) C(44) 1.711(4) . . yes P(1) C(21) 1.830(3) . . yes P(1) C(27) 1.842(3) . . yes P(1) C(38) 1.809(3) . . yes P(2) F(1) 1.606(3) . . yes P(2) F(2) 1.556(2) . . yes P(2) F(3) 1.591(2) . . yes P(2) F(4) 1.587(2) . . yes P(2) F(5) 1.574(3) . . yes P(2) F(6) 1.557(3) . . yes O(1) C(45) 1.218(4) . . yes N(1) C(1) 1.348(4) . . yes N(1) C(5) 1.365(4) . . yes N(2) C(6) 1.355(4) . . yes N(2) C(10) 1.352(4) . . yes N(3) C(11) 1.348(4) . . yes N(3) C(15) 1.360(3) . . yes N(4) C(16) 1.353(4) . . yes N(4) C(20) 1.342(4) . . yes C(1) C(2) 1.378(4) . . yes C(1) H(1) 0.98 . . no C(2) C(3) 1.372(5) . . yes C(2) H(2) 0.98 . . no C(3) C(4) 1.379(5) . . yes C(3) H(3) 0.98 . . no C(4) C(5) 1.390(4) . . yes C(4) H(4) 0.98 . . no C(5) C(6) 1.476(4) . . yes C(6) C(7) 1.397(4) . . yes C(7) C(8) 1.378(5) . . yes C(7) H(5) 0.98 . . no C(8) C(9) 1.387(5) . . yes C(8) H(6) 0.98 . . no C(9) C(10) 1.383(4) . . yes C(9) H(7) 0.98 . . no C(10) H(8) 0.98 . . no C(11) C(12) 1.387(4) . . yes C(11) H(9) 0.98 . . no C(12) C(13) 1.374(5) . . yes C(12) H(10) 0.98 . . no C(13) C(14) 1.383(5) . . yes C(13) H(11) 0.98 . . no C(14) C(15) 1.391(4) . . yes C(14) H(12) 0.98 . . no C(15) C(16) 1.477(4) . . yes C(16) C(17) 1.396(4) . . yes C(17) C(18) 1.380(5) . . yes C(17) H(13) 0.98 . . no C(18) C(19) 1.370(5) . . yes C(18) H(14) 0.98 . . no C(19) C(20) 1.392(4) . . yes C(19) H(15) 0.98 . . no C(20) H(16) 0.98 . . no C(21) C(22) 1.387(4) . . yes C(21) C(26) 1.394(4) . . yes C(22) C(23) 1.398(4) . . yes C(22) H(17) 0.98 . . no C(23) C(24) 1.382(6) . . yes C(23) H(18) 0.98 . . no C(24) C(25) 1.378(6) . . yes C(24) H(19) 0.98 . . no C(25) C(26) 1.394(4) . . yes C(25) H(20) 0.98 . . no C(26) H(21) 0.98 . . no C(27) C(28) 1.393(4) . . yes C(27) C(32) 1.397(4) . . yes C(28) C(29) 1.397(4) . . yes C(28) H(22) 0.98 . . no C(29) C(30) 1.370(5) . . yes C(29) H(23) 0.98 . . no C(30) C(31) 1.389(5) . . yes C(30) H(24) 0.98 . . no C(31) C(32) 1.388(4) . . yes C(31) H(25) 0.98 . . no C(32) H(26) 0.98 . . no C(33) C(34) 1.350(4) . . yes C(33) H(27) 0.98 . . no C(34) C(35) 1.431(4) . . yes C(34) H(28) 0.98 . . no C(35) C(36) 1.394(4) . . yes C(36) C(37) 1.445(4) . . yes C(37) C(38) 1.381(4) . . yes C(38) C(39) 1.432(4) . . yes C(39) C(40) 1.367(4) . . yes C(39) H(29) 0.98 . . no C(40) C(41) 1.454(4) . . yes C(41) C(42) 1.363(4) . . yes C(42) C(43) 1.422(5) . . yes C(42) H(30) 0.98 . . no C(43) C(44) 1.342(6) . . yes C(43) H(31) 0.98 . . no C(44) H(32) 0.98 . . no C(45) C(46) 1.494(5) . . yes C(45) C(47) 1.490(5) . . yes C(46) H(33) 0.98 . . no C(46) H(34) 0.98 . . no C(46) H(35) 0.98 . . no C(47) H(36) 0.98 . . no C(47) H(37) 0.98 . . no C(47) H(38) 0.98 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Ru(1) N(1) 98.55(7) . . . yes P(1) Ru(1) N(2) 176.29(6) . . . yes P(1) Ru(1) N(3) 97.51(6) . . . yes P(1) Ru(1) N(4) 89.36(6) . . . yes P(1) Ru(1) C(35) 89.28(8) . . . yes N(1) Ru(1) N(2) 77.81(9) . . . yes N(1) Ru(1) N(3) 102.80(9) . . . yes N(1) Ru(1) N(4) 172.01(9) . . . yes N(1) Ru(1) C(35) 82.8(1) . . . yes N(2) Ru(1) N(3) 84.10(9) . . . yes N(2) Ru(1) N(4) 94.26(9) . . . yes N(2) Ru(1) C(35) 89.5(1) . . . yes N(3) Ru(1) N(4) 77.04(9) . . . yes N(3) Ru(1) C(35) 170.39(9) . . . yes N(4) Ru(1) C(35) 96.3(1) . . . yes C(33) S(1) C(36) 90.9(1) . . . yes C(37) S(2) C(40) 92.5(1) . . . yes C(41) S(3) C(44) 91.9(2) . . . yes Ru(1) P(1) C(21) 114.84(8) . . . yes Ru(1) P(1) C(27) 119.3(1) . . . yes Ru(1) P(1) C(38) 114.5(1) . . . yes C(21) P(1) C(27) 100.7(1) . . . yes C(21) P(1) C(38) 102.4(1) . . . yes C(27) P(1) C(38) 102.7(1) . . . yes F(1) P(2) F(2) 178.5(2) . . . yes F(1) P(2) F(3) 88.6(1) . . . yes F(1) P(2) F(4) 87.8(2) . . . yes F(1) P(2) F(5) 90.0(2) . . . yes F(1) P(2) F(6) 90.2(2) . . . yes F(2) P(2) F(3) 90.3(1) . . . yes F(2) P(2) F(4) 91.2(2) . . . yes F(2) P(2) F(5) 91.0(2) . . . yes F(2) P(2) F(6) 90.8(2) . . . yes F(3) P(2) F(4) 89.2(2) . . . yes F(3) P(2) F(5) 177.9(2) . . . yes F(3) P(2) F(6) 90.2(2) . . . yes F(4) P(2) F(5) 89.1(2) . . . yes F(4) P(2) F(6) 177.9(2) . . . yes F(5) P(2) F(6) 91.5(2) . . . yes Ru(1) N(1) C(1) 127.3(2) . . . yes Ru(1) N(1) C(5) 115.7(2) . . . yes C(1) N(1) C(5) 116.5(2) . . . yes Ru(1) N(2) C(6) 115.3(2) . . . yes Ru(1) N(2) C(10) 125.4(2) . . . yes C(6) N(2) C(10) 119.3(2) . . . yes Ru(1) N(3) C(11) 126.7(2) . . . yes Ru(1) N(3) C(15) 115.0(2) . . . yes C(11) N(3) C(15) 117.7(2) . . . yes Ru(1) N(4) C(16) 117.7(2) . . . yes Ru(1) N(4) C(20) 123.9(2) . . . yes C(16) N(4) C(20) 118.4(2) . . . yes N(1) C(1) C(2) 124.0(3) . . . yes N(1) C(1) H(1) 118.1 . . . no C(2) C(1) H(1) 117.9 . . . no C(1) C(2) C(3) 118.9(3) . . . yes C(1) C(2) H(2) 120.3 . . . no C(3) C(2) H(2) 120.7 . . . no C(2) C(3) C(4) 118.9(3) . . . yes C(2) C(3) H(3) 120.5 . . . no C(4) C(3) H(3) 120.5 . . . no C(3) C(4) C(5) 119.5(3) . . . yes C(3) C(4) H(4) 120.4 . . . no C(5) C(4) H(4) 120.1 . . . no N(1) C(5) C(4) 122.2(3) . . . yes N(1) C(5) C(6) 115.4(2) . . . yes C(4) C(5) C(6) 122.4(3) . . . yes N(2) C(6) C(5) 115.0(2) . . . yes N(2) C(6) C(7) 120.8(3) . . . yes C(5) C(6) C(7) 124.2(3) . . . yes C(6) C(7) C(8) 119.4(3) . . . yes C(6) C(7) H(5) 120.3 . . . no C(8) C(7) H(5) 120.3 . . . no C(7) C(8) C(9) 119.7(3) . . . yes C(7) C(8) H(6) 120.1 . . . no C(9) C(8) H(6) 120.3 . . . no C(8) C(9) C(10) 118.6(3) . . . yes C(8) C(9) H(7) 120.6 . . . no C(10) C(9) H(7) 120.9 . . . no N(2) C(10) C(9) 122.2(3) . . . yes N(2) C(10) H(8) 118.9 . . . no C(9) C(10) H(8) 118.9 . . . no N(3) C(11) C(12) 123.1(3) . . . yes