#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2016-11-25 at 15:55:35 # Using CIFtbx version 3.0.4 1 Sep 2006 # Dictionary name : cif_core.dic # Dictionary vers : 2.4.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelx #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global loop_ _publ_author_name _publ_author_address 'Henri Brunner' ; Institut f\"ur Anorganische Chemie Universit\"at Regensburg D-93040 Regensburg Germany ; 'Takashi Tsuno' ; Department of Applied Molecular Chemistry College of Industrial Technology Nihon University Chiba 275-8575 Japan ; 'Haruka Iwabe' ; Department of Applied Molecular Chemistry College of Industrial Technology Nihon University Chiba 275-8575 Japan ; _publ_requested_journal 'ACS Omega' #\#CIF_1.1 #============================================================================== # publcif _publ_body_element loop start loop_ _publ_body_element _publ_body_title _publ_body_contents section ? ? # publcif _publ_body_element loop end #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Nov 17 14:35:32 2016' _audit_creation_method 'WinGX routine CIF_UPDATE orPLATON option' _audit_update_record ; ? 2016-11-17 # Formatted by publCIF ; #=============================================================================== # 1. SUBMISSION DETAILS #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; PPh3 Propeller Diastereomers. The Bonding Motif PhPPh3 Face-on \p-Ar in Half-Sandwich Compounds [ArLL'MPPh3] ; _publ_section_title_footnote . # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. #=============================================================================== # 4. TEXT _publ_section_synopsis . _publ_section_abstract ; (type here to add abstract) ; # Insert blank lines between paragraphs _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep ; (type here to add preparation details) ; _publ_section_exptl_refinement ; The data were collected at 123 K using an Oxford Diffraction Cryojet Cooler or at 173 K using a Rigaku RAXIS-RAPID. The structure was solved by direct methods (SIR-2004, or SIR-97 and refined byfull-matrix anisotropic least squares (SHELXL97). The H-atoms werecalculated geometrically and a riding model was used during refinement process. ; # Insert blank lines between references _publ_section_references ; Burla, M. C.; Caliandro, R.; Camalli, M.; Carrozzini, B.; Cascarano, G. L.; De Caro, L.; Giacovazzo, C.; Polidoria, G. & Spagnac R. (2005) J. Appl. Cryst., 38, 381--388 Altomare, A. Burla, M. C. Camalli, M. Cascarano, G. L. Giacovazzo, C. Guagliardi, A. Moliterni, A. G. G. Polidori, G. & Spagna, R. (1999), J.Appl. Cryst. 32, 115--119. Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105--107. Flack, H. D. (1983). Acta Cryst. A39, 876--881. L. J. Farrugia, (1997), J. Appl. Cryst. 30, 565. Scheldlink, G. M. (2008), Acta Cryst. Sect. A64, 112--122. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sheldrick, G.M. SHELXS97. Program for Crystal Structure solution. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194--201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7--13. Wilson, A. J. C. (1992). International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ? _publ_section_figure_captions ; View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. ; # start Validation Reply Form # ALERT LEVEL B _vrf_PLAT094_1519530 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.43 RESPONSE: This alert are generated because there is disorder in the structure. ; _vrf_PLAT220_1519530 ; PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 9.4 Ratio RESPONSE: This alert are generated because there is disorder in the structure. ; _vrf_PLAT242_1519530 ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C7 Check RESPONSE: This alert are generated because there is disorder in the structure. ; _vrf_PLAT990_1519531 ; PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE job ... ! Note RESPONSE: This was corrected with the SQUEEZE program. ; # end Validation Reply Form #=============================================================================== data_1519530 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C29 H30 Cl N O Ru' _chemical_formula_sum 'C29 H30 Cl N O Ru' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 545.06 _chemical_absolute_configuration rm #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.044(3) _cell_length_b 13.524(3) _cell_length_c 20.436(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2499.6(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 22815 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 _cell_measurement_temperature 173(2) #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ? _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _shelx_estimated_absorpt_T_min 0.773 _shelx_estimated_absorpt_T_max 0.822 _exptl_absorpt_correction_T_min 0.7317 _exptl_absorpt_correction_T_max 1.0000 _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 173(2) _diffrn_radiation_type MoK\a _diffrn_source 'sealed x-ray tube' _diffrn_detector 'curved image-plate' _diffrn_detector_area_resol_mean 10 _diffrn_measurement_device 'quarter \C-circle diffractometer' _diffrn_measurement_device_type 'Rigaku R-Axis Rapid' _diffrn_measurement_method 'phi or omega oscillation scans' _diffrn_orient_matrix_type fs_process _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_unetI/netI 0.029 _diffrn_reflns_number 19688 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.008 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_full 24.997 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_coverage 0.753 _reflns_number_total 4388 _reflns_number_gt 4289 _reflns_threshold_expression 'I > 2\s(I)' _computing_structure_solution 'SIR97 (Altomare et al, 1999)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+2.8687P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4388 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details ; Flack x determined using 1814 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.004(14) _refine_diff_density_max 2.3 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.088 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 1.03712(4) 0.82767(3) 0.72676(2) 0.01694(13) Uani 1 1 d . . . . . Cl1 Cl 0.94810(17) 0.93221(10) 0.81491(7) 0.0313(3) Uani 1 1 d . . . . . C12 C 0.7318(6) 0.9048(4) 0.6420(3) 0.0219(11) Uani 1 1 d . . . . . O1 O 0.9814(5) 0.9450(3) 0.66699(19) 0.0283(9) Uani 1 1 d . . . . . C5 C 1.1456(6) 0.6932(4) 0.7648(3) 0.0261(13) Uani 1 1 d . . . . . H5 H 1.11131 0.64187 0.792662 0.031 Uiso 1 1 calc R U . . . N1 N 0.8181(5) 0.7776(3) 0.7183(2) 0.0188(9) Uani 1 1 d . . . . . C29 C 0.5233(6) 0.5952(4) 0.7487(3) 0.0267(12) Uani 1 1 d . . . . . H29 H 0.499184 0.617131 0.791559 0.032 Uiso 1 1 calc R U . . . C24 C 0.6569(6) 0.6245(4) 0.7206(3) 0.0221(11) Uani 1 1 d . . . . . C20 C 0.8703(6) 1.0317(4) 0.5807(3) 0.0232(11) Uani 1 1 d . . . . . C4 C 1.2174(6) 0.7764(4) 0.7917(3) 0.0235(12) Uani 1 1 d . . . . . C3 C 1.2725(6) 0.8508(4) 0.7490(3) 0.0241(12) Uani 1 1 d . . . . . H3 H 1.323246 0.906449 0.766345 0.029 Uiso 1 1 calc R U . . . C21 C 0.7167(6) 0.8209(4) 0.6844(2) 0.0218(11) Uani 1 1 d . . . . . H21 H 0.620108 0.793814 0.687985 0.026 Uiso 1 1 calc R U . . . C1 C 1.1769(7) 0.7587(4) 0.6526(3) 0.0280(13) Uani 1 1 d . . . . . C16 C 0.7564(9) 1.1233(5) 0.4919(3) 0.0385(16) Uani 1 1 d . . . . . H16 H 0.673294 1.137945 0.465208 0.046 Uiso 1 1 calc R U . . . C15 C 0.7422(8) 1.0526(4) 0.5434(3) 0.0308(14) Uani 1 1 d . . . . . C2 C 1.2515(6) 0.8418(4) 0.6806(3) 0.0254(12) Uani 1 1 d . . . . . H2 H 1.287967 0.892288 0.652565 0.03 Uiso 1 1 calc R U . . . C26 C 0.5896(8) 0.5326(5) 0.6240(3) 0.0398(16) Uani 1 1 d . . . . . H26 H 0.612157 0.511121 0.58088 0.048 Uiso 1 1 calc R U . . . C19 C 1.0032(7) 1.0791(4) 0.5670(3) 0.0302(14) Uani 1 1 d . . . . . H19 H 1.088719 1.063558 0.591968 0.036 Uiso 1 1 calc R U . . . C10 C 1.2322(7) 0.7868(5) 0.8641(3) 0.0352(14) Uani 1 1 d . . . . . H10A H 1.284454 0.848432 0.874241 0.053 Uiso 1 1 calc R U . . . H10B H 1.133667 0.788302 0.884054 0.053 Uiso 1 1 calc R U . . . H10C H 1.288081 0.730634 0.881516 0.053 Uiso 1 1 calc R U . . . C6 C 1.1247(6) 0.6862(4) 0.6959(3) 0.0261(12) Uani 1 1 d . . . . . H6 H 1.073689 0.630602 0.678748 0.031 Uiso 1 1 calc R U . . . C23 C 0.7232(8) 0.7201(5) 0.8251(3) 0.0398(16) Uani 1 1 d . . . . . H23A H 0.692764 0.66204 0.85041 0.06 Uiso 1 1 calc R U . . . H23B H 0.80591 0.752897 0.847221 0.06 Uiso 1 1 calc R U . . . H23C H 0.63998 0.766178 0.82147 0.06 Uiso 1 1 calc R U . . . C27 C 0.4558(8) 0.5043(4) 0.6531(3) 0.0392(15) Uani 1 1 d . . . . . H27 H 0.387054 0.464413 0.629866 0.047 Uiso 1 1 calc R U . . . C22 C 0.7720(6) 0.6874(4) 0.7562(3) 0.0240(12) Uani 1 1 d . . . . . H22 H 0.86213 0.645418 0.761689 0.029 Uiso 1 1 calc R U . . . C11 C 0.8635(6) 0.9571(4) 0.6330(3) 0.0201(11) Uani 1 1 d . . . . . C13 C 0.6052(7) 0.9301(5) 0.6033(3) 0.0330(14) Uani 1 1 d . . . . . H13 H 0.515366 0.895316 0.610349 0.04 Uiso 1 1 calc R U . . . C14 C 0.6086(8) 1.0017(5) 0.5569(3) 0.0379(15) Uani 1 1 d . . . . . H14 H 0.521275 1.017851 0.533338 0.045 Uiso 1 1 calc R U . . . C25 C 0.6882(7) 0.5912(5) 0.6572(3) 0.0316(14) Uani 1 1 d . . . . . H25 H 0.778793 0.609338 0.636904 0.038 Uiso 1 1 calc R U . . . C17 C 0.8865(9) 1.1698(5) 0.4806(3) 0.0399(15) Uani 1 1 d . . . . . H17 H 0.89222 1.217877 0.446796 0.048 Uiso 1 1 calc R U . . . C18 C 1.0123(8) 1.1488(5) 0.5175(3) 0.0380(16) Uani 1 1 d . . . . . H18 H 1.102957 1.181751 0.508821 0.046 Uiso 1 1 calc R U . . . C7 C 1.1592(8) 0.7475(6) 0.5780(3) 0.0452(17) Uani 1 1 d . . . . . H7 H 1.166492 0.8144 0.557387 0.054 Uiso 1 1 calc R U . . . C28 C 0.4256(6) 0.5349(4) 0.7156(3) 0.0321(14) Uani 1 1 d . . . . . H28 H 0.336596 0.514522 0.736286 0.038 Uiso 1 1 calc R U . . . C9 C 1.030(2) 0.7049(18) 0.5594(8) 0.187(11) Uani 1 1 d . . . . . H9A H 0.946823 0.744522 0.57562 0.28 Uiso 1 1 calc R U . . . H9B H 1.025634 0.701513 0.511541 0.28 Uiso 1 1 calc R U . . . H9C H 1.023808 0.638016 0.577619 0.28 Uiso 1 1 calc R U . . . C8 C 1.2788(16) 0.6848(13) 0.5523(5) 0.130(7) Uani 1 1 d . . . . . H8A H 1.374682 0.712951 0.564649 0.195 Uiso 1 1 calc R U . . . H8B H 1.269822 0.618048 0.570547 0.195 Uiso 1 1 calc R U . . . H8C H 1.271648 0.681544 0.504469 0.195 Uiso 1 1 calc R U . . . 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 0.0153(2) 0.0126(2) 0.0230(2) 0.00132(17) -0.00156(17) -0.00091(16) Cl1 0.0281(7) 0.0233(6) 0.0426(8) -0.0128(6) -0.0011(7) 0.0051(6) C12 0.020(3) 0.022(3) 0.025(3) 0.005(2) 0.002(2) 0.003(2) O1 0.024(2) 0.0226(18) 0.038(2) 0.0119(17) -0.0077(18) -0.0059(17) C5 0.018(3) 0.019(3) 0.041(3) 0.004(3) 0.001(2) 0.004(2) N1 0.019(2) 0.017(2) 0.020(2) -0.0015(19) 0.0000(18) -0.0016(17) C29 0.023(3) 0.019(3) 0.038(3) 0.003(2) 0.003(3) -0.001(2) C24 0.019(3) 0.018(2) 0.030(3) 0.005(2) -0.001(2) 0.000(2) C20 0.029(3) 0.019(3) 0.022(2) -0.002(2) 0.002(2) 0.002(2) C4 0.016(3) 0.026(3) 0.029(3) 0.002(2) -0.003(2) 0.005(2) C3 0.015(2) 0.021(3) 0.037(3) 0.004(2) -0.001(2) -0.001(2) C21 0.018(3) 0.023(3) 0.024(3) 0.001(3) 0.001(2) -0.004(2) C1 0.026(3) 0.028(3) 0.030(3) -0.008(3) 0.002(2) 0.008(2) C16 0.061(5) 0.031(3) 0.024(3) 0.002(3) -0.011(3) 0.007(3) C15 0.044(4) 0.024(3) 0.025(3) 0.000(2) -0.004(3) 0.005(3) C2 0.018(3) 0.025(3) 0.033(3) 0.005(3) 0.007(2) -0.001(2) C26 0.055(4) 0.032(3) 0.033(3) -0.004(3) -0.011(3) -0.002(3) C19 0.036(4) 0.023(3) 0.032(3) 0.003(2) 0.003(2) 0.002(2) C10 0.033(3) 0.041(3) 0.032(3) 0.011(3) -0.011(3) -0.002(3) C6 0.022(3) 0.020(3) 0.036(3) -0.003(2) -0.002(2) 0.004(2) C23 0.054(4) 0.042(4) 0.023(3) 0.001(3) 0.000(3) -0.020(3) C27 0.038(4) 0.025(3) 0.054(4) 0.001(3) -0.020(3) -0.004(3) C22 0.022(3) 0.019(3) 0.031(3) 0.004(2) 0.000(2) -0.004(2) C11 0.021(3) 0.015(2) 0.024(2) -0.001(2) -0.001(2) 0.004(2) C13 0.018(3) 0.035(3) 0.045(4) 0.002(3) -0.008(3) 0.001(3) C14 0.031(3) 0.041(4) 0.042(3) 0.009(3) -0.016(3) 0.007(3) C25 0.029(3) 0.031(3) 0.035(3) -0.002(3) 0.004(3) -0.003(3) C17 0.071(5) 0.028(3) 0.021(3) 0.005(3) 0.003(3) 0.000(4) C18 0.048(4) 0.033(3) 0.032(3) 0.008(3) 0.012(3) -0.005(3) C7 0.046(4) 0.062(5) 0.028(3) -0.003(3) 0.000(3) 0.002(4) C28 0.017(3) 0.022(3) 0.057(4) 0.007(3) -0.005(3) -0.002(2) C9 0.107(12) 0.34(3) 0.117(12) -0.099(16) 0.004(10) -0.025(19) C8 0.118(11) 0.215(18) 0.056(6) -0.053(9) -0.015(6) 0.084(12) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 O1 2.065(4) . ? Ru1 N1 2.100(4) . ? Ru1 C6 2.164(6) . ? Ru1 C2 2.165(5) . ? Ru1 C1 2.183(6) . ? Ru1 C3 2.199(5) . ? Ru1 C5 2.208(5) . ? Ru1 C4 2.213(5) . ? Ru1 Cl1 2.4274(14) . ? C12 C11 1.398(8) . ? C12 C13 1.433(8) . ? C12 C21 1.435(8) . ? O1 C11 1.283(7) . ? C5 C4 1.410(8) . ? C5 C6 1.423(8) . ? C5 H5 0.95 . ? N1 C21 1.290(7) . ? N1 C22 1.503(7) . ? C29 C28 1.380(8) . ? C29 C24 1.395(8) . ? C29 H29 0.95 . ? C24 C25 1.402(9) . ? C24 C22 1.528(8) . ? C20 C19 1.390(8) . ? C20 C15 1.415(8) . ? C20 C11 1.472(7) . ? C4 C3 1.421(8) . ? C4 C10 1.493(8) . ? C3 C2 1.416(9) . ? C3 H3 0.95 . ? C21 H21 0.95 . ? C1 C6 1.403(9) . ? C1 C2 1.430(9) . ? C1 C7 1.539(9) . ? C16 C17 1.355(11) . ? C16 C15 1.427(9) . ? C16 H16 0.95 . ? C15 C14 1.417(10) . ? C2 H2 0.95 . ? C26 C25 1.372(9) . ? C26 C27 1.402(11) . ? C26 H26 0.95 . ? C19 C18 1.385(8) . ? C19 H19 0.95 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C6 H6 0.95 . ? C23 C22 1.541(9) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C27 C28 1.370(10) . ? C27 H27 0.95 . ? C22 H22 1 . ? C13 C14 1.355(9) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C25 H25 0.95 . ? C17 C18 1.394(10) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C7 C9 1.359(19) . ? C7 C8 1.473(14) . ? C7 H7 1 . ? C28 H28 0.95 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? 