Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal ; Journal ofthe Chemical Society, DALTON Transactions ; _publ_contact_author_name 'Dr Felix A Jalon' _publ_contact_author_address ; Dr Felix A Jalon Departamento de Quimica Inorganica, Organica y Bioquimica, Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela 10 E-13071-Ciudad Real SPAIN ; _publ_section_title ; Synthesis and Characterization of a Series of Ruthenium Scorpionate Complexes with B-H...M Agostic Interactions. X-ray Crystal Structure of the Complex [RuH(\k^2^-N,BH TpTn)(PMe~3~)(cod)]. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Caballero, A.' ; Departamento de Quimica Inorganica, Organica y Bioquimica. Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela, 10 E-13071, Ciudad Real Spain ; 'Gomez de la Torre, F.' ; Departamento de Quimica Inorganica, Organica y Bioquimica. Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela, 10 E-13071, Ciudad Real Spain ; 'Jalon, F.A.' ; Departamento de Quimica Inorganica, Organica y Bioquimica. Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela, 10 E-13071, Ciudad Real Spain ; 'Manzano, B.R.' ; Departamento de Quimica Inorganica, Organica y Bioquimica. Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela, 10 E-13071, Ciudad Real Spain ; 'Rodriguez, A.M.' ; Departamento de Quimica Inorganica, Organica y Bioquimica. Facultad de Quimicas Universidad de Castilla-La Mancha Avda. Camilo Jose Cela, 10 E-13071, Ciudad Real Spain ; 'Trofimenko, S' ; Department of Chemistry and Biochemistry University of Delaware Newwark, DE 19716 USA ; 'Sigalas, MP' ; Department of Chemistry Laboratory of Applied Quantum Chemistry Aristotle University of Thessaloniki 54006 Thessaloniki Greece ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use 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 ? #=========================================================================== data_7 _database_code_CSD 153203 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 B N6 P Ru S3' _chemical_formula_weight 745.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.682(5) _cell_length_b 11.427(5) _cell_length_c 14.375(5) _cell_angle_alpha 97.020(5) _cell_angle_beta 105.600(5) _cell_angle_gamma 94.070(5) _cell_volume 1667.