N(3) C(11) H(9) 118.6 . . . no C(12) C(11) H(9) 118.3 . . . no C(11) C(12) C(13) 118.7(3) . . . yes C(11) C(12) H(10) 120.8 . . . no C(13) C(12) H(10) 120.5 . . . no C(12) C(13) C(14) 119.4(3) . . . yes C(12) C(13) H(11) 120.2 . . . no C(14) C(13) H(11) 120.3 . . . no C(13) C(14) C(15) 119.2(3) . . . yes C(13) C(14) H(12) 120.4 . . . no C(15) C(14) H(12) 120.4 . . . no N(3) C(15) C(14) 121.8(3) . . . yes N(3) C(15) C(16) 114.7(2) . . . yes C(14) C(15) C(16) 123.4(3) . . . yes N(4) C(16) C(15) 115.3(2) . . . yes N(4) C(16) C(17) 121.0(3) . . . yes C(15) C(16) C(17) 123.7(3) . . . yes C(16) C(17) C(18) 119.7(3) . . . yes C(16) C(17) H(13) 120.2 . . . no C(18) C(17) H(13) 120.1 . . . no C(17) C(18) C(19) 119.3(3) . . . yes C(17) C(18) H(14) 120.4 . . . no C(19) C(18) H(14) 120.3 . . . no C(18) C(19) C(20) 118.5(3) . . . yes C(18) C(19) H(15) 120.7 . . . no C(20) C(19) H(15) 120.7 . . . no N(4) C(20) C(19) 123.0(3) . . . yes N(4) C(20) H(16) 118.7 . . . no C(19) C(20) H(16) 118.3 . . . no P(1) C(21) C(22) 121.1(2) . . . yes P(1) C(21) C(26) 119.7(2) . . . yes C(22) C(21) C(26) 118.9(3) . . . yes C(21) C(22) C(23) 120.4(3) . . . yes C(21) C(22) H(17) 119.8 . . . no C(23) C(22) H(17) 119.8 . . . no C(22) C(23) C(24) 119.9(4) . . . yes C(22) C(23) H(18) 120.0 . . . no C(24) C(23) H(18) 120.1 . . . no C(23) C(24) C(25) 120.4(3) . . . yes C(23) C(24) H(19) 119.8 . . . no C(25) C(24) H(19) 119.8 . . . no C(24) C(25) C(26) 119.7(3) . . . yes C(24) C(25) H(20) 120.2 . . . no C(26) C(25) H(20) 120.1 . . . no C(21) C(26) C(25) 120.7(3) . . . yes C(21) C(26) H(21) 119.5 . . . no C(25) C(26) H(21) 119.8 . . . no P(1) C(27) C(28) 119.4(2) . . . yes P(1) C(27) C(32) 121.9(2) . . . yes C(28) C(27) C(32) 118.8(3) . . . yes C(27) C(28) C(29) 120.4(3) . . . yes C(27) C(28) H(22) 119.8 . . . no C(29) C(28) H(22) 119.8 . . . no C(28) C(29) C(30) 120.2(3) . . . yes C(28) C(29) H(23) 119.8 . . . no C(30) C(29) H(23) 120.0 . . . no C(29) C(30) C(31) 120.1(3) . . . yes C(29) C(30) H(24) 119.9 . . . no C(31) C(30) H(24) 119.9 . . . no C(30) C(31) C(32) 120.1(3) . . . yes C(30) C(31) H(25) 119.8 . . . no C(32) C(31) H(25) 120.2 . . . no C(27) C(32) C(31) 120.4(3) . . . yes C(27) C(32) H(26) 119.8 . . . no C(31) C(32) H(26) 119.8 . . . no S(1) C(33) C(34) 111.5(2) . . . yes S(1) C(33) H(27) 124.4 . . . no C(34) C(33) H(27) 124.1 . . . no C(33) C(34) C(35) 116.1(3) . . . yes C(33) C(34) H(28) 121.9 . . . no C(35) C(34) H(28) 122.0 . . . no Ru(1) C(35) C(34) 122.3(2) . . . yes Ru(1) C(35) C(36) 128.8(2) . . . yes C(34) C(35) C(36) 108.5(3) . . . yes S(1) C(36) C(35) 113.0(2) . . . yes S(1) C(36) C(37) 118.4(2) . . . yes C(35) C(36) C(37) 128.5(3) . . . yes S(2) C(37) C(36) 121.0(2) . . . yes S(2) C(37) C(38) 110.6(2) . . . yes C(36) C(37) C(38) 128.4(2) . . . yes P(1) C(38) C(37) 121.0(2) . . . yes P(1) C(38) C(39) 126.2(2) . . . yes C(37) C(38) C(39) 112.7(2) . . . yes C(38) C(39) C(40) 113.6(3) . . . yes C(38) C(39) H(29) 123.2 . . . no C(40) C(39) H(29) 123.2 . . . no S(2) C(40) C(39) 110.6(2) . . . yes S(2) C(40) C(41) 120.7(2) . . . yes C(39) C(40) C(41) 128.7(3) . . . yes S(3) C(41) C(40) 120.0(2) . . . yes S(3) C(41) C(42) 110.7(2) . . . yes C(40) C(41) C(42) 129.3(3) . . . yes C(41) C(42) C(43) 112.5(3) . . . yes C(41) C(42) H(30) 123.8 . . . no C(43) C(42) H(30) 123.7 . . . no C(42) C(43) C(44) 113.2(3) . . . yes C(42) C(43) H(31) 123.3 . . . no C(44) C(43) H(31) 123.5 . . . no S(3) C(44) C(43) 111.7(3) . . . yes S(3) C(44) H(32) 124.1 . . . no C(43) C(44) H(32) 124.2 . . . no O(1) C(45) C(46) 121.7(4) . . . yes O(1) C(45) C(47) 121.1(3) . . . yes C(46) C(45) C(47) 117.3(3) . . . yes C(45) C(46) H(33) 109.3 . . . no C(45) C(46) H(34) 109.7 . . . no C(45) C(46) H(35) 109.7 . . . no H(33) C(46) H(34) 109.4 . . . no H(33) C(46) H(35) 109.1 . . . no H(34) C(46) H(35) 109.7 . . . no C(45) C(47) H(36) 109.7 . . . no C(45) C(47) H(37) 109.3 . . . no C(45) C(47) H(38) 109.5 . . . no H(36) C(47) H(37) 109.4 . . . no H(36) C(47) H(38) 109.6 . . . no H(37) C(47) H(38) 109.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(30) 3.357(4) . 2_666 no F(1) O(1) 3.380(4) . . no F(1) C(11) 3.526(4) . . no F(1) C(45) 3.553(5) . . no F(1) C(12) 3.588(4) . . no F(2) C(9) 3.276(4) . 1_455 no F(2) C(4) 3.331(4) . 2_656 no F(2) C(10) 3.524(4) . 1_455 no F(2) C(3) 3.567(5) . . no F(2) C(3) 3.584(5) . 2_656 no F(3) C(1) 3.207(4) . . no F(3) N(1) 3.224(3) . . no F(3) C(5) 3.277(4) . . no F(3) C(11) 3.283(4) . . no F(3) C(2) 3.304(4) . . no F(3) C(4) 3.347(4) . . no F(3) C(3) 3.363(4) . . no F(3) C(8) 3.442(4) . 2_756 no F(3) C(9) 3.553(4) . 2_756 no F(4) C(45) 3.063(4) . . no F(4) C(47) 3.214(5) . . no F(4) C(3) 3.226(4) . 2_656 no F(4) C(9) 3.333(4) . 2_756 no F(4) C(46) 3.390(5) . . no F(4) O(1) 3.475(4) . . no F(4) C(8) 3.580(4) . 2_756 no F(5) C(31) 3.373(4) . 2_666 no F(5) C(14) 3.437(5) . 1_455 no F(5) C(30) 3.449(5) . 2_666 no F(6) C(17) 2.946(4) . 1_455 no F(6) C(16) 3.453(4) . 1_455 no F(6) C(29) 3.507(5) . . no F(6) C(14) 3.545(5) . 1_455 no F(6) C(18) 3.572(4) . 1_455 no O(1) C(43) 3.310(4) . 1_654 no O(1) C(25) 3.319(4) . 2_766 no O(1) C(12) 3.414(4) . . no O(1) C(44) 3.459(4) . 1_654 no C(6) C(8) 3.546(5) . 2_756 no C(7) C(8) 3.438(5) . 2_756 no C(7) C(9) 3.599(5) . 2_756 no C(17) C(29) 3.591(4) . 1_655 no C(18) C(29) 3.536(4) . 1_655 no C(33) C(33) 3.430(7) . 2_757 no C(33) C(42) 3.468(5) . 2_657 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(21) C(22) . . . . -96.4(2) no Ru(1) P(1) C(21) C(26) . . . . 