# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gareth Owen' _publ_contact_author_email GARETH.OWEN@BRISTOL.AC.UK _publ_section_title ; A 'Sting' on Grubbs' Catalyst: An Insight into Hydride Migration Between Boron and Transition Metal. ; loop_ _publ_author_name 'Gareth Owen' 'Alex Hamilton' 'A Orpen' 'Georg C Rudolf' # Attachment 'Compound_5.cif' data_gro237 _database_code_depnum_ccdc_archive 'CCDC 690699' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H51 B Cl N4 P Ru S2, 2(C H2 Cl2)' _chemical_formula_sum 'C35 H55 B Cl5 N4 P Ru S2' _chemical_formula_weight 916.05 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.892(3) _cell_length_b 26.144(8) _cell_length_c 16.446(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.859(4) _cell_angle_gamma 90.00 _cell_volume 4248(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 988 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.6 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.68930 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24062 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.32 _reflns_number_total 10059 _reflns_number_gt 6311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^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 10059 _refine_ls_number_parameters 458 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.43285(3) 0.217119(13) 0.91845(2) 0.02156(10) Uani 1 1 d . . . S1 S 0.40339(10) 0.23878(4) 1.05731(6) 0.0241(2) Uani 1 1 d . . . S2 S 0.40471(11) 0.19919(4) 0.77474(7) 0.0264(2) Uani 1 1 d . . . N1 N 0.1477(4) 0.24977(14) 1.1136(2) 0.0276(8) Uani 1 1 d . . . N2 N 0.1520(3) 0.24396(13) 0.9811(2) 0.0225(7) Uani 1 1 d . . . N3 N 0.1521(3) 0.21963(14) 0.8261(2) 0.0252(7) Uani 1 1 d . . . N4 N 0.1478(4) 0.18658(14) 0.7036(2) 0.0279(8) Uani 1 1 d . . . P5 P 0.48653(10) 0.13482(4) 0.95341(7) 0.0228(2) Uani 1 1 d . . . B1 B 0.2285(5) 0.24154(19) 0.9023(3) 0.0237(10) Uani 1 1 d . . . Cl1A Cl 0.2803(19) 0.1147(3) 0.2818(5) 0.102(4) Uani 0.66(3) 1 d PD A 1 Cl1B Cl 0.194(2) 0.1068(3) 0.2621(6) 0.072(4) Uani 0.34(3) 1 d PD A 2 Cl2 Cl 0.1998(2) 0.07567(8) 0.43541(12) 0.0852(6) Uani 1 1 d . A . Cl3 Cl 0.34801(19) 1.03118(7) 0.62927(14) 0.0832(6) Uani 1 1 d . . . Cl4 Cl 0.08109(19) 1.00876(8) 0.68478(12) 0.0787(6) Uani 1 1 d . . . Cl7 Cl 0.66457(10) 0.25555(4) 0.91292(6) 0.0272(2) Uani 1 1 d . . . C1 C 0.5833(4) 0.12840(16) 1.0536(3) 0.0257(9) Uani 1 1 d . . . H1 H 0.5220 0.1438 1.0934 0.031 Uiso 1 1 calc R . . C2 C 0.6093(6) 0.07479(19) 1.0858(4) 0.0513(16) Uani 1 1 d . . . H2A H 0.6780 0.0580 1.0531 0.062 Uiso 1 1 calc R . . H2B H 0.5247 0.0546 1.0796 0.062 Uiso 1 1 calc R . . C3 C 0.6584(5) 0.0751(2) 1.1747(3) 0.0441(13) Uani 1 1 d . . . H3A H 0.5854 0.0881 1.2082 0.053 Uiso 1 1 calc R . . H3B H 0.6797 0.0397 