# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gareth Owen' _publ_contact_author_email GARETH.OWEN@BRISTOL.AC.UK _publ_section_title ; A New Hybrid Scorpionate Ligand: A Study of the Effect of Tautomerisation upon the Metal-Boron Bond within Metallaboratrane Complexes. ; loop_ _publ_author_name 'Gareth Owen' 'Jonathan Charmant' 'P. Hugh Gould' 'Alex Hamilton' 'Saowanit Saithong' # Attachment 'Complex_4.cif' data_gro172-p21-n- _database_code_depnum_ccdc_archive 'CCDC 736093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H29 B N5 O P Ru S3, 3(C H2 Cl2)' _chemical_formula_sum 'C35 H35 B Cl6 N5 O P Ru S3' _chemical_formula_weight 993.41 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' O O 0.0106 0.0060 '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 'P 21/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 16.376(3) _cell_length_b 10.867(2) _cell_length_c 24.024(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.38(3) _cell_angle_gamma 90.00 _cell_volume 4101.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5894 _cell_measurement_theta_min 2.279 _cell_measurement_theta_max 23.6335 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.387 _exptl_crystal_size_mid 0.141 _exptl_crystal_size_min 0.095 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details '(SADABS; Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size ? _diffrn_source_target Mo _diffrn_source_type ? _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45871 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9417 _reflns_number_gt 7491 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9417 _refine_ls_number_parameters 508 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.006 _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 0.73198(2) 0.77627(4) 0.063987(16) 0.01404(11) Uani 1 1 d . . . S1 S 0.81210(8) 0.74906(10) 0.16744(5) 0.0184(3) Uani 1 1 d . . . S2 S 0.63796(8) 0.60991(12) 0.06904(5) 0.0216(3) Uani 1 1 d . . . S3 S 0.79442(8) 0.97382(12) 0.06451(6) 0.0211(3) Uani 1 1 d . . . N1 N 0.6866(3) 0.9124(4) 0.16359(18) 0.0236(10) Uani 1 1 d . . . N2 N 0.7698(3) 0.8882(5) 0.2519(2) 0.0349(12) Uani 1 1 d . . . N3 N 0.5606(3) 0.8180(4) 0.09210(18) 0.0252(10) Uani 1 1 d . . . N4 N 0.4845(3) 0.6521(5) 0.09161(19) 0.0298(11) Uani 1 1 d . . . N5 N 0.6363(3) 1.0200(4) 0.06844(17) 0.0226(10) Uani 1 1 d . . . P1 P 0.84182(8) 0.66205(12) 0.03623(5) 0.0160(3) Uani 1 1 d . . . B1 B 0.6469(4) 0.8852(6) 0.0972(2) 0.0196(12) Uani 1 1 d . . . O1 O 0.6210(3) 0.8387(5) -0.05298(16) 0.0438(12) Uani 1 1 d . . . C1 C 0.8074(3) 0.5781(5) -0.0331(2) 0.0186(10) Uani 1 1 d . . . C2 C 0.7616(3) 0.6432(5) -0.0825(2) 0.0269(12) Uani 1 1 d . . . H2 H 0.7500 0.7283 -0.0795 0.032 Uiso 1 1 calc R . . C3 C 0.7334(3) 0.5839(6) -0.1355(2) 0.0288(13) Uani 1 1 d . . . H3 H 0.7042 0.6291 -0.1690 0.035 Uiso 1 1 calc R . . C4 C 0.7474(3) 0.4611(6) -0.1398(2) 0.0298(13) Uani 1 1 d . . . H4 H 0.7267 0.4207 -0.1761 0.036 Uiso 1 1 calc R . . C5 C 0.7916(3) 0.3955(5) -0.0916(2) 0.0287(12) Uani 1 1 d . . . H5 H 0.8015 0.3100 -0.0949 0.034 Uiso 1 1 calc R . . C6 C 0.8216(3) 0.4535(5) -0.0385(2) 0.0216(11) Uani 1 1 d . . . H6 H 0.8521 0.4077 -0.0055 0.026 Uiso 1 1 calc R . . C7 C 0.8989(3) 0.5418(4) 0.08594(19) 0.0167(10) Uani 1 1 d . . . C8 C 0.8518(3) 0.4666(5) 0.1120(2) 0.0244(12) Uani 1 1 d . . . H8 H 0.7922 0.4791 0.1042 0.029 Uiso 1 1 calc R . . C9 C 0.8913(4) 0.3735(5) 0.1494(2) 0.0301(13) Uani 1 1 d . . . H9 H 0.8582 0.3200 0.1656 0.036 Uiso 1 1 calc R . . C10 C 0.9787(4) 0.3581(5) 0.1632(2) 0.0288(13) Uani 1 1 d . . . H10 H 1.0058 0.2958 0.1898 0.035 Uiso 1 1 calc R . . C11 C 1.0263(3) 0.4344(5) 0.1379(2) 0.0237(11) Uani 1 1 d . . . H11 H 1.0863 0.4245 0.1474 0.028 Uiso 1 1 calc R . . C12 C 0.9871(3) 0.5239(5) 0.0993(2) 0.0199(11) Uani 1 1 d . . . H12 H 1.0200 0.5741 0.0814 0.024 Uiso 1 1 calc R . . C13 C 0.9319(3) 0.7543(4) 0.0288(2) 0.0196(11) Uani 1 1 d . . . C14 C 0.9630(4) 0.7483(5) -0.0196(2) 0.0249(12) Uani 1 1 d . . . H14 H 0.9360 0.6973 -0.0516 0.030 Uiso 1 1 calc R . . C15 C 1.0346(4) 0.8183(5) -0.0205(3) 0.0316(14) Uani 1 1 d . . . H15 H 1.0555 0.8157 -0.0536 0.038 Uiso 1 1 calc R . . C16 C 1.0749(4) 0.8910(5) 0.0262(3) 0.0315(14) Uani 1 1 d . . . H16 H 1.1243 0.9364 0.0257 0.038 Uiso 1 1 calc R . . C17 C 1.0437(3) 0.8975(5) 0.0735(2) 0.0273(12) Uani 1 1 d . . . H17 H 1.0710 0.9487 0.1053 0.033 Uiso 1 1 calc R . . C18 C 0.9724(3) 0.8297(5) 0.0749(2) 0.0223(11) Uani 1 1 d . . . H18 H 0.9512 0.8349 0.1078 0.027 Uiso 1 1 calc R . . C19 C 0.7543(3) 0.8506(5) 0.1959(2) 0.0198(11) Uani 1 1 d . . . C20 C 0.6576(4) 0.9907(5) 0.1992(2) 0.0323(14) Uani 1 1 d . . . H20 H 0.6099 1.0440 0.1867 0.039 Uiso 1 1 calc R . . C21 C 0.7068(4) 0.9804(5) 0.2541(2) 0.0369(16) Uani 1 1 d . . . H21 H 0.7015 1.0239 0.2872 0.044 Uiso 1 1 calc R . . C22 C 0.8339(4) 0.8443(6) 0.3000(3) 0.0430(16) Uani 1 1 d . . . H22A H 0.8150 0.7675 0.3138 0.065 Uiso 1 1 calc R . . H22B H 0.8454 0.9058 0.3311 0.065 Uiso 1 1 calc R . . H22C H 0.8859 0.8290 0.2886 0.065 Uiso 1 1 calc R . . C23 C 0.5580(3) 0.6947(5) 0.0836(2) 0.0222(11) Uani 1 1 d . . . C24 C 0.4871(4) 0.8503(6) 0.1078(2) 0.0329(14) Uani 1 1 d . . . H24 H 0.4730 0.9307 0.1176 0.040 Uiso 1 1 calc R . . C25 C 0.4402(4) 0.7494(6) 0.1067(3) 0.0339(14) Uani 1 1 d . . . H25 H 0.3867 0.7450 0.1147 0.041 Uiso 1 1 calc R . . C26 C 0.4597(4) 0.5248(6) 0.0879(3) 0.0345(14) Uani 1 1 d . . . H26A H 0.4613 0.4914 0.0503 0.052 Uiso 1 1 calc R . . H26B H 0.4018 0.5177 0.0916 0.052 Uiso 1 1 calc R . . H26C H 0.4991 0.4784 0.1191 0.052 Uiso 1 1 calc R . . C27 C 0.7083(3) 1.0680(5) 0.0605(2) 0.0238(12) Uani 1 1 d . . . C28 C 0.7125(5) 1.1963(6) 0.0474(3) 0.0403(16) Uani 1 1 d . . . H28 H 0.7639 1.2292 0.0426 0.048 Uiso 1 1 calc R . . C29 C 0.6461(4) 1.2698(6) 0.0419(3) 0.0425(16) Uani 1 1 d . . . H29 H 0.6494 1.3556 0.0353 0.051 Uiso 1 1 calc R . . C30 C 0.5717(4) 1.2155(6) 0.0463(2) 0.0363(14) Uani 1 1 d . . . H30 H 0.5217 1.2644 0.0393 0.044 Uiso 1 1 calc R . . C31 C 0.5674(3) 1.0950(5) 0.0601(2) 0.0243(12) Uani 1 1 d . . . H31 H 0.5155 1.0626 0.0640 0.029 Uiso 1 1 calc R . . C32 C 0.6647(3) 0.8111(5) -0.0082(2) 0.0229(11) Uani 1 1 d . . . C33A C 0.2573(12) -0.061(3) 0.1881(10) 0.077(6) Uani 0.671(5) 1 d PD A 1 H33A H 0.2602 0.0120 0.2132 0.092 Uiso 0.671(5) 1 calc PR A 1 H33B H 0.1996 -0.0970 0.1805 0.092 Uiso 0.671(5) 1 calc PR A 1 Cl1A Cl 0.2750(2) -0.0135(3) 0.11924(18) 0.0771(13) Uani 0.671(5) 1 d PD A 1 Cl2A Cl 0.3285(2) -0.1635(4) 0.22270(14) 0.0637(11) Uani 0.671(5) 1 d PD A 1 C33B C 0.255(2) 0.057(3) 0.1558(17) 0.113(14) Uani 0.329(5) 1 d PD A 2 H33C H 0.3022 0.1172 0.1609 0.136 Uiso 0.329(5) 1 calc PR A 2 H33D H 0.2320 0.0422 0.1136 0.136 Uiso 0.329(5) 1 calc PR A 2 Cl2B Cl 0.3008(14) -0.0871(18) 0.1894(10) 0.165(11) Uani 0.329(5) 1 d PD A 2 Cl1B Cl 0.1835(6) 0.1165(8) 0.1786(3) 0.097(3) Uani 0.329(5) 1 d PD A 2 C34 C 0.9321(5) 0.0553(6) 0.2109(3) 0.0482(19) Uani 1 1 d . . . H34A H 0.8992 -0.0223 0.2034 0.058 Uiso 1 1 calc R . . H34B H 0.9205 0.1009 0.1738 0.058 Uiso 1 1 calc R . . Cl3 Cl 0.89775(15) 0.14382(16) 0.26118(7) 0.0595(5) Uani 1 1 d . . . Cl4 Cl 1.04043(16) 0.0207(2) 0.23518(11) 0.0836(8) Uani 1 1 d . . . C35 C 0.0327(4) 0.6663(7) 0.2396(2) 0.0394(16) Uani 1 1 d . . . H35A H 0.0181 0.5792 0.2292 0.047 Uiso 1 1 calc R . . H35B H -0.0143 0.7181 0.2163 0.047 Uiso 1 1 calc R . . Cl5 Cl 0.04203(11) 0.68796(16) 0.31368(6) 0.0418(4) Uani 1 1 d . . . Cl6 Cl 0.12667(11) 0.70383(18) 0.22272(7) 0.0489(4) Uani 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 0.01449(19) 0.01353(19) 0.01557(19) 0.00112(16) 0.00663(14) 0.00320(16) S1 0.0205(6) 0.0103(6) 0.0238(6) 0.0029(5) 0.0054(5) 0.0009(5) S2 0.0207(6) 0.0203(7) 0.0251(7) -0.0040(5) 0.0088(5) -0.0032(5) S3 0.0226(6) 0.0151(6) 0.0293(7) 0.0051(5) 0.0134(5) 0.0031(5) N1 0.027(2) 0.026(2) 0.023(2) -0.0041(19) 0.0140(19) 0.006(2) N2 0.047(3) 0.031(3) 0.026(3) 0.000(2) 0.010(2) -0.015(2) N3 0.021(2) 0.030(3) 0.028(2) -0.0052(19) 0.0126(19) -0.0002(19) N4 0.029(3) 0.033(3) 0.031(3) -0.002(2) 0.014(2) -0.004(2) N5 0.022(2) 0.023(2) 0.021(2) -0.0048(18) 0.0042(18) 0.0131(19) P1 0.0183(6) 0.0125(6) 0.0201(6) 0.0031(5) 0.0104(5) 0.0039(5) B1 0.018(3) 0.025(3) 0.018(3) -0.002(2) 0.010(2) 0.007(2) O1 0.033(2) 0.075(3) 0.023(2) -0.001(2) 0.0063(18) 0.029(2) C1 0.016(2) 0.022(3) 0.020(2) 0.003(2) 0.009(2) 0.005(2) C2 0.033(3) 0.027(3) 0.026(3) 0.008(2) 0.017(2) 0.012(2) C3 0.021(3) 0.044(4) 0.023(3) 0.005(2) 0.008(2) 0.009(3) C4 0.022(3) 0.046(4) 0.021(3) -0.008(3) 0.005(2) 0.001(3) C5 0.024(3) 0.029(3) 0.034(3) -0.006(2) 0.010(2) -0.003(2) C6 0.022(3) 0.018(3) 0.027(3) -0.003(2) 0.010(2) 0.000(2) C7 0.025(3) 0.009(2) 0.017(2) 0.0008(18) 0.007(2) 0.006(2) C8 0.023(3) 0.019(3) 0.034(3) 0.008(2) 0.012(2) 0.006(2) C9 0.036(3) 0.022(3) 0.038(3) 0.013(2) 0.018(3) 0.004(2) C10 0.036(3) 0.019(3) 0.032(3) 0.012(2) 0.010(2) 0.012(2) C11 0.024(3) 0.020(3) 0.028(3) 0.000(2) 0.009(2) 0.006(2) C12 0.022(3) 0.016(3) 0.024(3) -0.002(2) 0.010(2) 0.000(2) C13 0.021(3) 0.012(3) 0.030(3) 0.006(2) 0.013(2) 0.0066(19) C14 0.033(3) 0.014(3) 0.032(3) 0.007(2) 0.014(2) 0.006(2) C15 0.034(3) 0.027(3) 0.045(4) 0.018(3) 0.029(3) 0.011(3) C16 0.024(3) 0.020(3) 0.057(4) 0.013(3) 0.022(3) 0.004(2) C17 0.022(3) 0.024(3) 0.037(3) 0.003(2) 0.009(2) 0.001(2) C18 0.020(3) 0.021(3) 0.030(3) 0.005(2) 0.013(2) 0.007(2) C19 0.027(3) 0.018(3) 0.016(2) -0.003(2) 0.010(2) -0.008(2) C20 0.041(4) 0.031(3) 0.029(3) -0.004(2) 0.017(3) 0.013(3) C21 0.075(5) 0.014(3) 0.032(3) -0.009(2) 0.031(3) 0.000(3) C22 0.062(5) 0.031(4) 0.034(3) 0.004(3) 0.009(3) -0.003(3) C23 0.020(3) 0.028(3) 0.020(3) 0.002(2) 0.007(2) -0.001(2) C24 0.025(3) 0.039(4) 0.040(3) -0.006(3) 0.018(3) 0.005(3) C25 0.027(3) 0.040(4) 0.040(3) -0.006(3) 0.016(3) 