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 O1 Ru1 N1 88.23(16) . . ? O1 Ru1 C6 126.62(19) . . ? N1 Ru1 C6 92.1(2) . . ? O1 Ru1 C2 83.8(2) . . ? N1 Ru1 C2 146.9(2) . . ? C6 Ru1 C2 67.9(2) . . ? O1 Ru1 C1 93.4(2) . . ? N1 Ru1 C1 110.6(2) . . ? C6 Ru1 C1 37.7(2) . . ? C2 Ru1 C1 38.4(2) . . ? O1 Ru1 C3 104.42(18) . . ? N1 Ru1 C3 167.34(18) . . ? C6 Ru1 C3 80.3(2) . . ? C2 Ru1 C3 37.9(2) . . ? C1 Ru1 C3 69.1(2) . . ? O1 Ru1 C5 161.8(2) . . ? N1 Ru1 C5 100.52(19) . . ? C6 Ru1 C5 38.0(2) . . ? C2 Ru1 C5 80.1(2) . . ? C1 Ru1 C5 68.6(2) . . ? C3 Ru1 C5 67.3(2) . . ? O1 Ru1 C4 140.80(19) . . ? N1 Ru1 C4 130.0(2) . . ? C6 Ru1 C4 68.2(2) . . ? C2 Ru1 C4 68.2(2) . . ? C1 Ru1 C4 81.7(2) . . ? C3 Ru1 C4 37.6(2) . . ? C5 Ru1 C4 37.2(2) . . ? O1 Ru1 Cl1 84.86(12) . . ? N1 Ru1 Cl1 86.32(12) . . ? C6 Ru1 Cl1 148.45(16) . . ? C2 Ru1 Cl1 124.68(17) . . ? C1 Ru1 Cl1 162.97(17) . . ? C3 Ru1 Cl1 94.86(16) . . ? C5 Ru1 Cl1 111.46(17) . . ? C4 Ru1 Cl1 88.96(15) . . ? C11 C12 C13 119.2(5) . . ? C11 C12 C21 124.1(5) . . ? C13 C12 C21 116.5(5) . . ? C11 O1 Ru1 128.4(3) . . ? C4 C5 C6 119.9(6) . . ? C4 C5 Ru1 71.6(3) . . ? C6 C5 Ru1 69.3(3) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? Ru1 C5 H5 131.9 . . ? C21 N1 C22 116.6(4) . . ? C21 N1 Ru1 124.6(4) . . ? C22 N1 Ru1 118.8(3) . . ? C28 C29 C24 121.4(6) . . ? C28 C29 H29 119.3 . . ? C24 C29 H29 119.3 . . ? C29 C24 C25 117.7(5) . . ? C29 C24 C22 123.6(5) . . ? C25 C24 C22 118.7(5) . . ? C19 C20 C15 120.5(5) . . ? C19 C20 C11 119.9(5) . . ? C15 C20 C11 119.6(5) . . ? C5 C4 C3 119.2(5) . . ? C5 C4 C10 120.2(5) . . ? C3 C4 C10 120.7(5) . . ? C5 C4 Ru1 71.2(3) . . ? C3 C4 Ru1 70.7(3) . . ? C10 C4 Ru1 129.1(4) . . ? C2 C3 C4 119.9(5) . . ? C2 C3 Ru1 69.8(3) . . ? C4 C3 Ru1 71.7(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? Ru1 C3 H3 131.1 . . ? N1 C21 C12 128.0(5) . . ? N1 C21 H21 116 . . ? C12 C21 H21 116 . . ? C6 C1 C2 117.1(5) . . ? C6 C1 C7 121.4(6) . . ? C2 C1 C7 121.5(6) . . ? C6 C1 Ru1 70.4(3) . . ? C2 C1 Ru1 70.1(3) . . ? C7 C1 Ru1 132.0(5) . . ? C17 C16 C15 121.0(7) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C20 C15 C14 119.8(5) . . ? C20 C15 C16 117.2(6) . . ? C14 C15 C16 123.0(6) . . ? C3 C2 C1 121.7(5) . . ? C3 C2 Ru1 72.4(3) . . ? C1 C2 Ru1 71.5(3) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? Ru1 C2 H2 129.6 . . ? C25 C26 C27 120.6(6) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C18 C19 C20 120.8(6) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 C6 C5 122.2(6) . . ? C1 C6 Ru1 71.9(3) . . ? C5 C6 Ru1 72.7(3) . . ? C1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? Ru1 C6 H6 129 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C27 C26 119.0(6) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? N1 C22 C24 113.3(4) . . ? N1 C22 C23 108.5(5) . . ? C24 C22 C23 113.5(5) . . ? N1 C22 H22 107 . . ? C24 C22 H22 107 . . ? C23 C22 H22 107 . . ? O1 C11 C12 125.0(5) . . ? O1 C11 C20 116.5(5) . . ? C12 C11 C20 118.5(5) . . ? C14 C13 C12 122.6(6) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C26 C25 C24 120.7(6) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C16 C17 C18 121.4(6) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 119.0(6) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C9 C7 C8 106.7(11) . . ? C9 C7 C1 114.1(9) . . ? C8 C7 C1 109.5(7) . . ? C9 C7 H7 108.8 . . ? C8 C7 H7 108.8 . . ? C1 C7 H7 108.8 . . ? C27 C28 C29 120.5(6) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 C28 C29 C24 C25 0.4(8) . . . . ? C28 C29 C24 C22 -177.3(5) . . . . ? C6 C5 C4 C3 -2.2(8) . . . . ? Ru1 C5 C4 C3 -53.8(4) . . . . ? C6 C5 C4 C10 176.6(5) . . . . ? Ru1 C5 C4 C10 124.9(5) . . . . ? C6 C5 C4 Ru1 51.6(5) . . . . ? C5 C4 C3 C2 1.6(8) . . . . ? C10 C4 C3 C2 -177.1(6) . . . . ? Ru1 C4 C3 C2 -52.5(5) . . . . ? C5 C4 C3 Ru1 54.1(4) . . . . ? C10 C4 C3 Ru1 -124.7(5) . . . . ? C22 N1 C21 C12 -177.0(5) . . . . ? Ru1 N1 C21 C12 5.5(8) . . . . ? C11 C12 C21 N1 -3.1(9) . . . . ? C13 C12 C21 N1 171.9(6) . . . . ? C19 C20 C15 C14 178.4(6) . . . . ? C11 C20 C15 C14 0.0(8) . . . . ? C19 C20 C15 C16 0.3(8) . . . . ? C11 C20 C15 C16 -178.1(5) . . . . ? C17 C16 C15 C20 -1.6(9) . . . . ? C17 C16 C15 C14 -179.6(6) . . . . ? C4 C3 C2 C1 -0.6(9) . . . . ? Ru1 C3 C2 C1 -54.0(5) . . . . ? C4 C3 C2 Ru1 53.4(5) . . . . ? C6 C1 C2 C3 0.2(9) . . . . ? C7 C1 C2 C3 -177.8(6) . . . . ? Ru1 C1 C2 C3 54.4(5) . . . . ? C6 C1 C2 Ru1 -54.2(5) . . . . ? C7 C1 C2 Ru1 127.8(6) . . . . ? C15 C20 C19 C18 1.0(9) . . . . ? C11 C20 C19 C18 179.4(5) . . . . ? C2 C1 C6 C5 -0.7(8) . . . . ? C7 C1 C6 C5 177.3(6) . . . . ? Ru1 C1 C6 C5 -54.8(5) . . . . ? C2 C1 C6 Ru1 54.1(5) . . . . ? C7 C1 C6 Ru1 -127.9(6) . . . . ? C4 C5 C6 C1 1.8(9) . . . . ? Ru1 C5 C6 C1 54.5(5) . . . . ? C4 C5 C6 Ru1 -52.7(5) . . . . ? C25 C26 C27 C28 -0.8(9) . . . . ? C21 N1 C22 C24 36.0(7) . . . . ? Ru1 N1 C22 C24 -146.4(4) . . . . ? C21 N1 C22 C23 -91.1(6) . . . . ? Ru1 N1 C22 C23 86.6(5) . . . . ? C29 C24 C22 N1 -127.3(5) . . . . ? C25 C24 C22 N1 55.0(7) . . . . ? C29 C24 C22 C23 -3.0(8) . . . . ? C25 C24 C22 C23 179.4(5) . . . . ? Ru1 O1 C11 C12 17.0(8) . . . . ? Ru1 O1 C11 C20 -162.6(3) . . . . ? C13 C12 C11 O1 176.1(5) . . . . ? C21 C12 C11 O1 -9.0(9) . . . . ? C13 C12 C11 C20 -4.3(8) . . . . ? C21 C12 C11 C20 170.5(5) . . . . ? C19 C20 C11 O1 4.9(7) . . . . ? C15 C20 C11 O1 -176.8(5) . . . . ? C19 C20 C11 C12 -174.7(5) . . . . ? C15 C20 C11 C12 3.6(8) . . . . ? C11 C12 C13 C14 1.5(9) . . . . ? C21 C12 C13 C14 -173.7(6) . . . . ? C12 C13 C14 C15 2.3(10) . . . . ? C20 C15 C14 C13 -2.9(10) . . . . ? C16 C15 C14 C13 175.0(6) . . . . ? C27 C26 C25 C24 -0.5(10) . . . . ? C29 C24 C25 C26 0.7(9) . . . . ? C22 C24 C25 C26 178.5(6) . . . . ? C15 C16 C17 C18 1.7(10) . . . . ? C20 C19 C18 C17 -1.0(9) . . . . ? C16 C17 C18 C19 -0.4(10) . . . . ? C6 C1 C7 C9 37.0(14) . . . . ? C2 C1 C7 C9 -145.1(12) . . . . ? Ru1 C1 C7 C9 -54.2(14) . . . . ? C6 C1 C7 C8 -82.6(11) . . . . ? C2 C1 C7 C8 95.3(11) . . . . ? Ru1 C1 C7 C8 -173.8(9) . . . . ? C26 C27 C28 C29 1.9(9) . . . . ? C24 C29 C28 C27 -1.7(9) . . . . ? #===END data_1519531 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety '(C47 H45 N O P Ru)3, (F6 P1)3' _chemical_formula_sum 'C141 H135 F18 N3 O3 P6 Ru3' _chemical_formula_weight 2750.54 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration rm #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.50060(10) _cell_length_b 17.86340(10) _cell_length_c 34.44680(10) _cell_angle_alpha 90 _cell_angle_beta 98.100(1) _cell_angle_gamma 90 _cell_volume 6396.99(7) _cell_formula_units_Z 2 _cell_measurement_temperature 110.00(2) _cell_measurement_reflns_used 31726 _cell_measurement_theta_min 3.5650 _cell_measurement_theta_max 66.5840 _cell_measurement_wavelength 1.54184 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.1924 _exptl_crystal_size_mid 0.0584 _exptl_crystal_size_min 0.0197 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2850 _exptl_special_details ? _exptl_absorpt_coefficient_mu 4.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46716 _exptl_absorpt_correction_T_max 1.00000 _shelx_estimated_absorpt_T_min 0.501 _shelx_estimated_absorpt_T_max 0.92 _diffrn_ambient_temperature 110.00(10) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_number 48030 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.583 _diffrn_reflns_theta_max 66.601 _diffrn_reflns_theta_full 66.601 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_Laue_measured_fraction_full 0.99 _diffrn_reflns_Laue_measured_fraction_max 0.99 _diffrn_reflns_point_group_measured_fraction_full 0.97 _diffrn_reflns_point_group_measured_fraction_max 0.97 _reflns_Friedel_fraction_full 0.949 _reflns_Friedel_fraction_max 0.949 _reflns_Friedel_coverage 0.893 _reflns_number_total 21912 _reflns_number_gt 21255 _reflns_threshold_expression 'I > 2\s(I)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+7.6114P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 21912 _refine_ls_number_parameters 1557 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.11 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details ; Flack x determined using 9590 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.014(3) _refine_diff_density_max 1.259 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.078 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.36063(4) 0.42960(2) 0.43516(2) 0.02682(11) Uani 1 1 d . . . . . Ru2 Ru 0.50974(4) 0.34946(3) 0.71636(2) 0.02847(12) Uani 1 1 d . . . . . Ru3 Ru 0.39069(4) 0.91796(3) 0.93234(2) 0.02478(11) Uani 1 1 d . . . . . P1 P 0.49655(15) 0.43928(9) 0.38555(4) 0.0275(3) Uani 1 1 d . . . . . P2 P 0.40181(15) 0.46544(9) 0.71149(5) 0.0306(3) Uani 1 1 d . . . . . P3 P 0.54572(16) 0.87383(11) 0.89361(5) 0.0337(4) Uani 1 1 d . . . . . P4 P 0.28786(19) 0.10529(11) 0.44208(6) 0.0432(4) Uani 1 1 d . . . . . P5 P 0.03852(17) 0.16891(11) 0.75855(6) 0.0402(4) Uani 1 1 d . . . . . O2 O 0.4974(4) 0.3679(2) 0.77467(13) 0.0295(9) Uani 1 1 d . . . . . P6 P 0.7965(2) 0.13479(14) 0.01363(7) 0.0560(6) Uani 1 1 d . . . . . O1 O 0.2510(4) 0.3672(2) 0.39288(11) 0.0243(8) Uani 1 1 d . . . . . O3 O 0.2718(4) 0.8464(3) 0.89726(11) 0.0294(9) Uani 1 1 d . . . . . C95 C 0.2558(6) 0.9271(5) 0.97858(16) 0.0364(15) Uani 1 1 d . . . . . N2 N 0.6884(5) 0.4049(4) 0.72753(17) 0.0391(14) Uani 1 1 d . . . . . N3 N 0.3448(5) 1.0039(3) 0.89067(15) 0.0290(11) Uani 1 1 d . . . . . C42 C 0.5903(6) 0.3545(4) 0.38348(18) 0.0293(13) Uani 1 1 d . . . . . C82 C 0.2200(6) 0.4100(4) 0.75669(19) 0.0332(14) Uani 1 1 d . . . . . H82 H 0.24032 0.361895 0.747561 0.04 Uiso 1 1 calc R U . . . C11 C 0.1530(6) 0.3889(3) 0.36779(17) 0.0247(12) Uani 1 1 d . . . . . C129 C 0.7008(7) 1.0002(6) 0.9090(2) 0.054(2) Uani 1 1 d . . . . . H129 H 0.647158 1.012064 0.928177 0.065 Uiso 1 1 calc R U . . . C97 C 0.4505(6) 0.8473(4) 0.98505(16) 0.0325(14) Uani 1 1 d . . . . . H97 H 0.487348 0.798642 0.986977 0.039 Uiso 1 1 calc R U . . . C49 C 0.3751(6) 0.2539(4) 0.7148(2) 0.0334(14) Uani 1 1 d . . . . . H49 H 0.306814 0.24817 0.729955 0.04 Uiso 1 1 calc R U . . . C36 C 0.6091(6) 0.5170(4) 0.3873(2) 0.0333(14) Uani 1 1 d . . . . . F8 F -0.0908(5) 0.1810(4) 0.7298(2) 0.096(3) Uani 1 1 d . . . . . C98 C 0.5310(6) 0.9110(4) 0.98778(16) 0.0321(14) Uani 1 1 d . . . . . C100 C 0.3365(7) 0.9897(4) 0.98145(18) 0.0355(15) Uani 1 1 d . . . . . H100 H 0.299192 1.038205 0.980726 0.043 Uiso 1 1 calc R U . . . C113 C 0.1048(7) 0.7349(4) 0.87031(19) 0.0374(15) Uani 1 1 d . . . . . H113 H 0.155476 0.729277 0.895255 0.045 Uiso 1 1 calc R U . . . C99 C 0.4723(7) 0.9830(4) 0.98542(17) 0.0336(15) Uani 1 1 d . . . . . H99 H 0.524248 1.026653 0.986503 0.04 Uiso 1 1 calc R U . . . C96 C 0.3153(6) 0.8557(4) 0.97947(17) 0.0352(15) Uani 1 1 d . . . . . H96 H 0.26278 0.81226 0.976203 0.042 Uiso 1 1 calc R U . . . C105 C 0.1991(6) 0.8605(4) 0.86435(16) 0.0266(12) Uani 1 1 d . . . . . C66 C 0.4397(7) 0.3337(4) 0.8481(2) 0.0363(15) Uani 1 1 d . . . . . H66 H 0.371414 0.341352 0.827246 0.044 Uiso 1 1 calc R U . . . C81 C 0.1310(6) 0.4169(5) 0.7829(2) 0.0409(15) Uani 1 1 d . . . . . H81 H 0.091588 0.373612 0.791881 0.049 Uiso 1 1 calc R U . . . C4 C 0.5264(6) 0.4020(5) 0.48218(19) 0.0429(18) Uani 1 1 d . . . . . C114 C 0.1135(6) 0.8014(4) 0.84889(18) 0.0318(14) Uani 1 1 d . . . . . C77 C 0.2792(6) 0.4730(4) 0.7439(2) 0.0318(14) Uani 1 1 d . . . . . C20 C 0.0841(6) 0.3302(3) 0.34512(17) 0.0266(12) Uani 1 1 d . . . . . C106 C 0.1994(5) 0.9282(4) 0.84359(16) 0.0283(12) Uani 1 1 d . . . . . C43 C 0.7219(6) 0.3539(4) 0.38021(18) 0.0341(14) Uani 1 1 d . . . . . H43 H 0.767284 0.399728 0.379267 0.041 Uiso 1 1 calc R U . . . C109 C 0.0390(6) 0.8091(5) 0.81176(19) 0.0377(15) Uani 1 1 d . . . . . C19 C 0.1167(6) 0.2537(4) 0.35292(19) 0.0315(14) Uani 1 1 d . . . . . H19 H 0.185939 0.241484 0.372746 0.038 Uiso 1 1 calc R U . . . C112 C 0.0241(8) 0.6780(5) 0.8556(2) 0.0465(18) Uani 1 1 d . . . . . H112 H 0.018894 0.633635 0.87054 0.056 Uiso 1 1 calc R U . . . F3 F 0.3834(6) 0.0421(4) 0.43383(16) 0.084(2) Uani 1 1 d . . . . . F10 F 0.1691(6) 0.1570(5) 0.78699(17) 0.095(2) Uani 1 1 d . . . . . C3 C 0.4612(8) 0.4653(5) 0.4937(2) 0.0458(19) Uani 1 1 d . . . . . H3 H 0.507067 0.510557 0.500042 0.055 Uiso 1 1 calc R U . . . C136 C 0.4856(6) 0.8557(4) 0.84172(17) 0.0297(13) Uani 1 1 d . . . . . C2 C 0.3288(7) 0.4621(4) 0.4959(2) 0.0393(16) Uani 1 1 d . . . . . H2 H 0.287776 0.505384 0.504276 0.047 Uiso 1 1 calc R U . . . C47 C 0.5268(6) 0.2854(4) 0.38537(18) 0.0298(13) Uani 1 1 d . . . . . H47 H 0.438199 0.284835 0.388329 0.036 Uiso 1 1 calc R U . . . C1 C 0.2544(7) 0.3979(4) 0.48620(18) 0.0355(15) Uani 1 1 d . . . . . C5 C 0.4536(7) 0.3364(4) 0.47201(18) 0.0372(15) Uani 1 1 d . . . . . H5 H 0.495327 0.292761 0.464301 0.045 Uiso 1 1 calc R U . . . C44 C 0.7854(7) 0.2863(4) 0.3784(2) 0.0384(15) Uani 1 1 d . . . . . H44 H 0.874794 0.286285 0.376442 0.046 Uiso 1 1 calc R U . . . C12 C 0.1134(6) 0.4630(4) 0.36158(19) 0.0306(14) Uani 1 1 d . . . . . N1 N 0.2690(6) 0.5256(3) 0.41099(19) 0.0365(13) Uani 1 1 d . . . . . C45 C 0.7216(8) 0.2191(4) 0.3792(2) 0.0414(17) Uani 1 1 d . . . . . H45 H 0.765989 0.173244 0.37728 0.05 Uiso 1 1 calc R U . . . C110 C -0.0420(7) 0.7485(5) 0.7968(2) 0.0469(18) Uani 1 1 d . . . . . H110 H -0.090551 0.752169 0.771415 0.056 Uiso 1 1 calc R U . . . C107 C 0.1235(6) 0.9340(4) 0.80536(18) 0.0348(14) Uani 1 1 d . . . . . H107 H 0.126693 0.978761 0.790678 0.042 Uiso 1 1 calc R U . . . C55 C 0.4475(7) 0.1055(4) 0.7585(2) 0.0424(17) Uani 1 1 d . . . . . H55A H 0.453845 0.075345 0.782507 0.064 Uiso 1 1 calc R U . . . H55B H 0.356716 0.113394 0.748174 0.064 Uiso 1 1 calc R U . . . H55C H 0.490045 0.079129 0.738949 0.064 Uiso 1 1 calc R U . . . C94 C 0.1823(7) 0.4883(4) 0.6559(2) 0.0375(15) Uani 1 1 d . . . . . H94 H 0.134417 0.47606 0.676404 0.045 Uiso 1 1 calc R U . . . C35 C 0.3736(7) 0.3862(4) 0.3125(2) 0.0378(15) Uani 1 1 d . . . . . H35 H 0.404691 0.337965 0.320714 0.045 Uiso 1 1 calc R U . . . F18 F 0.8411(8) 0.2047(4) -0.0078(2) 0.105(3) Uani 1 1 d . . . . . C46 C 0.5904(7) 0.2190(4) 0.3830(2) 0.0348(14) Uani 1 1 d . . . . . H46 H 0.545689 0.172974 0.383999 0.042 Uiso 1 1 calc R U . . . C67 C 0.5662(6) 0.3411(4) 0.84096(19) 0.0344(14) Uani 1 1 d . . . . . C13 C 0.0081(7) 0.4793(4) 0.3312(2) 0.0367(15) Uani 1 1 d . . . . . H13 H -0.017444 0.529843 0.326485 0.044 Uiso 1 1 calc R U . . . C40 C 0.7175(7) 0.6226(4) 0.4217(3) 0.0474(18) Uani 1 1 d . . . . . H40 H 0.735164 0.652112 0.444763 0.057 Uiso 1 1 calc R U . . . C89 C 0.3171(6) 0.4896(4) 0.6634(2) 0.0354(14) Uani 1 1 d . . . . . C17 C -0.0505(8) 0.2162(5) 0.3016(2) 0.052(2) Uani 1 1 d . . . . . H17 H -0.094151 0.177466 0.286216 0.063 Uiso 1 1 calc R U . . . C48 C 0.4990(7) 0.2242(4) 0.7293(2) 0.0349(15) Uani 1 1 d . . . . . C51 C 0.4523(7) 0.3008(4) 0.6552(2) 0.0385(15) Uani 1 1 d . . . . . C8 C 0.0975(8) 0.3436(5) 0.5259(2) 0.0503(19) Uani 1 1 d . . . . . H8A H 0.006496 0.341614 0.529299 0.075 Uiso 1 1 calc R U . . . H8B H 0.127578 0.293179 0.520637 0.075 Uiso 1 1 calc R U . . . H8C H 0.148017 0.36321 0.549823 0.075 Uiso 1 1 calc R U . . . C30 C 0.4075(6) 0.4473(4) 0.33602(19) 0.0319(14) Uani 1 1 d . . . . . F17 F 0.7409(8) 0.0635(4) 0.0356(3) 0.102(2) Uani 1 1 d . . . . . C50 C 0.3521(7) 0.2914(4) 0.6788(2) 0.0354(14) Uani 1 1 d . . . . . H50 H 0.268829 0.310837 0.669988 0.042 Uiso 1 1 calc R U . . . C32 C 