1.1923 0.053 Uiso 1 1 calc R . . C4 C 0.7824(5) 0.10805(19) 1.1885(3) 0.0371(11) Uani 1 1 d . . . H4A H 0.8597 0.0922 1.1619 0.045 Uiso 1 1 calc R . . H4B H 0.8060 0.1105 1.2476 0.045 Uiso 1 1 calc R . . C5 C 0.7568(7) 0.1611(2) 1.1539(4) 0.0645(19) Uani 1 1 d . . . H5A H 0.8408 0.1816 1.1610 0.077 Uiso 1 1 calc R . . H5B H 0.6861 0.1781 1.1848 0.077 Uiso 1 1 calc R . . C6 C 0.7117(6) 0.1599(2) 1.0638(3) 0.0528(16) Uani 1 1 d . . . H6A H 0.6946 0.1951 1.0438 0.063 Uiso 1 1 calc R . . H6B H 0.7836 0.1446 1.0318 0.063 Uiso 1 1 calc R . . C7 C 0.5731(4) 0.09948(16) 0.8722(3) 0.0275(10) Uani 1 1 d . . . H7 H 0.5135 0.1042 0.8218 0.033 Uiso 1 1 calc R . . C8 C 0.5884(5) 0.04158(17) 0.8817(3) 0.0420(13) Uani 1 1 d . . . H8A H 0.6553 0.0340 0.9269 0.050 Uiso 1 1 calc R . . H8B H 0.5006 0.0265 0.8955 0.050 Uiso 1 1 calc R . . C9 C 0.6342(5) 0.01771(19) 0.8045(3) 0.0396(12) Uani 1 1 d . . . H9A H 0.6462 -0.0195 0.8129 0.048 Uiso 1 1 calc R . . H9B H 0.5634 0.0227 0.7605 0.048 Uiso 1 1 calc R . . C10 C 0.7649(5) 0.04036(18) 0.7786(3) 0.0373(11) Uani 1 1 d . . . H10A H 0.7864 0.0262 0.7249 0.045 Uiso 1 1 calc R . . H10B H 0.8389 0.0307 0.8184 0.045 Uiso 1 1 calc R . . C11 C 0.7568(6) 0.0982(2) 0.7729(4) 0.0535(16) Uani 1 1 d . . . H11A H 0.6929 0.1078 0.7271 0.064 Uiso 1 1 calc R . . H11B H 0.8470 0.1120 0.7611 0.064 Uiso 1 1 calc R . . C12 C 0.7099(5) 0.12232(18) 0.8516(3) 0.0355(11) Uani 1 1 d . . . H12A H 0.7776 0.1156 0.8967 0.043 Uiso 1 1 calc R . . H12B H 0.7011 0.1598 0.8446 0.043 Uiso 1 1 calc R . . C13 C 0.3377(4) 0.09282(17) 0.9689(3) 0.0262(9) Uani 1 1 d . . . H13 H 0.3739 0.0581 0.9836 0.031 Uiso 1 1 calc R . . C14 C 0.2517(4) 0.11037(18) 1.0393(3) 0.0303(10) Uani 1 1 d . . . H14A H 0.3093 0.1116 1.0902 0.036 Uiso 1 1 calc R . . H14B H 0.2176 0.1454 1.0279 0.036 Uiso 1 1 calc R . . C15 C 0.1332(5) 0.07515(19) 1.0510(3) 0.0353(11) Uani 1 1 d . . . H15A H 0.0787 0.0886 1.0951 0.042 Uiso 1 1 calc R . . H15B H 0.1672 0.0409 1.0676 0.042 Uiso 1 1 calc R . . C16 C 0.0436(5) 0.07030(19) 0.9726(3) 0.0386(12) Uani 1 1 d . . . H16A H -0.0309 0.0459 0.9814 0.046 Uiso 1 1 calc R . . H16B H 0.0030 0.1040 0.9585 0.046 Uiso 1 1 calc R . . C17 C 0.1257(4) 0.05177(19) 0.9033(3) 0.0375(12) Uani 1 1 d . . . H17A H 0.0670 0.0504 0.8527 0.045 Uiso 1 1 calc R . . H17B H 0.1586 0.0167 0.9153 0.045 Uiso 1 1 calc R . . C18 C 0.2459(4) 0.08648(18) 0.8900(3) 0.0314(10) Uani 1 1 d . . . H18A H 0.2127 0.1205 0.8717 0.038 Uiso 1 1 calc R . . H18B H 0.3000 0.0720 0.8465 0.038 Uiso 1 1 calc R . . C19 C 0.2307(4) 0.20189(16) 0.7665(3) 0.0252(9) Uani 1 1 d . . . C20 C 0.0166(4) 0.21429(17) 0.7983(3) 0.0281(9) Uani 1 1 d . . . H20 H -0.0604 0.2234 0.8274 0.034 Uiso 1 1 calc R . . C21 C 0.0144(5) 0.19398(18) 0.7231(3) 0.0329(10) Uani 1 