77.2(2) no Ru(1) P(1) C(27) C(28) . . . . 21.9(2) no Ru(1) P(1) C(27) C(32) . . . . -159.2(2) no Ru(1) P(1) C(38) C(37) . . . . 24.8(3) no Ru(1) P(1) C(38) C(39) . . . . -159.8(2) no Ru(1) N(1) C(1) C(2) . . . . -171.0(2) no Ru(1) N(1) C(5) C(4) . . . . 173.0(2) no Ru(1) N(1) C(5) C(6) . . . . -6.7(3) no Ru(1) N(2) C(6) C(5) . . . . 6.3(3) no Ru(1) N(2) C(6) C(7) . . . . -174.9(2) no Ru(1) N(2) C(10) C(9) . . . . 175.8(2) no Ru(1) N(3) C(11) C(12) . . . . -171.0(2) no Ru(1) N(3) C(15) C(14) . . . . 172.1(3) no Ru(1) N(3) C(15) C(16) . . . . -5.6(3) no Ru(1) N(4) C(16) C(15) . . . . -3.4(3) no Ru(1) N(4) C(16) C(17) . . . . 176.5(2) no Ru(1) N(4) C(20) C(19) . . . . -176.3(2) no Ru(1) C(35) C(34) C(33) . . . . -174.0(2) no Ru(1) C(35) C(36) S(1) . . . . 173.5(1) no Ru(1) C(35) C(36) C(37) . . . . -10.0(4) no S(1) C(33) C(34) C(35) . . . . 0.0(4) no S(1) C(36) C(35) C(34) . . . . -0.1(3) no S(1) C(36) C(37) S(2) . . . . -10.7(3) no S(1) C(36) C(37) C(38) . . . . 165.9(2) no S(2) C(37) C(36) C(35) . . . . 172.9(2) no S(2) C(37) C(38) P(1) . . . . 176.4(1) no S(2) C(37) C(38) C(39) . . . . 0.4(3) no S(2) C(40) C(39) C(38) . . . . -0.9(3) no S(2) C(40) C(41) S(3) . . . . 161.6(2) no S(2) C(40) C(41) C(42) . . . . -17.2(5) no S(3) C(41) C(40) C(39) . . . . -17.3(4) no S(3) C(41) C(42) C(43) . . . . 0.7(4) no S(3) C(44) C(43) C(42) . . . . -0.4(4) no P(1) Ru(1) N(1) C(1) . . . . -0.8(3) no P(1) Ru(1) N(1) C(5) . . . . -171.7(2) no P(1) Ru(1) N(2) C(6) . . . . 4(1) no P(1) Ru(1) N(2) C(10) . . . . -174.4(9) no P(1) Ru(1) N(3) C(11) . . . . -98.4(2) no P(1) Ru(1) N(3) C(15) . . . . 90.6(2) no P(1) Ru(1) N(4) C(16) . . . . -97.6(2) no P(1) Ru(1) N(4) C(20) . . . . 80.4(2) no P(1) Ru(1) C(35) C(34) . . . . -160.4(2) no P(1) Ru(1) C(35) C(36) . . . . 26.9(2) no P(1) C(21) C(22) C(23) . . . . 174.4(3) no P(1) C(21) C(26) C(25) . . . . -174.9(2) no P(1) C(27) C(28) C(29) . . . . 179.4(2) no P(1) C(27) C(32) C(31) . . . . -178.5(2) no P(1) C(38) C(37) C(36) . . . . -0.5(4) no P(1) C(38) C(39) C(40) . . . . -175.5(2) no N(1) Ru(1) P(1) C(21) . . . . 170.5(1) no N(1) Ru(1) P(1) C(27) . . . . -69.8(1) no N(1) Ru(1) P(1) C(38) . . . . 52.4(1) no N(1) Ru(1) N(2) C(6) . . . . -7.5(2) no N(1) Ru(1) N(2) C(10) . . . . 174.2(3) no N(1) Ru(1) N(3) C(11) . . . . 2.2(2) no N(1) Ru(1) N(3) C(15) . . . . -168.8(2) no N(1) Ru(1) N(4) C(16) . . . . 90.1(7) no N(1) Ru(1) N(4) C(20) . . . . -91.9(7) no N(1) Ru(1) C(35) C(34) . . . . 100.9(2) no N(1) Ru(1) C(35) C(36) . . . . -71.8(2) no N(1) C(1) C(2) C(3) . . . . -1.0(5) no N(1) C(5) C(4) C(3) . . . . -1.0(5) no N(1) C(5) C(6) N(2) . . . . 0.2(4) no N(1) C(5) C(6) C(7) . . . . -178.6(3) no N(2) Ru(1) P(1) C(21) . . . . 159(1) no N(2) Ru(1) P(1) C(27) . . . . -81(1) no N(2) Ru(1) P(1) C(38) . . . . 41(1) no N(2) Ru(1) N(1) C(1) . . . . 178.4(3) no N(2) Ru(1) N(1) C(5) . . . . 7.6(2) no N(2) Ru(1) N(3) C(11) . . . . 78.3(2) no N(2) Ru(1) N(3) C(15) . . . . -92.7(2) no N(2) Ru(1) N(4) C(16) . . . . 83.2(2) no N(2) Ru(1) N(4) C(20) . . . . -98.8(2) no N(2) Ru(1) C(35) C(34) . . . . 23.2(2) no N(2) Ru(1) C(35) C(36) . . . . -149.6(2) no N(2) C(6) C(5) C(4) . . . . -179.5(3) no N(2) C(6) C(7) C(8) . . . . -1.3(5) no N(2) C(10) C(9) C(8) . . . . -0.8(5) no N(3) Ru(1) P(1) C(21) . . . . -85.2(1) no N(3) Ru(1) P(1) C(27) . . . . 34.4(1) no N(3) Ru(1) P(1) C(38) . . . . 156.6(1) no N(3) Ru(1) N(1) C(1) . . . . -100.6(3) no N(3) Ru(1) N(1) C(5) . . . . 88.5(2) no N(3) Ru(1) N(2) C(6) . . . . -112.0(2) no N(3) Ru(1) N(2) C(10) . . . . 69.7(2) no N(3) Ru(1) N(4) C(16) . . . . 0.3(2) no N(3) Ru(1) N(4) C(20) . . . . 178.3(2) no N(3) Ru(1) C(35) C(34) . . . . -25.2(7) no N(3) Ru(1) C(35) C(36) . . . . 162.0(5) no N(3) C(11) C(12) C(13) . . . . -0.7(5) no N(3) C(15) C(14) C(13) . . . . 0.8(6) no N(3) C(15) C(16) N(4) . . . . 5.9(4) no N(3) C(15) C(16) C(17) . . . . -173.9(3) no N(4) Ru(1) P(1) C(21) . . . . -8.4(1) no N(4) Ru(1) P(1) C(27) . . . . 111.3(1) no N(4) Ru(1) P(1) C(38) . . . . -126.5(1) no N(4) Ru(1) N(1) C(1) . . . . 171.4(6) no N(4) Ru(1) N(1) C(5) . . . . 0.6(8) no N(4) Ru(1) N(2) C(6) . . . . 171.6(2) no N(4) Ru(1) N(2) C(10) . . . . -6.8(2) no N(4) Ru(1) N(3) C(11) . . . . 174.0(2) no N(4) Ru(1) N(3) C(15) . . . . 3.0(2) no N(4) Ru(1) C(35) C(34) . . . . -71.1(2) no N(4) Ru(1) C(35) C(36) . . . . 116.1(2) no N(4) C(16) C(15) C(14) . . . . -171.7(3) no N(4) C(16) C(17) C(18) . . . . 0.3(4) no N(4) C(20) C(19) C(18) . . . . -0.5(5) no C(1) N(1) Ru(1) C(35) . . . . 87.4(3) no C(1) N(1) C(5) C(4) . . . . 1.1(4) no C(1) N(1) C(5) C(6) . . . . -178.6(3) no C(1) C(2) C(3) C(4) . . . . 1.1(5) no C(2) C(1) N(1) C(5) . . . . -0.1(5) no C(2) C(3) C(4) C(5) . . . . -0.1(6) no C(3) C(4) C(5) C(6) . . . . 178.7(3) no C(4) C(5) C(6) C(7) . . . . 1.7(5) no C(5) N(1) Ru(1) C(35) . . . . -83.5(2) no C(5) C(6) N(2) C(10) . . . . -175.3(3) no C(5) C(6) C(7) C(8) . . . . 177.4(3) no C(6) N(2) Ru(1) C(35) . . . . 75.2(2) no C(6) N(2) C(10) C(9) . . . . -2.5(5) no C(6) C(7) C(8) C(9) . . . . -2.0(5) no C(7) C(6) N(2) C(10) . . . . 3.5(4) no C(7) C(8) C(9) C(10) . . . . 3.1(5) no C(10) N(2) Ru(1) C(35) . . . . -103.1(2) no C(11) N(3) Ru(1) C(35) . . . . 127.0(6) no C(11) N(3) C(15) C(14) . . . . 0.2(4) no C(11) N(3) C(15) C(16) . . . . -177.5(2) no C(11) C(12) C(13) C(14) . . . . 1.8(6) no C(12) C(11) N(3) C(15) . . . . -0.3(4) no C(12) C(13) C(14) C(15) . . . . -1.8(6) no C(13) C(14) C(15) C(16) . . . . 178.3(3) no C(14) C(15) C(16) C(17) . . . . 