0.2820(7) 0.5259(5) 0.2876(2) 0.0413(16) Uani 1 1 d . . . . . H32 H 0.251009 0.574136 0.279331 0.05 Uiso 1 1 calc R U . . . C37 C 0.6647(6) 0.5369(4) 0.3539(2) 0.0376(15) Uani 1 1 d . . . . . H37 H 0.646929 0.508311 0.330502 0.045 Uiso 1 1 calc R U . . . C31 C 0.3619(6) 0.5178(4) 0.3229(2) 0.0350(14) Uani 1 1 d . . . . . H31 H 0.38623 0.560766 0.338441 0.042 Uiso 1 1 calc R U . . . C83 C 0.5001(7) 0.5466(4) 0.7281(3) 0.047(2) Uani 1 1 d . . . . . C90 C 0.3834(7) 0.5067(4) 0.6326(2) 0.0412(16) Uani 1 1 d . . . . . H90 H 0.474813 0.506693 0.636977 0.049 Uiso 1 1 calc R U . . . C140 C 0.4450(7) 0.8984(4) 0.7752(2) 0.0404(16) Uani 1 1 d . . . . . H140 H 0.447882 0.937541 0.756674 0.048 Uiso 1 1 calc R U . . . F11 F 0.1004(6) 0.1273(6) 0.7267(2) 0.121(4) Uani 1 1 d . . . . . F13 F 0.6784(6) 0.1247(5) -0.0198(2) 0.098(2) Uani 1 1 d . . . . . C124 C 0.6814(6) 0.9339(6) 0.88807(19) 0.047(2) Uani 1 1 d . . . . . C68 C 0.7584(6) 0.4009(5) 0.7614(2) 0.0446(18) Uani 1 1 d . . . . . H68 H 0.843462 0.419834 0.762852 0.053 Uiso 1 1 calc R U . . . C118 C 0.2909(8) 1.1322(4) 0.9129(3) 0.0475(19) Uani 1 1 d . . . . . C18 C 0.0498(8) 0.1979(5) 0.3323(2) 0.0472(19) Uani 1 1 d . . . . . H18 H 0.070042 0.14705 0.338416 0.057 Uiso 1 1 calc R U . . . F9 F -0.0211(6) 0.0963(4) 0.7727(3) 0.114(3) Uani 1 1 d . . . . . C88 C 0.5552(8) 0.5478(4) 0.7679(3) 0.057(2) Uani 1 1 d . . . . . H88 H 0.546973 0.504979 0.783754 0.068 Uiso 1 1 calc R U . . . C93 C 0.1176(7) 0.5047(4) 0.6189(2) 0.0436(17) Uani 1 1 d . . . . . H93 H 0.026323 0.502844 0.614202 0.052 Uiso 1 1 calc R U . . . C104 C 0.6755(6) 0.9025(5) 0.9953(2) 0.0413(17) Uani 1 1 d . . . . . H10A H 0.715813 0.952079 0.996314 0.062 Uiso 1 1 calc R U . . . H10B H 0.700191 0.876814 1.020396 0.062 Uiso 1 1 calc R U . . . H10C H 0.704278 0.873097 0.97417 0.062 Uiso 1 1 calc R U . . . C6 C 0.3204(7) 0.3350(4) 0.47320(18) 0.0346(14) Uani 1 1 d . . . . . H6 H 0.273173 0.290989 0.465118 0.041 Uiso 1 1 calc R U . . . C14 C -0.0546(6) 0.4253(5) 0.30944(18) 0.0421(16) Uani 1 1 d . . . . . H14 H -0.123401 0.438087 0.289594 0.051 Uiso 1 1 calc R U . . . C92 C 0.1853(8) 0.5234(4) 0.5891(2) 0.0444(17) Uani 1 1 d . . . . . H92 H 0.140664 0.536129 0.56402 0.053 Uiso 1 1 calc R U . . . C28 C 0.0295(9) 0.6281(5) 0.4890(2) 0.052(2) Uani 1 1 d . . . . . H28 H -0.057854 0.614061 0.488797 0.063 Uiso 1 1 calc R U . . . C15 C -0.0192(6) 0.3480(5) 0.31571(17) 0.0369(15) Uani 1 1 d . . . . . F7 F 0.0971(6) 0.2431(4) 0.7448(4) 0.140(4) Uani 1 1 d . . . . . C16 C -0.0847(8) 0.2891(6) 0.2941(2) 0.053(2) Uani 1 1 d . . . . . H16 H -0.15363 0.300272 0.27401 0.063 Uiso 1 1 calc R U . . . F15 F 0.8825(8) 0.0831(6) -0.0092(2) 0.123(3) Uani 1 1 d . . . . . C38 C 0.7464(7) 0.5990(4) 0.3554(3) 0.0449(18) Uani 1 1 d . . . . . H38 H 0.784621 0.612008 0.332971 0.054 Uiso 1 1 calc R U . . . C116 C 0.3937(7) 1.0815(4) 0.8991(2) 0.0346(14) Uani 1 1 d . . . . . H116 H 0.466254 1.078016 0.921201 0.042 Uiso 1 1 calc R U . . . C52 C 0.5760(7) 0.2759(4) 0.6712(2) 0.0403(16) Uani 1 1 d . . . . . H52 H 0.645905 0.28556 0.657142 0.048 Uiso 1 1 calc R U . . . C71 C 0.8042(7) 0.3966(6) 0.6688(3) 0.056(2) Uani 1 1 d . . . . . C54 C 0.5134(7) 0.1816(4) 0.7679(2) 0.0372(15) Uani 1 1 d . . . . . H54 H 0.46419 0.209144 0.786248 0.045 Uiso 1 1 calc R U . . . C60 C 0.8240(7) 0.3601(6) 0.8298(3) 0.056(2) Uani 1 1 d . . . . . H60 H 0.911023 0.368486 0.826286 0.067 Uiso 1 1 calc R U . . . C7 C 0.1141(7) 0.3956(5) 0.4910(2) 0.0443(17) Uani 1 1 d . . . . . H7 H 0.087791 0.447208 0.497736 0.053 Uiso 1 1 calc R U . . . C53 C 0.6004(7) 0.2367(4) 0.7076(2) 0.0384(15) Uani 1 1 d . . . . . H53 H 0.684555 0.219197 0.716979 0.046 Uiso 1 1 calc R U . . . C59 C 0.7237(7) 0.3714(4) 0.7970(2) 0.0414(16) Uani 1 1 d . . . . . F1 F 0.1882(7) 0.1686(4) 0.4518(3) 0.117(3) Uani 1 1 d . . . . . C69 C 0.7403(7) 0.4470(5) 0.6955(2) 0.051(2) Uani 1 1 d . . . . . H69 H 0.664735 0.470282 0.678979 0.061 Uiso 1 1 calc R U . . . C141 C 0.4858(6) 0.9111(4) 0.81425(17) 0.0307(13) Uani 1 1 d . . . . . H141 H 0.514929 0.959699 0.822467 0.037 Uiso 1 1 calc R U . . . C108 C 0.0476(7) 0.8768(4) 0.78995(19) 0.0400(16) Uani 1 1 d . . . . . H108 H -0.000114 0.881645 0.764526 0.048 Uiso 1 1 calc R U . . . C117 C 0.4479(8) 1.1163(4) 0.8644(2) 0.0432(17) Uani 1 1 d . . . . . H11A H 0.478732 1.167013 0.871245 0.065 Uiso 1 1 calc R U . . . H11B H 0.519395 1.085664 0.857888 0.065 Uiso 1 1 calc R U . . . H11C H 0.380245 1.118502 0.841678 0.065 Uiso 1 1 calc R U . . . C25 C 0.2823(10) 0.6700(5) 0.4893(3) 0.055(2) Uani 1 1 d . . . . . H25 H 0.369131 0.685275 0.489673 0.066 Uiso 1 1 calc R U . . . F16 F 0.9080(7) 0.1391(7) 0.0485(2) 0.137(4) Uani 1 1 d . . . . . C91 C 0.3199(8) 0.5238(4) 0.5954(2) 0.0448(17) Uani 1 1 d . . . . . H91 H 0.367235 0.535656 0.57463 0.054 Uiso 1 1 calc R U . . . C9 C 0.0269(7) 0.3711(5) 0.4546(2) 0.0490(19) Uani 1 1 d . . . . . H9A H -0.062502 0.370872 0.459771 0.074 Uiso 1 1 calc R U . . . H9B H 0.035492 0.405865 0.433085 0.074 Uiso 1 1 calc R U . . . H9C H 0.050992 0.320579 0.447182 0.074 Uiso 1 1 calc R U . . . C64 C 0.5115(10) 0.3022(6) 0.9148(2) 0.059(2) Uani 1 1 d . . . . . H64 H 0.492043 0.288602 0.939939 0.071 Uiso 1 1 calc R U . . . C61 C 0.7978(8) 0.3381(6) 0.8651(2) 0.060(2) Uani 1 1 d . . . . . H61 H 0.866602 0.328927 0.8856 0.072 Uiso 1 1 calc R U . . . C139 C 0.4001(8) 0.8291(5) 0.7629(2) 0.050(2) Uani 1 1 d . . . . . H139 H 0.374658 0.819737 0.735746 0.06 Uiso 1 1 calc R U . . . C21 C 0.1735(7) 0.5252(4) 0.3827(2) 0.0367(15) Uani 1 1 d . . . . . H21 H 0.138939 0.572949 0.374932 0.044 Uiso 1 1 calc R U . . . C41 C 0.6367(7) 0.5604(4) 0.4210(2) 0.0405(16) Uani 1 1 d . . . . . H41 H 0.600104 0.547495 0.44383 0.049 Uiso 1 1 calc R U . . . C80 C 0.1004(8) 0.4867(5) 0.7957(2) 0.053(2) Uani 1 1 d . . . . . H80 H 0.041484 0.491214 0.814101 0.064 Uiso 1 1 calc R U . . . C79 C 0.1550(8) 0.5505(5) 0.7820(3) 0.057(2) Uani 1 1 d . . . . . H79 H 0.131748 0.598671 0.790314 0.068 Uiso 1 1 calc R U . . . C22 C 0.3097(8) 0.5992(4) 0.4297(3) 0.053(2) Uani 1 1 d . . . . . H22 H 0.398112 0.59169 0.444262 0.064 Uiso 1 1 calc R U . . . C137 C 0.4327(10) 0.7849(4) 0.8288(2) 0.052(2) Uani 1 1 d . . . . . H137 H 0.425467 0.745876 0.847076 0.062 Uiso 1 1 calc R U . . . C101 C 0.1106(7) 0.9382(6) 0.9758(2) 0.052(2) Uani 1 1 d . . . . . H101 H 0.089498 0.990484 0.96666 0.062 Uiso 1 1 calc R U . . . C39 C 0.7720(8) 0.6411(4) 0.3885(3) 0.0480(19) Uani 1 1 d . . . . . H39 H 0.827317 0.6833 0.388883 0.058 Uiso 1 1 calc R U . . . C78 C 0.2435(8) 0.5433(4) 0.7560(3) 0.0469(18) Uani 1 1 d . . . . . H78 H 0.280351 0.586843 0.746368 0.056 Uiso 1 1 calc R U . . . F14 F 0.7082(7) 0.1854(3) 0.0367(2) 0.085(2) Uani 1 1 d . . . . . C56 C 0.6510(7) 0.1717(4) 0.7881(2) 0.0422(16) Uani 1 1 d . . . . . H56A H 0.650678 0.143764 0.812524 0.063 Uiso 1 1 calc R U . . . H56B H 0.700668 0.143975 0.770731 0.063 Uiso 1 1 calc R U . . . H56C H 0.690275 0.220925 0.793867 0.063 Uiso 1 1 calc R U . . . C34 C 0.2941(8) 0.3944(5) 0.2769(2) 0.0452(18) Uani 1 1 d . . . . . H34 H 0.271732 0.351726 0.260935 0.054 Uiso 1 1 calc R U . . . C125 C 0.7619(7) 0.9164(9) 0.8600(2) 0.079(4) Uani 1 1 d . . . . . H125 H 0.75098 0.870853 0.84571 0.095 Uiso 1 1 calc R U . . . C33 C 0.2471(7) 0.4642(5) 0.2644(2) 0.0442(17) Uani 1 1 d . . . . . H33 H 0.191646 0.469463 0.240312 0.053 Uiso 1 1 calc R U . . . C24 C 0.2258(8) 0.6240(4) 0.4597(2) 0.0406(16) Uani 1 1 d . . . . . C62 C 0.6688(8) 0.3282(5) 0.8724(2) 0.050(2) Uani 1 1 d . . . . . C57 C 0.4259(9) 0.3311(5) 0.6147(2) 0.051(2) Uani 1 1 d . . . . . H57A H 0.335043 0.34538 0.608951 0.077 Uiso 1 1 calc R U . . . H57B H 0.47994 0.375186 0.612487 0.077 Uiso 1 1 calc R U . . . H57C H 0.445145 0.292824 0.596031 0.077 Uiso 1 1 calc R U . . . C26 C 0.2147(12) 0.6943(5) 0.5185(3) 0.066(3) Uani 1 1 d . . . . . H26 H 0.255215 0.726092 0.538705 0.079 Uiso 1 1 calc R U . . . C119 C 0.3187(12) 1.1660(5) 0.9499(3) 0.067(3) Uani 1 1 d . . . . . H119 H 0.399836 1.157606 0.965269 0.08 Uiso 1 1 calc R U . . . C111 C -0.0504(7) 0.6849(5) 0.8188(2) 0.0463(18) Uani 1 1 d . . . . . H111 H -0.106898 0.645644 0.808958 0.056 Uiso 1 1 calc R U . . . C123 C 0.1763(9) 1.1490(5) 0.8896(4) 0.069(3) Uani 1 1 d . . . . . H123 H 0.158112 1.127957 0.864074 0.082 Uiso 1 1 calc R U . . . C29 C 0.0981(7) 0.6035(5) 0.4592(2) 0.0487(19) Uani 1 1 d . . . . . H29 H 0.057036 0.572791 0.438639 0.058 Uiso 1 1 calc R U . . . C84 C 0.5137(9) 0.6092(5) 0.7053(3) 0.063(3) Uani 1 1 d . . . . . H84 H 0.475399 0.610579 0.678611 0.076 Uiso 1 1 calc R U . . . C27 C 0.0911(11) 0.6732(5) 0.5186(2) 0.058(2) Uani 1 1 d . . . . . H27 H 0.046006 0.689334 0.539105 0.069 Uiso 1 1 calc R U . . . C130 C 0.6096(9) 0.7807(6) 0.9103(2) 0.062(3) Uani 1 1 d . . . . . F2 F 0.3472(14) 0.1116(6) 0.48489(17) 0.193(7) Uani 1 1 d . . . . . C72 C 0.7830(8) 0.4096(7) 0.6285(3) 0.068(3) Uani 1 1 d . . . . . H72 H 0.72466 0.447692 0.618219 0.082 Uiso 1 1 calc R U . . . C65 C 0.4121(8) 0.3155(5) 0.8846(2) 0.0488(19) Uani 1 1 d . . . . . H65 H 0.325239 0.312027 0.889275 0.059 Uiso 1 1 calc R U . . . C135 C 0.5216(11) 0.7266(6) 0.9188(3) 0.068(3) Uani 1 1 d . . . . . H135 H 0.432296 0.737672 0.91628 0.082 Uiso 1 1 calc R U . . . C134 C 0.5673(18) 0.6565(8) 0.9310(4) 0.123(7) Uani 1 1 d . . . . . H134 H 0.507445 0.622732 0.939696 0.148 Uiso 1 1 calc R U . . . C85 C 0.5859(11) 0.6714(6) 0.7224(4) 0.078(3) Uani 1 1 d . . . . . H85 H 0.601298 0.712708 0.706276 0.093 Uiso 1 1 calc R U . . . C138 C 0.3919(11) 0.7741(6) 0.7892(3) 0.069(3) Uani 1 1 d . . . . . H138 H 0.357428 0.726938 0.780454 0.082 Uiso 1 1 calc R U . . . C76 C 0.8891(7) 0.3403(6) 0.6823(2) 0.056(2) Uani 1 1 d . . . . . H76 H 0.906369 0.330961 0.709665 0.068 Uiso 1 1 calc R U . . . C75 C 0.9499(9) 0.2968(7) 0.6569(3) 0.072(3) Uani 1 1 d . . . . . H75 H 1.005647 0.257225 0.666861 0.087 Uiso 1 1 calc R U . . . C70 C 0.8312(9) 0.5110(6) 0.7101(3) 0.072(3) Uani 1 1 d . . . . . H70A H 0.861124 0.535829 0.687684 0.109 Uiso 1 1 calc R U . . . H70B H 0.785568 0.547262 0.72448 0.109 Uiso 1 1 calc R U . . . H70C H 0.905205 0.491028 0.727545 0.109 Uiso 1 1 calc R U . . . F5 F 0.2033(13) 0.0436(4) 0.4564(5) 0.218(9) Uani 1 1 d . . . . . F12 F -0.0181(8) 0.2121(8) 0.7920(4) 0.177(6) Uani 1 1 d . . . . . C63 C 0.6363(10) 0.3084(6) 0.9089(2) 0.060(2) Uani 1 1 d . . . . . H63 H 0.702725 0.298976 0.930073 0.072 Uiso 1 1 calc R U . . . C121 C 0.1097(17) 1.2270(7) 0.9399(6) 0.122(7) Uani 1 1 d . . . . . H121 H 0.04672 1.257888 0.949116 0.146 Uiso 1 1 calc R U . . . C103 C 0.0760(8) 0.9297(9) 1.0175(3) 0.085(4) Uani 1 1 d . . . . . H10D H 0.128285 0.964266 1.035191 0.128 Uiso 1 1 calc R U . . . H10E H -0.015324 0.941249 1.017299 0.128 Uiso 1 1 calc R U . . . H10F H 0.092945 0.878174 1.026507 0.128 Uiso 1 1 calc R U . . . C86 C 0.6347(10) 0.6730(5) 0.7624(4) 0.075(3) Uani 1 1 d . . . . . H86 H 0.676154 0.716433 0.773943 0.09 Uiso 1 1 calc R U . . . C10 C 0.6697(7) 0.4014(7) 0.4824(2) 0.061(3) Uani 1 1 d . . . . . H10G H 0.696224 0.352514 0.473482 0.091 Uiso 1 1 calc R U . . . H10H H 0.693485 0.440577 0.464872 0.091 Uiso 1 1 calc R U . . . H10I H 0.712742 0.410784 0.509125 0.091 Uiso 1 1 calc R U . . . C23 C 0.3200(13) 0.6622(5) 0.4000(4) 0.080(4) Uani 1 1 d . . . . . H23A H 0.346837 0.708603 0.414033 0.12 Uiso 1 1 calc R U . . . H23B H 0.38364 0.648517 0.382993 0.12 Uiso 1 1 calc R U . . . H23C H 0.236124 0.669811 0.384035 0.12 Uiso 1 1 calc R U . . . C128 C 0.7975(9) 1.0493(8) 0.9023(3) 0.079(4) Uani 1 1 d . . . . . H128 H 0.812052 1.094252 0.917031 0.094 Uiso 1 1 calc R U . . . C131 C 0.7406(11) 0.7646(9) 0.9142(3) 0.088(4) Uani 1 1 d . . . . . H131 H 0.802803 0.800493 0.909036 0.105 Uiso 1 1 calc R U . . . C133 C 0.6833(14) 0.6328(8) 0.9316(4) 0.097(5) Uani 1 1 d . . . . . H133 H 0.705268 0.581385 0.935103 0.116 Uiso 1 1 calc R U . . . C73 C 0.8461(11) 0.3676(8) 0.6031(3) 0.085(4) Uani 1 1 d . . . . . H73 H 0.831884 0.37765 0.575735 0.103 Uiso 1 1 calc R U . . . C126 C 0.8557(9) 0.9656(10) 0.8536(3) 0.107(6) Uani 1 1 d . . . . . H126 H 0.910648 0.953987 0.834744 0.128 Uiso 1 1 calc R U . . . C102 C 0.0318(9) 0.8863(8) 0.9498(3) 0.084(4) Uani 1 1 d . . . . . H10J H -0.059417 0.897792 0.949963 0.126 Uiso 1 1 calc R U . . . H10K H 0.052663 0.891518 0.923095 0.126 Uiso 1 1 calc R U . . . H10L H 0.049278 0.834901 0.95894 0.126 Uiso 1 1 calc R U . . . C132 C 0.7752(12) 0.6876(8) 0.9268(4) 0.096(4) Uani 1 1 d . . . . . H132 H 0.86365 0.674564 0.931922 0.116 Uiso 1 1 calc R U . . . C122 C 0.0873(11) 1.1965(7) 0.9032(5) 0.099(5) Uani 1 1 d . . . . . H122 H 0.009498 1.207987 0.886697 0.119 Uiso 1 1 calc R U . . . C74 C 0.9292(11) 0.3112(9) 0.6175(3) 0.088(4) Uani 1 1 d . . . . . H74 H 0.97213 0.282445 0.600137 0.106 Uiso 1 1 calc R U . . . C87 C 0.6212(10) 0.6101(5) 0.7845(3) 0.072(3) Uani 1 1 d . . . . . H87 H 0.657304 0.609307 0.811394 0.086 Uiso 1 1 calc R U . . . C115 C 0.2696(6) 0.9941(4) 0.85766(18) 0.0296(13) Uani 1 1 d . . . . . H115 H 0.259846 1.036065 0.84059 0.036 Uiso 1 1 calc R U . . . C58 C 0.5965(6) 0.3598(4) 0.80253(19) 0.0328(14) Uani 1 1 d . . . . . C120 C 0.2286(18) 1.2119(6) 0.9642(5) 0.103(5) Uani 1 1 d . . . . . H120 H 0.246003 1.232864 0.989728 0.124 Uiso 1 1 calc R U . . . C127 C 0.8720(11) 1.0312(10) 0.8737(3) 0.112(6) Uani 1 1 d . . . . . H127 H 0.936212 1.065337 0.867977 0.134 Uiso 1 1 calc R U . . . F6 F 0.3599(7) 0.1740(5) 0.4269(2) 0.093(2) Uiso 1 1 d . . . . . F4 F 0.2044(11) 0.0957(6) 0.4022(3) 0.137(3) 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 Ru1 0.0235(2) 0.0296(3) 0.0286(2) -0.00924(19) 0.00796(16) -0.00704(19) Ru2 0.0212(2) 0.0305(2) 0.0348(2) 0.01137(19) 0.00777(17) 0.00253(18) Ru3 0.0206(2) 0.0344(3) 0.01945(19) -0.00165(18) 0.00313(15) -0.00007(19) P1 0.0238(7) 0.0283(8) 0.0318(7) -0.0059(6) 0.0089(6) -0.0043(6) P2 0.0220(7) 0.0271(8) 0.0416(9) 0.0104(7) 0.0007(6) -0.0010(6) P3 0.0246(8) 0.0548(11) 0.0219(7) -0.0011(7) 0.0037(6) 0.0104(7) P4 0.0403(10) 0.0385(10) 0.0501(11) 0.0161(8) 0.0040(8) 0.0034(8) P5 0.0265(8) 0.0374(10) 0.0574(11) -0.0013(8) 0.0076(8) 0.0024(7) O2 0.021(2) 0.031(2) 0.036(2) 0.0080(18) 0.0053(17) 0.0039(17) P6 0.0437(11) 0.0642(14) 0.0609(13) -0.0315(11) 0.0107(10) -0.0044(10) O1 0.023(2) 0.026(2) 0.0240(19) -0.0001(16) 0.0021(16) 0.0002(16) O3 0.032(2) 0.031(2) 0.0228(19) 0.0014(18) -0.0036(16) 0.0003(19) C95 0.027(3) 0.062(4) 0.021(3) -0.002(3) 0.007(2) -0.005(3) N2 0.023(3) 0.051(4) 0.045(3) 0.023(3) 0.007(2) -0.003(2) N3 0.032(3) 0.030(3) 0.027(2) -0.002(2) 0.009(2) -0.003(2) C42 0.031(3) 0.028(3) 0.031(3) -0.003(3) 0.011(2) -0.002(3) C82 