0.003(3) C26 0.025(3) 0.038(4) 0.042(4) -0.002(3) 0.011(3) -0.004(3) C27 0.026(3) 0.026(3) 0.018(3) 0.003(2) 0.005(2) 0.014(2) C28 0.057(4) 0.029(3) 0.033(3) 0.000(3) 0.009(3) 0.020(3) C29 0.056(4) 0.026(3) 0.038(3) 0.000(3) 0.001(3) 0.002(3) C30 0.041(4) 0.034(4) 0.030(3) -0.002(3) 0.005(3) -0.004(3) C31 0.022(3) 0.025(3) 0.025(3) -0.004(2) 0.006(2) 0.007(2) C32 0.019(3) 0.032(3) 0.020(3) -0.002(2) 0.009(2) 0.011(2) C33A 0.060(10) 0.090(14) 0.079(12) -0.031(10) 0.018(9) -0.025(10) Cl1A 0.0533(19) 0.055(2) 0.129(3) 0.025(2) 0.035(2) -0.0001(15) Cl2A 0.0425(17) 0.091(3) 0.0490(18) -0.0191(17) -0.0014(13) 0.0071(18) C33B 0.12(3) 0.08(2) 0.19(4) 0.00(3) 0.13(3) -0.01(2) Cl2B 0.25(3) 0.110(14) 0.188(18) -0.062(13) 0.15(2) -0.089(17) Cl1B 0.111(7) 0.087(6) 0.078(5) 0.010(4) 0.002(4) -0.046(5) C34 0.066(5) 0.037(4) 0.035(4) -0.002(3) 0.004(3) -0.029(4) Cl3 0.1029(16) 0.0331(9) 0.0400(9) 0.0074(7) 0.0159(10) -0.0105(10) Cl4 0.0764(16) 0.0600(14) 0.0919(17) 0.0009(12) -0.0128(13) 0.0136(12) C35 0.030(3) 0.058(4) 0.028(3) -0.013(3) 0.005(3) -0.006(3) Cl5 0.0492(10) 0.0498(10) 0.0292(8) -0.0069(7) 0.0154(7) -0.0183(8) Cl6 0.0425(9) 0.0703(13) 0.0381(9) -0.0075(8) 0.0180(7) -0.0096(9) _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 C32 1.813(5) . ? Ru1 B1 2.146(5) . ? Ru1 S3 2.3764(14) . ? Ru1 S2 2.3999(14) . ? Ru1 P1 2.4283(13) . ? Ru1 S1 2.4790(15) . ? S1 C19 1.717(5) . ? S2 C23 1.716(5) . ? S3 C27 1.722(5) . ? N1 C19 1.340(7) . ? N1 C20 1.384(6) . ? N1 B1 1.571(7) . ? N2 C19 1.359(6) . ? N2 C22 1.408(7) . ? N2 C21 1.450(8) . ? N3 C23 1.354(7) . ? N3 C24 1.404(7) . ? N3 B1 1.566(7) . ? N4 C23 1.353(7) . ? N4 C25 1.388(7) . ? N4 C26 1.437(7) . ? N5 C27 1.351(7) . ? N5 C31 1.360(6) . ? N5 B1 1.608(7) . ? P1 C13 1.833(5) . ? P1 C7 1.838(5) . ? P1 C1 1.842(5) . ? O1 C32 1.152(6) . ? C1 C6 1.386(7) . ? C1 C2 1.403(7) . ? C2 C3 1.385(7) . ? C2 H2 0.9500 . ? C3 C4 1.363(8) . ? C3 H3 0.9500 . ? C4 C5 1.378(8) . ? C4 H4 0.9500 . ? C5 C6 1.383(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.388(7) . ? C7 C12 1.402(7) . ? C8 C9 1.386(7) . ? C8 H8 0.9500 . ? C9 C10 1.385(8) . ? C9 H9 0.9500 . ? C10 C11 1.391(8) . ? C10 H10 0.9500 . ? C11 C12 1.373(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.387(7) . ? C13 C14 1.397(7) . ? C14 C15 1.403(8) . ? C14 H14 0.9500 . ? C15 C16 1.380(8) . ? C15 H15 0.9500 . ? C16 C17 1.371(8) . ? C16 H16 0.9500 . ? C17 C18 1.390(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C20 C21 1.341(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.334(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.436(8) . ? C28 C29 1.325(9) . ? C28 H28 0.9500 . ? C29 C30 1.384(9) . ? C29 H29 0.9500 . ? C30 C31 1.358(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C33A Cl2A 1.66(3) . ? C33A Cl1A 1.83(2) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C33B Cl1B 1.57(3) . ? C33B Cl2B 1.82(4) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34 Cl4 1.745(8) . ? C34 Cl3 1.756(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 Cl6 1.748(6) . ? C35 Cl5 1.758(6) . ? 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 C32 Ru1 B1 87.6(2) . . ? C32 Ru1 S3 87.76(18) . . ? B1 Ru1 S3 79.81(17) . . ? C32 Ru1 S2 88.87(18) . . ? B1 Ru1 S2 84.48(17) . . ? S3 Ru1 S2 164.05(5) . . ? C32 Ru1 P1 98.11(15) . . ? B1 Ru1 P1 173.11(16) . . ? S3 Ru1 P1 96.45(5) . . ? S2 Ru1 P1 99.46(5) . . ? C32 Ru1 S1 172.25(16) . . ? B1 Ru1 S1 84.75(15) . . ? S3 Ru1 S1 89.84(4) . . ? S2 Ru1 S1 91.44(5) . . ? P1 Ru1 S1 89.47(5) . . ? C19 S1 Ru1 97.32(17) . . ? C23 S2 Ru1 98.21(19) . . ? C27 S3 Ru1 101.1(2) . . ? C19 N1 C20 108.8(4) . . ? C19 N1 B1 122.1(4) . . ? C20 N1 B1 128.9(4) . . ? C19 N2 C22 126.8(5) . . ? C19 N2 C21 107.9(5) . . ? C22 N2 C21 125.3(5) . . ? C23 N3 C24 107.2(5) . . ? C23 N3 B1 117.5(4) . . ? C24 N3 B1 133.4(5) . . ? C23 N4 C25 109.1(5) . . ? C23 N4 C26 124.6(5) . . ? C25 N4 C26 126.1(5) . . ? C27 N5 C31 118.0(5) . . ? C27 N5 B1 114.8(4) . . ? C31 N5 B1 126.5(5) . . ? C13 P1 C7 100.2(2) . . ? C13 P1 C1 103.5(2) . . ? C7 P1 C1 101.8(2) . . ? C13 P1 Ru1 115.20(16) . . ? C7 P1 Ru1 117.74(16) . . ? C1 P1 Ru1 116.08(16) . . ? N3 B1 N1 105.8(4) . . ? N3 B1 N5 113.9(4) . . ? N1 B1 N5 103.2(4) . . ? N3 B1 Ru1 112.4(4) . . ? N1 B1 Ru1 110.8(3) . . ? N5 B1 Ru1 110.2(3) . . ? C6 C1 C2 118.5(5) . . ? C6 C1 P1 123.5(4) . . ? C2 C1 P1 118.0(4) . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.5(5) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 118.9(4) . . ? C8 C7 P1 117.8(4) . . ? C12 C7 P1 123.3(4) . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 120.4(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.5(5) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 120.6(5) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 119.2(5) . . ? C18 C13 P1 117.5(4) . . ? C14 C13 P1 123.2(4) . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.4(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.4(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.6(5) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? N1 C19 N2 108.4(5) . . ? N1 C19 S1 123.3(4) . . ? N2 C19 S1 128.1(4) . . ? C21 C20 N1 109.9(5) . . ? C21 C20 H20 125.1 . . ? N1 C20 H20 125.1 . . ? C20 C21 N2 105.0(5) . . ? C20 C21 H21 127.5 . . ? N2 C21 H21 127.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 N3 108.0(5) . . ? N4 C23 S2 127.2(4) . . ? N3 C23 S2 124.7(4) . . ? C25 C24 N3 108.7(5) . . ? C25 C24 H24 125.6 . . ? N3 C24 H24 125.6 . . ? C24 C25 N4 106.9(5) . . ? C24 C25 H25 126.5 . . ? N4 C25 H25 126.5 . . ? N4 C26 H26A 109.5 . . ? N4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 120.2(5) . . ? N5 C27 S3 119.8(4) . . ? C28 C27 S3 120.0(5) . . ? C29 C28 C27 121.2(7) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 116.8(6) . . ? C28 C29 H29 121.6 . . ? C30 C29 H29 121.6 . . ? C31 C30 C29 122.5(6) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 N5 121.1(6) . . ? C30 C31 H31 119.4 . . ? N5 C31 H31 119.4 . . ? O1 C32 Ru1 176.6(5) . . ? Cl2A C33A Cl1A 112.0(10) . . ? Cl2A C33A H33A 109.2 . . ? Cl1A C33A H33A 109.2 . . ? Cl2A C33A H33B 109.2 . . ? Cl1A C33A H33B 109.2 . . ? H33A C33A H33B 107.9 . . ? Cl1B C33B Cl2B 116.9(19) . . ? Cl1B C33B H33C 108.1 . . ? Cl2B C33B H33C 108.1 . . ? Cl1B C33B H33D 108.1 . . ? Cl2B C33B H33D 108.1 . . ? H33C C33B H33D 107.3 . . ? Cl4 C34 Cl3 112.4(3) . . ? Cl4 C34 H34A 109.1 . . ? Cl3 C34 H34A 109.1 . . ? Cl4 C34 H34B 109.1 . . ? Cl3 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? Cl6 C35 Cl5 111.9(3) . . ? Cl6 C35 H35A 109.2 . . ? Cl5 C35 H35A 109.2 . . ? Cl6 C35 H35B 109.2 . . ? Cl5 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? 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 C19 -7.2(2) . . . . ? S3 Ru1 S1 C19 72.54(17) . . . . ? S2 Ru1 S1 C19 -91.56(17) . . . . ? P1 Ru1 S1 C19 168.99(17) . . . . ? C32 Ru1 S2 C23 -77.9(2) . . . . ? B1 Ru1 S2 C23 9.7(2) . . . . ? S3 Ru1 S2 C23 -0.1(3) . . . . ? P1 Ru1 S2 C23 -175.99(17) . . . . ? S1 Ru1 S2 C23 94.31(17) . . . . ? C32 Ru1 S3 C27 63.5(2) . . . . ? B1 Ru1 S3 C27 -24.4(2) . . . . ? S2 Ru1 S3 C27 -14.4(3) . . . . ? P1 Ru1 S3 C27 161.46(17) . . . . ? S1 Ru1 S3 C27 -109.09(17) . . . . ? C32 Ru1 P1 C13 91.4(3) . . . . ? S3 Ru1 P1 C13 2.72(19) . . . . ? S2 Ru1 P1 C13 -178.43(18) . . . . ? S1 Ru1 P1 C13 -87.06(19) . . . . ? C32 Ru1 P1 C7 -150.8(3) . . . . ? S3 Ru1 P1 C7 120.59(19) . . . . ? S2 Ru1 P1 C7 -60.56(19) . . . . ? S1 Ru1 P1 C7 30.81(19) . . . . ? C32 Ru1 P1 C1 -29.8(3) . . . . ? S3 Ru1 P1 C1 -118.40(19) . . . . ? S2 Ru1 P1 C1 60.45(19) . . . . ? S1 Ru1 P1 C1 151.82(19) . . . . ? C23 N3 B1 N1 -103.5(5) . . . . ? C24 N3 B1 N1 58.4(7) . . . . ? C23 N3 B1 N5 143.8(4) . . . . ? C24 N3 B1 N5 -54.3(7) . . . . ? C23 N3 B1 Ru1 17.6(5) . . . . ? C24 N3 B1 Ru1 179.4(5) . . . . ? C19 N1 B1 N3 107.7(5) . . . . ? C20 N1 B1 N3 -66.7(7) . . . . ? C19 N1 B1 N5 -132.3(5) . . . . ? C20 N1 B1 N5 53.3(7) . . . . ? C19 N1 B1 Ru1 -14.4(6) . . . . ? C20 N1 B1 Ru1 171.3(5) . . . . ? C27 N5 B1 N3 -165.7(4) . . . . ? C31 N5 B1 N3 25.0(7) . . . . ? C27 N5 B1 N1 80.1(5) . . . . ? C31 N5 B1 N1 -89.2(5) . . . . ? C27 N5 B1 Ru1 -38.3(5) . . . . ? C31 N5 B1 Ru1 152.4(4) . . . . ? C32 Ru1 B1 N3 74.1(4) . . . . ? S3 Ru1 B1 N3 162.3(4) . . . . ? S2 Ru1 B1 N3 -15.0(3) . . . . ? S1 Ru1 B1 N3 -106.9(3) . . . . ? C32 Ru1 B1 N1 -167.7(4) . . . . ? S3 Ru1 B1 N1 -79.6(3) . . . . ? S2 Ru1 B1 N1 103.2(4) . . . . ? S1 Ru1 B1 N1 11.2(3) . . . . ? C32 Ru1 B1 N5 -54.1(4) . . . . ? S3 Ru1 B1 N5 34.0(3) . . . . ? S2 Ru1 B1 N5 -143.2(3) . . . . ? S1 Ru1 B1 N5 124.8(3) . . . . ? C13 P1 C1 C6 106.9(4) . . . . ? C7 P1 C1 C6 3.3(5) . . . . ? Ru1 P1 C1 C6 -125.9(4) . . . . ? C13 P1 C1 C2 -75.5(4) . . . . ? C7 P1 C1 C2 -179.1(4) . . . . ? Ru1 P1 C1 C2 51.7(4) . . . . ? C6 C1 C2 C3 -1.5(7) . . . . ? P1 C1 C2 C3 -179.2(4) . . . . ? C1 C2 C3 C4 2.1(8) . . . . ? C2 C3 C4 C5 -1.5(8) . . . . ? C3 C4 C5 C6 0.4(8) . . . . ? C4 C5 C6 C1 0.2(8) . . . . ? C2 C1 C6 C5 0.4(7) . . . . ? P1 C1 C6 C5 178.0(4) . . . . ? C13 P1 C7 C8 166.9(4) . . . . ? C1 P1 C7 C8 -86.9(4) . . . . ? Ru1 P1 C7 C8 41.2(4) . . . . ? C13 P1 C7 C12 -12.1(5) . . . . ? C1 P1 C7 C12 94.1(4) . . . . ? Ru1 P1 C7 C12 -137.8(4) . . . . ? C12 C7 C8 C9 -1.7(8) . . . . ? P1 C7 C8 C9 179.3(4) . . . . ? C7 C8 C9 C10 3.0(8) . . . . ? C8 C9 C10 C11 -2.0(9) . . . . ? C9 C10 C11 C12 -0.4(8) . . . . ? C10 C11 C12 C7 1.7(8) . . . . ? C8 C7 C12 C11 -0.6(7) . . . . ? P1 C7 C12 C11 178.3(4) . . . . ? C7 P1 C13 C18 -75.3(4) . . . . ? C1 P1 C13 C18 179.8(4) . . . . ? Ru1 P1 C13 C18 52.1(4) . . . . ? C7 P1 C13 C14 102.1(4) . . . . ? C1 P1 C13 C14 -2.8(5) . . . . ? Ru1 P1 C13 C14 -130.5(4) . . . . ? C18 C13 C14 C15 0.1(7) . . . . ? P1 C13 C14 C15 -177.3(4) . . . . ? C13 C14 C15 C16 1.1(8) . . . . ? C14 C15 C16 C17 -1.7(8) . . . . ? C15 C16 C17 