1 d . . . H21 H -0.0638 0.1862 0.6895 0.040 Uiso 1 1 calc R . . C22 C 0.1915(5) 0.16510(19) 0.6268(3) 0.0341(11) Uani 1 1 d . . . H22A H 0.1745 0.1900 0.5829 0.051 Uiso 1 1 calc R . . H22B H 0.1408 0.1337 0.6142 0.051 Uiso 1 1 calc R . . H22C H 0.2885 0.1573 0.6320 0.051 Uiso 1 1 calc R . . C23 C 0.2310(4) 0.24487(15) 1.0501(2) 0.0224(9) Uani 1 1 d . . . C24 C 0.0174(4) 0.24976(17) 1.0006(3) 0.0276(10) Uani 1 1 d . . . H24 H -0.0589 0.2510 0.9632 0.033 Uiso 1 1 calc R . . C25 C 0.0153(4) 0.25331(17) 1.0821(3) 0.0297(10) Uani 1 1 d . . . H25 H -0.0629 0.2575 1.1127 0.036 Uiso 1 1 calc R . . C26 C 0.1923(4) 0.24881(19) 1.2000(3) 0.0336(11) Uani 1 1 d . . . H26A H 0.2805 0.2318 1.2063 0.050 Uiso 1 1 calc R . . H26B H 0.1260 0.2301 1.2309 0.050 Uiso 1 1 calc R . . H26C H 0.2003 0.2839 1.2206 0.050 Uiso 1 1 calc R . . C27 C 0.3057(4) 0.29650(16) 0.8814(3) 0.0254(9) Uani 1 1 d . . . H27A H 0.4048 0.2914 0.8883 0.030 Uiso 1 1 calc R . . H27B H 0.2846 0.3053 0.8236 0.030 Uiso 1 1 calc R . . C28 C 0.2663(4) 0.34117(17) 0.9339(3) 0.0275(10) Uani 1 1 d . . . C29 C 0.1363(5) 0.36138(18) 0.9272(3) 0.0392(12) Uani 1 1 d . . . H29 H 0.0730 0.3483 0.8871 0.047 Uiso 1 1 calc R . . C30 C 0.0979(6) 0.4005(2) 0.9783(4) 0.0531(16) Uani 1 1 d . . . H30 H 0.0081 0.4135 0.9731 0.064 Uiso 1 1 calc R . . C31 C 0.1864(7) 0.4208(2) 1.0359(4) 0.0524(15) Uani 1 1 d . . . H31 H 0.1590 0.4474 1.0707 0.063 Uiso 1 1 calc R . . C32 C 0.3154(6) 0.4019(2) 1.0425(3) 0.0444(13) Uani 1 1 d . . . H32 H 0.3785 0.4159 1.0818 0.053 Uiso 1 1 calc R . . C33 C 0.3553(5) 0.36269(18) 0.9926(3) 0.0352(11) Uani 1 1 d . . . H33 H 0.4454 0.3502 0.9985 0.042 Uiso 1 1 calc R . . C34 C 0.2077(6) 0.9909(2) 0.6208(4) 0.0610(17) Uani 1 1 d . . . H34A H 0.1706 0.9913 0.5637 0.073 Uiso 1 1 calc R . . H34B H 0.2367 0.9555 0.6340 0.073 Uiso 1 1 calc R . . C35 C 0.1438(7) 0.1142(2) 0.3539(4) 0.0631(18) Uani 1 1 d D . . H35A H 0.1256 0.1494 0.3729 0.076 Uiso 1 1 calc R A 1 H35B H 0.0596 0.1002 0.3276 0.076 Uiso 1 1 calc R A 1 H100 H 0.283(4) 0.1892(14) 0.922(2) 0.010(9) 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 0.01509(16) 0.02873(17) 0.02124(17) 0.00034(15) 0.00461(12) -0.00026(14) S1 0.0175(5) 0.0323(6) 0.0230(5) -0.0009(4) 0.0038(4) 0.0001(4) S2 0.0189(5) 0.0381(6) 0.0228(6) 0.0000(5) 0.0057(4) -0.0008(4) N1 0.023(2) 0.037(2) 0.0233(19) -0.0022(16) 0.0047(15) 0.0021(15) N2 0.0172(18) 0.0286(19) 0.0223(18) -0.0006(15) 0.0068(14) 0.0003(14) N3 0.0184(17) 0.035(2) 0.0221(18) 0.0022(16) 0.0025(14) -0.0001(15) N4 0.030(2) 0.035(2) 0.0190(19) 0.0008(16) 0.0013(15) -0.0033(16) P5 0.0148(5) 0.0283(6) 0.0258(6) -0.0005(5) 0.0052(4) -0.0016(4) B1 0.018(2) 0.032(3) 0.021(2) 0.004(2) 0.0048(19) 0.0020(19) Cl1A 0.160(10) 0.085(3) 0.063(3) -0.007(2) 0.032(4) 0.047(4) Cl1B 