0.026(3) 0.030(3) 0.044(3) -0.001(3) 0.006(3) 0.003(3) C11 0.023(3) 0.029(3) 0.024(3) 0.003(2) 0.010(2) 0.002(2) C129 0.027(4) 0.104(7) 0.034(4) -0.007(4) 0.008(3) -0.017(4) C97 0.037(3) 0.044(4) 0.017(3) 0.002(3) 0.004(2) -0.002(3) C49 0.031(3) 0.030(3) 0.042(4) 0.001(3) 0.015(3) 0.001(3) C36 0.025(3) 0.028(3) 0.050(4) -0.006(3) 0.014(3) -0.004(3) F8 0.031(3) 0.105(5) 0.144(6) 0.080(5) -0.015(3) -0.012(3) C98 0.029(3) 0.051(4) 0.016(2) -0.004(3) 0.003(2) 0.002(3) C100 0.032(4) 0.052(4) 0.023(3) -0.005(3) 0.006(3) 0.005(3) C113 0.050(4) 0.038(4) 0.025(3) -0.004(3) 0.009(3) -0.011(3) C99 0.032(3) 0.051(4) 0.018(3) -0.008(3) 0.003(2) -0.002(3) C96 0.031(3) 0.055(4) 0.020(3) 0.008(3) 0.003(2) -0.010(3) C105 0.023(3) 0.032(3) 0.025(3) 0.000(2) 0.003(2) 0.004(2) C66 0.039(4) 0.034(4) 0.036(3) -0.003(3) 0.007(3) -0.007(3) C81 0.029(3) 0.043(4) 0.050(4) 0.001(3) 0.005(3) 0.006(3) C4 0.027(3) 0.073(5) 0.027(3) -0.006(3) -0.001(3) -0.008(3) C114 0.027(3) 0.043(4) 0.027(3) -0.001(3) 0.007(2) 0.000(3) C77 0.023(3) 0.030(3) 0.040(3) 0.001(3) -0.004(3) 0.000(3) C20 0.024(3) 0.033(3) 0.023(3) -0.001(2) 0.003(2) 0.000(2) C106 0.023(3) 0.036(3) 0.025(3) 0.003(3) 0.002(2) 0.001(3) C43 0.030(3) 0.035(3) 0.037(3) 0.005(3) 0.007(3) -0.004(3) C109 0.025(3) 0.058(5) 0.030(3) -0.003(3) 0.003(3) -0.004(3) C19 0.027(3) 0.033(3) 0.032(3) -0.009(3) -0.001(2) 0.005(3) C112 0.059(5) 0.043(4) 0.038(4) -0.006(3) 0.009(3) -0.017(4) F3 0.065(3) 0.120(5) 0.062(3) -0.040(3) -0.010(3) 0.045(3) F10 0.048(3) 0.179(8) 0.054(3) -0.004(4) -0.006(2) -0.006(4) C3 0.045(4) 0.066(5) 0.029(3) -0.021(3) 0.011(3) -0.024(4) C136 0.026(3) 0.036(3) 0.028(3) -0.003(3) 0.010(2) 0.002(3) C2 0.045(4) 0.045(4) 0.031(3) -0.010(3) 0.013(3) -0.008(3) C47 0.028(3) 0.032(3) 0.031(3) -0.003(3) 0.010(2) -0.004(3) C1 0.037(4) 0.046(4) 0.027(3) -0.001(3) 0.014(3) -0.008(3) C5 0.034(3) 0.049(4) 0.027(3) -0.002(3) -0.002(3) 0.007(3) C44 0.029(3) 0.042(4) 0.046(4) 0.004(3) 0.014(3) 0.002(3) C12 0.027(3) 0.036(3) 0.032(3) 0.007(3) 0.016(3) 0.006(3) N1 0.036(3) 0.021(3) 0.056(4) -0.011(2) 0.022(3) -0.004(2) C45 0.044(4) 0.035(4) 0.049(4) 0.003(3) 0.019(3) 0.007(3) C110 0.038(4) 0.064(5) 0.038(4) -0.010(3) 0.002(3) -0.014(4) C107 0.030(3) 0.041(4) 0.031(3) 0.007(3) -0.003(2) 0.006(3) C55 0.044(4) 0.033(4) 0.054(4) 0.013(3) 0.021(3) 0.007(3) C94 0.032(4) 0.041(4) 0.039(4) 0.006(3) 0.002(3) 0.002(3) C35 0.044(4) 0.040(4) 0.032(3) -0.002(3) 0.013(3) -0.001(3) F18 0.104(5) 0.106(5) 0.122(6) -0.028(4) 0.075(5) -0.044(4) C46 0.036(4) 0.032(3) 0.038(3) -0.004(3) 0.012(3) -0.003(3) C67 0.037(3) 0.033(3) 0.033(3) 0.010(3) 0.003(3) -0.004(3) C13 0.031(3) 0.042(4) 0.041(4) 0.014(3) 0.016(3) 0.009(3) C40 0.033(4) 0.038(4) 0.071(5) -0.011(4) 0.007(4) -0.008(3) C89 0.031(3) 0.029(3) 0.045(4) 0.011(3) 0.001(3) 0.001(3) C17 0.043(4) 0.067(6) 0.042(4) -0.022(4) -0.010(3) -0.005(4) C48 0.042(4) 0.023(3) 0.042(4) 0.009(3) 0.013(3) 0.003(3) C51 0.043(4) 0.037(4) 0.037(4) 0.007(3) 0.012(3) 0.007(3) C8 0.049(4) 0.069(5) 0.035(3) 0.008(4) 0.014(3) -0.014(4) C30 0.027(3) 0.037(4) 0.035(3) 0.001(3) 0.015(3) -0.003(3) F17 0.116(6) 0.069(4) 0.118(6) -0.004(4) 0.007(5) -0.001(4) C50 0.031(3) 0.028(3) 0.047(4) -0.003(3) 0.006(3) 0.002(3) C32 0.031(4) 0.051(4) 0.044(4) 0.010(3) 0.014(3) -0.002(3) C37 0.026(3) 0.036(4) 0.053(4) 0.004(3) 0.013(3) -0.001(3) C31 0.027(3) 0.036(4) 0.045(4) 0.000(3) 0.015(3) 0.003(3) C83 0.028(4) 0.035(4) 0.075(5) 0.020(4) -0.007(3) -0.006(3) C90 0.036(4) 0.041(4) 0.046(4) 0.015(3) 0.006(3) 0.005(3) C140 0.035(4) 0.054(4) 0.033(3) 0.000(3) 0.005(3) 0.008(3) F11 0.057(4) 0.189(8) 0.123(6) -0.112(6) 0.031(4) -0.024(4) F13 0.060(4) 0.122(6) 0.107(5) -0.007(4) -0.007(3) -0.027(4) C124 0.019(3) 0.093(6) 0.028(3) -0.016(4) 0.004(2) -0.006(4) C68 0.020(3) 0.059(5) 0.054(4) 0.024(4) 0.003(3) 0.001(3) C118 0.056(5) 0.026(3) 0.068(5) -0.009(3) 0.034(4) -0.010(3) C18 0.043(4) 0.048(4) 0.047(4) -0.023(3) -0.005(3) 0.003(3) F9 0.062(4) 0.101(5) 0.176(8) 0.091(6) 0.003(4) -0.009(4) C88 0.046(5) 0.031(4) 0.083(6) 0.006(4) -0.026(4) -0.006(3) C93 0.038(4) 0.045(4) 0.046(4) 0.004(3) -0.003(3) 0.006(3) C104 0.024(3) 0.065(5) 0.033(3) 0.002(3) -0.003(3) 0.005(3) C6 0.038(4) 0.035(4) 0.029(3) 0.000(3) -0.001(3) -0.009(3) C14 0.033(3) 0.063(5) 0.030(3) 0.016(4) 0.004(3) 0.014(4) C92 0.052(5) 0.037(4) 0.040(4) 0.002(3) -0.004(3) 0.004(3) C28 0.056(5) 0.058(5) 0.045(4) -0.002(4) 0.013(4) 0.028(4) C15 0.031(3) 0.059(4) 0.021(3) 0.004(3) 0.003(2) 0.004(3) F7 0.045(3) 0.078(5) 0.287(13) 0.078(6) -0.008(5) -0.020(3) C16 0.044(4) 0.080(6) 0.030(4) -0.005(4) -0.005(3) -0.004(4) F15 0.115(6) 0.174(8) 0.078(4) -0.047(5) 0.007(4) 0.080(6) C38 0.030(4) 0.037(4) 0.072(5) 0.004(4) 0.022(3) -0.004(3) C116 0.033(3) 0.041(4) 0.033(3) -0.005(3) 0.014(3) -0.003(3) C52 0.039(4) 0.035(4) 0.052(4) 0.010(3) 0.023(3) 0.009(3) C71 0.029(4) 0.086(6) 0.055(5) 0.034(4) 0.013(3) -0.007(4) C54 0.040(4) 0.032(4) 0.043(4) 0.009(3) 0.020(3) 0.009(3) C60 0.030(4) 0.076(6) 0.059(5) 0.022(4) -0.003(3) -0.006(4) C7 0.035(4) 0.052(4) 0.048(4) 0.007(3) 0.014(3) -0.007(3) C53 0.038(4) 0.036(4) 0.045(4) 0.006(3) 0.019(3) 0.012(3) C59 0.030(3) 0.046(4) 0.048(4) 0.012(3) 0.004(3) -0.004(3) F1 0.076(4) 0.050(3) 0.231(10) -0.003(5) 0.042(5) 0.017(3) C69 0.024(3) 0.071(6) 0.058(4) 0.039(4) 0.005(3) -0.006(3) C141 0.031(3) 0.035(3) 0.027(3) -0.001(3) 0.009(2) 0.002(3) C108 0.028(3) 0.060(5) 0.028(3) 0.002(3) -0.008(3) -0.002(3) C117 0.045(4) 0.041(4) 0.047(4) -0.002(3) 0.019(3) -0.013(3) C25 0.073(6) 0.036(4) 0.055(5) -0.004(4) 0.006(4) -0.009(4) F16 0.070(4) 0.260(12) 0.077(4) -0.088(6) -0.001(4) -0.020(6) C91 0.057(5) 0.038(4) 0.040(4) 0.009(3) 0.010(3) 0.003(3) C9 0.032(4) 0.070(6) 0.046(4) 0.007(4) 0.010(3) -0.006(3) C64 0.076(6) 0.069(6) 0.032(4) 0.008(4) 0.010(4) -0.028(5) C61 0.043(4) 0.088(7) 0.045(4) 0.023(5) -0.009(3) -0.004(4) C139 0.042(4) 0.078(6) 0.031(3) -0.017(4) 0.005(3) -0.014(4) C21 0.037(4) 0.026(3) 0.053(4) 0.003(3) 0.024(3) 0.003(3) C41 0.031(4) 0.045(4) 0.047(4) -0.013(3) 0.013(3) -0.012(3) C80 0.041(4) 0.071(6) 0.048(4) -0.018(4) 0.007(3) 0.009(4) C79 0.049(5) 0.050(5) 0.071(6) -0.031(4) 0.009(4) 0.007(4) C22 0.049(5) 0.028(4) 0.088(6) -0.021(4) 0.026(4) -0.009(3) C137 0.085(6) 0.038(4) 0.036(4) -0.007(3) 0.020(4) -0.008(4) C101 0.025(3) 0.087(7) 0.044(4) 0.013(4) 0.007(3) 0.005(4) C39 0.037(4) 0.036(4) 0.072(5) 0.002(4) 0.013(4) -0.008(3) C78 0.043(4) 0.032(4) 0.062(5) -0.008(3) -0.005(4) -0.003(3) F14 0.090(4) 0.065(4) 0.116(5) -0.014(3) 0.067(4) 0.000(3) C56 0.044(4) 0.041(4) 0.042(4) 0.010(3) 0.010(3) 0.010(3) C34 0.050(4) 0.053(5) 0.033(4) -0.004(3) 0.007(3) -0.007(3) C125 0.025(4) 0.173(12) 0.041(4) -0.034(6) 0.011(3) -0.028(6) C33 0.041(4) 0.059(5) 0.032(3) 0.009(3) 0.004(3) -0.010(3) C24 0.046(4) 0.023(3) 0.053(4) -0.005(3) 0.007(3) 0.005(3) C62 0.051(5) 0.055(5) 0.040(4) 0.014(3) -0.007(3) -0.009(4) C57 0.068(5) 0.046(5) 0.038(4) 0.008(3) 0.007(4) 0.003(4) C26 0.107(9) 0.046(5) 0.046(5) -0.010(4) 0.011(5) -0.022(5) C119 0.103(8) 0.036(4) 0.073(6) -0.014(4) 0.054(6) -0.010(5) C111 0.033(4) 0.055(5) 0.051(4) -0.013(4) 0.006(3) -0.015(3) C123 0.038(5) 0.050(5) 0.122(9) -0.026(5) 0.023(5) -0.004(4) C29 0.038(4) 0.059(5) 0.050(4) -0.017(4) 0.009(3) 0.016(4) C84 0.056(5) 0.038(4) 0.092(7) 0.026(5) -0.007(5) -0.013(4) C27 0.101(8) 0.039(4) 0.036(4) 0.001(3) 0.017(4) 0.024(5) C130 0.063(6) 0.091(7) 0.034(4) 0.007(4) 0.014(4) 0.050(5) F2 0.380(17) 0.161(8) 0.029(3) 0.001(4) -0.007(5) 0.195(11) C72 0.042(4) 0.101(8) 0.063(5) 0.051(6) 0.013(4) -0.002(5) C65 0.053(5) 0.052(5) 0.043(4) -0.004(3) 0.013(3) -0.017(4) C135 0.093(7) 0.069(6) 0.052(5) 0.028(5) 0.043(5) 0.038(6) C134 0.196(16) 0.090(9) 0.106(10) 0.057(8) 0.101(11) 0.099(11) C85 0.078(7) 0.043(5) 0.107(8) 0.027(5) -0.007(6) -0.024(5) C138 0.088(7) 0.069(6) 0.055(5) -0.030(5) 0.028(5) -0.041(5) C76 0.032(4) 0.087(6) 0.055(4) 0.034(5) 0.019(3) 0.010(4) C75 0.043(5) 0.110(8) 0.070(6) 0.034(6) 0.028(4) 0.012(5) C70 0.049(5) 0.079(7) 0.089(7) 0.045(6) 0.005(5) -0.024(5) F5 0.233(13) 0.049(4) 0.43(2) -0.016(8) 0.254(16) -0.019(6) F12 0.079(5) 0.230(13) 0.235(12) -0.155(11) 0.066(7) -0.013(6) C63 0.070(6) 0.077(6) 0.030(4) 0.014(4) -0.008(4) -0.021(5) C121 0.107(11) 0.064(8) 0.22(2) -0.055(10) 0.105(13) -0.010(8) C103 0.034(4) 0.169(12) 0.056(5) 0.002(7) 0.023(4) 0.002(7) C86 0.071(6) 0.042(5) 0.099(8) 0.010(5) -0.031(6) -0.017(5) C10 0.028(4) 0.114(8) 0.039(4) -0.002(4) -0.001(3) -0.008(4) C23 0.116(9) 0.034(4) 0.109(8) -0.023(5) 0.078(8) -0.029(5) C128 0.047(5) 0.137(10) 0.054(5) -0.024(6) 0.014(4) -0.051(6) C131 0.067(7) 0.155(12) 0.045(5) 0.029(6) 0.022(5) 0.067(8) C133 0.099(9) 0.092(9) 0.111(10) 0.041(8) 0.057(8) 0.045(8) C73 0.074(7) 0.133(11) 0.055(5) 0.043(6) 0.032(5) -0.002(7) C126 0.044(5) 0.226(17) 0.057(6) -0.066(8) 0.030(4) -0.060(8) C102 0.039(5) 0.144(11) 0.067(6) -0.028(7) 0.003(4) 0.005(6) C132 0.066(7) 0.113(10) 0.113(10) 0.009(8) 0.021(7) 0.057(8) C122 0.054(6) 0.064(7) 0.185(15) -0.048(8) 0.039(8) -0.005(5) C74 0.059(6) 0.138(11) 0.073(7) 0.038(7) 0.033(5) 0.018(7) C87 0.058(6) 0.048(5) 0.096(7) 0.017(5) -0.036(5) -0.012(4) C115 0.024(3) 0.038(3) 0.028(3) 0.007(3) 0.006(2) 0.006(3) C58 0.026(3) 0.030(3) 0.042(3) 0.014(3) 0.004(3) 0.001(3) C120 0.160(15) 0.048(6) 0.123(11) -0.038(7) 0.094(11) -0.020(8) C127 0.066(7) 0.209(17) 0.068(7) -0.042(9) 0.034(6) -0.088(10) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 O1 2.053(4) . ? Ru1 N1 2.082(6) . ? Ru1 C6 2.215(7) . ? Ru1 C3 2.234(7) . ? Ru1 C5 2.234(7) . ? Ru1 C2 2.241(7) . ? Ru1 C4 2.259(7) . ? Ru1 C1 2.283(6) . ? Ru1 P1 2.3818(15) . ? Ru2 O2 2.057(4) . ? Ru2 N2 2.108(6) . ? Ru2 C50 2.210(7) . ? Ru2 C49 2.211(7) . ? Ru2 C52 2.223(7) . ? Ru2 C53 2.267(7) . ? Ru2 C51 2.281(7) . ? Ru2 C48 2.288(6) . ? Ru2 P2 2.3561(17) . ? Ru3 O3 2.057(4) . ? Ru3 N3 2.111(5) . ? Ru3 C96 2.204(6) . ? Ru3 C97 2.228(6) . ? Ru3 C99 2.232(6) . ? Ru3 C98 2.245(6) . ? Ru3 C100 2.258(7) . ? Ru3 C95 2.282(6) . ? Ru3 P3 2.3799(17) . ? P1 C42 1.813(7) . ? P1 C36 1.819(7) . ? P1 C30 1.832(7) . ? P2 C89 1.817(7) . ? P2 C77 1.823(7) . ? P2 C83 1.824(8) . ? P3 C124 1.815(8) . ? P3 C136 1.839(6) . ? P3 C130 1.855(9) . ? P4 F2 1.522(7) . ? P4 F4 1.531(11) . ? P4 F5 1.538(8) . ? P4 F3 1.562(6) . ? P4 F6 1.569(8) . ? P4 F1 1.608(7) . ? P5 F11 1.541(6) . ? P5 F9 1.549(6) . ? P5 F7 1.563(7) . ? P5 F12 1.572(8) . ? P5 F8 1.578(5) . ? P5 F10 1.583(6) . ? O2 C58 1.320(8) . ? P6 F18 1.555(8) . ? P6 F16 1.556(7) . ? P6 F15 1.576(6) . ? P6 F13 1.580(7) . ? P6 F14 1.587(6) . ? P6 F17 1.630(8) . ? O1 C11 1.306(7) . ? O3 C105 1.299(7) . ? C95 C100 1.398(11) . ? C95 C96 1.418(12) . ? C95 C101 1.527(9) . ? N2 C68 1.291(9) . ? N2 C69 1.500(8) . ? N3 C115 1.302(8) . ? N3 C116 1.493(9) . ? C42 C43 1.402(9) . ? C42 C47 1.409(9) . ? C82 C77 1.387(10) . ? C82 C81 1.393(10) . ? C82 H82 0.95 . ? C11 C12 1.396(9) . ? C11 C20 1.439(9) . ? C129 C128 1.385(13) . ? C129 C124 1.387(13) . ? C129 H129 0.95 . ? C97 C98 1.413(10) . ? C97 C96 1.413(10) . ? C97 H97 0.95 . ? C49 C50 1.401(10) . ? C49 C48 1.428(10) . ? C49 H49 0.95 . ? C36 C41 1.391(10) . ? C36 C37 1.408(10) . ? C98 C99 1.423(10) . ? C98 C104 1.511(9) . ? C100 C99 1.419(10) . ? C100 H100 0.95 . ? C113 C112 1.374(10) . ? C113 C114 1.408(10) . ? C113 H113 0.95 . ? C99 H99 0.95 . ? C96 H96 0.95 . ? C105 C106 1.405(9) . ? C105 C114 1.440(9) . ? C66 C65 1.371(10) . ? C66 C67 1.389(10) . ? C66 H66 0.95 . ? C81 C80 1.374(12) . ? C81 H81 0.95 . ? C4 C3 1.408(12) . ? C4 C5 1.417(11) . ? C4 C10 1.503(10) . ? C114 C109 1.409(9) . ? C77 C78 1.391(10) . ? C20 C15 1.412(8) . ? C20 C19 1.426(9) . ? C106 C115 1.436(10) . ? C106 C107 1.444(8) . ? C43 C44 1.386(10) . ? C43 H43 0.95 . ? C109 C110 1.427(11) . ? C109 C108 1.433(11) . ? C19 C18 1.359(10) . ? C19 H19 0.95 . ? C112 C111 1.399(12) . ? C112 H112 0.95 . ? C3 C2 1.404(11) . ? C3 H3 0.95 . ? C136 C141 1.370(9) . ? C136 C137 1.426(10) . ? C2 C1 1.401(10) . ? C2 H2 0.95 . ? C47 C46 1.368(10) . ? C47 H47 0.95 . ? C1 C6 1.426(10) . ? C1 C7 1.505(10) . ? C5 C6 1.405(10) . ? C5 H5 0.95 . ? C44 C45 1.377(11) . ? C44 H44 0.95 . ? C12 C21 1.426(10) . ? C12 C13 1.440(10) . ? N1 C21 1.296(10) . ? N1 C22 1.500(9) . ? C45 C46 1.402(10) . ? C45 H45 0.95 . ? C110 C111 1.375(12) . ? C110 H110 0.95 . ? C107 C108 1.356(10) . ? C107 H107 0.95 . ? C55 C54 1.540(11) . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C94 C93 1.388(10) . ? C94 C89 1.403(10) . ? C94 H94 0.95 . ? C35 C30 1.376(10) . ? C35 C34 1.392(11) . ? C35 H35 0.95 . ? C46 H46 0.95 . ? C67 C62 1.435(10) . ? C67 C58 1.444(9) . ? C13 C14 1.337(11) . ? C13 H13 0.95 . ? C40 C39 1.389(12) . ? C40 C41 1.397(10) . ? C40 H40 0.95 . ? C89 C90 1.383(10) . ? C17 C16 1.364(13) . ? C17 C18 1.423(11) . ? C17 H17 0.95 . ? C48 C53 1.404(10) . ? C48 C54 1.519(9) . ? C51 C52 1.409(11) . ? C51 C50 1.428(10) . ? C51 C57 1.484(10) . ? C8 C7 1.548(10) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C30 C31 1.399(10) . ? C50 H50 0.95 . ? C32 C33 1.380(12) . ? C32 C31 1.384(10) . ? C32 H32 0.95 . ? C37 C38 1.399(10) . ? C37 H37 0.95 . ? C31 H31 0.95 . ? C83 C84 1.384(11) . ? C83 C88 1.413(13) . ? C90 C91 1.395(11) . ? C90 H90 0.95 . ? C140 C139 1.370(12) . ? C140 C141 1.373(9) . ? C140 H140 0.95 . ? C124 C125 1.406(10) . ? C68 C59 1.426(10) . ? C68 H68 0.95 . ? C118 C123 1.384(14) . ? C118 C119 1.401(13) . ? C118 C116 1.535(10) . ? C18 H18 0.95 . ? C88 C87 1.392(12) . ? C88 H88 0.95 . ? C93 C92 1.369(12) . ? C93 H93 0.95 . ? C104 H10A 0.98 . ? C104 H10B 0.98 . ? C104 H10C 0.98 . ? C6 H6 0.95 . ? C14 C15 1.438(12) . ? C14 H14 0.95 . ? C92 C91 1.400(12) . ? C92 H92 0.95 . ? C28 C27 1.386(13) . ? C28 C29 1.404(11) . ? C28 H28 0.95 . ? C15 C16 1.410(12) . ? C16 H16 0.95 . ? C38 C39 1.360(12) . ? C38 H38 0.95 . ? C116 C117 1.527(9) . ? C116 H116 1 . ? C52 C53 1.428(10) . ? C52 H52 0.95 . ? C71 C76 1.381(12) . ? C71 C72 1.394(12) . ? C71 C69 1.511(14) . ? C54 C56 1.523(11) . ? C54 H54 1 . ? C60 C61 1.344(12) . ? C60 C59 1.447(10) . ? C60 H60 0.95 . ? C7 C9 1.509(11) . ? C7 H7 1 . ? C53 H53 0.95 . ? C59 C58 1.392(10) . ? C69 C70 1.528(13) . ? C69 H69 1 . ? C141 H141 0.95 . ? C108 H108 0.95 . ? C117 H11A 0.98 . ? C117 H11B 0.98 . ? C117 H11C 0.98 . ? C25 C24 1.378(11) . ? C25 C26 1.380(14) . ? C25 H25 0.95 . ? C91 H91 0.95 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C64 C63 1.359(14) . ? C64 C65 1.385(13) . ? C64 H64 0.95 . ? C61 C62 1.423(12) . ? C61 H61 0.95 . ? C139 C138 1.348(14) . ? C139 H139 0.95 . ? C21 H21 0.95 . ? C41 H41 0.95 . ? C80 C79 1.389(14) . ? C80 H80 0.95 . ? C79 C78 1.383(13) . ? C79 H79 0.95 . ? C22 C24 1.516(11) . ? C22 C23 1.535(14) . ? C22 H22 1 . ? C137 C138 1.383(12) . ? C137 H137 0.95 . ? C101 C102 1.463(15) . ? C101 C103 1.536(11) . ? C101 H101 1 . ? C39 H39 0.95 . ? C78 H78 0.95 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C34 C33 1.386(12) . ? C34 H34 0.95 . ? C125 C126 1.362(16) . ? C125 H125 0.95 . ? C33 H33 0.95 . ? C24 C29 1.387(11) . ? C62 C63 1.394(11) . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? C26 C27 1.352(15) . ? C26 H26 0.95 . ? C119 C120 1.394(16) . ? C119 H119 0.95 . ? C111 H111 0.95 . ? C123 C122 1.392(14) . ? C123 H123 0.95 . ? C29 H29 0.95 . ? C84 C85 1.425(14) . ? C84 H84 0.95 . ? C27 H27 0.95 . ? C130 C135 1.396(16) . ? C130 C131 1.394(13) . ? C72 C73 1.389(17) . ? C72 H72 0.95 . ? C65 H65 0.95 . ? C135 C134 1.386(14) . ? C135 H135 0.95 . ? C134 C133 1.287(19) . ? C134 H134 0.95 . ? C85 C86 1.401(16) . ? C85 H85 0.95 . ? C138 H138 0.95 . ? C76 C75 1.391(15) . ? C76 H76 0.95 . ? C75 C74 1.367(15) . ? C75 H75 0.95 . ? C70 H70A 0.98 . ? C70 H70B 0.98 . ? C70 H70C 0.98 . ? C63 H63 0.95 . ? C121 C122 1.36(2) . ? C121 C120 1.43(2) . ? C121 H121 0.95 . ? C103 H10D 0.98 . ? C103 H10E 0.98 . ? C103 H10F 0.98 . ? C86 C87 1.375(14) . ? C86 H86 0.95 . ? C10 H10G 0.98 . ? C10 H10H 0.98 . ? C10 H10I 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C128 C127 1.381(15) . ? C128 H128 0.95 . ? C131 C132 1.472(19) . ? C131 H131 0.95 . ? C133 C132 1.40(2) . ? C133 H133 0.95 . ? C73 C74 1.378(17) . ? C73 H73 0.95 . ? C126 C127 1.36(2) . ? C126 H126 0.95 . ? C102 H10J 0.98 . ? C102 H10K 0.98 . ? C102 H10L 0.98 . ? C132 H132 0.95 . ? C122 H122 0.95 . ? C74 H74 0.95 . ? C87 H87 0.95 . ? C115 H115 0.95 . ? C120 H120 0.95 . ? C127 H127 0.95 . ? 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 O1 Ru1 N1 89.0(2) . . ? O1 Ru1 C6 82.6(2) . . ? N1 Ru1 C6 138.5(2) . . ? O1 Ru1 C3 160.4(2) . . ? N1 Ru1 C3 105.0(3) . . ? C6 Ru1 C3 77.8(3) . . ? O1 Ru1 C5 98.9(2) . . ? N1 Ru1 C5 169.1(2) . . ? C6 Ru1 C5 36.8(3) . . ? C3 Ru1 C5 65.6(3) . . ? O1 Ru1 C2 131.3(2) . . ? N1 Ru1 C2 92.2(3) . . ? C6 Ru1 C2 65.1(3) . . ? C3 Ru1 C2 36.6(3) . . ? C5 Ru1 C2 76.9(3) . . ? O1 Ru1 C4 133.5(2) . . ? N1 Ru1 C4 137.1(3) . . ? C6 Ru1 C4 66.5(3) . . ? C3 Ru1 C4 36.5(3) . . ? C5 Ru1 C4 36.8(3) . . ? C2 Ru1 C4 65.7(3) . . ? O1 Ru1 C1 97.2(2) . . ? N1 Ru1 C1 105.3(2) . . ? C6 Ru1 C1 36.9(3) . . ? C3 Ru1 C1 66.2(3) . . ? C5 Ru1 C1 66.4(3) . . ? C2 Ru1 C1 36.1(3) . . ? C4 Ru1 C1 78.7(3) . . ? O1 Ru1 P1 82.16(12) . . ? N1 Ru1 P1 86.74(16) . . ? C6 Ru1 P1 131.54(19) . . ? C3 Ru1 P1 111.84(19) . . ? C5 Ru1 P1 101.76(19) . . ? C2 Ru1 P1 146.53(19) . . ? C4 Ru1 P1 92.93(18) . . ? C1 Ru1 P1 167.94(19) . . ? O2 Ru2 N2 85.6(2) . . ? O2 Ru2 C50 120.1(2) . . ? N2 Ru2 C50 154.3(2) . . ? O2 Ru2 C49 91.1(2) . . ? N2 Ru2 C49 156.4(2) . . ? C50 Ru2 C49 36.9(3) . . ? O2 Ru2 C52 147.9(2) . . ? N2 Ru2 C52 92.7(3) . . ? C50 Ru2 C52 66.1(3) . . ? C49 Ru2 C52 77.8(3) . . ? O2 Ru2 C53 111.0(2) . . ? N2 Ru2 C53 93.6(3) . . ? C50 Ru2 C53 78.4(3) . . ? C49 Ru2 C53 65.8(3) . . ? C52 Ru2 C53 37.1(3) . . ? O2 Ru2 C51 156.6(2) . . ? N2 Ru2 C51 117.4(3) . . ? C50 Ru2 C51 37.0(3) . . ? C49 Ru2 C51 66.3(3) . . ? C52 Ru2 C51 36.4(3) . . ? C53 Ru2 C51 66.4(3) . . ? O2 Ru2 C48 87.4(2) . . ? N2 Ru2 C48 119.4(2) . . ? C50 Ru2 C48 66.5(3) . . ? C49 Ru2 C48 37.0(3) . . ? C52 Ru2 C48 65.6(2) . . ? C53 Ru2 C48 35.9(2) . . ? C51 Ru2 C48 78.1(3) . . ? O2 Ru2 P2 80.39(12) . . ? N2 Ru2 P2 90.39(17) . . ? C50 Ru2 P2 93.31(18) . . ? C49 Ru2 P2 112.17(18) . . ? C52 Ru2 P2 131.67(19) . . ? C53 Ru2 P2 168.19(19) . . ? C51 Ru2 P2 101.97(18) . . ? C48 Ru2 P2 146.87(19) . . ? O3 Ru3 N3 89.51(19) . . ? O3 Ru3 C96 82.4(2) . . ? N3 Ru3 C96 142.8(2) . . ? O3 Ru3 C97 101.8(2) . . ? N3 Ru3 C97 167.8(2) . . ? C96 Ru3 C97 37.2(2) . . ? O3 Ru3 C99 159.4(2) . . ? N3 Ru3 C99 101.7(2) . . ? C96 Ru3 C99 78.2(3) . . ? C97 Ru3 C99 66.1(3) . . ? O3 Ru3 C98 137.5(2) . . ? N3 Ru3 C98 132.7(2) . . ? C96 Ru3 C98 66.8(2) . . ? C97 Ru3 C98 36.8(3) . . ? C99 Ru3 C98 37.0(3) . . ? O3 Ru3 C100 126.6(2) . . ? N3 Ru3 C100 92.2(2) . . ? C96 Ru3 C100 65.2(3) . . ? C97 Ru3 C100 77.5(3) . . ? C99 Ru3 C100 36.8(2) . . ? C98 Ru3 C100 66.3(2) . . ? O3 Ru3 C95 94.0(2) . . ? N3 Ru3 C95 108.5(2) . . ? C96 Ru3 C95 36.8(3) . . ? C97 Ru3 C95 66.6(3) . . ? C99 Ru3 C95 66.2(2) . . ? C98 Ru3 C95 78.9(2) . . ? C100 Ru3 C95 35.9(3) . . ? O3 Ru3 P3 82.60(13) . . ? N3 Ru3 P3 88.19(15) . . ? C96 Ru3 P3 126.2(2) . . ? C97 Ru3 P3 97.62(18) . . ? C99 Ru3 P3 114.68(18) . . ? C98 Ru3 P3 92.28(16) . . ? C100 Ru3 P3 150.76(19) . . ? C95 Ru3 P3 162.9(2) . . ? C42 P1 C36 106.6(3) . . ? C42 P1 C30 103.7(3) . . ? C36 P1 C30 102.4(3) . . ? C42 P1 Ru1 110.6(2) . . ? C36 P1 Ru1 118.9(2) . . ? C30 P1 Ru1 113.3(2) . . ? C89 P2 C77 104.0(3) . . ? C89 P2 C83 106.2(3) . . ? C77 P2 C83 99.6(4) . . ? C89 P2 Ru2 116.3(2) . . ? C77 P2 Ru2 113.3(2) . . ? C83 P2 Ru2 115.6(2) . . ? C124 P3 C136 99.7(3) . . ? C124 P3 C130 107.9(5) . . ? C136 P3 C130 101.7(4) . . ? C124 P3 Ru3 118.2(3) . . ? C136 P3 Ru3 115.8(2) . . ? C130 P3 Ru3 111.6(3) . . ? F2 P4 F4 169.0(8) . . ? F2 P4 F5 85.4(9) . . ? F4 P4 F5 85.6(9) . . ? F2 P4 F3 92.5(4) . . ? F4 P4 F3 93.3(5) . . ? F5 P4 F3 87.4(5) . . ? F2 P4 F6 96.5(7) . . ? F4 P4 F6 91.8(5) . . ? F5 P4 F6 173.4(6) . . ? F3 P4 F6 98.8(4) . . ? F2 P4 F1 86.3(5) . . ? F4 P4 F1 87.7(6) . . ? F5 P4 F1 90.8(4) . . ? F3 P4 F1 178.0(5) . . ? F6 P4 F1 83.0(4) . . ? F11 P5 F9 92.9(6) . . ? F11 P5 F7 88.3(6) . . ? F9 P5 F7 178.8(6) . . ? F11 P5 F12 177.3(5) . . ? F9 P5 F12 88.2(7) . . ? F7 P5 F12 90.6(7) . . ? F11 P5 F8 91.8(5) . . ? F9 P5 F8 87.8(3) . . ? F7 P5 F8 92.0(4) . . ? F12 P5 F8 90.7(6) . . ? F11 P5 F10 87.7(4) . . ? F9 P5 F10 92.6(4) . . ? F7 P5 F10 87.6(4) . . ? F12 P5 F10 89.8(5) . . ? F8 P5 F10 179.4(4) . . ? C58 O2 Ru2 122.7(4) . . ? F18 P6 F16 94.7(6) . . ? F18 P6 F15 90.1(5) . . ? F16 P6 F15 89.5(4) . . ? F18 P6 F13 90.2(5) . . ? F16 P6 F13 175.0(6) . . ? F15 P6 F13 90.9(4) . . ? F18 P6 F14 90.9(4) . . ? F16 P6 F14 90.9(4) . . ? F15 P6 F14 178.9(5) . . ? F13 P6 F14 88.6(4) . . ? F18 P6 F17 176.5(5) . . ? F16 P6 F17 87.7(5) . . ? F15 P6 F17 92.4(5) . . ? F13 P6 F17 87.3(4) . . ? F14 P6 F17 86.6(4) . . ? C11 O1 Ru1 128.3(4) . . ? C105 O3 Ru3 128.7(4) . . ? C100 C95 C96 117.1(6) . . ? C100 C95 C101 119.3(8) . . ? C96 C95 C101 123.5(7) . . ? C100 C95 Ru3 71.1(4) . . ? C96 C95 Ru3 68.6(3) . . ? C101 C95 Ru3 132.7(4) . . ? C68 N2 C69 118.2(6) . . ? C68 N2 Ru2 121.2(5) . . ? C69 N2 Ru2 120.5(4) . . ? C115 N3 C116 116.5(6) . . ? C115 N3 Ru3 123.2(4) . . ? C116 N3 Ru3 120.2(4) . . ? C43 C42 C47 118.4(6) . . ? C43 C42 P1 123.8(5) . . ? C47 C42 P1 117.8(5) . . ? C77 C82 C81 120.4(6) . . ? C77 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? O1 C11 C12 124.9(6) . . ? O1 C11 C20 115.6(5) . . ? C12 C11 C20 119.5(6) . . ? C128 C129 C124 120.8(8) . . ? C128 C129 H129 119.6 . . ? C124 C129 H129 119.6 . . ? C98 C97 C96 120.2(7) . . ? C98 C97 Ru3 72.2(4) . . ? C96 C97 Ru3 70.5(4) . . ? C98 C97 H97 119.9 . . ? C96 C97 H97 119.9 . . ? Ru3 C97 H97 129.8 . . ? C50 C49 C48 121.5(6) . . ? C50 C49 Ru2 71.5(4) . . ? C48 C49 Ru2 74.4(4) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? Ru2 C49 H49 126.9 . . ? C41 C36 C37 118.8(6) . . ? C41 C36 P1 120.7(5) . . ? C37 C36 P1 120.4(5) . . ? C97 C98 C99 118.3(6) . . ? C97 C98 C104 120.5(7) . . ? C99 C98 C104 121.2(6) . . ? C97 C98 Ru3 70.9(3) . . ? C99 C98 Ru3 71.0(3) . . ? C104 C98 Ru3 132.4(4) . . ? C95 C100 C99 122.0(7) . . ? C95 C100 Ru3 73.0(4) . . ? C99 C100 Ru3 70.6(4) . . ? C95 C100 H100 119 . . ? C99 C100 H100 119 . . ? Ru3 C100 H100 130.1 . . ? C112 C113 C114 120.9(7) . . ? C112 C113 H113 119.6 . . ? C114 C113 H113 119.6 . . ? C100 C99 C98 120.2(7) . . ? C100 C99 Ru3 72.6(4) . . ? C98 C99 Ru3 72.0(4) . . ? C100 C99 H99 119.9 . . ? C98 C99 H99 119.9 . . ? Ru3 C99 H99 127.7 . . ? C97 C96 C95 122.0(7) . . ? C97 C96 Ru3 72.3(4) . . ? C95 C96 Ru3 74.6(4) . . ? C97 C96 H96 119 . . ? C95 C96 H96 119 . . ? Ru3 C96 H96 126 . . ? O3 C105 C106 124.7(6) . . ? O3 C105 C114 116.0(6) . . ? C106 C105 C114 119.3(5) . . ? C65 C66 C67 121.0(7) . . ? C65 C66 H66 119.5 . . ? C67 C66 H66 119.5 . . ? C80 C81 C82 119.8(8) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C3 C4 C5 117.9(6) . . ? C3 C4 C10 122.0(7) . . ? C5 C4 C10 120.0(8) . . ? C3 C4 Ru1 70.8(4) . . ? C5 C4 Ru1 70.6(4) . . ? C10 C4 Ru1 132.5(5) . . ? C113 C114 C109 119.3(6) . . ? C113 C114 C105 120.6(6) . . ? C109 C114 C105 120.1(6) . . ? C82 C77 C78 118.9(7) . . ? C82 C77 P2 121.4(5) . . ? C78 C77 P2 119.6(6) . . ? C15 C20 C19 119.4(6) . . ? C15 C20 C11 120.1(6) . . ? C19 C20 C11 120.5(5) . . ? C105 C106 C115 124.8(5) . . ? C105 C106 C107 119.0(6) . . ? C115 C106 C107 116.2(6) . . ? C44 C43 C42 119.8(6) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C114 C109 C110 118.7(7) . . ? C114 C109 C108 119.4(6) . . ? C110 C109 C108 121.9(6) . . ? C18 C19 C20 120.8(6) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C113 C112 C111 120.4(7) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C2 C3 C4 120.4(7) . . ? C2 C3 Ru1 72.0(4) . . ? C4 C3 Ru1 72.7(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? Ru1 C3 H3 127.6 . . ? C141 C136 C137 117.6(6) . . ? C141 C136 P3 120.7(5) . . ? C137 C136 P3 121.7(5) . . ? C1 C2 C3 123.0(7) . . ? C1 C2 Ru1 73.6(4) . . ? C3 C2 Ru1 71.4(4) . . ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? Ru1 C2 H2 129 . . ? C46 C47 C42 121.2(6) . . ? C46 C47 H47 119.4 . . ? C42 C47 H47 119.4 . . ? C2 C1 C6 116.1(6) . . ? C2 C1 C7 121.2(7) . . ? C6 C1 C7 122.6(6) . . ? C2 C1 Ru1 70.3(4) . . ? C6 C1 Ru1 69.0(4) . . ? C7 C1 Ru1 133.0(5) . . ? C6 C5 C4 120.8(7) . . ? C6 C5 Ru1 70.9(4) . . ? C4 C5 Ru1 72.6(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? Ru1 C5 H5 129.4 . . ? C45 C44 C43 121.3(6) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C11 C12 C21 124.1(6) . . ? C11 C12 C13 118.9(6) . . ? C21 C12 C13 117.0(6) . . ? C21 N1 C22 118.1(6) . . ? C21 N1 Ru1 124.1(4) . . ? C22 N1 Ru1 117.6(5) . . ? C44 C45 C46 119.4(7) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C111 C110 C109 120.5(7) . . ? C111 C110 H110 119.7 . . ? C109 C110 H110 119.7 . . ? C108 C107 C106 121.5(6) . . ? C108 C107 H107 119.3 . . ? C106 C107 H107 119.3 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C93 C94 C89 121.2(7) . . ? C93 C94 H94 119.4 . . ? C89 C94 H94 119.4 . . ? C30 C35 C34 120.6(7) . . ? C30 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C47 C46 C45 119.9(6) . . ? C47 C46 H46 120 . . ? C45 C46 H46 120 . . ? C66 C67 C62 119.1(6) . . ? C66 C67 C58 121.5(6) . . ? C62 C67 C58 119.4(6) . . ? C14 C13 C12 122.0(7) . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C39 C40 C41 119.7(8) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C90 C89 C94 117.7(6) . . ? C90 C89 P2 121.1(5) . . ? C94 C89 P2 121.2(5) . . ? C16 C17 C18 120.5(7) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C53 C48 C49 118.4(6) . . ? C53 C48 C54 123.8(6) . . ? C49 C48 C54 117.8(6) . . ? C53 C48 Ru2 71.2(4) . . ? C49 C48 Ru2 68.6(4) . . ? C54 C48 Ru2 131.2(5) . . ? C52 C51 C50 116.9(6) . . ? C52 C51 C57 121.5(7) . . ? C50 C51 C57 121.5(7) . . ? C52 C51 Ru2 69.5(4) . . ? C50 C51 Ru2 68.8(4) . . ? C57 C51 Ru2 135.9(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C35 C30 C31 118.4(6) . . ? C35 C30 P1 122.8(5) . . ? C31 C30 P1 118.6(5) . . ? C49 C50 C51 120.8(6) . . ? C49 C50 Ru2 71.6(4) . . ? C51 C50 Ru2 74.2(4) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? Ru2 C50 H50 126.6 . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C38 C37 C36 119.4(7) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C32 C31 C30 121.1(7) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C84 C83 C88 118.6(8) . . ? C84 C83 P2 124.3(7) . . ? C88 C83 P2 116.8(6) . . ? C89 C90 C91 121.8(7) . . ? C89 C90 H90 119.1 . . ? C91 C90 H90 119.1 . . ? C139 C140 C141 120.0(7) . . ? C139 C140 H140 120 . . ? C141 C140 H140 120 . . ? C129 C124 C125 119.3(9) . . ? C129 C124 P3 120.7(5) . . ? C125 C124 P3 119.9(8) . . ? N2 C68 C59 128.0(6) . . ? N2 C68 H68 116 . . ? C59 C68 H68 116 . . ? C123 C118 C119 119.2(9) . . ? C123 C118 C116 122.7(8) . . ? C119 C118 C116 118.1(9) . . ? C19 C18 C17 119.6(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C87 C88 C83 121.5(8) . . ? C87 C88 H88 119.2 . . ? C83 C88 H88 119.2 . . ? C92 C93 C94 120.0(7) . . ? C92 C93 H93 120 . . ? C94 C93 H93 120 . . ? C98 C104 H10A 109.5 . . ? C98 C104 H10B 109.5 . . ? H10A C104 H10B 109.5 . . ? C98 C104 H10C 109.5 . . ? H10A C104 H10C 109.5 . . ? H10B C104 H10C 109.5 . . ? C5 C6 C1 121.7(6) . . ? C5 C6 Ru1 72.3(4) . . ? C1 C6 Ru1 74.1(4) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? Ru1 C6 H6 126.4 . . ? C13 C14 C15 120.8(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C93 C92 C91 120.3(7) . . ? C93 C92 H92 119.8 . . ? C91 C92 H92 119.8 . . ? C27 C28 C29 119.0(9) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C16 C15 C20 118.6(7) . . ? C16 C15 C14 122.7(6) . . ? C20 C15 C14 118.7(6) . . ? C17 C16 C15 121.1(7) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C39 C38 C37 121.3(7) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? N3 C116 C117 112.4(5) . . ? N3 C116 C118 111.7(5) . . ? C117 C116 C118 111.1(6) . . ? N3 C116 H116 107.1 . . ? C117 C116 H116 107.1 . . ? C118 C116 H116 107.1 . . ? C51 C52 C53 122.7(6) . . ? C51 C52 Ru2 74.0(4) . . ? C53 C52 Ru2 73.1(4) . . ? C51 C52 H52 118.7 . . ? C53 C52 H52 118.7 . . ? Ru2 C52 H52 126.1 . . ? C76 C71 C72 117.5(9) . . ? C76 C71 C69 123.4(7) . . ? C72 C71 C69 119.1(8) . . ? C48 C54 C56 115.3(6) . . ? C48 C54 C55 105.8(6) . . ? C56 C54 C55 111.2(6) . . ? C48 C54 H54 108.1 . . ? C56 C54 H54 108.1 . . ? C55 C54 H54 108.1 . . ? C61 C60 C59 121.9(7) . . ? C61 C60 H60 119 . . ? C59 C60 H60 119 . . ? C1 C7 C9 114.0(6) . . ? C1 C7 C8 108.6(6) . . ? C9 C7 C8 110.5(6) . . ? C1 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C48 C53 C52 119.4(7) . . ? C48 C53 Ru2 72.8(4) . . ? C52 C53 Ru2 69.8(4) . . ? C48 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? Ru2 C53 H53 129.4 . . ? C58 C59 C68 122.6(6) . . ? C58 C59 C60 118.6(7) . . ? C68 C59 C60 118.5(7) . . ? N2 C69 C71 112.8(7) . . ? N2 C69 C70 114.1(7) . . ? C71 C69 C70 109.7(7) . . ? N2 C69 H69 106.6 . . ? C71 C69 H69 106.6 . . ? C70 C69 H69 106.6 . . ? C140 C141 C136 121.8(7) . . ? C140 C141 H141 119.1 . . ? C136 C141 H141 119.1 . . ? C107 C108 C109 120.5(6) . . ? C107 C108 H108 119.8 . . ? C109 C108 H108 119.8 . . ? C116 C117 H11A 109.5 . . ? C116 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C116 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C24 C25 C26 121.0(9) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C90 C91 C92 118.9(7) . . ? C90 C91 H91 120.6 . . ? C92 C91 H91 120.6 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C63 C64 C65 121.0(7) . . ? C63 C64 H64 119.5 . . ? C65 C64 H64 119.5 . . ? C60 C61 C62 121.2(7) . . ? C60 C61 H61 119.4 . . ? C62 C61 H61 119.4 . . ? C138 C139 C140 120.1(7) . . ? C138 C139 H139 120 . . ? C140 C139 H139 120 . . ? N1 C21 C12 128.9(6) . . ? N1 C21 H21 115.5 . . ? C12 C21 H21 115.5 . . ? C36 C41 C40 120.7(7) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C81 C80 C79 120.6(7) . . ? C81 C80 H80 119.7 . . ? C79 C80 H80 119.7 . . ? C78 C79 C80 119.4(7) . . ? C78 C79 H79 120.3 . . ? C80 C79 H79 120.3 . . ? N1 C22 C24 113.0(6) . . ? N1 C22 C23 113.5(8) . . ? C24 C22 C23 110.1(7) . . ? N1 C22 H22 106.6 . . ? C24 C22 H22 106.6 . . ? C23 C22 H22 106.6 . . ? C138 C137 C136 119.0(8) . . ? C138 C137 H137 120.5 . . ? C136 C137 H137 120.5 . . ? C102 C101 C95 115.4(8) . . ? C102 C101 C103 108.7(9) . . ? C95 C101 C103 107.1(6) . . ? C102 C101 H101 108.5 . . ? C95 C101 H101 108.5 . . ? C103 C101 H101 108.5 . . ? C38 C39 C40 120.1(7) . . ? C38 C39 H39 120 . . ? C40 C39 H39 120 . . ? C79 C78 C77 120.9(8) . . ? C79 C78 H78 119.6 . . ? C77 C78 H78 119.6 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C33 C34 C35 120.7(7) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C126 C125 C124 119.2(11) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C32 C33 C34 119.1(7) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C25 C24 C29 118.8(8) . . ? C25 C24 C22 116.6(8) . . ? C29 C24 C22 124.6(7) . . ? C63 C62 C61 123.4(7) . . ? C63 C62 C67 117.9(8) . . ? C61 C62 C67 118.6(7) . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C27 C26 C25 120.3(8) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C120 C119 C118 120.7(13) . . ? C120 C119 H119 119.7 . . ? C118 C119 H119 119.7 . . ? C110 C111 C112 120.1(7) . . ? C110 C111 H111 119.9 . . ? C112 C111 H111 119.9 . . ? C118 C123 C122 120.4(12) . . ? C118 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C24 C29 C28 120.2(8) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C83 C84 C85 119.2(10) . . ? C83 C84 H84 120.4 . . ? C85 C84 H84 120.4 . . ? C26 C27 C28 120.7(8) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C135 C130 C131 120.7(10) . . ? C135 C130 P3 117.7(7) . . ? C131 C130 P3 121.6(10) . . ? C73 C72 C71 120.9(9) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C66 C65 C64 119.7(8) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C134 C135 C130 118.5(12) . . ? C134 C135 H135 120.7 . . ? C130 C135 H135 120.7 . . ? C133 C134 C135 126.1(16) . . ? C133 C134 H134 116.9 . . ? C135 C134 H134 116.9 . . ? C86 C85 C84 121.4(9) . . ? C86 C85 H85 119.3 . . ? C84 C85 H85 119.3 . . ? C139 C138 C137 121.5(8) . . ? C139 C138 H138 119.3 . . ? C137 C138 H138 119.3 . . ? C71 C76 C75 121.8(8) . . ? C71 C76 H76 119.1 . . ? C75 C76 H76 119.1 . . ? C74 C75 C76 119.7(10) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C64 C63 C62 121.2(8) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C122 C121 C120 119.3(11) . . ? C122 C121 H121 120.3 . . ? C120 C121 H121 120.3 . . ? C101 C103 H10D 109.5 . . ? C101 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C101 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C87 C86 C85 118.5(9) . . ? C87 C86 H86 120.7 . . ? C85 C86 H86 120.7 . . ? C4 C10 H10G 109.5 . . ? C4 C10 H10H 109.5 . . ? H10G C10 H10H 109.5 . . ? C4 C10 H10I 109.5 . . ? H10G C10 H10I 109.5 . . ? H10H C10 H10I 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C127 C128 C129 118.2(11) . . ? C127 C128 H128 120.9 . . ? C129 C128 H128 120.9 . . ? C130 C131 C132 114.9(13) . . ? C130 C131 H131 122.6 . . ? C132 C131 H131 122.6 . . ? C134 C133 C132 115.7(13) . . ? C134 C133 H133 122.2 . . ? C132 C133 H133 122.2 . . ? C74 C73 C72 120.1(9) . . ? C74 C73 H73 120 . . ? C72 C73 H73 120 . . ? C127 C126 C125 121.0(9) . . ? C127 C126 H126 119.5 . . ? C125 C126 H126 119.5 . . ? C101 C102 H10J 109.5 . . ? C101 C102 H10K 109.5 . . ? H10J C102 H10K 109.5 . . ? C101 C102 H10L 109.5 . . ? H10J C102 H10L 109.5 . . ? H10K C102 H10L 109.5 . . ? C133 C132 C131 122.9(11) . . ? C133 C132 H132 118.6 . . ? C131 C132 H132 118.6 . . ? C121 C122 C123 121.3(15) . . ? C121 C122 H122 119.4 . . ? C123 C122 H122 119.4 . . ? C75 C74 C73 120.0(12) . . ? C75 C74 H74 120 . . ? C73 C74 H74 120 . . ? C86 C87 C88 120.6(10) . . ? C86 C87 H87 119.7 . . ? C88 C87 H87 119.7 . . ? N3 C115 C106 128.7(6) . . ? N3 C115 H115 115.6 . . ? C106 C115 H115 115.6 . . ? O2 C58 C59 123.9(6) . . ? O2 C58 C67 116.0(6) . . ? C59 C58 C67 120.0(6) . . ? C119 C120 C121 119.0(13) . . ? C119 C120 H120 120.5 . . ? C121 C120 H120 120.5 . . ? C126 C127 C128 121.5(10) . . ? C126 C127 H127 119.2 . . ? C128 C127 H127 119.2 . . ? 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 C36 P1 C42 C43 -5.3(6) . . . . ? C30 P1 C42 C43 102.4(6) . . . . ? Ru1 P1 C42 C43 -135.9(5) . . . . ? C36 P1 C42 C47 174.5(5) . . . . ? C30 P1 C42 C47 -77.8(5) . . . . ? Ru1 P1 C42 C47 43.9(5) . . . . ? Ru1 O1 C11 C12 8.8(8) . . . . ? Ru1 O1 C11 C20 -171.9(4) . . . . ? C42 P1 C36 C41 -111.5(6) . . . . ? C30 P1 C36 C41 139.9(6) . . . . ? Ru1 P1 C36 C41 14.2(7) . . . . ? C42 P1 C36 C37 71.9(6) . . . . ? C30 P1 C36 C37 -36.7(6) . . . . ? Ru1 P1 C36 C37 -162.4(5) . . . . ? C96 C97 C98 C99 1.0(8) . . . . ? Ru3 C97 C98 C99 54.7(5) . . . . ? C96 C97 C98 C104 177.6(5) . . . . ? Ru3 C97 C98 C104 -128.7(5) . . . . ? C96 C97 C98 Ru3 -53.7(5) . . . . ? C96 C95 C100 C99 -0.5(8) . . . . ? C101 C95 C100 C99 177.8(6) . . . . ? Ru3 C95 C100 C99 -53.1(5) . . . . ? C96 C95 C100 Ru3 52.6(5) . . . . ? C101 C95 C100 Ru3 -129.1(5) . . . . ? C95 C100 C99 C98 -1.9(9) . . . . ? Ru3 C100 C99 C98 -56.0(5) . . . . ? C95 C100 C99 Ru3 54.1(5) . . . . ? C97 C98 C99 C100 1.6(8) . . . . ? C104 C98 C99 C100 -174.9(6) . . . . ? Ru3 C98 C99 C100 56.3(5) . . . . ? C97 C98 C99 Ru3 -54.7(4) . . . . ? C104 C98 C99 Ru3 128.7(5) . . . . ? C98 C97 C96 C95 -3.6(9) . . . . ? Ru3 C97 C96 C95 -58.1(5) . . . . ? C98 C97 C96 Ru3 54.5(5) . . . . ? C100 C95 C96 C97 3.2(8) . . . . ? C101 C95 C96 C97 -175.0(6) . . . . ? Ru3 C95 C96 C97 57.0(5) . . . . ? C100 C95 C96 Ru3 -53.8(5) . . . . ? C101 C95 C96 Ru3 127.9(6) . . . . ? Ru3 O3 C105 C106 7.8(9) . . . . ? Ru3 O3 C105 C114 -172.2(4) . . . . ? C77 C82 C81 C80 0.9(10) . . . . ? C112 C113 C114 C109 -0.6(11) . . . . ? C112 C113 C114 C105 -179.5(7) . . . . ? O3 C105 C114 C113 4.3(9) . . . . ? C106 C105 C114 C113 -175.7(6) . . . . ? O3 C105 C114 C109 -174.6(6) . . . . ? C106 C105 C114 C109 5.4(9) . . . . ? C81 C82 C77 C78 -3.2(10) . . . . ? C81 C82 C77 P2 177.0(5) . . . . ? C89 P2 C77 C82 102.1(6) . . . . ? C83 P2 C77 C82 -148.5(6) . . . . ? Ru2 P2 C77 C82 -25.1(6) . . . . ? C89 P2 C77 C78 -77.8(6) . . . . ? C83 P2 C77 C78 31.7(6) . . . . ? Ru2 P2 C77 C78 155.0(5) . . . . ? O1 C11 C20 C15 -176.7(5) . . . . ? C12 C11 C20 C15 2.7(9) . . . . ? O1 C11 C20 C19 5.3(8) . . . . ? C12 C11 C20 C19 -175.3(6) . . . . ? O3 C105 C106 C115 -7.0(10) . . . . ? C114 C105 C106 C115 173.1(6) . . . . ? O3 C105 C106 C107 173.7(6) . . . . ? C114 C105 C106 C107 -6.2(9) . . . . ? C47 C42 C43 C44 0.9(9) . . . . ? P1 C42 C43 C44 -179.2(5) . . . . ? C113 C114 C109 C110 -0.8(10) . . . . ? C105 C114 C109 C110 178.2(6) . . . . ? C113 C114 C109 C108 179.9(7) . . . . ? C105 C114 C109 C108 -1.2(10) . . . . ? C15 C20 C19 C18 0.2(10) . . . . ? C11 C20 C19 C18 178.3(7) . . . . ? C114 C113 C112 C111 0.5(12) . . . . ? C5 C4 C3 C2 1.6(11) . . . . ? C10 C4 C3 C2 -175.3(7) . . . . ? Ru1 C4 C3 C2 56.0(6) . . . . ? C5 C4 C3 Ru1 -54.4(6) . . . . ? C10 C4 C3 Ru1 128.7(7) . . . . ? C124 P3 C136 C141 -38.5(6) . . . . ? C130 P3 C136 C141 -149.3(6) . . . . ? Ru3 P3 C136 C141 89.5(5) . . . . ? C124 P3 C136 C137 144.1(7) . . . . ? C130 P3 C136 C137 33.3(7) . . . . ? Ru3 P3 C136 C137 -87.9(6) . . . . ? C4 C3 C2 C1 -1.3(11) . . . . ? Ru1 C3 C2 C1 55.1(7) . . . . ? C4 C3 C2 Ru1 -56.4(6) . . . . ? C43 C42 C47 C46 -1.7(9) . . . . ? P1 C42 C47 C46 178.4(5) . . . . ? C3 C2 C1 C6 -0.9(10) . . . . ? Ru1 C2 C1 C6 53.2(5) . . . . ? C3 C2 C1 C7 176.8(7) . . . . ? Ru1 C2 C1 C7 -129.1(6) . . . . ? C3 C2 C1 Ru1 -54.1(6) . . . . ? C3 C4 C5 C6 0.4(10) . . . . ? C10 C4 C5 C6 177.3(6) . . . . ? Ru1 C4 C5 C6 -54.1(6) . . . . ? C3 C4 C5 Ru1 54.5(6) . . . . ? C10 C4 C5 Ru1 -128.6(6) . . . . ? C42 C43 C44 C45 0.7(11) . . . . ? O1 C11 C12 C21 -1.5(10) . . . . ? C20 C11 C12 C21 179.2(6) . . . . ? O1 C11 C12 C13 176.2(5) . . . . ? C20 C11 C12 C13 -3.0(9) . . . . ? C43 C44 C45 C46 -1.6(11) . . . . ? C114 C109 C110 C111 2.2(11) . . . . ? C108 C109 C110 C111 -178.5(7) . . . . ? C105 C106 C107 C108 3.1(10) . . . . ? C115 C106 C107 C108 -176.3(6) . . . . ? C42 C47 C46 C45 0.9(10) . . . . ? C44 C45 C46 C47 0.8(11) . . . . ? C65 C66 C67 C62 1.0(11) . . . . ? C65 C66 C67 C58 179.7(7) . . . . ? C11 C12 C13 C14 1.7(9) . . . . ? C21 C12 C13 C14 179.6(6) . . . . ? C93 C94 C89 C90 -0.9(11) . . . . ? C93 C94 C89 P2 -178.1(6) . . . . ? C77 P2 C89 C90 165.2(6) . . . . ? C83 P2 C89 C90 60.7(7) . . . . ? Ru2 P2 C89 C90 -69.4(6) . . . . ? C77 P2 C89 C94 -17.7(7) . . . . ? C83 P2 C89 C94 -122.3(6) . . . . ? Ru2 P2 C89 C94 107.6(6) . . . . ? C50 C49 C48 C53 3.3(10) . . . . ? Ru2 C49 C48 C53 -52.8(6) . . . . ? C50 C49 C48 C54 -177.5(6) . . . . ? Ru2 C49 C48 C54 126.4(6) . . . . ? C50 C49 C48 Ru2 56.1(6) . . . . ? C34 C35 C30 C31 -1.0(10) . . . . ? C34 C35 C30 P1 172.9(5) . . . . ? C42 P1 C30 C35 28.5(6) . . . . ? C36 P1 C30 C35 139.3(6) . . . . ? Ru1 P1 C30 C35 -91.4(6) . . . . ? C42 P1 C30 C31 -157.5(5) . . . . ? C36 P1 C30 C31 -46.7(6) . . . . ? Ru1 P1 C30 C31 82.6(5) . . . . ? C48 C49 C50 C51 0.3(10) . . . . ? Ru2 C49 C50 C51 57.8(6) . . . . ? C48 C49 C50 Ru2 -57.5(6) . . . . ? C52 C51 C50 C49 -4.7(10) . . . . ? C57 C51 C50 C49 171.7(7) . . . . ? Ru2 C51 C50 C49 -56.6(6) . . . . ? C52 C51 C50 Ru2 51.8(6) . . . . ? C57 C51 C50 Ru2 -131.7(7) . . . . ? C41 C36 C37 C38 0.4(10) . . . . ? P1 C36 C37 C38 177.1(6) . . . . ? C33 C32 C31 C30 -0.8(10) . . . . ? C35 C30 C31 C32 1.6(9) . . . . ? P1 C30 C31 C32 -172.6(5) . . . . ? C89 P2 C83 C84 -6.3(10) . . . . ? C77 P2 C83 C84 -114.0(9) . . . . ? Ru2 P2 C83 C84 124.3(8) . . . . ? C89 P2 C83 C88 167.5(7) . . . . ? C77 P2 C83 C88 59.8(7) . . . . ? Ru2 P2 C83 C88 -61.9(8) . . . . ? C94 C89 C90 C91 1.5(11) . . . . ? P2 C89 C90 C91 178.6(6) . . . . ? C128 C129 C124 C125 0.6(14) . . . . ? C128 C129 C124 P3 -174.3(8) . . . . ? C136 P3 C124 C129 132.7(7) . . . . ? C130 P3 C124 C129 -121.4(7) . . . . ? Ru3 P3 C124 C129 6.4(8) . . . . ? C136 P3 C124 C125 -42.1(9) . . . . ? C130 P3 C124 C125 63.8(8) . . . . ? Ru3 P3 C124 C125 -168.4(7) . . . . ? C69 N2 C68 C59 172.4(8) . . . . ? Ru2 N2 C68 C59 -10.6(12) . . . . ? C20 C19 C18 C17 2.5(12) . . . . ? C16 C17 C18 C19 -3.5(13) . . . . ? C84 C83 C88 C87 0.5(15) . . . . ? P2 C83 C88 C87 -173.6(8) . . . . ? C89 C94 C93 C92 -0.8(12) . . . . ? C4 C5 C6 C1 -2.8(10) . . . . ? Ru1 C5 C6 C1 -57.7(6) . . . . ? C4 C5 C6 Ru1 54.9(6) . . . . ? C2 C1 C6 C5 3.0(10) . . . . ? C7 C1 C6 C5 -174.7(6) . . . . ? Ru1 C1 C6 C5 56.8(6) . . . . ? C2 C1 C6 Ru1 -53.8(5) . . . . ? C7 C1 C6 Ru1 128.5(6) . . . . ? C12 C13 C14 C15 0.2(10) . . . . ? C94 C93 C92 C91 2.1(12) . . . . ? C19 C20 C15 C16 -1.9(9) . . . . ? C11 C20 C15 C16 -179.9(6) . . . . ? C19 C20 C15 C14 177.2(6) . . . . ? C11 C20 C15 C14 -0.9(9) . . . . ? C13 C14 C15 C16 178.4(7) . . . . ? C13 C14 C15 C20 -0.6(9) . . . . ? C18 C17 C16 C15 1.9(13) . . . . ? C20 C15 C16 C17 0.8(11) . . . . ? C14 C15 C16 C17 -178.2(8) . . . . ? C36 C37 C38 C39 -0.7(11) . . . . ? C115 N3 C116 C117 -48.2(8) . . . . ? Ru3 N3 C116 C117 134.7(5) . . . . ? C115 N3 C116 C118 77.5(7) . . . . ? Ru3 N3 C116 C118 -99.6(6) . . . . ? C123 C118 C116 N3 -62.7(10) . . . . ? C119 C118 C116 N3 121.3(7) . . . . ? C123 C118 C116 C117 63.6(10) . . . . ? C119 C118 C116 C117 -112.4(8) . . . . ? C50 C51 C52 C53 5.7(11) . . . . ? C57 C51 C52 C53 -170.7(7) . . . . ? Ru2 C51 C52 C53 57.2(7) . . . . ? C50 C51 C52 Ru2 -51.5(6) . . . . ? C57 C51 C52 Ru2 132.1(7) . . . . ? C53 C48 C54 C56 16.8(10) . . . . ? C49 C48 C54 C56 -162.4(6) . . . . ? Ru2 C48 C54 C56 -77.4(8) . . . . ? C53 C48 C54 C55 -106.6(8) . . . . ? C49 C48 C54 C55 74.2(8) . . . . ? Ru2 C48 C54 C55 159.3(5) . . . . ? C2 C1 C7 C9 127.6(8) . . . . ? C6 C1 C7 C9 -54.8(10) . . . . ? Ru1 C1 C7 C9 36.0(10) . . . . ? C2 C1 C7 C8 -108.7(8) . . . . ? C6 C1 C7 C8 68.9(9) . . . . ? Ru1 C1 C7 C8 159.7(6) . . . . ? C49 C48 C53 C52 -2.4(11) . . . . ? C54 C48 C53 C52 178.5(7) . . . . ? Ru2 C48 C53 C52 -53.9(6) . . . . ? C49 C48 C53 Ru2 51.6(6) . . . . ? C54 C48 C53 Ru2 -127.6(7) . . . . ? C51 C52 C53 C48 -2.2(12) . . . . ? Ru2 C52 C53 C48 55.4(6) . . . . ? C51 C52 C53 Ru2 -57.6(7) . . . . ? N2 C68 C59 C58 -17.1(14) . . . . ? N2 C68 C59 C60 169.0(9) . . . . ? C61 C60 C59 C58 0.7(14) . . . . ? C61 C60 C59 C68 174.8(9) . . . . ? C68 N2 C69 C71 96.3(9) . . . . ? Ru2 N2 C69 C71 -80.7(7) . . . . ? C68 N2 C69 C70 -29.7(11) . . . . ? Ru2 N2 C69 C70 153.3(6) . . . . ? C76 C71 C69 N2 -45.2(10) . . . . ? C72 C71 C69 N2 138.5(8) . . . . ? C76 C71 C69 C70 83.1(10) . . . . ? C72 C71 C69 C70 -93.1(9) . . . . ? C139 C140 C141 C136 1.4(10) . . . . ? C137 C136 C141 C140 -4.4(10) . . . . ? P3 C136 C141 C140 178.1(5) . . . . ? C106 C107 C108 C109 1.2(11) . . . . ? C114 C109 C108 C107 -2.1(11) . . . . ? C110 C109 C108 C107 178.6(7) . . . . ? C89 C90 C91 C92 -0.3(12) . . . . ? C93 C92 C91 C90 -1.5(12) . . . . ? C59 C60 C61 C62 -3.0(16) . . . . ? C141 C140 C139 C138 2.2(12) . . . . ? C22 N1 C21 C12 -176.8(6) . . . . ? Ru1 N1 C21 C12 -1.8(10) . . . . ? C11 C12 C21 N1 -2.1(11) . . . . ? C13 C12 C21 N1 -179.9(6) . . . . ? C37 C36 C41 C40 0.3(11) . . . . ? P1 C36 C41 C40 -176.4(6) . . . . ? C39 C40 C41 C36 -0.6(12) . . . . ? C82 C81 C80 C79 1.7(12) . . . . ? C81 C80 C79 C78 -1.8(13) . . . . ? C21 N1 C22 C24 80.6(9) . . . . ? Ru1 N1 C22 C24 -94.7(7) . . . . ? C21 N1 C22 C23 -45.6(10) . . . . ? Ru1 N1 C22 C23 139.0(7) . . . . ? C141 C136 C137 C138 4.1(12) . . . . ? P3 C136 C137 C138 -178.5(7) . . . . ? C100 C95 C101 C102 142.6(9) . . . . ? C96 C95 C101 C102 -39.2(11) . . . . ? Ru3 C95 C101 C102 51.8(12) . . . . ? C100 C95 C101 C103 -96.2(10) . . . . ? C96 C95 C101 C103 82.0(10) . . . . ? Ru3 C95 C101 C103 173.0(8) . . . . ? C37 C38 C39 C40 0.4(12) . . . . ? C41 C40 C39 C38 0.2(12) . . . . ? C80 C79 C78 C77 -0.6(13) . . . . ? C82 C77 C78 C79 3.1(11) . . . . ? P2 C77 C78 C79 -177.1(6) . . . . ? C30 C35 C34 C33 -0.3(11) . . . . ? C129 C124 