8.4(5) no C(15) N(3) Ru(1) C(35) . . . . -44.0(7) no C(15) C(16) N(4) C(20) . . . . 178.5(2) no C(15) C(16) C(17) C(18) . . . . -179.8(3) no C(16) N(4) Ru(1) C(35) . . . . 173.2(2) no C(16) N(4) C(20) C(19) . . . . 1.7(4) no C(16) C(17) C(18) C(19) . . . . 0.9(5) no C(17) C(16) N(4) C(20) . . . . -1.6(4) no C(17) C(18) C(19) C(20) . . . . -0.8(5) no C(20) N(4) Ru(1) C(35) . . . . -8.8(2) no C(21) P(1) Ru(1) C(35) . . . . 87.9(1) no C(21) P(1) C(27) C(28) . . . . 148.6(2) no C(21) P(1) C(27) C(32) . . . . -32.6(2) no C(21) P(1) C(38) C(37) . . . . -100.2(2) no C(21) P(1) C(38) C(39) . . . . 75.2(3) no C(21) C(22) C(23) C(24) . . . . -0.2(5) no C(21) C(26) C(25) C(24) . . . . 0.8(5) no C(22) C(21) P(1) C(27) . . . . 134.1(2) no C(22) C(21) P(1) C(38) . . . . 28.4(3) no C(22) C(21) C(26) C(25) . . . . -1.2(4) no C(22) C(23) C(24) C(25) . . . . -0.2(6) no C(23) C(22) C(21) C(26) . . . . 0.8(5) no C(23) C(24) C(25) C(26) . . . . -0.2(5) no C(26) C(21) P(1) C(27) . . . . -52.3(2) no C(26) C(21) P(1) C(38) . . . . -158.1(2) no C(27) P(1) Ru(1) C(35) . . . . -152.4(1) no C(27) P(1) C(38) C(37) . . . . 155.6(2) no C(27) P(1) C(38) C(39) . . . . -28.9(3) no C(27) C(28) C(29) C(30) . . . . -1.1(4) no C(27) C(32) C(31) C(30) . . . . -0.6(5) no C(28) C(27) P(1) C(38) . . . . -105.9(2) no C(28) C(27) C(32) C(31) . . . . 0.3(4) no C(28) C(29) C(30) C(31) . . . . 0.8(5) no C(29) C(28) C(27) C(32) . . . . 0.6(4) no C(29) C(30) C(31) C(32) . . . . 0.1(5) no C(32) C(27) P(1) C(38) . . . . 72.9(2) no C(33) S(1) C(36) C(35) . . . . 0.0(2) no C(33) S(1) C(36) C(37) . . . . -176.9(2) no C(33) C(34) C(35) C(36) . . . . 0.1(4) no C(34) C(33) S(1) C(36) . . . . 0.0(3) no C(34) C(35) C(36) C(37) . . . . 176.5(3) no C(35) Ru(1) P(1) C(38) . . . . -30.2(1) no C(35) C(36) C(37) C(38) . . . . -10.5(5) no C(36) C(37) S(2) C(40) . . . . 176.4(2) no C(36) C(37) C(38) C(39) . . . . -176.5(3) no C(37) S(2) C(40) C(39) . . . . 0.9(2) no C(37) S(2) C(40) C(41) . . . . -178.1(2) no C(37) C(38) C(39) C(40) . . . . 0.3(4) no C(38) C(37) S(2) C(40) . . . . -0.8(2) no C(38) C(39) C(40) C(41) . . . . 178.1(3) no C(39) C(40) C(41) C(42) . . . . 163.9(3) no C(40) C(41) S(3) C(44) . . . . -179.8(3) no C(40) C(41) C(42) C(43) . . . . 179.6(3) no C(41) S(3) C(44) C(43) . . . . 0.7(3) no C(41) C(42) C(43) C(44) . . . . -0.2(5) no C(42) C(41) S(3) C(44) . . . . -0.8(3) no #---------------------------------------------- #---END data_mw015/1a _database_code_CSD 193872 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H39 F12 N4 O P3 Ru S3' _chemical_formula_weight 1194.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9127(4) _cell_length_b 11.2475(4) _cell_length_c 20.5749(4) _cell_angle_alpha 74.704(6) _cell_angle_beta 76.606(7) _cell_angle_gamma 91.102(8) _cell_volume 2360.96(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14384 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.87 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7576 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 11.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22282 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.87 _reflns_number_total 9749 _reflns_number_gt 7610 _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 w=1/[\s^2^(Fo^2^)+(0.0487P)^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 9749 _refine_ls_number_parameters 644 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.61510(2) 0.12267(2) 0.758277(12) 0.01152(7) Uani 1 d . A 1 S1 S 0.63897(7) 0.34007(7) 0.71171(4) 0.01680(16) Uani 1 d . A 1 S2 S 0.36935(7) 0.44540(8) 0.58884(5) 0.02305(18) Uani 1 d . A 1 P1 P 0.55166(6) 0.11086(7) 0.65982(4) 0.01087(15) Uani 1 d . A 1 P2 P 1.02888(9) -0.15334(9) 0.89750(5) 0.0278(2) Uani 1 d . B 1 P3 P 1.01892(9) -0.54089(11) 0.74684(5) 0.0355(2) Uani 1 d . C 1 F1 F 1.0451(2) -0.0385(2) 0.83125(12) 0.0498(6) Uani 1 d . B 1 F2 F 0.8785(2) -0.1481(3) 0.91321(14) 0.0533(7) Uani 1 d . B 1 F3 F 1.0366(2) -0.0621(2) 0.94405(11) 0.0414(6) Uani 1 d . B 1 F4 F 1.18027(19) -0.1581(3) 0.88204(12) 0.0456(6) Uani 1 d . B 1 F5 F 1.0212(2) -0.2455(2) 0.85123(12) 0.0401(5) Uani 1 d . B 1 F6 F 1.0116(3) -0.2667(2) 0.96451(12) 0.0539(7) Uani 1 d . B 1 F7 F 0.9440(4) -0.4289(4) 0.7481(3) 0.149(2) Uani 1 d . C 1 F8 F 1.1326(3) -0.4772(4) 0.76224(18) 0.0994(15) Uani 1 d . C 1 F9 F 0.9717(4) -0.6093(5) 0.82521(17) 0.1249(18) Uani 1 d . C 1 F10 F 0.9059(2) -0.6077(3) 0.73037(16) 0.0691(9) Uani 1 d . C 1 F11 F 1.0736(3) -0.4837(4) 0.66680(15) 0.1006(15) Uani 1 d . C 1 F12 F 1.0985(5) -0.6552(5) 0.7398(3) 0.1357(18) Uani 1 d . C 1 O1 O 1.3703(4) -0.5431(4) 0.9629(2) 0.0856(13) Uani 1 d . D 1 N1 N 0.4418(2) 0.1456(2) 0.82122(13) 0.0157(5) Uani 1 d . A 1 N2 N 0.6679(2) 0.1359(2) 0.84888(13) 0.0162(5) Uani 1 d . A 1 N3 N 0.6110(2) -0.0661(2) 0.80041(13) 0.0174(5) Uani 1 d . A 1 N4 N 0.7970(2) 0.0870(2) 0.71263(13) 0.0163(5) Uani 1 d . A 1 C1 C 0.3292(3) 0.1549(3) 0.80473(16) 0.0175(6) Uani 1 d . A 1 H1 H 0.3253 0.1506 0.7597 0.021 Uiso 1 calc R A 1 C2 C 0.2197(3) 0.1702(3) 0.84957(17) 0.0224(7) Uani 1 d . A 1 H2 H 0.1426 0.1773 0.8354 0.027 Uiso 1 calc R A 1 C3 C 0.2233(3) 0.1751(4) 0.91514(19) 0.0303(8) Uani 1 d . A 1 H3 H 0.1483 0.1829 0.9476 0.036 Uiso 1 calc R A 1 C4 C 0.3375(3) 0.1686(4) 0.93281(18) 0.0293(8) Uani 1 d . A 1 H4 H 0.3422 0.1738 0.9775 0.035 Uiso 1 calc R A 1 C5 C 0.4459(3) 0.1545(3) 0.88550(15) 0.0173(6) Uani 1 d . A 1 C6 C 0.5716(3) 0.1484(3) 0.90063(16) 0.0205(7) Uani 1 d . A 1 C7 C 0.5932(3) 0.1550(4) 0.96357(18) 