0.099(10) 0.068(4) 0.049(4) -0.007(3) 0.014(5) 0.015(4) Cl2 0.0769(13) 0.0985(15) 0.0796(14) 0.0259(11) -0.0022(10) 0.0154(10) Cl3 0.0643(12) 0.0741(12) 0.1101(17) 0.0128(11) -0.0056(11) -0.0072(9) Cl4 0.0763(13) 0.0921(13) 0.0696(12) 0.0034(10) 0.0221(10) 0.0303(10) Cl7 0.0182(5) 0.0339(6) 0.0297(6) 0.0015(4) 0.0043(4) -0.0027(4) C1 0.018(2) 0.028(2) 0.032(2) 0.0029(18) 0.0039(18) 0.0007(16) C2 0.051(3) 0.032(3) 0.068(4) 0.011(3) -0.029(3) -0.004(2) C3 0.036(3) 0.041(3) 0.054(4) 0.018(3) -0.007(3) -0.003(2) C4 0.035(3) 0.048(3) 0.028(3) 0.004(2) -0.005(2) -0.002(2) C5 0.081(5) 0.062(4) 0.046(4) 0.021(3) -0.031(3) -0.039(3) C6 0.048(4) 0.068(4) 0.041(3) 0.015(3) -0.013(3) -0.032(3) C7 0.021(2) 0.033(2) 0.029(2) -0.0017(19) 0.0042(18) -0.0037(17) C8 0.042(3) 0.028(3) 0.059(4) -0.003(2) 0.032(3) -0.003(2) C9 0.029(3) 0.036(3) 0.055(3) -0.013(2) 0.008(2) 0.000(2) C10 0.034(3) 0.039(3) 0.041(3) -0.006(2) 0.012(2) 0.001(2) C11 0.068(4) 0.040(3) 0.056(4) -0.002(3) 0.046(3) -0.002(3) C12 0.031(3) 0.034(3) 0.043(3) -0.005(2) 0.018(2) -0.0074(19) C13 0.021(2) 0.030(2) 0.027(2) 0.0015(18) 0.0046(18) -0.0040(17) C14 0.022(2) 0.037(3) 0.032(3) -0.001(2) 0.0067(19) -0.0013(18) C15 0.023(2) 0.040(3) 0.044(3) 0.009(2) 0.012(2) -0.0026(19) C16 0.022(2) 0.038(3) 0.057(3) 0.007(2) 0.007(2) -0.0066(19) C17 0.020(2) 0.038(3) 0.055(3) -0.006(2) 0.004(2) -0.0061(19) C18 0.019(2) 0.042(3) 0.034(3) -0.002(2) 0.0014(19) -0.0063(18) C19 0.025(2) 0.028(2) 0.022(2) 0.0033(17) 0.0017(18) -0.0045(16) C20 0.017(2) 0.039(3) 0.028(2) 0.001(2) -0.0004(17) 0.0017(18) C21 0.033(3) 0.039(3) 0.027(3) 0.004(2) 0.000(2) -0.007(2) C22 0.035(3) 0.046(3) 0.021(2) -0.004(2) 0.005(2) -0.002(2) C23 0.022(2) 0.025(2) 0.021(2) 0.0004(17) 0.0044(17) 0.0006(16) C24 0.014(2) 0.040(3) 0.029(2) 0.000(2) 0.0040(17) -0.0009(17) C25 0.018(2) 0.040(3) 0.031(2) 0.003(2) 0.0089(18) 0.0014(18) C26 0.025(2) 0.051(3) 0.026(2) -0.002(2) 0.0102(19) 0.000(2) C27 0.017(2) 0.037(3) 0.021(2) 0.0046(17) 0.0012(17) 0.0015(16) C28 0.023(2) 0.032(2) 0.029(2) 0.0010(19) 0.0074(18) -0.0017(17) C29 0.026(3) 0.036(3) 0.056(3) 0.005(2) 0.006(2) 0.003(2) C30 0.042(3) 0.043(3) 0.076(4) 0.000(3) 0.024(3) 0.008(2) C31 0.069(4) 0.039(3) 0.051(4) -0.008(3) 0.029(3) 0.004(3) C32 0.060(4) 0.041(3) 0.032(3) 0.000(2) 0.005(3) -0.005(3) C33 0.039(3) 0.036(3) 0.031(3) 0.002(2) 0.001(2) 0.002(2) C34 0.071(4) 0.054(4) 0.060(4) -0.006(3) 0.026(3) -0.002(3) C35 0.075(5) 0.047(4) 0.067(4) -0.010(3) -0.004(4) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 B1 2.124(5) . ? Ru1 P5 2.2829(13) . ? Ru1 S1 2.3847(13) . ? Ru1 S2 2.4119(13) . ? Ru1 C27 2.487(4) . ? Ru1 Cl7 2.5085(12) . ? Ru1 H100 1.66(4) . ? S1 C23 1.711(4) . ? S2 C19 1.721(4) . ? N1 C23 1.369(5) . ? N1 C25 1.387(6) . ? N1 C26 