C125 C126 -1.1(16) . . . . ? P3 C124 C125 C126 173.8(10) . . . . ? C31 C32 C33 C34 -0.5(11) . . . . ? C35 C34 C33 C32 1.1(11) . . . . ? C26 C25 C24 C29 1.4(13) . . . . ? C26 C25 C24 C22 -178.7(8) . . . . ? N1 C22 C24 C25 153.0(8) . . . . ? C23 C22 C24 C25 -78.9(10) . . . . ? N1 C22 C24 C29 -27.0(12) . . . . ? C23 C22 C24 C29 101.0(10) . . . . ? C60 C61 C62 C63 -177.4(10) . . . . ? C60 C61 C62 C67 1.0(15) . . . . ? C66 C67 C62 C63 0.3(12) . . . . ? C58 C67 C62 C63 -178.4(8) . . . . ? C66 C67 C62 C61 -178.2(8) . . . . ? C58 C67 C62 C61 3.1(12) . . . . ? C24 C25 C26 C27 0.1(14) . . . . ? C123 C118 C119 C120 4.6(13) . . . . ? C116 C118 C119 C120 -179.3(8) . . . . ? C109 C110 C111 C112 -2.2(12) . . . . ? C113 C112 C111 C110 0.9(13) . . . . ? C119 C118 C123 C122 -2.6(15) . . . . ? C116 C118 C123 C122 -178.6(9) . . . . ? C25 C24 C29 C28 -1.5(12) . . . . ? C22 C24 C29 C28 178.5(8) . . . . ? C27 C28 C29 C24 0.3(12) . . . . ? C88 C83 C84 C85 1.9(15) . . . . ? P2 C83 C84 C85 175.6(8) . . . . ? C25 C26 C27 C28 -1.3(14) . . . . ? C29 C28 C27 C26 1.2(13) . . . . ? C124 P3 C130 C135 176.2(7) . . . . ? C136 P3 C130 C135 -79.3(7) . . . . ? Ru3 P3 C130 C135 44.8(8) . . . . ? C124 P3 C130 C131 -4.2(9) . . . . ? C136 P3 C130 C131 100.2(8) . . . . ? Ru3 P3 C130 C131 -135.7(7) . . . . ? C76 C71 C72 C73 -0.5(14) . . . . ? C69 C71 C72 C73 176.0(9) . . . . ? C67 C66 C65 C64 -1.8(12) . . . . ? C63 C64 C65 C66 1.3(14) . . . . ? C131 C130 C135 C134 -0.2(15) . . . . ? P3 C130 C135 C134 179.4(9) . . . . ? C130 C135 C134 C133 -8(2) . . . . ? C83 C84 C85 C86 -5.1(18) . . . . ? C140 C139 C138 C137 -2.5(16) . . . . ? C136 C137 C138 C139 -0.7(16) . . . . ? C72 C71 C76 C75 -1.2(14) . . . . ? C69 C71 C76 C75 -177.5(9) . . . . ? C71 C76 C75 C74 2.2(16) . . . . ? C65 C64 C63 C62 0.0(16) . . . . ? C61 C62 C63 C64 177.6(10) . . . . ? C67 C62 C63 C64 -0.8(14) . . . . ? C84 C85 C86 C87 5.6(19) . . . . ? C124 C129 C128 C127 1.3(17) . . . . ? C135 C130 C131 C132 1.0(15) . . . . ? P3 C130 C131 C132 -178.5(8) . . . . ? C135 C134 C133 C132 13(3) . . . . ? C71 C72 C73 C74 1.2(17) . . . . ? C124 C125 C126 C127 0(2) . . . . ? C134 C133 C132 C131 -12(2) . . . . ? C130 C131 C132 C133 4.9(18) . . . . ? C120 C121 C122 C123 2(2) . . . . ? C118 C123 C122 C121 -0.8(19) . . . . ? C76 C75 C74 C73 -1.5(19) . . . . ? C72 C73 C74 C75 -0.2(19) . . . . ? C85 C86 C87 C88 -3.0(19) . . . . ? C83 C88 C87 C86 0.0(17) . . . . ? C116 N3 C115 C106 -173.6(6) . . . . ? Ru3 N3 C115 C106 3.4(9) . . . . ? C105 C106 C115 N3 0.8(11) . . . . ? C107 C106 C115 N3 -179.8(6) . . . . ? Ru2 O2 C58 C59 29.9(9) . . . . ? Ru2 O2 C58 C67 -152.9(5) . . . . ? C68 C59 C58 O2 6.7(12) . . . . ? C60 C59 C58 O2 -179.4(7) . . . . ? C68 C59 C58 C67 -170.3(7) . . . . ? C60 C59 C58 C67 3.5(11) . . . . ? C66 C67 C58 O2 -1.3(10) . . . . ? C62 C67 C58 O2 177.3(7) . . . . ? C66 C67 C58 C59 176.0(7) . . . . ? C62 C67 C58 C59 -5.4(11) . . . . ? C118 C119 C120 C121 -3.1(17) . . . . ? C122 C121 C120 C119 0(2) . . . . ? C125 C126 C127 C128 2(2) . . . . ? C129 C128 C127 C126 -3(2) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.098 0.002 0.117 164 16 ' ' 2 0.079 0.502 0.883 164 16 ' ' _platon_squeeze_details ; ; data_1519532 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C47 H45 N O P Ru, F6 P, (C H2 Cl2)2' _chemical_formula_sum 'C49 H49 Cl4 F6 N O P2 Ru' _chemical_formula_weight 1086.7 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration rm #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.429(3) _cell_length_b 16.431(5) _cell_length_c 14.060(5) _cell_angle_alpha 90 _cell_angle_beta 98.590(14) _cell_angle_gamma 90 _cell_volume 2382.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20559 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7749 _exptl_absorpt_correction_T_max 1.0000 _shelx_estimated_absorpt_T_min 0.722 _shelx_estimated_absorpt_T_max 0.876 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed x-ray tube' _diffrn_detector 'curved image-plate' _diffrn_detector_area_resol_mean 10 _diffrn_measurement_device 'quarter \C-circle diffractometer' _diffrn_measurement_device_type 'Rigaku R-Axis Rapid' _diffrn_measurement_method 'phi or omega oscillation scans' _diffrn_orient_matrix_type fs_process _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_number 18634 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_full 24.999 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _reflns_Friedel_fraction_full 0.977 _reflns_Friedel_fraction_max 0.977 _reflns_Friedel_coverage 0.907 _reflns_number_total 8291 _reflns_number_gt 7733 _reflns_threshold_expression 'I > 2\s(I)' _computing_structure_solution 'SIR97 (Altomare et al, 1999)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+3.6529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0062(16) _refine_ls_number_reflns 8291 _refine_ls_number_parameters 578 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.06 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details ; Flack x determined using 3305 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.029(14) _refine_diff_density_max 2.326 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.11 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0 '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 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45483(5) 0.19406(4) 0.12543(4) 0.0259(2) Uani 1 1 d . . . . . P1 P 0.6317(2) 0.28478(14) 0.16836(15) 0.0301(5) Uani 1 1 d . . . . . P2 P 0.1943(2) 0.38784(17) 0.81579(18) 0.0410(6) Uani 1 1 d . . . . . Cl1 Cl -0.1093(5) 0.2028(4) 0.6079(3) 0.1088(14) Uani 1 1 d . . . . . F4 F 0.2550(7) 0.4635(4) 0.7669(5) 0.0640(18) Uani 1 1 d . . . . . C43 C 0.7925(9) 0.1618(7) 0.2546(7) 0.036(2) Uani 1 1 d . . . . . H43 H 0.737247 0.126933 0.212954 0.043 Uiso 1 1 calc R U . . . F2 F 0.1356(7) 0.3114(5) 0.8656(6) 0.074(2) Uani 1 1 d . . . . . F5 F 0.0907(9) 0.3783(7) 0.7225(6) 0.095(3) Uani 1 1 d . . . . . O1 O 0.3427(6) 0.2969(4) 0.1199(4) 0.0325(14) Uani 1 1 d . . . . . F6 F 0.2961(9) 0.4018(6) 0.9095(6) 0.096(3) Uani 1 1 d . . . . . C5 C 0.4972(10) 0.0649(5) 0.0966(6) 0.037(2) Uani 1 1 d . . . . . H5 H 0.547126 0.02777 0.138766 0.045 Uiso 1 1 calc R U . . . N1 N 0.4455(6) 0.1873(6) 0.2729(4) 0.0313(15) Uani 1 1 d . . . . . C24 C 0.4137(9) 0.0464(6) 0.3405(6) 0.035(2) Uani 1 1 d . . . . . C36 C 0.7011(9) 0.3209(6) 0.0636(7) 0.037(2) Uani 1 1 d . . . . . C30 C 0.5889(9) 0.3772(6) 0.2281(6) 0.036(2) Uani 1 1 d . . . . . C22 C 0.5079(9) 0.1168(6) 0.3293(7) 0.038(2) Uani 1 1 d . . . . . H22 H 0.574521 0.094687 0.29194 0.045 Uiso 1 1 calc R U . . . C20 C 0.2476(9) 0.3572(6) 0.3522(7) 0.035(2) Uani 1 1 d . . . . . C11 C 0.3060(8) 0.3075(5) 0.2848(6) 0.0311(18) Uani 1 1 d . . . . . F1 F 0.0994(10) 0.4461(6) 0.8581(7) 0.096(3) Uani 1 1 d . . . . . C21 C 0.3807(8) 0.2378(6) 0.3185(6) 0.0328(19) Uani 1 1 d . . . . . H21 H 0.383418 0.226452 0.385021 0.039 Uiso 1 1 calc R U . . . Cl2 Cl -0.2568(10) 0.1788(6) 0.7577(7) 0.205(5) Uani 1 1 d . . . . . C2 C 0.3503(10) 0.1776(7) -0.0208(7) 0.052(3) Uani 1 1 d . . . . . H2 H 0.302602 0.218647 -0.058338 0.062 Uiso 1 1 calc R U . . . C1 C 0.2864(9) 0.1280(7) 0.0399(8) 0.046(2) Uani 1 1 d . . . . . F3 F 0.2920(9) 0.3309(5) 0.7728(9) 0.103(3) Uani 1 1 d . . . . . C48 C 0.8559(9) 0.2957(7) 0.3091(7) 0.044(2) Uani 1 1 d . . . . . H48 H 0.844821 0.353006 0.304808 0.053 Uiso 1 1 calc R U . . . C12 C 0.2873(8) 0.3300(5) 0.1867(6) 0.0307(18) Uani 1 1 d . . . . . C31 C 0.5898(9) 0.3790(6) 0.3272(6) 0.037(2) Uani 1 1 d . . . . . H31 H 0.619386 0.332846 0.364954 0.045 Uiso 1 1 calc R U . . . C3 C 0.4788(10) 0.1677(6) -0.0265(6) 0.041(2) Uani 1 1 d . . . . . H3 H 0.516676 0.199431 -0.071512 0.049 Uiso 1 1 calc R U . . . C23 C 0.5805(10) 0.1413(8) 0.4283(7) 0.052(3) Uani 1 1 d . . . . . H23A H 0.619073 0.09278 0.461728 0.078 Uiso 1 1 calc R U . . . H23B H 0.649028 0.180268 0.420109 0.078 Uiso 1 1 calc R U . . . H23C H 0.519589 0.166316 0.466408 0.078 Uiso 1 1 calc R U . . . C4 C 0.5584(8) 0.1113(6) 0.0330(7) 0.036(2) Uani 1 1 d . . . . . C42 C 0.7692(9) 0.2460(7) 0.2505(7) 0.035(2) Uani 1 1 d . . . . . C25 C 0.2839(11) 0.0576(7) 0.3494(10) 0.055(3) Uani 1 1 d . . . . . H25 H 0.247345 0.11069 0.346027 0.067 Uiso 1 1 calc R U . . . C41 C 0.8332(10) 0.3232(7) 0.0621(7) 0.046(2) Uani 1 1 d . . . . . H41 H 0.891644 0.306516 0.116953 0.055 Uiso 1 1 calc R U . . . C15 C 0.1624(11) 0.4203(7) 0.3193(8) 0.048(3) Uani 1 1 d . . . . . C6 C 0.3639(12) 0.0721(7) 0.0995(8) 0.048(3) Uani 1 1 d . . . . . H6 H 0.324879 0.038757 0.142329 0.057 Uiso 1 1 calc R U . . . C44 C 0.6987(10) 0.0995(8) 0.0186(9) 0.056(3) Uani 1 1 d . . . . . H44A H 0.720358 0.138579 -0.02915 0.083 Uiso 1 1 calc R U . . . H44B H 0.755541 0.108349 0.079826 0.083 Uiso 1 1 calc R U . . . H44C H 0.710629 0.044002 -0.003989 0.083 Uiso 1 1 calc R U . . . C19 C 0.2750(10) 0.3431(7) 0.4540(7) 0.049(3) Uani 1 1 d . . . . . H19 H 0.331406 0.300497 0.47953 0.059 Uiso 1 1 calc R U . . . C46 C 0.9747(9) 0.1805(10) 0.3753(8) 0.060(4) Uani 1 1 d . . . . . H46 H 1.045245 0.158926 0.418428 0.072 Uiso 1 1 calc R U . . . C13 C 0.1987(10) 0.3949(6) 0.1549(7) 0.043(2) Uani 1 1 d . . . . . H13 H 0.182043 0.407942 0.088359 0.052 Uiso 1 1 calc R U . . . C37 C 0.6154(9) 0.3453(6) -0.0181(6) 0.0352(19) Uani 1 1 d . . . . . H37 H 0.524559 0.34465 -0.016874 0.042 Uiso 1 1 calc R U . . . C29 C 0.4636(12) -0.0309(7) 0.3468(7) 0.049(3) Uani 1 1 d . . . . . H29 H 0.551927 -0.039672 0.340317 0.059 Uiso 1 1 calc R U . . . C32 C 0.5477(12) 0.4478(8) 0.3716(7) 0.055(3) Uani 1 1 d . . . . . H32 H 0.556382 0.450025 0.439787 0.066 Uiso 1 1 calc R U . . . C47 C 0.9562(10) 0.2649(9) 0.3723(8) 0.054(3) Uani 1 1 d . . . . . H47 H 1.012064 0.299905 0.413363 0.065 Uiso 1 1 calc R U . . . C45 C 0.8952(9) 0.1276(8) 0.3184(8) 0.046(3) Uani 1 1 d . . . . . H45 H 0.908817 0.070415 0.321998 0.055 Uiso 1 1 calc R U . . . C38 C 0.6623(12) 0.3704(6) -0.1002(7) 0.050(3) Uani 1 1 d . . . . . H38 H 0.604246 0.386614 -0.155497 0.06 Uiso 1 1 calc R U . . . C18 C 0.2161(13) 0.3940(9) 0.5143(9) 0.069(4) Uani 1 1 d . . . . . H18 H 0.235266 0.386133 0.581861 0.083 Uiso 1 1 calc R U . . . C40 C 0.8804(10) 0.3499(8) -0.0194(8) 0.054(3) Uani 1 1 d . . . . . H40 H 0.971354 0.353323 -0.01924 0.065 Uiso 1 1 calc R U . . . C26 C 0.2089(13) -0.0090(8) 0.3630(10) 0.064(3) Uani 1 1 d . . . . . H26 H 0.119228 -0.001194 0.365698 0.077 Uiso 1 1 calc R U . . . C35 C 0.5404(13) 0.4446(7) 0.1757(8) 0.055(3) Uani 1 1 d . . . . . H35 H 0.538287 0.444991 0.107907 0.066 Uiso 1 1 calc R U . . . C28 C 0.3849(14) -0.0968(7) 0.3628(8) 0.061(3) Uani 1 1 d . . . . . H28 H 0.420347 -0.150173 0.366722 0.073 Uiso 1 1 calc R U . . . C14 C 0.1382(12) 0.4379(7) 0.2175(9) 0.056(3) Uani 1 1 d . . . . . H14 H 0.079495 0.480116 0.194291 0.067 Uiso 1 1 calc R U . . . C33 C 0.4951(16) 0.5109(8) 0.3191(9) 0.068(4) Uani 1 1 d . . . . . H33 H 0.458138 0.554931 0.349376 0.082 Uiso 1 1 calc R U . . . C39 C 0.7966(12) 0.3715(7) -0.1010(8) 0.054(3) Uani 1 1 d . . . . . H39 H 0.82993 0.387134 -0.157592 0.065 Uiso 1 1 calc R U . . . C17 C 0.1326(15) 0.4543(9) 0.4803(11) 0.075(4) Uani 1 1 d . . . . . H17 H 0.093974 0.486779 0.52419 0.09 Uiso 1 1 calc R U . . . C27 C 0.2582(13) -0.0857(7) 0.3727(8) 0.057(3) Uani 1 1 d . . . . . H27 H 0.205666 -0.130236 0.386143 0.069 Uiso 1 1 calc R U . . . C34 C 0.4948(17) 0.5115(8) 0.2203(9) 0.075(4) Uani 1 1 d . . . . . H34 H 0.46334 0.557675 0.183408 0.09 Uiso 1 1 calc R U . . . C7 C 0.1428(11) 0.1435(11) 0.0358(11) 0.081(5) Uani 1 1 d . . . . . H7 H 0.124981 0.200314 0.011921 0.097 Uiso 1 1 calc R U . . . C9 C 0.0948(12) 0.1361(13) 0.1272(11) 0.094(6) Uani 1 1 d . . . . . H9A H 0.00145 0.147118 0.117849 0.141 Uiso 1 1 calc R U . . . H9B H 0.11105 0.080869 0.152348 0.141 Uiso 1 1 calc R U . . . H9C H 0.139647 0.175421 0.173009 0.141 Uiso 1 1 calc R U . . . C8 C 0.0714(12) 0.0845(15) -0.0407(12) 0.115(8) Uani 1 1 d . . . . . H8A H 0.105975 0.091014 -0.101319 0.172 Uiso 1 1 calc R U . . . H8B H 0.084611 0.028295 -0.018026 0.172 Uiso 1 1 calc R U . . . H8C H -0.021565 0.096977 -0.050977 0.172 Uiso 1 1 calc R U . . . C16 C 0.1027(16) 0.4690(9) 0.3821(10) 0.074(4) Uani 1 1 d . . . . . H16 H 0.043651 0.510843 0.358243 0.088 Uiso 1 1 calc R U . . . C49 C -0.1157(19) 0.2078(16) 0.7258(14) 0.124(8) Uani 1 1 d . . . . . H49A H -0.045898 0.173223 0.759992 0.149 Uiso 1 1 calc R U . . . H49B H -0.097908 0.264602 0.747439 0.149 Uiso 1 1 calc R U . . . Cl3 Cl 0.2557(9) 0.1249(7) 0.5633(7) 0.204(4) Uani 1 1 d . . . . . Cl4 Cl 0.1946(11) 0.0859(10) 0.7393(9) 0.261(7) Uani 1 1 d . . . . . C52 C 0.202(6) 0.144(2) 0.656(3) 0.36(4) Uani 1 1 d . . . . . H52A H 0.112296 0.162951 0.635039 0.427 Uiso 1 1 calc R U . . . H52B H 0.251574 0.191537 0.683846 0.427 Uiso 1 1 calc R U . . . 