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\2q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 8005 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.98 _reflns_number_total 8005 _reflns_number_gt 5254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8005 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.75950(4) -0.85606(4) 0.71042(3) 0.02460(12) Uani 1 1 d . . . HA H 0.766(4) -0.949(4) 0.758(3) 0.019(12) Uiso 1 1 d . . . HB H 0.760(5) -0.689(4) 0.669(4) 0.027(13) Uiso 1 1 d . . . P1 P 0.82047(13) -0.77484(12) 0.87477(9) 0.0276(3) Uani 1 1 d . . . S2 S 0.53681(14) -1.04310(14) 0.81303(14) 0.0479(4) Uani 1 1 d . . . S4 S 0.62512(17) -0.39428(16) 0.98032(12) 0.0504(4) Uani 1 1 d . . . S3 S 0.9239(11) -0.5281(9) 0.3831(7) 0.067(3) Uani 0.50 1 d P A 1 S3A S 0.9237(10) -0.5761(9) 0.3602(6) 0.062(2) Uani 0.50 1 d P A 2 N21 N 0.5641(4) -0.8193(3) 0.6961(3) 0.0247(8) Uani 1 1 d . . . N22 N 0.5504(4) -0.7100(3) 0.6648(3) 0.0262(9) Uani 1 1 d . . . N31 N 0.6431(4) -0.6417(4) 0.5353(3) 0.0258(9) Uani 1 1 d . . . N32 N 0.7411(4) -0.6037(4) 0.4977(3) 0.0292(9) Uani 1 1 d . . . N41 N 0.6982(4) -0.5208(4) 0.7017(3) 0.0268(9) Uani 1 1 d . . . N42 N 0.6728(4) -0.4961(4) 0.7893(3) 0.0266(9) Uani 1 1 d . . . B1 B 0.6665(5) -0.6451(5) 0.6436(4) 0.0281(12) Uani 1 1 d . . . C1 C 0.9385(5) -0.9448(5) 0.7223(4) 0.0323(12) Uani 1 1 d . . . H1 H 0.9407 -0.9458 0.7873 0.039 Uiso 1 1 calc . . . C2 C 0.9560(5) -0.8355(5) 0.6921(4) 0.0350(12) Uani 1 1 d . . . H2 H 0.9735 -0.7685 0.7392 0.042 Uiso 1 1 calc . . . C3 C 0.9488(5) -0.8174(5) 0.5901(4) 0.0394(13) Uani 1 1 d . . . H3A H 1.0291 -0.8382 0.5762 0.047 Uiso 1 1 calc . . . H3B H 0.9438 -0.7338 0.5853 0.047 Uiso 1 1 calc . . . C4 C 0.8337(6) -0.8887(5) 0.5124(4) 0.0386(13) Uani 1 1 d . . . H4A H 0.8121 -0.8470 0.4562 0.046 Uiso 1 1 calc . . . H4B H 0.8601 -0.9647 0.4915 0.046 Uiso 1 1 calc . . . C5 C 0.7131(5) -0.9100(4) 0.5459(4) 0.0284(11) Uani 1 1 d . . . H5 H 0.6533 -0.8542 0.5375 0.034 Uiso 1 1 calc . . . C6 C 0.6862(5) -1.0069(4) 0.5880(4) 0.0289(11) Uani 1 1 d . . . H6 H 0.6100 -1.0119 0.6075 0.035 Uiso 1 1 calc . . . C7 C 0.7718(5) -1.1049(5) 0.6044(4) 0.0385(13) Uani 1 1 d . . . H7A H 0.7650 -1.1513 0.5417 0.046 Uiso 1 1 calc . . . H7B H 0.7390 -1.1566 0.6433 0.046 Uiso 1 1 calc . . . C8 C 0.9157(5) -1.0644(5) 0.6552(4) 0.0360(12) Uani 1 1 d . . . H8A H 0.9617 -1.0579 0.6060 0.043 Uiso 1 1 calc . . . H8B H 0.9526 -1.1242 0.6936 0.043 Uiso 1 1 calc . . . C9 C 0.8888(6) -0.8741(5) 0.9612(4) 0.0411(13) Uani 1 1 d . . . H9A H 0.8303 -0.9456 0.9488 