1.467(6) . ? N2 C23 1.345(5) . ? N2 C24 1.394(5) . ? N2 B1 1.534(5) . ? N3 C19 1.364(5) . ? N3 C20 1.402(5) . ? N3 B1 1.540(6) . ? N4 C19 1.347(5) . ? N4 C21 1.386(6) . ? N4 C22 1.468(5) . ? P5 C13 1.864(4) . ? P5 C7 1.867(4) . ? P5 C1 1.871(5) . ? B1 C27 1.671(6) . ? B1 H100 1.50(4) . ? Cl1A C35 1.841(11) . ? Cl1B C35 1.624(9) . ? Cl2 C35 1.745(6) . ? Cl3 C34 1.742(6) . ? Cl4 C34 1.740(6) . ? C1 C2 1.516(6) . ? C1 C6 1.516(6) . ? C1 H1 1.0000 . ? C2 C3 1.518(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.516(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.529(6) . ? C7 C12 1.532(6) . ? C7 H7 1.0000 . ? C8 C9 1.505(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.502(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.541(6) . ? C13 C18 1.556(6) . ? C13 H13 1.0000 . ? C14 C15 1.510(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.533(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.513(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 C21 1.345(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.345(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.515(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.389(6) . ? C28 C33 1.392(6) . ? C29 C30 1.389(7) . ? C29 H29 0.9500 . ? C30 C31 1.364(9) . ? C30 H30 0.9500 . ? C31 C32 1.368(8) . ? C31 H31 0.9500 . ? C32 C33 1.383(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? 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 B1 Ru1 P5 121.52(14) . . ? B1 Ru1 S1 83.55(13) . . ? P5 Ru1 S1 91.18(4) . . ? B1 Ru1 S2 82.70(13) . . ? P5 Ru1 S2 94.46(4) . . ? S1 Ru1 S2 166.13(4) . . ? B1 Ru1 C27 41.58(16) . . ? P5 Ru1 C27 163.10(10) . . ? S1 Ru1 C27 87.26(10) . . ? S2 Ru1 C27 83.67(10) . . ? B1 Ru1 Cl7 137.80(14) . . ? P5 Ru1 Cl7 100.67(4) . . ? S1 Ru1 Cl7 95.46(4) . . ? S2 Ru1 Cl7 95.93(4) . . ? C27 Ru1 Cl7 96.24(10) . . ? B1 Ru1 H100 44.6(12) . . ? P5 Ru1 H100 76.9(12) . . ? S1 Ru1 H100 85.2(13) . . ? S2 Ru1 H100 83.8(13) . . ? C27 Ru1 H100 86.2(12) . . ? Cl7 Ru1 H100 177.5(12) . . ? C23 S1 Ru1 97.15(14) . . ? C19 S2 Ru1 97.80(15) . . ? C23 N1 C25 108.3(4) . . ? C23 N1 C26 125.1(4) . . ? C25 N1 C26 126.6(3) . . ? C23 N2 C24 108.9(3) . . ? C23 N2 B1 115.0(3) . . ? C24 N2 B1 135.8(4) . . ? C19 N3 C20 107.6(4) . . ? C19 N3 B1 115.9(3) . . ? C20 N3 B1 136.5(3) . . ? C19 N4 C21 109.4(4) . . ? C19 N4 C22 125.4(4) . . ? C21 N4 C22 125.2(4) . . ? C13 P5 C7 101.52(19) . . ? C13 P5 C1 101.52(19) . . ? C7 P5 C1 110.6(2) . . ? C13 P5 Ru1 114.48(15) . . ? C7 P5 Ru1 113.29(15) . . ? C1 P5 Ru1 114.13(14) . . ? N2 B1 N3 117.4(3) . . ? N2 B1 C27 112.8(4) . . ? N3 B1 C27 111.3(3) . . ? N2 B1 Ru1 114.4(3) . . ? N3 B1 Ru1 114.5(3) . . ? C27 B1 Ru1 80.9(2) . . ? N2 B1 H100 92.2(14) . . ? N3 B1 H100 89.7(14) . . ? C27 B1 H100 131.9(14) . . ? Ru1 