0.0332(9) Uani 1 d . A 1 H7 H 0.5249 0.1639 0.9996 0.040 Uiso 1 calc R A 1 C8 C 0.7137(3) 0.1486(4) 0.97386(19) 0.0362(9) Uani 1 d . A 1 H8 H 0.7291 0.1531 1.0168 0.043 Uiso 1 calc R A 1 C9 C 0.8111(3) 0.1356(3) 0.92085(18) 0.0279(8) Uani 1 d . A 1 H9 H 0.8949 0.1306 0.9266 0.034 Uiso 1 calc R A 1 C10 C 0.7850(3) 0.1300(3) 0.85925(17) 0.0232(7) Uani 1 d . A 1 H10 H 0.8526 0.1217 0.8226 0.028 Uiso 1 calc R A 1 C11 C 0.5128(3) -0.1363(3) 0.84874(17) 0.0244(7) Uani 1 d . A 1 H11 H 0.4365 -0.0994 0.8613 0.029 Uiso 1 calc R A 1 C12 C 0.5189(4) -0.2586(3) 0.8803(2) 0.0348(9) Uani 1 d . A 1 H12 H 0.4481 -0.3057 0.9141 0.042 Uiso 1 calc R A 1 C13 C 0.6296(4) -0.3123(4) 0.8621(2) 0.0441(11) Uani 1 d . A 1 H13 H 0.6357 -0.3973 0.8830 0.053 Uiso 1 calc R A 1 C14 C 0.7307(4) -0.2420(4) 0.8137(2) 0.0356(9) Uani 1 d . A 1 H14 H 0.8076 -0.2780 0.8011 0.043 Uiso 1 calc R A 1 C15 C 0.7206(3) -0.1177(3) 0.78302(17) 0.0230(7) Uani 1 d . A 1 C16 C 0.8244(3) -0.0321(3) 0.73278(17) 0.0218(7) Uani 1 d . A 1 C17 C 0.9433(3) -0.0686(4) 0.7085(2) 0.0356(9) Uani 1 d . A 1 H17 H 0.9604 -0.1528 0.7224 0.043 Uiso 1 calc R A 1 C18 C 1.0364(3) 0.0196(4) 0.6639(2) 0.0398(10) Uani 1 d . A 1 H18 H 1.1190 -0.0031 0.6478 0.048 Uiso 1 calc R A 1 C19 C 1.0089(3) 0.1398(4) 0.64309(19) 0.0344(9) Uani 1 d . A 1 H19 H 1.0717 0.2013 0.6119 0.041 Uiso 1 calc R A 1 C20 C 0.8881(3) 0.1705(3) 0.66817(17) 0.0237(7) Uani 1 d . A 1 H20 H 0.8691 0.2539 0.6533 0.028 Uiso 1 calc R A 1 C21 C 0.6851(3) 0.1253(3) 0.58465(15) 0.0135(6) Uani 1 d . A 1 C22 C 0.7304(3) 0.2409(3) 0.53854(16) 0.0195(7) Uani 1 d . A 1 H22 H 0.6906 0.3123 0.5458 0.023 Uiso 1 calc R A 1 C23 C 0.8327(3) 0.2531(4) 0.48217(17) 0.0269(8) Uani 1 d . A 1 H23 H 0.8637 0.3324 0.4514 0.032 Uiso 1 calc R A 1 C24 C 0.8896(3) 0.1486(4) 0.47101(18) 0.0289(8) Uani 1 d . A 1 H24 H 0.9584 0.1562 0.4318 0.035 Uiso 1 calc R A 1 C25 C 0.8464(3) 0.0335(4) 0.51665(18) 0.0274(8) Uani 1 d . A 1 H25 H 0.8854 -0.0378 0.5087 0.033 Uiso 1 calc R A 1 C26 C 0.7468(3) 0.0220(3) 0.57373(16) 0.0177(6) Uani 1 d . A 1 H26 H 0.7199 -0.0569 0.6059 0.021 Uiso 1 calc R A 1 C27 C 0.4556(3) -0.0255(3) 0.66056(15) 0.0122(6) Uani 1 d . A 1 C28 C 0.3667(3) -0.0886(3) 0.72112(16) 0.0179(6) Uani 1 d . A 1 H28 H 0.3598 -0.0636 0.7624 0.021 Uiso 1 calc R A 1 C29 C 0.2879(3) -0.1879(3) 0.72178(17) 0.0229(7) Uani 1 d . A 1 H29 H 0.2275 -0.2299 0.7634 0.027 Uiso 1 calc R A 1 C30 C 0.2968(3) -0.2259(3) 0.66243(17) 0.0224(7) Uani 1 d . A 1 H30 H 0.2436 -0.2942 0.6631 0.027 Uiso 1 calc R A 1 C31 C 0.3841(3) -0.1635(3) 0.60199(17) 0.0225(7) Uani 1 d . A 1 H31 H 0.3903 -0.1890 0.5609 0.027 Uiso 1 calc R A 1 C32 C 0.4625(3) -0.0642(3) 0.60064(16) 0.0166(6) Uani 1 d . A 1 H32 H 0.5216 -0.0220 0.5586 0.020 Uiso 1 calc R A 1 C33 C 0.6207(3) 0.4200(3) 0.77487(18) 0.0271(8) Uani 1 d . A 1 H33 H 0.6768 0.4195 0.8040 0.033 Uiso 1 calc R A 1 C34 C 0.5171(3) 0.4824(4) 0.7769(2) 0.0333(9) Uani 1 d . A 1 H34 H 0.4928 0.5330 0.8073 0.040 Uiso 1 calc R A 1 C35 C 0.4466(3) 0.4657(3) 0.7291(2) 0.0294(8) Uani 1 d . A 1 H35 H 0.3716 0.5048 0.7242 0.035 Uiso 1 calc R A 1 C36 C 0.4976(3) 0.3884(3) 0.69132(17) 0.0183(6) Uani 1 d . A 1 C37 C 0.4515(3) 0.3472(3) 0.63943(16) 0.0166(6) Uani 1 d . A 1 C38 C 0.4633(2) 0.2362(3) 0.62297(15) 0.0134(6) Uani 1 d . A 1 C39 C 0.4022(3) 0.2314(3) 0.56944(16) 0.0169(6) Uani 1 d . A 1 H39 H 0.4004 0.1616 0.5517 0.020 Uiso 1 calc R A 1 C40 C 0.3465(3) 0.3370(3) 0.54597(16) 0.0194(7) Uani 1 d . A 1 S3 S 0.3147(2) 0.3082(3) 0.42301(13) 0.0309(6) Uani 0.641(4) d PD A 1 C41 C 0.2791(3) 0.3632(3) 0.49144(18) 0.0251(8) Uani 1 d D A 1 C42 C 0.1656(6) 0.4454(7) 0.4940(4) 0.0188(19) Uiso 0.641(4) d PD A 1 H42 H 0.1297 0.4848 0.5287 0.023 Uiso 0.641(4) calc PR A 1 C43 C 0.1283(5) 0.4469(6) 0.4313(3) 0.0261(13) Uiso 0.641(4) d PD A 1 H43 H 0.0620 0.4938 0.4183 0.031 Uiso 0.641(4) calc PR A 1 C44 C 0.1923(6) 0.3781(6) 0.3911(3) 0.0233(12) Uiso 0.641(4) d PD A 1 H44 H 0.1719 0.3694 0.3500 0.028 Uiso 0.641(4) calc PR A 1 C45 C 1.1883(6) -0.4829(5) 1.0307(3) 0.0756(17) Uani 1 d . D 1 H45A H 1.1344 -0.5561 1.0616 0.113 Uiso 1 calc R D 1 H45B H 1.1353 -0.4160 1.0169 0.113 Uiso 1 calc R D 1 H45C H 1.2463 -0.4563 1.0550 0.113 Uiso 1 calc R D 1 C46 C 1.2624(5) -0.5136(4) 0.9676(3) 0.0519(12) Uani 1 d . D 1 C47 C 1.1988(5) -0.5077(5) 0.9107(3) 0.0609(14) Uani 1 d . D 1 H47A H 1.1862 -0.4215 0.8895 0.091 Uiso 1 calc R D 1 H47B H 1.1166 -0.5563 0.9295 0.091 Uiso 1 calc R D 1 H47C H 1.2514 -0.5416 0.8755 0.091 Uiso 1 calc R D 1 S3B S 0.1560(4) 0.4311(4) 0.4848(2) 0.0354(13) Uiso 0.359(4) d PD A 2 C42B C 0.3108(13) 0.3257(14) 0.4318(5) 0.025(6) Uiso 0.359(4) d PD A 2 H42B H 0.3848 0.2835 0.4228 0.030 Uiso 0.359(4) calc PR A 2 C43B C 0.2333(9) 0.3496(9) 0.3831(5) 0.023(2) Uiso 0.359(4) d PD A 2 H43B H 0.2432 0.3267 0.3410 0.028 Uiso 0.359(4) calc PR A 2 C44B C 0.1413(8) 0.4139(9) 0.4127(4) 0.0168(19) Uiso 0.359(4) d PD A 2 H44B H 0.0749 0.4453 0.3921 0.020 Uiso 0.359(4) calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01319(12) 0.01424(13) 0.00839(12) -0.00595(9) -0.00181(8) 0.00148(8) S1 0.0193(4) 0.0153(4) 0.0160(4) -0.0068(3) -0.0024(3) -0.0017(3) S2 0.0248(4) 0.0162(4) 0.0287(5) -0.0050(3) -0.0088(3) 0.0073(3) P1 0.0124(3) 0.0120(4) 0.0085(4) -0.0043(3) -0.0016(3) 0.0015(3) P2 0.0311(5) 0.0327(6) 0.0198(5) -0.0096(4) -0.0045(4) 0.0001(4) P3 0.0280(5) 0.0422(6) 0.0320(6) -0.0011(5) -0.0106(4) -0.0075(4) F1 0.0779(17) 0.0406(15) 0.0309(13) -0.0011(11) -0.0245(12) -0.0063(12) F2 0.0330(13) 0.073(2) 