0.062 Uiso 1 1 calc . . . H9B H 0.8999 -0.8357 1.0266 0.062 Uiso 1 1 calc . . . H9C H 0.9719 -0.8931 0.9537 0.062 Uiso 1 1 calc . . . C10 C 0.6893(6) -0.7258(5) 0.9222(4) 0.0383(13) Uani 1 1 d . . . H10A H 0.6184 -0.7881 0.9054 0.057 Uiso 1 1 calc . . . H10B H 0.6591 -0.6571 0.8944 0.057 Uiso 1 1 calc . . . H10C H 0.7206 -0.7060 0.9920 0.057 Uiso 1 1 calc . . . C11 C 0.9427(6) -0.6469(5) 0.9134(4) 0.0411(14) Uani 1 1 d . . . H11A H 1.0178 -0.6642 0.8917 0.062 Uiso 1 1 calc . . . H11B H 0.9681 -0.6288 0.9834 0.062 Uiso 1 1 calc . . . H11C H 0.9070 -0.5801 0.8856 0.062 Uiso 1 1 calc . . . C21 C 0.4281(5) -0.6821(5) 0.6575(4) 0.0308(11) Uani 1 1 d . . . H21 H 0.3951 -0.6132 0.6378 0.037 Uiso 1 1 calc . . . C22 C 0.3612(5) -0.7716(5) 0.6838(4) 0.0306(11) Uani 1 1 d . . . H22 H 0.2747 -0.7755 0.6858 0.037 Uiso 1 1 calc . . . C23 C 0.4485(5) -0.8583(5) 0.7079(3) 0.0274(10) Uani 1 1 d . . . C24 C 0.4201(5) -0.9666(5) 0.7447(4) 0.0305(11) Uani 1 1 d . . . C25 C 0.2989(5) -1.0165(5) 0.7396(4) 0.0373(13) Uani 1 1 d . . . H25 H 0.2225 -0.9885 0.7060 0.045 Uiso 1 1 calc . . . C26 C 0.3000(6) -1.1151(5) 0.7902(5) 0.0432(15) Uani 1 1 d . . . H26 H 0.2243 -1.1582 0.7932 0.052 Uiso 1 1 calc . . . C27 C 0.4204(6) -1.1405(5) 0.8334(5) 0.0445(15) Uani 1 1 d . . . H27 H 0.4386 -1.2025 0.8696 0.053 Uiso 1 1 calc . . . C31 C 0.5303(4) -0.6678(5) 0.4628(4) 0.0299(11) Uani 1 1 d . . . H31 H 0.4499 -0.6932 0.4711 0.036 Uiso 1 1 calc . . . C32 C 0.5514(5) -0.6514(6) 0.3769(4) 0.0400(14) Uani 1 1 d . . . H32 H 0.4915 -0.6640 0.3153 0.048 Uiso 1 1 calc . . . C33 C 0.6860(5) -0.6105(4) 0.4023(4) 0.0263(10) Uani 1 1 d . A . C34 C 0.7591(5) -0.5736(4) 0.3360(4) 0.0277(11) Uani 1 1 d . . . C35 C 0.7081(5) -0.5552(4) 0.2381(4) 0.0287(11) Uani 1 1 d . A . H35 H 0.6202 -0.5670 0.2031 0.034 Uiso 1 1 calc . . . C36 C 0.8117(6) -0.5159(6) 0.2014(4) 0.0474(15) Uani 1 1 d . . . H36 H 0.8012 -0.5091 0.1360 0.057 Uiso 1 1 calc . B 1 C37 C 0.932(2) -0.4882(15) 0.2738(18) 0.042(5) Uani 0.50 1 d P A 1 H37 H 1.0068 -0.4524 0.2635 0.050 Uiso 0.50 1 calc P C 1 C37A C 0.926(3) -0.5374(17) 0.2487(18) 0.051(5) Uani 0.50 1 d P A 2 H37A H 0.9991 -0.5327 0.2259 0.061 Uiso 0.50 1 calc P D 2 C41 C 0.7659(5) -0.4255(5) 0.6845(4) 0.0355(12) Uani 1 1 d . . . H41 H 0.7947 -0.4217 0.6293 0.043 Uiso 1 1 calc . . . C42 C 0.7856(5) -0.3355(5) 0.7603(4) 0.0388(13) Uani 1 1 d . . . H42 H 0.8296 -0.2603 0.7678 0.047 Uiso 1 1 