B1 H100 51.0(13) . . ? C2 C1 C6 109.7(4) . . ? C2 C1 P5 117.5(3) . . ? C6 C1 P5 116.0(3) . . ? C2 C1 H1 103.9 . . ? C6 C1 H1 103.9 . . ? P5 C1 H1 103.9 . . ? C1 C2 C3 111.9(4) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 111.6(4) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 110.3(4) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 112.4(5) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C1 C6 C5 108.8(4) . . ? C1 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? C1 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8 C7 C12 108.9(4) . . ? C8 C7 P5 117.6(3) . . ? C12 C7 P5 114.0(3) . . ? C8 C7 H7 105.0 . . ? C12 C7 H7 105.0 . . ? P5 C7 H7 105.0 . . ? C9 C8 C7 110.9(4) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 112.0(4) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 111.5(4) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 112.0(4) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C7 C12 C11 109.5(4) . . ? C7 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C7 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C18 109.7(4) . . ? C14 C13 P5 113.4(3) . . ? C18 C13 P5 112.4(3) . . ? C14 C13 H13 107.0 . . ? C18 C13 H13 107.0 . . ? P5 C13 H13 107.0 . . ? C15 C14 C13 112.1(4) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 111.3(4) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 110.5(4) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.7(4) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C13 111.9(4) . . ? C17 C18 H18A 109.2 . . ? C13 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? C13 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N4 C19 N3 107.8(4) . . ? N4 C19 S2 128.1(3) . . ? N3 C19 S2 124.1(3) . . ? C21 C20 N3 108.1(4) . . ? C21 C20 H20 126.0 . . ? N3 C20 H20 126.0 . . ? C20 C21 N4 107.2(4) . . ? C20 C21 H21 126.4 . . ? N4 C21 H21 126.4 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 N1 107.4(3) . . ? N2 C23 S1 126.3(3) . . ? N1 C23 S1 126.2(3) . . ? C25 C24 N2 107.4(4) . . ? C25 C24 H24 126.3 . . ? N2 C24 H24 126.3 . . ? C24 C25 N1 107.9(4) . . ? C24 C25 H25 126.1 . . ? N1 C25 H25 126.1 . . ? N1 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 B1 114.3(3) . . ? C28 C27 Ru1 130.1(3) . . ? B1 C27 Ru1 57.5(2) . . ? C28 C27 H27A 108.7 . . ? B1 C27 H27A 108.7 . . ? Ru1 C27 H27A 51.2 . . ? C28 C27 H27B 108.7 . . ? B1 C27 H27B 108.7 . . ? Ru1 C27 H27B 120.6 . . ? H27A C27 H27B 107.6 . . ? C29 C28 C33 116.9(4) . . ? C29 C28 C27 120.7(4) . . ? C33 C28 C27 122.3(4) . . ? C28 C29 C30 120.8(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 121.4(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 118.6(5) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C31 C32 C33 120.9(5) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 