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 0.0204(3) 0.0340(3) 0.0232(3) 0.0024(3) 0.00348(19) 0.0010(3) P1 0.0249(10) 0.0403(11) 0.0251(10) 0.0047(9) 0.0040(8) -0.0051(9) P2 0.0346(12) 0.0529(14) 0.0362(13) 0.0065(11) 0.0073(10) -0.0069(11) Cl1 0.138(4) 0.094(3) 0.097(3) -0.019(3) 0.025(3) 0.010(3) F4 0.066(4) 0.077(5) 0.050(4) 0.019(3) 0.012(3) -0.023(4) C43 0.017(4) 0.055(6) 0.037(5) 0.010(4) 0.006(4) -0.004(4) F2 0.063(4) 0.068(4) 0.093(6) 0.031(4) 0.015(4) -0.013(4) F5 0.078(5) 0.134(8) 0.065(5) 0.016(5) -0.019(4) -0.046(6) O1 0.029(3) 0.041(4) 0.027(3) 0.000(3) 0.004(3) 0.004(3) F6 0.092(6) 0.112(7) 0.072(5) 0.033(5) -0.029(5) -0.041(5) C5 0.048(5) 0.035(5) 0.029(4) 0.000(4) 0.005(4) 0.008(4) N1 0.023(3) 0.042(4) 0.029(3) 0.008(4) 0.002(2) -0.006(4) C24 0.039(5) 0.039(5) 0.027(4) 0.013(4) 0.003(4) 0.001(4) C36 0.036(5) 0.049(5) 0.029(5) 0.005(4) 0.014(4) 0.000(4) C30 0.039(5) 0.043(5) 0.025(4) 0.004(4) 0.005(4) -0.014(4) C22 0.029(4) 0.052(6) 0.031(5) 0.010(4) 0.004(4) 0.004(4) C20 0.030(5) 0.040(5) 0.037(5) -0.009(4) 0.008(4) -0.009(4) C11 0.023(4) 0.037(4) 0.033(4) -0.003(4) 0.005(3) -0.006(3) F1 0.099(6) 0.081(6) 0.124(7) -0.005(5) 0.073(6) 0.003(5) C21 0.024(4) 0.049(5) 0.024(4) 0.006(4) -0.002(3) 0.001(4) Cl2 0.246(9) 0.188(8) 0.208(8) -0.061(6) 0.128(7) -0.127(8) C2 0.049(5) 0.068(9) 0.033(5) -0.011(5) -0.012(4) 0.023(6) C1 0.026(5) 0.054(6) 0.056(6) -0.019(5) -0.001(4) -0.003(4) F3 0.083(6) 0.073(5) 0.170(10) -0.011(6) 0.070(7) 0.000(5) C48 0.024(5) 0.063(7) 0.046(6) 0.009(5) 0.006(4) -0.004(5) C12 0.033(4) 0.031(4) 0.029(4) -0.004(3) 0.004(3) -0.005(3) C31 0.038(5) 0.047(5) 0.028(4) 0.002(4) 0.006(4) -0.015(4) C3 0.056(6) 0.043(5) 0.023(4) -0.004(3) 0.004(4) 0.002(4) C23 0.034(5) 0.081(8) 0.039(6) 0.021(5) -0.003(4) 0.002(5) C4 0.030(5) 0.042(5) 0.037(5) -0.008(4) 0.006(4) 0.000(4) C42 0.031(5) 0.049(6) 0.027(5) 0.010(4) 0.009(4) 0.000(4) C25 0.042(6) 0.043(6) 0.084(9) 0.015(6) 0.020(6) -0.003(5) C41 0.038(5) 0.064(6) 0.038(5) 0.001(5) 0.012(4) -0.012(5) C15 0.046(6) 0.046(6) 0.056(6) -0.017(5) 0.021(5) 0.004(5) C6 0.062(7) 0.041(6) 0.044(6) -0.013(5) 0.024(5) -0.020(5) C44 0.035(5) 0.078(8) 0.058(7) -0.027(6) 0.018(5) 0.010(5) C19 0.037(5) 0.070(7) 0.040(5) -0.018(5) 0.004(4) -0.012(5) C46 0.025(4) 0.110(13) 0.044(5) 0.029(7) -0.001(4) 0.020(7) C13 0.048(5) 0.043(5) 0.038(5) 0.001(4) 0.005(4) 0.014(4) C37 0.043(5) 0.037(5) 0.027(4) 0.002(4) 0.010(4) 0.000(4) C29 0.053(6) 0.058(7) 0.035(5) 0.004(5) 0.002(4) 0.016(5) C32 0.067(8) 0.067(7) 0.032(5) -0.005(5) 0.013(5) -0.020(6) C47 0.028(5) 0.092(9) 0.038(6) 0.001(5) -0.006(4) -0.011(6) C45 0.023(5) 0.072(7) 0.043(6) 0.014(5) 0.005(4) 0.004(5) C38 0.074(8) 0.045(6) 0.032(5) 0.003(4) 0.012(5) -0.003(5) C18 0.066(8) 0.102(11) 0.044(6) -0.045(7) 0.025(6) -0.042(8) C40 0.039(6) 0.078(8) 0.049(6) 0.010(5) 0.016(5) -0.012(5) C26 0.047(7) 0.061(8) 0.087(10) 0.012(7) 0.021(6) -0.021(6) C35 0.081(8) 0.051(6) 0.034(5) 0.000(5) 0.011(5) 0.003(6) C28 0.096(10) 0.045(6) 0.036(6) 0.004(5) -0.007(6) -0.007(6) C14 0.060(7) 0.042(6) 0.067(7) 0.000(5) 0.016(6) 0.022(5) C33 0.111(11) 0.055(7) 0.040(6) -0.015(5) 0.016(7) 0.006(7) C39 0.067(7) 0.059(6) 0.043(6) 0.002(5) 0.031(5) -0.014(6) C17 0.083(10) 0.066(8) 0.082(10) -0.040(7) 0.030(8) -0.001(8) C27 0.071(8) 0.055(7) 0.046(6) 0.006(5) 0.009(6) -0.019(6) C34 0.132(13) 0.046(6) 0.046(7) 0.000(5) 0.012(7) 0.010(7) C7 0.030(6) 0.115(11) 0.094(11) -0.043(9) -0.005(6) -0.005(7) C9 0.039(7) 0.162(17) 0.086(10) -0.035(11) 0.024(7) -0.009(8) C8 0.029(6) 0.21(2) 0.100(12) -0.081(14) -0.009(7) -0.007(9) C16 0.097(11) 0.061(8) 0.068(9) -0.021(6) 0.030(7) 0.013(7) C49 0.103(13) 0.14(2) 0.117(14) 0.053(15) -0.015(11) -0.027(14) Cl3 0.188(8) 0.251(10) 0.156(7) 0.019(7) -0.028(6) 0.099(8) Cl4 0.188(10) 0.357(17) 0.251(12) 0.093(12) 0.073(9) 0.112(11) C52 0.70(10) 0.24(4) 0.20(3) 0.13(3) 0.31(5) 0.26(6) #=============================================================================== # 10. MOLECULAR GEOMETRY _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 O1 2.050(6) . ? Ru1 N1 2.093(6) . ? Ru1 C2 2.195(9) . ? Ru1 C5 2.217(9) . ? Ru1 C6 2.223(10) . ? Ru1 C3 2.230(9) . ? Ru1 C1 2.253(9) . ? Ru1 C4 2.264(9) . ? Ru1 P1 2.378(2) . ? P1 C42 1.817(10) . ? P1 C30 1.822(10) . ? P1 C36 1.834(9) . ? P2 F1 1.558(8) . ? P2 F3 1.569(8) . ? P2 F5 1.578(8) . ? P2 F6 1.580(8) . ? P2 F4 1.596(7) . ? P2 F2 1.605(7) . ? Cl1 C49 1.67(2) . ? C43 C42 1.403(14) . ? C43 C45 1.408(14) . ? C43 H43 0.95 . ? O1 C12 1.294(10) . ? C5 C4 1.399(13) . ? C5 C6 1.402(16) . ? C5 H5 0.95 . ? N1 C21 1.298(12) . ? N1 C22 1.496(12) . ? C24 C29 1.370(14) . ? C24 C25 1.391(15) . ? C24 C22 1.541(13) . ? C36 C41 1.382(13) . ? C36 C37 1.404(13) . ? C30 C35 1.384(15) . ? C30 C31 1.393(12) . ? C22 C23 1.536(15) . ? C22 H22 1 . ? C20 C15 1.398(15) . ? C20 C19 1.436(15) . ? C20 C11 1.452(13) . ? C11 C12 1.413(12) . ? C11 C21 1.426(13) . ? C21 H21 0.95 . ? Cl2 C49 1.67(2) . ? C2 C3 1.365(15) . ? C2 C1 1.417(16) . ? C2 H2 0.95 . ? C1 C6 1.412(17) . ? C1 C7 1.511(15) . ? C48 C47 1.365(15) . ? C48 C42 1.393(15) . ? C48 H48 0.95 . ? C12 C13 1.438(13) . ? C31 C32 1.393(16) . ? C31 H31 0.95 . ? C3 C4 1.429(13) . ? C3 H3 0.95 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C4 C44 1.519(13) . ? C25 C26 1.375(16) . ? C25 H25 0.95 . ? C41 C40 1.384(14) . ? C41 H41 0.95 . ? C15 C16 1.405(15) . ? C15 C14 1.445(17) . ? C6 H6 0.95 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C19 C18 1.397(16) . ? C19 H19 0.95 . ? C46 C45 1.373(19) . ? C46 C47 1.40(2) . ? C46 H46 0.95 . ? C13 C14 1.356(14) . ? C13 H13 0.95 . ? C37 C38 1.382(13) . ? C37 H37 0.95 . ? C29 C28 1.397(17) . ? C29 H29 0.95 . ? C32 C33 1.342(18) . ? C32 H32 0.95 . ? C47 H47 0.95 . ? C45 H45 0.95 . ? C38 C39 1.403(17) . ? C38 H38 0.95 . ? C18 C17 1.36(2) . ? C18 H18 0.95 . ? C40 C39 1.380(16) . ? C40 H40 0.95 . ? C26 C27 1.359(19) . ? C26 H26 0.95 . ? C35 C34 1.384(17) . ? C35 H35 0.95 . ? C28 C27 1.363(19) . ? C28 H28 0.95 . ? C14 H14 0.95 . ? C33 C34 1.389(17) . ? C33 H33 0.95 . ? C39 H39 0.95 . ? C17 C16 1.39(2) . ? C17 H17 0.95 . ? C27 H27 0.95 . ? C34 H34 0.95 . ? C7 C9 1.45(2) . ? C7 C8 1.553(19) . ? C7 H7 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C16 H16 0.95 . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? Cl3 C52 1.52(3) . ? Cl4 C52 1.52(3) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? 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 O1 Ru1 N1 88.3(3) . . ? O1 Ru1 C2 82.2(3) . . ? N1 Ru1 C2 146.2(4) . . ? O1 Ru1 C5 155.5(3) . . ? N1 Ru1 C5 99.8(4) . . ? C2 Ru1 C5 78.2(4) . . ? O1 Ru1 C6 120.6(4) . . ? N1 Ru1 C6 91.9(4) . . ? C2 Ru1 C6 66.1(5) . . ? C5 Ru1 C6 36.8(4) . . ? O1 Ru1 C3 105.6(3) . . ? N1 Ru1 C3 165.3(4) . . ? C2 Ru1 C3 35.9(4) . . ? C5 Ru1 C3 65.5(3) . . ? C6 Ru1 C3 76.9(4) . . ? O1 Ru1 C1 89.0(3) . . ? N1 Ru1 C1 110.8(4) . . ? C2 Ru1 C1 37.1(4) . . ? C5 Ru1 C1 66.6(4) . . ? C6 Ru1 C1 36.8(4) . . ? C3 Ru1 C1 65.5(4) . . ? O1 Ru1 C4 142.3(3) . . ? N1 Ru1 C4 129.3(3) . . ? C2 Ru1 C4 66.5(4) . . ? C5 Ru1 C4 36.4(3) . . ? C6 Ru1 C4 66.0(4) . . ? C3 Ru1 C4 37.1(3) . . ? C1 Ru1 C4 78.8(3) . . ? O1 Ru1 P1 84.79(19) . . ? N1 Ru1 P1 86.0(2) . . ? C2 Ru1 P1 124.9(3) . . ? C5 Ru1 P1 118.6(3) . . ? C6 Ru1 P1 154.4(3) . . ? C3 Ru1 P1 99.9(3) . . ? C1 Ru1 P1 161.9(3) . . ? C4 Ru1 P1 96.0(2) . . ? C42 P1 C30 102.9(5) . . ? C42 P1 C36 104.8(4) . . ? C30 P1 C36 104.7(4) . . ? C42 P1 Ru1 116.7(4) . . ? C30 P1 Ru1 113.9(3) . . ? C36 P1 Ru1 112.5(3) . . ? F1 P2 F3 178.7(5) . . ? F1 P2 F5 89.1(6) . . ? F3 P2 F5 91.4(7) . . ? F1 P2 F6 88.8(6) . . ? F3 P2 F6 90.8(6) . . ? F5 P2 F6 177.3(6) . . ? F1 P2 F4 90.1(5) . . ? F3 P2 F4 88.6(5) . . ? F5 P2 F4 89.2(4) . . ? F6 P2 F4 89.2(4) . . ? F1 P2 F2 90.5(5) . . ? F3 P2 F2 90.8(5) . . ? F5 P2 F2 91.5(5) . . ? F6 P2 F2 90.1(4) . . ? F4 P2 F2 179.1(4) . . ? C42 C43 C45 122.0(10) . . ? C42 C43 H43 119 . . ? C45 C43 H43 119 . . ? C12 O1 Ru1 129.2(6) . . ? C4 C5 C6 121.4(9) . . ? C4 C5 Ru1 73.6(5) . . ? C6 C5 Ru1 71.8(6) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? Ru1 C5 H5 127.3 . . ? C21 N1 C22 116.8(7) . . ? C21 N1 Ru1 124.0(6) . . ? C22 N1 Ru1 119.0(6) . . ? C29 C24 C25 118.8(10) . . ? C29 C24 C22 117.5(9) . . ? C25 C24 C22 123.6(9) . . ? C41 C36 C37 119.5(8) . . ? C41 C36 P1 122.4(8) . . ? C37 C36 P1 118.0(7) . . ? C35 C30 C31 117.6(9) . . ? C35 C30 P1 121.1(7) . . ? C31 C30 P1 120.9(7) . . ? N1 C22 C23 113.2(8) . . ? N1 C22 C24 113.7(7) . . ? C23 C22 C24 109.8(8) . . ? N1 C22 H22 106.5 . . ? C23 C22 H22 106.5 . . ? C24 C22 H22 106.5 . . ? C15 C20 C19 118.1(9) . . ? C15 C20 C11 120.6(9) . . ? C19 C20 C11 121.3(10) . . ? C12 C11 C21 121.6(8) . . ? C12 C11 C20 118.7(8) . . ? C21 C11 C20 119.8(8) . . ? N1 C21 C11 130.4(8) . . ? N1 C21 H21 114.8 . . ? C11 C21 H21 114.8 . . ? C3 C2 C1 121.4(10) . . ? C3 C2 Ru1 73.4(5) . . ? C1 C2 Ru1 73.7(6) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? Ru1 C2 H2 125.4 . . ? C6 C1 C2 116.9(9) . . ? C6 C1 C7 127.5(12) . . ? C2 C1 C7 115.6(11) . . ? C6 C1 Ru1 70.5(6) . . ? C2 C1 Ru1 69.2(5) . . ? C7 C1 Ru1 128.9(8) . . ? C47 C48 C42 122.3(11) . . ? C47 C48 H48 118.8 . . ? C42 C48 H48 118.8 . . ? O1 C12 C11 126.0(8) . . ? O1 C12 C13 114.9(8) . . ? C11 C12 C13 119.1(8) . . ? C30 C31 C32 120.7(10) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C2 C3 C4 122.2(9) . . ? C2 C3 Ru1 70.7(6) . . ? C4 C3 Ru1 72.8(5) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? Ru1 C3 H3 130.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C5 C4 C3 116.6(8) . . ? C5 C4 C44 123.8(10) . . ? C3 C4 C44 119.4(10) . . ? C5 C4 Ru1 70.0(5) . . ? C3 C4 Ru1 70.2(5) . . ? C44 C4 Ru1 134.8(7) . . ? C48 C42 C43 117.4(10) . . ? C48 C42 P1 123.4(8) . . ? C43 C42 P1 119.1(9) . . ? C26 C25 C24 119.3(11) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C36 C41 C40 120.1(10) . . ? C36 C41 H41 120 . . ? C40 C41 H41 120 . . ? C20 C15 C16 122.3(12) . . ? C20 C15 C14 119.0(9) . . ? C16 C15 C14 118.7(11) . . ? C5 C6 C1 121.3(10) . . ? C5 C6 Ru1 71.4(6) . . ? C1 C6 Ru1 72.8(6) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? Ru1 C6 H6 129 . . ? C4 C44 H44A 109.5 . . ? C4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C18 C19 C20 117.9(12) . . ? C18 C19 H19 121 . . ? C20 C19 H19 121 . . ? C45 C46 C47 122.8(10) . . ? C45 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C14 C13 C12 121.6(9) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C38 C37 C36 120.4(9) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C24 C29 C28 120.2(11) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C33 C32 C31 120.7(10) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C48 C47 C46 118.3(11) . . ? C48 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C46 C45 C43 117.0(11) . . ? C46 C45 H45 121.5 . . ? C43 C45 H45 121.5 . . ? C37 C38 C39 119.3(10) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C17 C18 C19 122.7(12) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C39 C40 C41 120.7(10) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C27 C26 C25 122.5(12) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C30 C35 C34 121.2(10) . . ? C30 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C27 C28 C29 121.0(11) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C13 C14 C15 120.6(10) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C32 C33 C34 119.7(12) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C40 C39 C38 119.9(9) . . ? C40 C39 H39 120 . . ? C38 C39 H39 120 . . ? C18 C17 C16 120.9(11) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C28 C27 C26 118.2(11) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C33 C34 C35 119.9(12) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C9 C7 C1 115.0(13) . . ? C9 C7 C8 111.6(14) . . ? C1 C7 C8 106.9(11) . . ? C9 C7 H7 107.7 . . ? C1 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C17 C16 C15 118.0(14) . . ? C17 C16 H16 121 . . ? C15 C16 H16 121 . . ? Cl2 C49 Cl1 114.8(12) . . ? Cl2 C49 H49A 108.6 . . ? Cl1 C49 H49A 108.6 . . ? Cl2 C49 H49B 108.6 . . ? Cl1 C49 H49B 108.6 . . ? H49A C49 H49B 107.5 . . ? Cl3 C52 Cl4 127(2) . . ? Cl3 C52 H52A 105.6 . . ? Cl4 C52 H52A 105.6 . . ? Cl3 C52 H52B 105.6 . . ? Cl4 C52 H52B 105.6 . . ? H52A C52 H52B 106.1 . . ? 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 C42 P1 C36 C41 -6.5(10) . . . . ? C30 P1 C36 C41 101.4(9) . . . . ? Ru1 P1 C36 C41 -134.4(8) . . . . ? C42 P1 C36 C37 172.2(8) . . . . ? C30 P1 C36 C37 -79.9(9) . . . . ? Ru1 P1 C36 C37 44.3(9) . . . . ? C42 P1 C30 C35 146.4(9) . . . . ? C36 P1 C30 C35 37.1(10) . . . . ? Ru1 P1 C30 C35 -86.2(9) . . . . ? C42 P1 C30 C31 -41.1(8) . . . . ? C36 P1 C30 C31 -150.5(8) . . . . ? Ru1 P1 C30 C31 86.2(8) . . . . ? C21 N1 C22 C23 -46.0(11) . . . . ? Ru1 N1 C22 C23 138.7(7) . . . . ? C21 N1 C22 C24 80.2(10) . . . . ? Ru1 N1 C22 C24 -95.1(7) . . . . ? C29 C24 C22 N1 149.1(8) . . . . ? C25 C24 C22 N1 -34.3(13) . . . . ? C29 C24 C22 C23 -82.9(11) . . . . ? C25 C24 C22 C23 93.8(12) . . . . ? C15 C20 C11 C12 7.4(13) . . . . ? C19 C20 C11 C12 -172.9(8) . . . . ? C15 C20 C11 C21 -172.8(9) . . . . ? C19 C20 C11 C21 7.0(13) . . . . ? C22 N1 C21 C11 -176.6(9) . . . . ? Ru1 N1 C21 C11 -1.5(13) . . . . ? C12 C11 C21 N1 3.2(15) . . . . ? C20 C11 C21 N1 -176.6(9) . . . . ? C3 C2 C1 C6 4.6(14) . . . . ? Ru1 C2 C1 C6 -53.6(8) . . . . ? C3 C2 C1 C7 -177.5(10) . . . . ? Ru1 C2 C1 C7 124.3(9) . . . . ? C3 C2 C1 Ru1 58.2(9) . . . . ? Ru1 O1 C12 C11 8.9(13) . . . . ? Ru1 O1 C12 C13 -170.7(6) . . . . ? C21 C11 C12 O1 -6.9(14) . . . . ? C20 C11 C12 O1 172.9(8) . . . . ? C21 C11 C12 C13 172.6(8) . . . . ? C20 C11 C12 C13 -7.5(13) . . . . ? C35 C30 C31 C32 -2.4(14) . . . . ? P1 C30 C31 C32 -175.1(8) . . . . ? C1 C2 C3 C4 -4.6(15) . . . . ? Ru1 C2 C3 C4 53.7(8) . . . . ? C1 C2 C3 Ru1 -58.3(8) . . . . ? C6 C5 C4 C3 1.8(13) . . . . ? Ru1 C5 C4 C3 -54.1(7) . . . . ? C6 C5 C4 C44 -172.9(9) . . . . ? Ru1 C5 C4 C44 131.2(9) . . . . ? C6 C5 C4 Ru1 55.9(8) . . . . ? C2 C3 C4 C5 1.3(13) . . . . ? Ru1 C3 C4 C5 54.1(7) . . . . ? C2 C3 C4 C44 176.2(9) . . . . ? Ru1 C3 C4 C44 -131.0(9) . . . . ? C2 C3 C4 Ru1 -52.8(8) . . . . ? C47 C48 C42 C43 -3.5(15) . . . . ? C47 C48 C42 P1 178.0(8) . . . . ? C45 C43 C42 C48 3.2(15) . . . . ? C45 C43 C42 P1 -178.3(7) . . . . ? C30 P1 C42 C48 -30.3(9) . . . . ? C36 P1 C42 C48 78.9(9) . . . . ? Ru1 P1 C42 C48 -155.9(7) . . . . ? C30 P1 C42 C43 151.2(8) . . . . ? C36 P1 C42 C43 -99.6(9) . . . . ? Ru1 P1 C42 C43 25.7(9) . . . . ? C29 C24 C25 C26 -0.8(18) . . . . ? C22 C24 C25 C26 -177.4(11) . . . . ? C37 C36 C41 C40 0.3(16) . . . . ? P1 C36 C41 C40 179.0(9) . . . . ? C19 C20 C15 C16 -0.6(16) . . . . ? C11 C20 C15 C16 179.2(11) . . . . ? C19 C20 C15 C14 177.1(10) . . . . ? C11 C20 C15 C14 -3.1(15) . . . . ? C4 C5 C6 C1 -1.6(14) . . . . ? Ru1 C5 C6 C1 55.2(9) . . . . ? C4 C5 C6 Ru1 -56.8(8) . . . . ? C2 C1 C6 C5 -1.5(14) . . . . ? C7 C1 C6 C5 -179.1(10) . . . . ? Ru1 C1 C6 C5 -54.5(9) . . . . ? C2 C1 C6 Ru1 53.0(8) . . . . ? C7 C1 C6 Ru1 -124.6(11) . . . . ? C15 C20 C19 C18 -0.8(14) . . . . ? C11 C20 C19 C18 179.4(9) . . . . ? O1 C12 C13 C14 -176.7(10) . . . . ? C11 C12 C13 C14 3.7(15) . . . . ? C41 C36 C37 C38 1.0(15) . . . . ? P1 C36 C37 C38 -177.7(8) . . . . ? C25 C24 C29 C28 -0.6(15) . . . . ? C22 C24 C29 C28 176.2(9) . . . . ? C30 C31 C32 C33 5.8(17) . . . . ? C42 C48 C47 C46 2.5(16) . . . . ? C45 C46 C47 C48 -1.0(17) . . . . ? C47 C46 C45 C43 0.7(15) . . . . ? C42 C43 C45 C46 -1.8(15) . . . . ? C36 C37 C38 C39 -0.3(15) . . . . ? C20 C19 C18 C17 1.6(17) . . . . ? C36 C41 C40 C39 -2.4(18) . . . . ? C24 C25 C26 C27 3(2) . . . . ? C31 C30 C35 C34 0.2(18) . . . . ? P1 C30 C35 C34 172.9(11) . . . . ? C24 C29 C28 C27 -0.3(16) . . . . ? C12 C13 C14 C15 0.7(18) . . . . ? C20 C15 C14 C13 -1.0(17) . . . . ? C16 C15 C14 C13 176.9(12) . . . . ? C31 C32 C33 C34 -7(2) . . . . ? C41 C40 C39 C38 3.1(18) . . . . ? C37 C38 C39 C40 -1.8(16) . . . . ? C19 C18 C17 C16 -1(2) . . . . ? C29 C28 C27 C26 2.5(18) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C32 C33 C34 C35 5(2) . . . . ? C30 C35 C34 C33 -1(2) . . . . ? C6 C1 C7 C9 34(2) . . . . ? C2 C1 C7 C9 -143.2(14) . . . . ? Ru1 C1 C7 C9 -60(2) . . . . ? C6 C1 C7 C8 -90.0(17) . . . . ? C2 C1 C7 C8 92.4(16) . . . . ? Ru1 C1 C7 C8 175.6(12) . . . . ? C18 C17 C16 C15 -1(2) . . . . ? C20 C15 C16 C17 1(2) . . . . ? C14 C15 C16 C17 -176.4(13) . . . . ? # END loop_ _publcif_info_cif.paper_type ?