C18 1.1(8) . . . . ? C14 C13 C18 C17 -0.7(7) . . . . ? P1 C13 C18 C17 176.8(4) . . . . ? C16 C17 C18 C13 0.1(8) . . . . ? C20 N1 C19 N2 -0.3(6) . . . . ? B1 N1 C19 N2 -175.7(4) . . . . ? C20 N1 C19 S1 -176.9(4) . . . . ? B1 N1 C19 S1 7.8(7) . . . . ? C22 N2 C19 N1 178.4(5) . . . . ? C21 N2 C19 N1 0.0(6) . . . . ? C22 N2 C19 S1 -5.3(8) . . . . ? C21 N2 C19 S1 176.3(4) . . . . ? Ru1 S1 C19 N1 2.0(5) . . . . ? Ru1 S1 C19 N2 -173.8(4) . . . . ? C19 N1 C20 C21 0.6(7) . . . . ? B1 N1 C20 C21 175.6(5) . . . . ? N1 C20 C21 N2 -0.6(7) . . . . ? C19 N2 C21 C20 0.4(6) . . . . ? C22 N2 C21 C20 -178.1(6) . . . . ? C25 N4 C23 N3 -1.3(6) . . . . ? C26 N4 C23 N3 -178.3(5) . . . . ? C25 N4 C23 S2 175.5(4) . . . . ? C26 N4 C23 S2 -1.4(8) . . . . ? C24 N3 C23 N4 2.1(6) . . . . ? B1 N3 C23 N4 168.4(4) . . . . ? C24 N3 C23 S2 -174.8(4) . . . . ? B1 N3 C23 S2 -8.6(6) . . . . ? Ru1 S2 C23 N4 -179.9(4) . . . . ? Ru1 S2 C23 N3 -3.6(5) . . . . ? C23 N3 C24 C25 -2.2(6) . . . . ? B1 N3 C24 C25 -165.4(5) . . . . ? N3 C24 C25 N4 1.4(7) . . . . ? C23 N4 C25 C24 0.0(6) . . . . ? C26 N4 C25 C24 176.8(5) . . . . ? C31 N5 C27 C28 4.0(7) . . . . ? B1 N5 C27 C28 -166.3(5) . . . . ? C31 N5 C27 S3 -174.6(4) . . . . ? B1 N5 C27 S3 15.2(6) . . . . ? Ru1 S3 C27 N5 11.7(4) . . . . ? Ru1 S3 C27 C28 -166.8(4) . . . . ? N5 C27 C28 C29 -1.1(8) . . . . ? S3 C27 C28 C29 177.4(5) . . . . ? C27 C28 C29 C30 -3.4(9) . . . . ? C28 C29 C30 C31 5.2(9) . . . . ? C29 C30 C31 N5 -2.4(9) . . . . ? C27 N5 C31 C30 -2.3(7) . . . . ? B1 N5 C31 C30 166.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.918 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.139 # Attachment 'Complex_5.cif' data_gro160-p21-c _database_code_depnum_ccdc_archive 'CCDC 736094' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C34 H27 B N3 O P Ru S3, C H2 Cl2' _chemical_formula_sum 'C35 H29 B Cl2 N3 O P Ru S3' _chemical_formula_weight 817.54 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' 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.948(3) _cell_length_b 13.124(3) _cell_length_c 19.139(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.87(3) _cell_angle_gamma 90.00 _cell_volume 3370.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5303 _cell_measurement_theta_min 2.1705 _cell_measurement_theta_max 27.1775 _exptl_crystal_description plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details '(SADABS; Bruker, 1998)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size ? _diffrn_source_target Mo _diffrn_source_type ? _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37481 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7715 _reflns_number_gt 6274 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. An isotropic restraint was applied to the boron atom and rigid bond restraints were applied to the bonds made by this atom to the nitrogen and ruthenium atoms. ; _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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7715 _refine_ls_number_parameters 424 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.000 _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 0.26679(2) 0.50650(3) 0.221032(19) 0.00836(9) Uani 1 1 d U . . S1 S 0.38082(8) 0.41659(8) 0.32145(6) 0.0126(2) Uani 1 1 d . . . S2 S 0.22328(7) 0.62878(8) 0.29996(6) 0.0115(2) Uani 1 1 d . . . S3 S 0.34382(8) 0.42590(8) 0.14058(6) 0.0128(2) Uani 1 1 d . . . P1 P 0.12241(8) 0.39871(9) 0.21557(6) 0.0098(2) Uani 1 1 d . . . B1 B 0.3868(3) 0.6082(4) 0.2401(3) 0.0071(9) Uani 1 1 d U . . N1 N 0.4609(2) 0.6010(3) 0.32109(19) 0.0093(7) Uani 1 1 d U . . N2 N 0.3470(2) 0.7238(3) 0.23663(18) 0.0091(7) Uani 1 1 d U . . N3 N 0.4581(2) 0.5912(3) 0.18743(18) 0.0092(7) Uani 1 1 d U . . O1 O 0.1635(2) 0.6296(2) 0.09119(17) 0.0195(7) Uani 1 1 d . . . C1 C 0.0073(3) 0.4634(3) 0.1656(2) 0.0094(9) Uani 1 1 d . . . C2 C -0.0395(3) 0.5296(3) 0.2032(3) 0.0162(10) Uani 1 1 d . . . H2 H -0.0157 0.5344 0.2546 0.019 Uiso 1 1 calc R . . C3 C -0.1196(3) 0.5881(4) 0.1669(3) 0.0194(10) Uani 1 1 d . . . H3 H -0.1503 0.6329 0.1933 0.023 Uiso 1 1 calc R . . C4 C -0.1555(3) 0.5820(4) 0.0920(3) 0.0163(10) Uani 1 1 d . . . H4 H -0.2110 0.6222 0.0671 0.020 Uiso 1 1 calc R . . C5 C -0.1106(3) 0.5176(3) 0.0536(3) 0.0181(10) Uani 1 1 d . . . H5 H -0.1351 0.5134 0.0023 0.022 Uiso 1 1 calc R . . C6 C -0.0288(3) 0.4582(3) 0.0904(2) 0.0148(10) Uani 1 1 d . . . H6 H 0.0023 0.4141 0.0638 0.018 Uiso 1 1 calc R . . C7 C 0.1121(3) 0.2723(3) 0.1724(2) 0.0107(9) Uani 1 1 d . . . C8 C 0.0226(3) 0.2215(3) 0.1437(2) 0.0132(9) Uani 1 1 d . . . H8 H -0.0385 0.2543 0.1428 0.016 Uiso 1 1 calc R . . C9 C 0.0214(3) 0.1232(3) 0.1163(2) 0.0139(9) Uani 1 1 d . . . H9 H -0.0404 0.0895 0.0968 0.017 Uiso 1 1 calc R . . C10 C 0.1094(3) 0.0743(4) 0.1171(2) 0.0179(10) Uani 1 1 d . . . H10 H 0.1086 0.0065 0.0996 0.021 Uiso 1 1 calc R . . C11 C 0.1995(3) 0.1262(3) 0.1441(3) 