121.4(5) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? Cl4 C34 Cl3 112.6(3) . . ? Cl4 C34 H34A 109.1 . . ? Cl3 C34 H34A 109.1 . . ? Cl4 C34 H34B 109.1 . . ? Cl3 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? Cl1B C35 Cl2 123.1(6) . . ? Cl2 C35 Cl1A 106.4(5) . . ? Cl1B C35 H35A 118.2 . . ? Cl2 C35 H35A 110.4 . . ? Cl1A C35 H35A 110.4 . . ? Cl1B C35 H35B 80.7 . . ? Cl2 C35 H35B 110.4 . . ? Cl1A C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 Ru1 S1 C23 12.70(19) . . . . ? P5 Ru1 S1 C23 -108.89(14) . . . . ? S2 Ru1 S1 C23 5.2(2) . . . . ? C27 Ru1 S1 C23 54.26(17) . . . . ? Cl7 Ru1 S1 C23 150.27(14) . . . . ? B1 Ru1 S2 C19 -15.6(2) . . . . ? P5 Ru1 S2 C19 105.69(15) . . . . ? S1 Ru1 S2 C19 -8.0(2) . . . . ? C27 Ru1 S2 C19 -57.43(17) . . . . ? Cl7 Ru1 S2 C19 -153.08(15) . . . . ? B1 Ru1 P5 C13 -1.7(2) . . . . ? S1 Ru1 P5 C13 81.49(16) . . . . ? S2 Ru1 P5 C13 -85.83(16) . . . . ? C27 Ru1 P5 C13 -3.0(4) . . . . ? Cl7 Ru1 P5 C13 177.27(15) . . . . ? B1 Ru1 P5 C7 114.1(2) . . . . ? S1 Ru1 P5 C7 -162.73(16) . . . . ? S2 Ru1 P5 C7 29.95(16) . . . . ? C27 Ru1 P5 C7 112.8(4) . . . . ? Cl7 Ru1 P5 C7 -66.94(16) . . . . ? B1 Ru1 P5 C1 -118.0(2) . . . . ? S1 Ru1 P5 C1 -34.89(15) . . . . ? S2 Ru1 P5 C1 157.79(15) . . . . ? C27 Ru1 P5 C1 -119.3(4) . . . . ? Cl7 Ru1 P5 C1 60.89(15) . . . . ? C23 N2 B1 N3 156.6(4) . . . . ? C24 N2 B1 N3 -30.0(7) . . . . ? C23 N2 B1 C27 -72.0(5) . . . . ? C24 N2 B1 C27 101.5(5) . . . . ? C23 N2 B1 Ru1 18.2(5) . . . . ? C24 N2 B1 Ru1 -168.4(4) . . . . ? C19 N3 B1 N2 -158.7(4) . . . . ? C20 N3 B1 N2 24.5(7) . . . . ? C19 N3 B1 C27 69.2(5) . . . . ? C20 N3 B1 C27 -107.6(5) . . . . ? C19 N3 B1 Ru1 -20.3(5) . . . . ? C20 N3 B1 Ru1 162.8(4) . . . . ? P5 Ru1 B1 N2 69.5(3) . . . . ? S1 Ru1 B1 N2 -17.9(3) . . . . ? S2 Ru1 B1 N2 160.3(3) . . . . ? C27 Ru1 B1 N2 -111.0(4) . . . . ? Cl7 Ru1 B1 N2 -108.9(3) . . . . ? P5 Ru1 B1 N3 -70.1(3) . . . . ? S1 Ru1 B1 N3 -157.5(3) . . . . ? S2 Ru1 B1 N3 20.7(3) . . . . ? C27 Ru1 B1 N3 109.4(4) . . . . ? Cl7 Ru1 B1 N3 111.5(3) . . . . ? P5 Ru1 B1 C27 -179.43(17) . . . . ? S1 Ru1 B1 C27 93.1(2) . . . . ? S2 Ru1 B1 C27 -88.7(2) . . . . ? Cl7 Ru1 B1 C27 2.1(3) . . . . ? C13 P5 C1 C2 49.6(4) . . . . ? C7 P5 C1 C2 -57.5(4) . . . . ? Ru1 P5 C1 C2 173.3(3) . . . . ? C13 P5 C1 C6 -177.8(4) . . . . ? C7 P5 C1 C6 75.0(4) . . . . ? Ru1 P5 C1 C6 -54.1(4) . . . . ? C6 C1 C2 C3 58.1(6) . . . . ? P5 C1 C2 C3 -166.6(4) . . . . ? C1 C2 C3 C4 -55.4(6) . . . . ? C2 C3 C4 C5 53.1(6) . . . . ? C3 C4 C5 C6 -55.9(7) . . . . ? C2 C1 C6 C5 -58.5(7) . . . . ? P5 C1 C6 C5 165.4(4) . . . . ? C4 C5 C6 C1 58.7(7) . . . . ? C13 P5 C7 C8 -44.9(4) . . . . ? C1 P5 C7 C8 62.2(4) . . . . ? Ru1 P5 C7 C8 -168.1(3) . . . . ? C13 P5 C7 C12 -174.2(4) . . . . ? C1 