0.0645(18) -0.0397(15) -0.0092(11) 0.0073(12) F3 0.0491(13) 0.0509(16) 0.0313(13) -0.0240(12) -0.0092(10) 0.0028(11) F4 0.0299(12) 0.0792(19) 0.0345(13) -0.0293(13) -0.0052(9) 0.0057(11) F5 0.0458(13) 0.0418(14) 0.0370(13) -0.0232(11) -0.0046(10) -0.0006(10) F6 0.0724(17) 0.0499(17) 0.0277(13) -0.0004(12) -0.0013(12) 0.0056(13) F7 0.148(4) 0.124(4) 0.285(7) -0.158(4) -0.144(4) 0.098(3) F8 0.081(2) 0.112(3) 0.087(2) 0.033(2) -0.0593(19) -0.054(2) F9 0.121(3) 0.183(5) 0.0394(19) 0.001(2) -0.0031(19) -0.084(3) F10 0.0543(16) 0.088(2) 0.071(2) -0.0281(18) -0.0210(14) -0.0252(15) F11 0.064(2) 0.166(4) 0.0398(18) 0.023(2) -0.0133(15) -0.026(2) F12 0.164(4) 0.125(4) 0.155(4) -0.046(3) -0.095(3) 0.095(3) O1 0.063(3) 0.098(4) 0.091(3) -0.014(3) -0.024(2) -0.016(2) N1 0.0177(13) 0.0150(14) 0.0134(13) -0.0059(11) 0.0003(9) 0.0003(9) N2 0.0214(13) 0.0173(14) 0.0119(13) -0.0069(11) -0.0048(10) 0.0005(10) N3 0.0289(14) 0.0168(14) 0.0117(13) -0.0070(11) -0.0114(10) 0.0058(10) N4 0.0133(12) 0.0260(15) 0.0149(13) -0.0124(11) -0.0062(9) 0.0048(10) C1 0.0143(15) 0.0199(17) 0.0180(16) -0.0072(13) -0.0014(11) -0.0009(11) C2 0.0155(15) 0.0233(18) 0.0268(19) -0.0090(15) 0.0000(12) 0.0010(12) C3 0.0221(17) 0.039(2) 0.0270(19) -0.0159(17) 0.0066(13) 0.0016(14) C4 0.0309(19) 0.042(2) 0.0155(17) -0.0156(16) 0.0018(13) 0.0001(15) C5 0.0211(16) 0.0195(17) 0.0094(15) -0.0062(13) 0.0023(11) -0.0026(12) C6 0.0267(17) 0.0242(18) 0.0104(15) -0.0068(13) -0.0024(12) -0.0048(13) C7 0.036(2) 0.054(3) 0.0118(17) -0.0171(17) -0.0015(14) -0.0038(17) C8 0.040(2) 0.056(3) 0.0166(18) -0.0131(18) -0.0120(15) -0.0059(18) C9 0.0317(19) 0.035(2) 0.0222(19) -0.0103(16) -0.0144(14) -0.0010(15) C10 0.0223(17) 0.030(2) 0.0223(18) -0.0116(15) -0.0098(13) 0.0038(13) C11 0.0370(19) 0.0218(18) 0.0139(17) -0.0052(14) -0.0053(13) -0.0034(14) C12 0.060(3) 0.020(2) 0.027(2) -0.0035(16) -0.0200(18) -0.0058(17) C13 0.077(3) 0.016(2) 0.050(3) -0.0058(18) -0.040(2) 0.0036(19) C14 0.051(2) 0.026(2) 0.045(2) -0.0167(19) -0.033(2) 0.0165(17) C15 0.0370(19) 0.0208(18) 0.0220(18) -0.0138(14) -0.0188(14) 0.0128(14) C16 0.0254(17) 0.031(2) 0.0187(17) -0.0168(15) -0.0129(13) 0.0153(13) C17 0.039(2) 0.049(3) 0.032(2) -0.0234(19) -0.0181(17) 0.0274(18) C18 0.0238(19) 0.070(3) 0.035(2) -0.027(2) -0.0099(16) 0.0213(19) C19 0.0178(17) 0.058(3) 0.028(2) -0.0184(19) -0.0009(14) 0.0026(16) C20 0.0169(16) 0.036(2) 0.0200(17) -0.0124(15) -0.0030(12) 0.0006(13) C21 0.0124(14) 0.0181(16) 0.0126(15) -0.0077(12) -0.0043(10) -0.0006(11) C22 0.0187(15) 0.0236(18) 0.0177(16) -0.0092(14) -0.0037(12) 0.0000(12) C23 0.0220(17) 0.039(2) 0.0141(17) -0.0056(15) 0.0030(12) -0.0102(14) C24 0.0174(16) 0.048(2) 0.0190(18) -0.0143(17) 0.0045(12) -0.0041(14) C25 0.0169(16) 0.038(2) 0.032(2) -0.0224(17) 0.0001(13) 0.0058(14) C26 0.0135(14) 0.0218(17) 0.0208(17) -0.0109(14) -0.0041(11) 0.0047(11) C27 0.0143(14) 0.0102(15) 0.0123(15) -0.0037(12) -0.0030(10) 0.0006(10) C28 0.0221(16) 0.0196(17) 0.0104(15) -0.0041(13) -0.0012(11) -0.0005(12) C29 0.0217(16) 0.0221(18) 0.0200(17) -0.0035(14) 0.0014(12) -0.0052(12) C30 0.0225(16) 0.0190(18) 0.0258(18) -0.0068(14) -0.0061(13) -0.0048(12) C31 0.0252(17) 0.0262(19) 0.0209(17) -0.0161(15) -0.0044(13) 0.0000(13) C32 0.0177(15) 0.0196(17) 0.0120(15) -0.0061(13) -0.0008(11) -0.0007(11) C33 0.0368(19) 0.0231(19) 0.0266(19) -0.0150(16) -0.0089(15) -0.0030(14) C34 0.040(2) 0.029(2) 0.039(2) -0.0250(18) -0.0052(16) 0.0018(16) C35 0.0325(19) 0.0228(19) 0.038(2) -0.0186(17) -0.0060(15) 0.0052(14) C36 0.0218(15) 0.0130(16) 0.0201(17) -0.0069(13) -0.0025(12) 0.0012(11) C37 0.0166(15) 0.0153(16) 0.0150(16) -0.0010(13) -0.0017(11) 0.0034(11) C38 0.0105(13) 0.0154(15) 0.0140(15) -0.0051(12) -0.0008(10) 0.0004(10) C39 0.0168(15) 0.0163(16) 0.0175(16) -0.0033(13) -0.0059(11) 0.0028(11) C40 0.0182(15) 0.0189(17) 0.0188(17) -0.0014(13) -0.0042(12) 0.0018(12) S3 0.0446(12) 0.0301(11) 0.0289(10) -0.0169(9) -0.0195(7) 0.0166(8) C41 0.0240(17) 0.0214(18) 0.0255(19) 0.0065(14) -0.0130(13) -0.0049(13) C45 0.117(5) 0.053(4) 0.070(4) -0.016(3) -0.050(4) 0.020(3) C46 0.058(3) 0.032(3) 0.058(3) 0.002(2) -0.019(2) -0.013(2) C47 0.075(3) 0.052(3) 0.058(3) -0.011(3) -0.026(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.066(3) . ? Ru1 N4 2.086(2) . ? Ru1 N1 2.093(2) . ? Ru1 N2 2.114(2) . ? Ru1 P1 2.3215(7) . ? Ru1 S1 2.3640(8) . ? S1 C33 1.744(3) . ? S1 C36 1.751(3) . ? S2 C37 1.724(3) . ? S2 C40 1.727(3) . ? P1 C38 1.822(3) . ? P1 C21 1.831(3) . ? P1 C27 1.836(3) . ? P2 F6 1.583(3) . ? P2 F1 1.583(2) . ? P2 F3 1.590(2) . ? P2 F5 1.595(2) . ? P2 F2 1.603(2) . ? P2 F4 1.613(2) . ? P3 F7 1.517(3) . ? P3 F9 1.550(3) . ? P3 F8 1.556(3) . ? P3 F11 1.566(3) . ? P3 F10 1.579(3) . ? P3 F12 1.584(4) . ? O1 C46 1.219(6) . ? N1 C1 1.347(4) . ? N1 C5 1.363(4) . ? N2 C10 1.344(4) . ? N2 C6 1.351(4) . ? N3 C11 1.350(4) . ? N3 C15 1.354(4) . ? N4 C20 1.340(4) . ? N4 C16 1.355(4) . ? C1 C2 1.375(4) . ? C2 C3 1.374(5) . ? C3 C4 1.375(5) . ? C4 C5 1.388(4) . ? C5 C6 1.474(4) . ? C6 C7 1.389(4) . ? C7 C8 1.380(5) . ? C8 C9 1.376(5) . ? C9 C10 1.378(4) . ? C11 C12 1.368(5) . ? C12 C13 1.379(6) . ? C13 C14 1.371(6) . ? C14 C15 1.392(5) . ? C15 C16 1.473(5) . ? C16 C17 1.389(4) . ? C17 C18 1.381(6) . ? C18 C19 1.368(6) . ? C19 C20 1.385(5) . ? C21 C22 1.394(4) . ? C21 C26 1.397(4) . ? C22 C23 1.386(4) . ? C23 C24 1.387(5) . ? C24 C25 1.382(5) . ? C25 C26 1.378(4) . ? C27 C28 1.395(4) . ? C27 C32 1.399(4) . ? C28 C29 1.392(4) . ? C29 C30 1.380(5) . ? C30 C31 1.382(5) . ? C31 C32 