calc . . . C43 C 0.7244(5) -0.3824(5) 0.8243(4) 0.0309(11) Uani 1 1 d . . . C44 C 0.7090(5) -0.3230(5) 0.9141(4) 0.0333(12) Uani 1 1 d . . . C45 C 0.7508(5) -0.2062(5) 0.9607(4) 0.0328(12) Uani 1 1 d . . . H45 H 0.7972 -0.1506 0.9369 0.039 Uiso 1 1 calc . . . C46 C 0.7156(7) -0.1835(6) 1.0446(6) 0.062(2) Uani 1 1 d . . . H46 H 0.7368 -0.1102 1.0843 0.075 Uiso 1 1 calc . . . C47 C 0.6488(7) -0.2738(7) 1.0652(4) 0.0577(19) Uani 1 1 d . . . H47 H 0.6185 -0.2710 1.1203 0.069 Uiso 1 1 calc . . . 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 0.01938(19) 0.0295(2) 0.0238(2) 0.00242(16) 0.00527(15) 0.00153(14) P1 0.0299(7) 0.0294(7) 0.0213(6) 0.0045(5) 0.0040(5) -0.0004(5) S2 0.0321(7) 0.0432(8) 0.0737(12) 0.0285(8) 0.0158(8) 0.0013(6) S4 0.0626(11) 0.0593(10) 0.0334(8) 0.0081(7) 0.0193(8) 0.0080(8) S3 0.038(3) 0.126(8) 0.038(4) 0.024(4) 0.011(2) -0.007(4) S3A 0.033(2) 0.126(7) 0.036(4) 0.040(4) 0.011(3) 0.018(4) N21 0.0221(19) 0.023(2) 0.028(2) 0.0004(17) 0.0076(17) 0.0026(16) N22 0.027(2) 0.026(2) 0.025(2) 0.0043(17) 0.0059(17) 0.0004(17) N31 0.027(2) 0.029(2) 0.023(2) 0.0042(17) 0.0101(17) -0.0015(17) N32 0.027(2) 0.037(2) 0.025(2) 0.0075(19) 0.0091(18) -0.0038(18) N41 0.031(2) 0.030(2) 0.018(2) 0.0015(17) 0.0047(17) 0.0006(17) N42 0.033(2) 0.028(2) 0.019(2) 0.0061(17) 0.0072(17) -0.0018(17) B1 0.025(3) 0.038(3) 0.026(3) 0.010(2) 0.012(2) 0.005(2) C1 0.026(3) 0.041(3) 0.027(3) 0.000(2) 0.003(2) 0.011(2) C2 0.019(2) 0.048(3) 0.034(3) -0.003(3) 0.004(2) 0.004(2) C3 0.033(3) 0.044(3) 0.049(4) 0.004(3) 0.025(3) 0.005(2) C4 0.047(3) 0.049(3) 0.030(3) 0.007(3) 0.024(3) 0.015(3) C5 0.030(3) 0.034(3) 0.021(2) -0.004(2) 0.008(2) 0.009(2) C6 0.027(2) 0.031(3) 0.027(3) -0.001(2) 0.008(2) 0.000(2) C7 0.039(3) 0.042(3) 0.034(3) 0.002(3) 0.010(3) 0.008(2) C8 0.029(3) 0.037(3) 0.042(3) 0.004(3) 0.010(2) 0.006(2) C9 0.045(3) 0.041(3) 0.034(3) 0.009(3) 0.004(3) 0.001(3) C10 0.044(3) 0.045(3) 0.028(3) 0.001(2) 0.016(3) 0.003(3) C11 0.041(3) 0.043(3) 0.030(3) 0.001(2) 0.001(2) -0.014(3) C21 0.035(3) 0.037(3) 0.023(3) 0.002(2) 0.012(2) 0.017(2) C22 0.020(2) 0.049(3) 0.026(3) 0.008(2) 0.010(2) 0.009(2) C23 0.026(2) 0.037(3) 0.018(2) -0.002(2) 0.0091(19) -0.001(2) C24 0.025(2) 0.035(3) 0.032(3) 0.003(2) 0.010(2) 0.003(2) C25 0.031(3) 0.041(3) 0.038(3) -0.003(3) 0.011(2) -0.003(2) C26 0.037(3) 0.038(3) 0.054(4) -0.003(3) 0.022(3) -0.016(3) C27 0.045(3) 0.028(3) 0.065(4) 0.014(3) 