0.0181(10) Uani 1 1 d . . . H11 H 0.2605 0.0941 0.1438 0.022 Uiso 1 1 calc R . . C12 C 0.2003(3) 0.2236(3) 0.1711(2) 0.0130(9) Uani 1 1 d . . . H12 H 0.2621 0.2581 0.1891 0.016 Uiso 1 1 calc R . . C13 C 0.0928(3) 0.3684(3) 0.3010(2) 0.0117(9) Uani 1 1 d . . . C14 C 0.0049(3) 0.3182(4) 0.3016(3) 0.0184(10) Uani 1 1 d . . . H14 H -0.0392 0.2961 0.2571 0.022 Uiso 1 1 calc R . . C15 C -0.0192(3) 0.3000(4) 0.3658(3) 0.0207(11) Uani 1 1 d . . . H15 H -0.0805 0.2676 0.3649 0.025 Uiso 1 1 calc R . . C16 C 0.0449(3) 0.3286(3) 0.4310(3) 0.0182(10) Uani 1 1 d . . . H16 H 0.0289 0.3144 0.4752 0.022 Uiso 1 1 calc R . . C17 C 0.1328(3) 0.3781(4) 0.4321(3) 0.0180(10) Uani 1 1 d . . . H17 H 0.1770 0.3983 0.4771 0.022 Uiso 1 1 calc R . . C18 C 0.1567(3) 0.3986(3) 0.3672(2) 0.0152(10) Uani 1 1 d . . . H18 H 0.2168 0.4333 0.3683 0.018 Uiso 1 1 calc R . . C19 C 0.4652(3) 0.5111(3) 0.3570(2) 0.0123(9) Uani 1 1 d . . . C20 C 0.5375(3) 0.4977(4) 0.4242(2) 0.0172(9) Uani 1 1 d . . . H20 H 0.5453 0.4329 0.4473 0.021 Uiso 1 1 calc R . . C21 C 0.5966(3) 0.5776(4) 0.4563(2) 0.0186(10) Uani 1 1 d . . . H21 H 0.6437 0.5693 0.5023 0.022 Uiso 1 1 calc R . . C22 C 0.5869(3) 0.6712(4) 0.4207(2) 0.0164(10) Uani 1 1 d . . . H22 H 0.6262 0.7280 0.4424 0.020 Uiso 1 1 calc R . . C23 C 0.5205(3) 0.6799(3) 0.3544(2) 0.0130(9) Uani 1 1 d . . . H23 H 0.5150 0.7435 0.3300 0.016 Uiso 1 1 calc R . . C24 C 0.2781(3) 0.7361(3) 0.2755(2) 0.0096(9) Uani 1 1 d . . . C25 C 0.2507(3) 0.8353(3) 0.2898(2) 0.0124(9) Uani 1 1 d . . . H25 H 0.2086 0.8449 0.3208 0.015 Uiso 1 1 calc R . . C26 C 0.2834(3) 0.9177(3) 0.2601(2) 0.0136(9) Uani 1 1 d . . . H26 H 0.2633 0.9845 0.2692 0.016 Uiso 1 1 calc R . . C27 C 0.3474(3) 0.9025(3) 0.2158(2) 0.0140(9) Uani 1 1 d . . . H27 H 0.3696 0.9587 0.1931 0.017 Uiso 1 1 calc R . . C28 C 0.3771(3) 0.8065(3) 0.2059(2) 0.0119(9) Uani 1 1 d . . . H28 H 0.4209 0.7969 0.1762 0.014 Uiso 1 1 calc R . . C29 C 0.4405(3) 0.5082(3) 0.1427(2) 0.0121(9) Uani 1 1 d . . . C30 C 0.5038(3) 0.4870(3) 0.0979(2) 0.0143(9) Uani 1 1 d . . . H30 H 0.4915 0.4291 0.0669 0.017 Uiso 1 1 calc R . . C31 C 0.5823(3) 0.5497(4) 0.0990(2) 0.0158(10) Uani 1 1 d . . . H31 H 0.6238 0.5368 0.0680 0.019 Uiso 1 1 calc R . . C32 C 0.6012(3) 0.6333(3) 0.1463(2) 0.0147(10) Uani 1 1 d . . . H32 H 0.6558 0.6774 0.1480 0.018 Uiso 1 1 calc R . . C33 C 0.5406(3) 0.6504(3) 0.1896(2) 0.0123(9) Uani 1 1 d . . . H33 H 0.5556 0.7056 0.2230 0.015 Uiso 1 1 calc R . . C34 C 0.2005(3) 0.5816(3) 0.1416(2) 0.0104(9) Uani 1 1 d . . . C35 C 0.7520(3) 0.2459(4) 0.0236(2) 0.0212(11) Uani 1 1 d . . . H35A H 0.7972 0.3026 0.0200 0.025 Uiso 1 1 calc R . . H35B H 0.7658 0.2265 0.0754 0.025 Uiso 1 1 calc R . . Cl1 Cl 0.77550(9) 0.14102(10) -0.02676(7) 0.0292(3) Uani 1 1 d . . . Cl2 Cl 0.62671(10) 0.28730(12) -0.00873(8) 0.0414(4) Uani 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 0.00741(15) 0.00671(17) 0.01119(17) -0.00136(15) 0.00290(11) -0.00061(14) S1 0.0113(5) 0.0093(6) 0.0170(6) 0.0023(5) 0.0033(4) -0.0007(4) S2 0.0112(5) 0.0101(5) 0.0147(6) -0.0016(4) 0.0062(4) -0.0021(4) S3 0.0113(5) 0.0112(6) 0.0169(6) -0.0034(5) 0.0057(4) -0.0016(4) P1 0.0075(5) 0.0105(6) 0.0123(6) -0.0016(5) 0.0040(4) -0.0004(4) B1 0.0069(12) 0.0079(12) 0.0072(12) -0.0009(9) 0.0029(9) 0.0010(9) N1 0.0065(16) 0.0104(19) 0.0112(18) -0.0015(15) 0.0025(13) -0.0001(14) N2 0.0071(16) 0.0109(18) 0.0085(18) -0.0013(15) 0.0005(13) -0.0007(13) N3 0.0085(16) 0.0097(19) 0.0088(18) -0.0007(14) 0.0014(13) -0.0009(14) O1 0.0260(18) 0.0165(18) 0.0155(18) 0.0011(14) 0.0047(14) 0.0010(14) C1 0.008(2) 0.007(2) 0.013(2) -0.0021(17) 0.0027(16) -0.0036(15) C2 0.016(2) 0.017(3) 0.016(2) -0.0042(19) 0.0038(18) 0.0013(18) C3 0.016(2) 0.017(3) 0.025(3) -0.003(2) 0.007(2) 0.0018(19) C4 0.006(2) 0.016(2) 0.025(3) 0.004(2) 0.0009(18) 0.0003(17) C5 0.020(2) 0.015(3) 0.016(2) -0.001(2) 0.0003(18) -0.0034(19) C6 0.014(2) 0.015(2) 0.017(2) -0.0034(19) 0.0061(18) -0.0008(18) C7 0.016(2) 0.006(2) 0.011(2) 0.0010(17) 0.0059(17) -0.0001(17) C8 0.014(2) 0.011(2) 0.015(2) -0.0014(19) 0.0048(18) -0.0004(18) C9 0.017(2) 0.011(2) 0.014(2) -0.0018(18) 0.0060(18) -0.0092(18) C10 0.032(3) 0.010(2) 0.014(2) 0.0006(19) 0.012(2) -0.002(2) C11 0.021(2) 0.014(2) 0.025(3) 0.007(2) 0.015(2) 0.0055(19) C12 0.011(2) 0.014(2) 0.015(2) 0.0033(19) 0.0049(17) -0.0032(17) C13 0.017(2) 0.009(2) 0.010(2) 0.0017(18) 0.0057(17) 0.0051(17) C14 0.015(2) 0.021(3) 0.017(3) -0.004(2) 0.0015(19) -0.008(2) C15 0.016(2) 0.024(3) 0.025(3) -0.005(2) 0.011(2) -0.009(2) C16 0.025(3) 0.016(3) 0.016(3) 0.003(2) 0.009(2) 0.001(2) C17 0.019(2) 0.018(3) 0.015(2) 0.001(2) 0.0010(19) -0.0029(19) C18 0.013(2) 0.015(2) 0.017(2) -0.0017(19) 0.0042(18) -0.0033(18) C19 0.0104(19) 0.011(2) 0.017(2) -0.0027(19) 0.0073(16) 0.0000(18) C20 0.012(2) 0.024(3) 0.017(2) 0.003(2) 0.0062(17) 0.001(2) C21 0.011(2) 0.028(3) 0.015(2) 0.001(2) 0.0000(18) 0.0014(19) C22 