P5 C7 C12 -67.1(4) . . . . ? Ru1 P5 C7 C12 62.5(4) . . . . ? C12 C7 C8 C9 -59.6(6) . . . . ? P5 C7 C8 C9 168.7(3) . . . . ? C7 C8 C9 C10 57.1(6) . . . . ? C8 C9 C10 C11 -53.3(6) . . . . ? C9 C10 C11 C12 53.3(7) . . . . ? C8 C7 C12 C11 58.8(6) . . . . ? P5 C7 C12 C11 -167.6(4) . . . . ? C10 C11 C12 C7 -56.4(6) . . . . ? C7 P5 C13 C14 175.1(3) . . . . ? C1 P5 C13 C14 61.0(4) . . . . ? Ru1 P5 C13 C14 -62.4(3) . . . . ? C7 P5 C13 C18 -59.8(4) . . . . ? C1 P5 C13 C18 -173.9(3) . . . . ? Ru1 P5 C13 C18 62.7(3) . . . . ? C18 C13 C14 C15 54.3(5) . . . . ? P5 C13 C14 C15 -179.2(3) . . . . ? C13 C14 C15 C16 -56.7(5) . . . . ? C14 C15 C16 C17 56.8(5) . . . . ? C15 C16 C17 C18 -56.3(5) . . . . ? C16 C17 C18 C13 55.5(5) . . . . ? C14 C13 C18 C17 -53.4(5) . . . . ? P5 C13 C18 C17 179.5(3) . . . . ? C21 N4 C19 N3 -0.6(5) . . . . ? C22 N4 C19 N3 179.8(4) . . . . ? C21 N4 C19 S2 178.0(3) . . . . ? C22 N4 C19 S2 -1.7(6) . . . . ? C20 N3 C19 N4 0.6(5) . . . . ? B1 N3 C19 N4 -177.2(3) . . . . ? C20 N3 C19 S2 -178.1(3) . . . . ? B1 N3 C19 S2 4.2(5) . . . . ? Ru1 S2 C19 N4 -167.5(4) . . . . ? Ru1 S2 C19 N3 10.9(4) . . . . ? C19 N3 C20 C21 -0.3(5) . . . . ? B1 N3 C20 C21 176.7(5) . . . . ? N3 C20 C21 N4 0.0(5) . . . . ? C19 N4 C21 C20 0.4(5) . . . . ? C22 N4 C21 C20 -180.0(4) . . . . ? C24 N2 C23 N1 1.6(5) . . . . ? B1 N2 C23 N1 176.8(3) . . . . ? C24 N2 C23 S1 179.6(3) . . . . ? B1 N2 C23 S1 -5.2(5) . . . . ? C25 N1 C23 N2 -1.6(5) . . . . ? C26 N1 C23 N2 175.6(4) . . . . ? C25 N1 C23 S1 -179.6(3) . . . . ? C26 N1 C23 S1 -2.3(6) . . . . ? Ru1 S1 C23 N2 -8.0(4) . . . . ? Ru1 S1 C23 N1 169.5(3) . . . . ? C23 N2 C24 C25 -1.0(5) . . . . ? B1 N2 C24 C25 -174.8(4) . . . . ? N2 C24 C25 N1 0.0(5) . . . . ? C23 N1 C25 C24 1.0(5) . . . . ? C26 N1 C25 C24 -176.2(4) . . . . ? N2 B1 C27 C28 -10.7(5) . . . . ? N3 B1 C27 C28 123.7(4) . . . . ? Ru1 B1 C27 C28 -123.4(3) . . . . ? N2 B1 C27 Ru1 112.7(4) . . . . ? N3 B1 C27 Ru1 -112.9(3) . . . . ? B1 Ru1 C27 C28 95.8(4) . . . . ? P5 Ru1 C27 C28 97.5(5) . . . . ? S1 Ru1 C27 C28 12.5(3) . . . . ? S2 Ru1 C27 C28 -178.0(4) . . . . ? Cl7 Ru1 C27 C28 -82.7(4) . . . . ? P5 Ru1 C27 B1 1.7(5) . . . . ? S1 Ru1 C27 B1 -83.4(2) . . . . ? S2 Ru1 C27 B1 86.1(2) . . . . ? Cl7 Ru1 C27 B1 -178.6(2) . . . . ? B1 C27 C28 C29 -67.7(5) . . . . ? Ru1 C27 C28 C29 -134.7(4) . . . . ? B1 C27 C28 C33 110.1(5) . . . . ? Ru1 C27 C28 C33 43.1(6) . . . . ? C33 C28 C29 C30 -1.4(7) . . . . ? C27 C28 C29 C30 176.5(5) . . . . ? C28 C29 C30 C31 0.8(8) . . . . ? C29 C30 C31 C32 0.3(9) . . . . ? C30 C31 C32 C33 -0.8(8) . . . . ? C31 C32 C33 C28 0.2(8) . . . . ? C29 C28 C33 C32 0.8(7) . . . . ? C27 C28 C33 C32 -177.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.749 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.111