0.023(3) -0.009(2) C31 0.018(2) 0.044(3) 0.027(3) 0.009(2) 0.003(2) 0.005(2) C32 0.032(3) 0.060(4) 0.021(3) 0.002(3) -0.004(2) 0.005(3) C33 0.027(2) 0.025(2) 0.025(3) 0.004(2) 0.003(2) 0.0013(19) C34 0.028(3) 0.032(3) 0.024(3) 0.006(2) 0.008(2) 0.008(2) C35 0.023(2) 0.028(3) 0.039(3) 0.016(2) 0.011(2) 0.0030(19) C36 0.056(4) 0.061(4) 0.036(3) 0.019(3) 0.021(3) 0.023(3) C37 0.034(8) 0.044(11) 0.052(13) 0.022(9) 0.011(8) 0.005(9) C37A 0.045(9) 0.065(14) 0.050(13) 0.028(11) 0.022(9) -0.007(12) C41 0.039(3) 0.035(3) 0.034(3) 0.001(2) 0.015(2) 0.001(2) C42 0.037(3) 0.041(3) 0.032(3) 0.000(2) 0.004(2) -0.004(2) C43 0.031(3) 0.033(3) 0.026(3) 0.003(2) 0.004(2) 0.004(2) C44 0.033(3) 0.037(3) 0.027(3) 0.007(2) 0.000(2) 0.011(2) C45 0.027(3) 0.030(3) 0.039(3) -0.001(2) 0.008(2) 0.002(2) C46 0.054(4) 0.051(4) 0.062(5) -0.028(4) -0.001(4) 0.009(3) C47 0.062(4) 0.086(5) 0.026(3) -0.005(3) 0.013(3) 0.034(4) _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 N21 2.119(4) . ? Ru1 C2 2.184(5) . ? Ru1 C1 2.204(5) . ? Ru1 C6 2.237(5) . ? Ru1 C5 2.278(5) . ? Ru1 P1 2.3276(15) . ? P1 C11 1.814(5) . ? P1 C10 1.810(6) . ? P1 C9 1.827(6) . ? S2 C27 1.718(5) . ? S2 C24 1.729(5) . ? S4 C47 1.680(7) . ? S4 C44 1.708(6) . ? S3 C37 1.71(3) . ? S3 C34 1.723(12) . ? S3A C34 1.701(11) . ? S3A C37A 1.72(3) . ? N21 C23 1.345(6) . ? N21 N22 1.383(5) . ? N22 C21 1.347(6) . ? N22 B1 1.519(7) . ? N31 C31 1.350(6) . ? N31 N32 1.369(5) . ? N31 B1 1.515(7) . ? N32 C33 1.329(6) . ? N41 N42 1.360(5) . ? N41 C41 1.348(7) . ? N41 B1 1.522(7) . ? N42 C43 1.354(6) . ? C1 C2 1.388(8) . ? C1 C8 1.536(7) . ? C2 C3 1.489(8) . ? C3 C4 1.523(8) . ? C4 C5 1.506(7) . ? C5 C6 1.374(7) . ? C6 C7 1.496(7) . ? C7 C8 1.524(7) . ? C21 C22 1.355(7) . ? C22 C23 1.419(7) . ? C23 C24 1.447(7) . ? C24 C25 1.356(7) . ? C25 C26 1.413(8) . ? C26 C27 1.339(8) . ? C31 C32 1.346(7) . ? C32 C33 1.414(7) . ? C33 C34 1.466(7) . ? C34 C35 1.414(7) . ? C35 C36 1.416(8) . ? C36 C37A 1.28(3) . ? C36 C37 1.40(2) . ? C41 C42 1.365(7) . ? C42 C43 1.397(8) . ? C43 C44 1.439(7) . ? C44 C45 1.402(7) . ? C45 C46 1.357(9) . ? C46 C47 1.322(10) . ? 