1.385(4) . ? C33 C34 1.340(5) . ? C34 C35 1.426(5) . ? C35 C36 1.359(5) . ? C36 C37 1.452(4) . ? C37 C38 1.378(4) . ? C38 C39 1.424(4) . ? C39 C40 1.370(4) . ? C40 C41 1.451(4) . ? S3 C41 1.653(5) . ? S3 C44 1.735(7) . ? C41 C42B 1.374(5) . ? C41 C42 1.559(8) . ? C42 C43 1.437(10) . ? C43 C44 1.364(9) . ? C45 C46 1.489(8) . ? C46 C47 1.481(7) . ? S3B C44B 1.588(6) . ? C42B C43B 1.432(5) . ? C43B C44B 1.372(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 N4 78.31(10) . . ? N3 Ru1 N1 96.33(10) . . ? N4 Ru1 N1 169.54(10) . . ? N3 Ru1 N2 84.94(10) . . ? N4 Ru1 N2 92.22(9) . . ? N1 Ru1 N2 78.27(10) . . ? N3 Ru1 P1 95.81(7) . . ? N4 Ru1 P1 89.44(7) . . ? N1 Ru1 P1 100.11(7) . . ? N2 Ru1 P1 178.29(7) . . ? N3 Ru1 S1 174.65(7) . . ? N4 Ru1 S1 97.67(8) . . ? N1 Ru1 S1 87.08(7) . . ? N2 Ru1 S1 91.73(7) . . ? P1 Ru1 S1 87.63(3) . . ? C33 S1 C36 91.47(16) . . ? C33 S1 Ru1 113.46(12) . . ? C36 S1 Ru1 108.42(11) . . ? C37 S2 C40 91.91(15) . . ? C38 P1 C21 99.62(13) . . ? C38 P1 C27 101.55(13) . . ? C21 P1 C27 102.81(13) . . ? C38 P1 Ru1 116.39(10) . . ? C21 P1 Ru1 112.72(9) . . ? C27 P1 Ru1 120.83(10) . . ? F6 P2 F1 179.05(16) . . ? F6 P2 F3 89.14(14) . . ? F1 P2 F3 90.04(14) . . ? F6 P2 F5 90.50(14) . . ? F1 P2 F5 90.33(14) . . ? F3 P2 F5 179.63(14) . . ? F6 P2 F2 89.66(15) . . ? F1 P2 F2 89.86(15) . . ? F3 P2 F2 89.83(13) . . ? F5 P2 F2 90.24(13) . . ? F6 P2 F4 90.29(14) . . ? F1 P2 F4 90.18(14) . . ? F3 P2 F4 89.81(13) . . ? F5 P2 F4 90.13(13) . . ? F2 P2 F4 179.63(14) . . ? F7 P3 F9 96.9(3) . . ? F7 P3 F8 91.6(2) . . ? F9 P3 F8 89.71(19) . . ? F7 P3 F11 88.9(3) . . ? F9 P3 F11 174.2(3) . . ? F8 P3 F11 90.74(18) . . ? F7 P3 F10 89.7(2) . . ? F9 P3 F10 90.70(18) . . ? F8 P3 F10 178.6(2) . . ? F11 P3 F10 88.71(18) . . ? F7 P3 F12 176.0(3) . . ? F9 P3 F12 86.9(3) . . ? F8 P3 F12 89.6(3) . . ? F11 P3 F12 87.3(3) . . ? F10 P3 F12 89.0(2) . . ? C1 N1 C5 117.3(3) . . ? C1 N1 Ru1 127.4(2) . . ? C5 N1 Ru1 115.24(19) . . ? C10 N2 C6 118.9(3) . . ? C10 N2 Ru1 126.2(2) . . ? C6 N2 Ru1 114.89(19) . . ? C11 N3 C15 119.0(3) . . ? C11 N3 Ru1 124.5(2) . . ? C15 N3 Ru1 116.1(2) . . ? C20 N4 C16 118.3(3) . . ? C20 N4 Ru1 126.3(2) . . ? C16 N4 Ru1 115.3(2) . . ? N1 C1 C2 123.5(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 118.6(3) . . ? C3 C4 C5 120.2(3) . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 115.7(3) . . ? C4 C5 C6 123.1(3) . . ? N2 C6 C7 120.6(3) . . ? N2 C6 C5 115.9(3) . . ? C7 C6 C5 123.5(3) . . ? C8 C7 C6 120.2(3) . . ? C9 C8 C7 118.8(3) . . ? C8 C9 C10 118.9(3) . . ? N2 C10 C9 122.7(3) . . ? N3 C11 C12 122.4(3) . . ? C11 C12 C13 118.9(4) . . ? C14 C13 C12 119.4(4) . . ? C13 C14 C15 119.9(4) . . ? N3 C15 C14 120.4(3) . . ? N3 C15 C16 115.0(3) . . ? C14 C15 C16 124.6(3) . . ? N4 C16 C17 121.6(3) . . ? N4 C16 C15 115.1(3) . . ? C17 C16 C15 123.2(3) . . ? C18 C17 C16 118.9(4) . . ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 118.9(4) . . ? N4 C20 C19 122.5(3) . . ? C22 C21 C26 118.6(3) . . ? C22 C21 P1 120.4(2) . . ? C26 C21 P1 121.0(2) . . ? C23 C22 C21 120.8(3) . . ? C22 C23 C24 119.5(3) . . ? C25 C24 C23 120.2(3) . . ? C26 C25 C24 120.2(3) . . ? C25 C26 C21 120.6(3) . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P1 119.7(2) . . ? C32 C27 P1 122.0(2) . . ? C29 C28 C27 120.7(3) . . ? C30 C29 C28 120.4(3) . . ? C29 C30 C31 119.3(3) . . ? C30 C31 C32 120.7(3) . . ? C31 C32 C27 120.6(3) . . ? C34 C33 S1 111.1(3) . . ? C33 C34 C35 113.7(3) . . ? C36 C35 C34 113.2(3) . . ? C35 C36 C37 129.1(3) . . ? C35 C36 S1 110.4(3) . . ? C37 C36 S1 120.6(2) . . ? C38 C37 C36 129.2(3) . . ? C38 C37 S2 111.8(2) . . ? C36 C37 S2 119.0(2) . . ? C37 C38 C39 111.7(3) . . ? C37 C38 P1 126.0(2) . . ? C39 C38 P1 122.2(2) . . ? C40 C39 C38 113.5(3) . . ? C39 C40 C41 127.6(3) . . ? C39 C40 S2 111.0(2) . . ? C41 C40 S2 121.4(2) . . ? C41 S3 C44 91.8(3) . . ? C42B C41 C40 124.8(6) . . ? C42B C41 C42 113.4(6) . . ? C40 C41 C42 121.7(4) . . ? C42B C41 S3 3.9(8) . . ? C40 C41 S3 123.2(3) . . ? C42 C41 S3 115.1(4) . . ? C43 C42 C41 103.1(5) . . ? C44 C43 C42 117.2(5) . . ? C43 C44 S3 112.7(4) . . ? O1 C46 C47 121.2(5) . . ? O1 C46 C45 121.8(5) . . ? C47 C46 C45 117.0(5) . . ? C41 C42B C43B 120.5(9) . . ? C44B C43B C42B 102.2(8) . . ? C43B C44B S3B 113.7(6) . . ? 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 N3 Ru1 S1 C33 -76.8(8) . . . . ? N4 Ru1 S1 C33 -117.75(15) . . . . ? N1 Ru1 S1 C33 52.88(15) . . . . ? N2 Ru1 S1 C33 -25.28(15) . . . . ? P1 Ru1 S1 C33 153.14(13) . . . . ? N3 Ru1 S1 C36 -176.8(8) . . . . ? N4 Ru1 S1 C36 142.23(13) . . . . ? N1 Ru1 S1 C36 -47.14(13) . . . . ? N2 Ru1 S1 C36 -125.30(13) . . . . ? P1 Ru1 S1 C36 53.12(12) . . . . ? N3 Ru1 P1 C38 150.33(12) . . . . ? N4 Ru1 P1 C38 -131.48(13) . . . . ? N1 Ru1 P1 C38 52.82(13) . . . . ? N2 Ru1 P1 C38 34(2) . . . . ? S1 Ru1 P1 C38 -33.79(10) . . . . ? N3 Ru1 P1 C21 -95.47(13) . . . . ? N4 Ru1 P1 C21 -17.28(13) . . . . ? N1 Ru1 P1 C21 167.02(13) . . . . ? N2 Ru1 P1 C21 148(2) . . . . ? S1 Ru1 P1 C21 80.41(11) . . . . ? N3 Ru1 P1 C27 26.52(13) . . . . ? N4 Ru1 P1 C27 104.71(13) . . . . ? N1 Ru1 P1 C27 -70.99(13) . . . . ? N2 Ru1 P1 C27 -90(2) . . . . ? S1 Ru1 P1 C27 -157.60(11) . . . . ? N3 Ru1 N1 C1 -99.3(3) . . . . ? N4 Ru1 N1 C1 -157.8(5) . . . . ? N2 Ru1 N1 C1 177.2(3) . . . . ? P1 Ru1 N1 C1 -2.2(3) . . . . ? S1 Ru1 N1 C1 84.9(3) . . . . ? N3 Ru1 N1 C5 82.2(2) . . . . ? N4 Ru1 N1 C5 23.7(7) . . . . ? N2 Ru1 N1 C5 -1.3(2) . . . . ? P1 Ru1 N1 C5 179.3(2) . . . . ? S1 Ru1 N1 C5 -93.6(2) . . . . ? N3 Ru1 N2 C10 