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 N21 Ru1 C2 157.24(19) . . ? N21 Ru1 C1 164.15(17) . . ? C2 Ru1 C1 36.9(2) . . ? N21 Ru1 C6 89.33(17) . . ? C2 Ru1 C6 94.49(19) . . ? C1 Ru1 C6 79.64(19) . . ? N21 Ru1 C5 90.78(16) . . ? C2 Ru1 C5 79.75(19) . . ? C1 Ru1 C5 86.79(18) . . ? C6 Ru1 C5 35.41(18) . . ? N21 Ru1 P1 90.84(11) . . ? C2 Ru1 P1 95.76(14) . . ? C1 Ru1 P1 93.83(14) . . ? C6 Ru1 P1 152.82(14) . . ? C5 Ru1 P1 171.64(14) . . ? C11 P1 C10 102.8(3) . . ? C11 P1 C9 101.8(3) . . ? C10 P1 C9 100.6(3) . . ? C11 P1 Ru1 117.57(19) . . ? C10 P1 Ru1 115.55(19) . . ? C9 P1 Ru1 116.1(2) . . ? C27 S2 C24 92.4(3) . . ? C47 S4 C44 92.1(3) . . ? C37 S3 C34 91.0(10) . . ? C34 S3A C37A 92.8(10) . . ? C23 N21 N22 106.9(4) . . ? C23 N21 Ru1 145.0(4) . . ? N22 N21 Ru1 108.0(3) . . ? C21 N22 N21 109.6(4) . . ? C21 N22 B1 131.8(4) . . ? N21 N22 B1 118.6(4) . . ? C31 N31 N32 109.4(4) . . ? C31 N31 B1 128.8(4) . . ? N32 N31 B1 121.7(4) . . ? C33 N32 N31 105.4(4) . . ? N42 N41 C41 109.6(4) . . ? N42 N41 B1 121.4(4) . . ? C41 N41 B1 128.5(4) . . ? C43 N42 N41 105.7(4) . . ? N31 B1 N22 111.5(4) . . ? N31 B1 N41 111.4(4) . . ? N22 B1 N41 110.3(4) . . ? C2 C1 C8 124.2(5) . . ? C2 C1 Ru1 70.8(3) . . ? C8 C1 Ru1 113.3(3) . . ? C1 C2 C3 125.0(5) . . ? C1 C2 Ru1 72.3(3) . . ? C3 C2 Ru1 110.1(3) . . ? C2 C3 C4 114.8(5) . . ? C5 C4 C3 114.1(4) . . ? C6 C5 C4 124.0(5) . . ? C6 C5 Ru1 70.7(3) . . ? C4 C5 Ru1 110.5(3) . . ? C5 C6 C7 124.1(5) . . ? C5 C6 Ru1 73.9(3) . . ? C7 C6 Ru1 109.9(3) . . ? C6 C7 C8 114.9(5) . . ? C7 C8 C1 113.4(4) . . ? N22 C21 C22 108.4(4) . . ? C21 C22 C23 106.8(4) . . ? N21 C23 C22 108.2(4) . . ? N21 C23 C24 125.9(5) . . ? C22 C23 C24 125.7(4) . . ? C25 C24 C23 125.4(5) . . ? C25 C24 S2 109.7(4) . . ? C23 C24 S2 124.6(4) . . ? C24 C25 C26 113.5(5) . . ? C27 C26 C25 113.5(5) . . ? C26 C27 S2 110.8(4) . . ? N31 C31 C32 110.0(4) . . ? C31 C32 C33 103.7(4) . . ? N32 C33 C32 111.4(4) . . ? N32 C33 C34 122.1(4) . . ? C32 C33 C34 126.4(5) . . ? C35 C34 C33 127.6(4) . . ? C35 C34 S3A 108.9(5) . . ? C33 C34 S3A 122.4(5) . . ? C35 C34 S3 113.5(5) . . ? C33 C34 S3 118.4(5) . . ? S3A C34 S3 20.3(4) . . ? C36 C35 C34 109.5(5) . . ? C37A C36 C37 26.1(11) . . ? C37A C36 C35 115.3(12) . . ? C37 C36 C35 113.1(11) . . ? C36 C37 S3 112.2(16) . . ? C36 C37A S3A 110.6(16) . . ? N41 C41 C42 109.8(5) . . ? C41 C42 C43 104.1(5) . . ? N42 C43 C42 110.9(5) . . ? N42 C43 C44 121.3(5) . . ? C42 C43 C44 127.7(5) . . ? C45 C44 C43 130.1(5) . . ? C45 C44 S4 109.0(4) . . ? C43 C44 S4 120.8(4) . . ? C46 C45 C44 112.2(5) . . ? C47 C46 C45 114.6(6) . . ? C46 C47 S4 112.0(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.735 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.124