82.4(3) . . . . ? N4 Ru1 N2 C10 4.3(3) . . . . ? N1 Ru1 N2 C10 180.0(3) . . . . ? P1 Ru1 N2 C10 -161(2) . . . . ? S1 Ru1 N2 C10 -93.4(3) . . . . ? N3 Ru1 N2 C6 -96.0(2) . . . . ? N4 Ru1 N2 C6 -174.0(2) . . . . ? N1 Ru1 N2 C6 1.6(2) . . . . ? P1 Ru1 N2 C6 20(3) . . . . ? S1 Ru1 N2 C6 88.2(2) . . . . ? N4 Ru1 N3 C11 175.8(3) . . . . ? N1 Ru1 N3 C11 4.9(3) . . . . ? N2 Ru1 N3 C11 82.4(2) . . . . ? P1 Ru1 N3 C11 -96.0(2) . . . . ? S1 Ru1 N3 C11 134.2(7) . . . . ? N4 Ru1 N3 C15 3.3(2) . . . . ? N1 Ru1 N3 C15 -167.6(2) . . . . ? N2 Ru1 N3 C15 -90.1(2) . . . . ? P1 Ru1 N3 C15 91.5(2) . . . . ? S1 Ru1 N3 C15 -38.3(9) . . . . ? N3 Ru1 N4 C20 -179.6(3) . . . . ? N1 Ru1 N4 C20 -119.7(6) . . . . ? N2 Ru1 N4 C20 -95.3(3) . . . . ? P1 Ru1 N4 C20 84.3(2) . . . . ? S1 Ru1 N4 C20 -3.2(3) . . . . ? N3 Ru1 N4 C16 -2.1(2) . . . . ? N1 Ru1 N4 C16 57.8(6) . . . . ? N2 Ru1 N4 C16 82.2(2) . . . . ? P1 Ru1 N4 C16 -98.2(2) . . . . ? S1 Ru1 N4 C16 174.3(2) . . . . ? C5 N1 C1 C2 -1.4(5) . . . . ? Ru1 N1 C1 C2 -179.8(2) . . . . ? N1 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 2.1(5) . . . . ? C2 C3 C4 C5 -1.5(6) . . . . ? C1 N1 C5 C4 2.0(5) . . . . ? Ru1 N1 C5 C4 -179.3(3) . . . . ? C1 N1 C5 C6 -177.9(3) . . . . ? Ru1 N1 C5 C6 0.8(4) . . . . ? C3 C4 C5 N1 -0.7(5) . . . . ? C3 C4 C5 C6 179.2(3) . . . . ? C10 N2 C6 C7 -0.1(5) . . . . ? Ru1 N2 C6 C7 178.4(3) . . . . ? C10 N2 C6 C5 179.8(3) . . . . ? Ru1 N2 C6 C5 -1.7(4) . . . . ? N1 C5 C6 N2 0.6(4) . . . . ? C4 C5 C6 N2 -179.3(3) . . . . ? N1 C5 C6 C7 -179.5(3) . . . . ? C4 C5 C6 C7 0.6(6) . . . . ? N2 C6 C7 C8 -0.1(6) . . . . ? C5 C6 C7 C8 -180.0(4) . . . . ? C6 C7 C8 C9 0.0(6) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C6 N2 C10 C9 0.4(5) . . . . ? Ru1 N2 C10 C9 -177.9(3) . . . . ? C8 C9 C10 N2 -0.5(6) . . . . ? C15 N3 C11 C12 -1.0(5) . . . . ? Ru1 N3 C11 C12 -173.3(2) . . . . ? N3 C11 C12 C13 0.1(5) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C11 N3 C15 C14 1.2(4) . . . . ? Ru1 N3 C15 C14 174.1(2) . . . . ? C11 N3 C15 C16 -176.7(3) . . . . ? Ru1 N3 C15 C16 -3.8(3) . . . . ? C13 C14 C15 N3 -0.5(5) . . . . ? C13 C14 C15 C16 177.2(3) . . . . ? C20 N4 C16 C17 0.0(4) . . . . ? Ru1 N4 C16 C17 -177.7(2) . . . . ? C20 N4 C16 C15 178.5(3) . . . . ? Ru1 N4 C16 C15 0.8(3) . . . . ? N3 C15 C16 N4 1.9(4) . . . . ? C14 C15 C16 N4 -175.9(3) . . . . ? N3 C15 C16 C17 -179.5(3) . . . . ? C14 C15 C16 C17 2.7(5) . . . . ? N4 C16 C17 C18 1.4(5) . . . . ? C15 C16 C17 C18 -177.0(3) . . . . ? C16 C17 C18 C19 -1.8(6) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C16 N4 C20 C19 -1.0(5) . . . . ? Ru1 N4 C20 C19 176.4(2) . . . . ? C18 C19 C20 N4 0.6(5) . . . . ? C38 P1 C21 C22 32.9(3) . . . . ? C27 P1 C21 C22 137.2(2) . . . . ? Ru1 P1 C21 C22 -91.1(2) . . . . ? C38 P1 C21 C26 -149.7(2) . . . . ? C27 P1 C21 C26 -45.4(3) . . . . ? Ru1 P1 C21 C26 86.3(2) . . . . ? C26 C21 C22 C23 1.4(4) . . . . ? P1 C21 C22 C23 178.9(2) . . . . ? C21 C22 C23 C24 0.9(5) . . . . ? C22 C23 C24 C25 -1.5(5) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C24 C25 C26 C21 2.6(5) . . . . ? C22 C21 C26 C25 -3.2(4) . . . . ? P1 C21 C26 C25 179.4(2) . . . . ? C38 P1 C27 C28 -96.5(3) . . . . ? C21 P1 C27 C28 160.7(2) . . . . ? Ru1 P1 C27 C28 34.0(3) . . . . ? C38 P1 C27 C32 79.1(3) . . . . ? C21 P1 C27 C32 -23.6(3) . . . . ? Ru1 P1 C27 C32 -150.3(2) . . . . ? C32 C27 C28 C29 0.5(4) . . . . ? P1 C27 C28 C29 176.3(2) . . . . ? C27 C28 C29 C30 0.2(5) . . . . ? C28 C29 C30 C31 -0.7(5) . . . . ? C29 C30 C31 C32 0.3(5) . . . . ? C30 C31 C32 C27 0.4(5) . . . . ? C28 C27 C32 C31 -0.8(4) . . . . ? P1 C27 C32 C31 -176.6(2) . . . . ? C36 S1 C33 C34 -2.6(3) . . . . ? Ru1 S1 C33 C34 -113.5(3) . . . . ? S1 C33 C34 C35 1.6(4) . . . . ? C33 C34 C35 C36 0.8(5) . . . . ? C34 C35 C36 C37 178.4(3) . . . . ? C34 C35 C36 S1 -2.7(4) . . . . ? C33 S1 C36 C35 3.0(3) . . . . ? Ru1 S1 C36 C35 118.4(2) . . . . ? C33 S1 C36 C37 -177.9(3) . . . . ? Ru1 S1 C36 C37 -62.6(3) . . . . ? C35 C36 C37 C38 -148.2(4) . . . . ? S1 C36 C37 C38 33.0(4) . . . . ? C35 C36 C37 S2 31.8(5) . . . . ? S1 C36 C37 S2 -147.02(19) . . . . ? C40 S2 C37 C38 1.2(2) . . . . ? C40 S2 C37 C36 -178.8(2) . . . . ? C36 C37 C38 C39 178.9(3) . . . . ? S2 C37 C38 C39 -1.1(3) . . . . ? C36 C37 C38 P1 -4.2(5) . . . . ? S2 C37 C38 P1 175.75(16) . . . . ? C21 P1 C38 C37 -108.2(3) . . . . ? C27 P1 C38 C37 146.5(3) . . . . ? Ru1 P1 C38 C37 13.2(3) . . . . ? C21 P1 C38 C39 68.4(3) . . . . ? C27 P1 C38 C39 -37.0(3) . . . . ? Ru1 P1 C38 C39 -170.2(2) . . . . ? C37 C38 C39 C40 0.4(4) . . . . ? P1 C38 C39 C40 -176.6(2) . . . . ? C38 C39 C40 C41 178.8(3) . . . . ? C38 C39 C40 S2 0.6(3) . . . . ? C37 S2 C40 C39 -1.0(2) . . . . ? C37 S2 C40 C41 -179.4(3) . . . . ? C39 C40 C41 C42B -36.5(10) . . . . ? S2 C40 C41 C42B 141.7(9) . . . . ? C39 C40 C41 C42 147.2(4) . . . . ? S2 C40 C41 C42 -34.7(5) . . . . ? C39 C40 C41 S3 -32.2(5) . . . . ? S2 C40 C41 S3 146.0(2) . . . . ? C44 S3 C41 C42B -66(8) . . . . ? C44 S3 C41 C40 178.5(3) . . . . ? C44 S3 C41 C42 -0.9(4) . . . . ? C42B C41 C42 C43 3.2(9) . . . . ? C40 C41 C42 C43 179.9(4) . . . . ? S3 C41 C42 C43 -0.7(5) . . . . ? C41 C42 C43 C44 2.6(7) . . . . ? C42 C43 C44 S3 -3.5(7) . . . . ? C41 S3 C44 C43 2.5(5) . . . . ? C40 C41 C42B C43B 176.0(8) . . . . ? C42 C41 C42B C43B -7.4(15) . . . . ? S3 C41 C42B C43B 109(9) . . . . ? C41 C42B C43B C44B 2.0(15) . . . . ? C42B C43B C44B S3B -1.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 0.894 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.092