0.013(2) 0.017(3) 0.021(3) -0.002(2) 0.0063(19) -0.0039(18) C23 0.009(2) 0.014(2) 0.017(2) -0.0025(19) 0.0058(17) -0.0009(17) C24 0.0055(19) 0.013(2) 0.010(2) -0.0019(17) 0.0000(16) 0.0009(16) C25 0.010(2) 0.013(2) 0.014(2) -0.0021(18) 0.0014(17) 0.0025(17) C26 0.012(2) 0.010(2) 0.017(2) -0.0027(19) 0.0008(17) 0.0009(17) C27 0.013(2) 0.010(2) 0.019(2) 0.0065(19) 0.0047(18) 0.0006(17) C28 0.008(2) 0.017(2) 0.010(2) 0.0053(18) 0.0020(16) 0.0036(17) C29 0.0078(18) 0.011(2) 0.017(2) 0.0061(19) 0.0020(16) 0.0025(18) C30 0.016(2) 0.014(2) 0.013(2) 0.0004(19) 0.0037(17) 0.0027(18) C31 0.013(2) 0.022(3) 0.016(2) 0.006(2) 0.0099(18) 0.0056(18) C32 0.009(2) 0.013(2) 0.021(3) 0.005(2) 0.0027(18) -0.0007(17) C33 0.009(2) 0.011(2) 0.015(2) 0.0018(18) 0.0001(17) -0.0005(17) C34 0.010(2) 0.010(2) 0.012(2) -0.0019(18) 0.0025(17) -0.0008(17) C35 0.026(3) 0.024(3) 0.011(2) -0.001(2) 0.0014(19) -0.002(2) Cl1 0.0242(6) 0.0276(7) 0.0322(8) -0.0058(6) 0.0017(5) 0.0037(5) Cl2 0.0374(8) 0.0444(9) 0.0402(9) -0.0005(7) 0.0070(6) 0.0206(7) _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 C34 1.835(4) . ? Ru1 B1 2.093(5) . ? Ru1 S3 2.3555(12) . ? Ru1 S2 2.3931(12) . ? Ru1 S1 2.4380(13) . ? Ru1 P1 2.4398(12) . ? S1 C19 1.718(4) . ? S2 C24 1.727(4) . ? S3 C29 1.720(4) . ? P1 C13 1.836(4) . ? P1 C1 1.837(4) . ? P1 C7 1.841(4) . ? B1 N2 1.611(6) . ? B1 N3 1.613(5) . ? B1 N1 1.614(6) . ? N1 C19 1.359(5) . ? N1 C23 1.371(5) . ? N2 C28 1.355(5) . ? N2 C24 1.376(5) . ? N3 C29 1.366(5) . ? N3 C33 1.380(5) . ? O1 C34 1.149(5) . ? C1 C6 1.391(6) . ? C1 C2 1.398(6) . ? C2 C3 1.377(6) . ? C2 H2 0.9500 . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.377(6) . ? C4 H4 0.9500 . ? C5 C6 1.402(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(6) . ? C7 C12 1.393(6) . ? C8 C9 1.391(6) . ? C8 H8 0.9500 . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 C11 1.399(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.392(6) . ? C13 C14 1.395(6) . ? C14 C15 1.381(6) . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.382(6) . ? C16 H16 0.9500 . ? C17 C18 1.397(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.412(6) . ? C20 C21 1.372(6) . ? C20 H20 0.9500 . ? C21 C22 1.394(6) . ? C21 H21 0.9500 . ? C22 C23 1.355(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.406(6) . ? C25 C26 1.357(6) . ? C25 H25 0.9500 . ? C26 C27 1.404(6) . ? C26 H26 0.9500 . ? C27 C28 1.355(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.416(6) . ? C30 C31 1.366(6) . ? C30 H30 0.9500 . ? C31 C32 1.400(6) . ? C31 H31 0.9500 . ? C32 C33 1.354(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C35 Cl1 1.762(5) . ? C35 Cl2 1.772(5) . ? 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 C34 Ru1 B1 90.00(18) . . ? C34 Ru1 S3 85.20(13) . . ? B1 Ru1 S3 85.07(13) . . ? C34 Ru1 S2 90.31(13) . . ? B1 Ru1 S2 77.95(13) . . ? S3 Ru1 S2 162.45(4) . . ? C34 Ru1 S1 170.13(13) . . ? B1 Ru1 S1 81.55(13) . . ? S3 Ru1 S1 88.97(4) . . ? S2 Ru1 S1 92.89(4) . . ? C34 Ru1 P1 93.01(13) . . ? B1 Ru1 P1 171.29(13) . . ? S3 Ru1 P1 103.31(4) . . ? S2 Ru1 P1 93.85(4) . . ? S1 Ru1 P1 96.09(4) . . ? C19 S1 Ru1 101.03(15) . . ? C24 S2 Ru1 99.67(14) . . ? C29 S3 Ru1 101.40(15) . . ? C13 P1 C1 100.69(19) . . ? C13 P1 C7 101.26(19) . . ? C1 P1 C7 103.50(19) . . ? C13 P1 Ru1 118.12(15) . . ? C1 P1 Ru1 110.38(14) . . ? C7 P1 Ru1 120.27(14) . . ? N2 B1 N3 111.6(3) . . ? N2 B1 N1 102.5(3) . . ? N3 B1 N1 104.5(3) . . ? N2 B1 Ru1 110.1(3) . . ? N3 B1 Ru1 113.8(3) . . ? N1 B1 Ru1 113.7(3) . . ? C19 N1 C23 118.9(4) . . ? C19 N1 B1 117.7(3) . . ? C23 N1 B1 123.4(3) . . ? C28 N2 C24 119.0(4) . . ? C28 N2 B1 129.0(3) . . ? C24 N2 B1 111.8(3) . . ? C29 N3 C33 118.2(3) . . ? C29 N3 B1 117.8(3) . . ? C33 N3 B1 123.7(3) . . ? C6 C1 C2 118.4(4) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 P1 119.0(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 120.4(4) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C12 118.4(4) . . ? C8 C7 P1 124.2(3) . . ? C12 C7 P1 117.4(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 118.9(4) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 121.0(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C18 C13 C14 118.2(4) . . ? C18 C13 P1 120.3(3) . . ? C14 C13 P1 121.5(3) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.3(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.3(4) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? N1 C19 C20 119.4(4) . . ? N1 C19 S1 119.7(3) . . ? C20 C19 S1 120.8(4) . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.3(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 118.8(4) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 N1 123.0(4) . . ? C22 C23 H23 118.5 . . ? N1 C23 H23 118.5 . . ? N2 C24 C25 118.8(4) . . ? N2 C24 S2 118.5(3) . . ? C25 C24 S2 122.6(3) . . ? C26 C25 C24 121.1(4) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 118.8(4) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 119.0(4) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? N2 C28 C27 122.8(4) . . ? N2 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? N3 C29 C30 120.1(4) . . ? N3 C29 S3 121.4(3) . . ? C30 C29 S3 118.5(3) . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.4(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 119.1(4) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 N3 122.9(4) . . ? C32 C33 H33 118.5 . . ? N3 C33 H33 118.5 . . ? O1 C34 Ru1 176.5(4) . . ? Cl1 C35 Cl2 111.2(3) . . ? Cl1 C35 H35A 109.4 . . ? Cl2 C35 H35A 109.4 . . ? Cl1 C35 H35B 109.4 . . ? Cl2 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? 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 C19 16.66(18) . . . . ? S3 Ru1 S1 C19 101.83(14) . . . . ? S2 Ru1 S1 C19 -60.71(14) . . . . ? P1 Ru1 S1 C19 -154.89(14) . . . . ? C34 Ru1 S2 C24 -59.31(19) . . . . ? B1 Ru1 S2 C24 30.62(19) . . . . ? S3 Ru1 S2 C24 15.6(2) . . . . ? S1 Ru1 S2 C24 111.35(14) . . . . ? P1 Ru1 S2 C24 -152.35(14) . . . . ? C34 Ru1 S3 C29 84.90(19) . . . . ? B1 Ru1 S3 C29 -5.52(19) . . . . ? S2 Ru1 S3 C29 9.2(2) . . . . ? S1 Ru1 S3 C29 -87.12(15) . . . . ? P1 Ru1 S3 C29 176.86(14) . . . . ? C34 Ru1 P1 C13 -137.0(2) . . . . ? S3 Ru1 P1 C13 137.26(16) . . . . ? S2 Ru1 P1 C13 -46.45(16) . . . . ? S1 Ru1 P1 C13 46.87(16) . . . . ? C34 Ru1 P1 C1 -21.9(2) . . . . ? S3 Ru1 P1 C1 -107.72(15) . . . . ? S2 Ru1 P1 C1 68.57(15) . . . . ? S1 Ru1 P1 C1 161.90(15) . . . . ? C34 Ru1 P1 C7 98.4(2) . . . . ? S3 Ru1 P1 C7 12.63(16) . . . . ? S2 Ru1 P1 C7 -171.08(16) . . . . ? S1 Ru1 P1 C7 -77.76(16) . . . . ? C34 Ru1 B1 N2 47.9(3) . . . . ? S3 Ru1 B1 N2 133.1(3) . . . . ? S2 Ru1 B1 N2 -42.4(2) . . . . ? S1 Ru1 B1 N2 -137.2(3) . . . . ? C34 Ru1 B1 N3 -78.3(3) . . . . ? S3 Ru1 B1 N3 6.9(3) . . . . ? S2 Ru1 B1 N3 -168.6(3) . . . . ? S1 Ru1 B1 N3 96.6(3) . . . . ? C34 Ru1 B1 N1 162.3(3) . . . . ? S3 Ru1 B1 N1 -112.5(3) . . . . ? S2 Ru1 B1 N1 72.0(3) . . . . ? S1 Ru1 B1 N1 -22.9(2) . . . . ? N2 B1 N1 C19 144.7(3) . . . . ? N3 B1 N1 C19 -98.7(4) . . . . ? Ru1 B1 N1 C19 25.9(4) . . . . ? N2 B1 N1 C23 -36.7(4) . . . . ? N3 B1 N1 C23 79.9(4) . . . . ? Ru1 B1 N1 C23 -155.5(3) . . . . ? N3 B1 N2 C28 -11.1(6) . . . . ? N1 B1 N2 C28 100.2(4) . . . . ? Ru1 B1 N2 C28 -138.5(4) . . . . ? N3 B1 N2 C24 173.7(3) . . . . ? N1 B1 N2 C24 -75.0(4) . . . . ? Ru1 B1 N2 C24 46.3(4) . . . . ? N2 B1 N3 C29 -132.3(4) . . . . ? N1 B1 N3 C29 117.7(4) . . . . ? Ru1 B1 N3 C29 -6.9(4) . . . . ? N2 B1 N3 C33 53.6(5) . . . . ? N1 B1 N3 C33 -56.4(5) . . . . ? Ru1 B1 N3 C33 179.0(3) . . . . ? C13 P1 C1 C6 -148.2(4) . . . . ? C7 P1 C1 C6 -43.8(4) . . . . ? Ru1 P1 C1 C6 86.2(4) . . . . ? C13 P1 C1 C2 39.5(4) . . . . ? C7 P1 C1 C2 143.9(3) . . . . ? Ru1 P1 C1 C2 -86.1(3) . . . . ? C6 C1 C2 C3 0.3(6) . . . . ? P1 C1 C2 C3 172.9(3) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C2 C1 C6 C5 -0.5(6) . . . . ? P1 C1 C6 C5 -172.9(3) . . . . ? C4 C5 C6 C1 0.3(7) . . . . ? C13 P1 C7 C8 71.5(4) . . . . ? C1 P1 C7 C8 -32.5(4) . . . . ? Ru1 P1 C7 C8 -156.2(3) . . . . ? C13 P1 C7 C12 -106.2(3) . . . . ? C1 P1 C7 C12 149.8(3) . . . . ? Ru1 P1 C7 C12 26.1(4) . . . . ? C12 C7 C8 C9 1.9(6) . . . . ? P1 C7 C8 C9 -175.7(3) . . . . ? C7 C8 C9 C10 0.0(7) . . . . ? C8 C9 C10 C11 -1.8(7) . . . . ? C9 C10 C11 C12 1.6(7) . . . . ? C10 C11 C12 C7 0.3(7) . . . . ? C8 C7 C12 C11 -2.0(6) . . . . ? P1 C7 C12 C11 175.8(3) . . . . ? C1 P1 C13 C18 -126.0(4) . . . . ? C7 P1 C13 C18 127.7(4) . . . . ? Ru1 P1 C13 C18 -5.9(4) . . . . ? C1 P1 C13 C14 51.7(4) . . . . ? C7 P1 C13 C14 -54.5(4) . . . . ? Ru1 P1 C13 C14 171.9(3) . . . . ? C18 C13 C14 C15 1.0(7) . . . . ? P1 C13 C14 C15 -176.8(4) . . . . ? C13 C14 C15 C16 -2.0(7) . . . . ? C14 C15 C16 C17 1.7(7) . . . . ? C15 C16 C17 C18 -0.3(7) . . . . ? C14 C13 C18 C17 0.4(6) . . . . ? P1 C13 C18 C17 178.2(3) . . . . ? C16 C17 C18 C13 -0.7(7) . . . . ? C23 N1 C19 C20 -6.3(6) . . . . ? B1 N1 C19 C20 172.4(3) . . . . ? C23 N1 C19 S1 172.0(3) . . . . ? B1 N1 C19 S1 -9.3(5) . . . . ? Ru1 S1 C19 N1 -8.3(3) . . . . ? Ru1 S1 C19 C20 170.0(3) . . . . ? N1 C19 C20 C21 6.1(6) . . . . ? S1 C19 C20 C21 -172.2(3) . . . . ? C19 C20 C21 C22 -2.2(6) . . . . ? C20 C21 C22 C23 -1.3(6) . . . . ? C21 C22 C23 N1 1.1(6) . . . . ? C19 N1 C23 C22 2.8(6) . . . . ? B1 N1 C23 C22 -175.8(4) . . . . ? C28 N2 C24 C25 -8.0(6) . . . . ? B1 N2 C24 C25 167.7(3) . . . . ? C28 N2 C24 S2 168.2(3) . . . . ? B1 N2 C24 S2 -16.0(4) . . . . ? Ru1 S2 C24 N2 -15.4(3) . . . . ? Ru1 S2 C24 C25 160.7(3) . . . . ? N2 C24 C25 C26 6.6(6) . . . . ? S2 C24 C25 C26 -169.5(3) . . . . ? C24 C25 C26 C27 -1.5(6) . . . . ? C25 C26 C27 C28 -2.1(6) . . . . ? C24 N2 C28 C27 4.6(6) . . . . ? B1 N2 C28 C27 -170.3(4) . . . . ? C26 C27 C28 N2 0.5(7) . . . . ? C33 N3 C29 C30 -2.6(6) . . . . ? B1 N3 C29 C30 -177.0(4) . . . . ? C33 N3 C29 S3 176.0(3) . . . . ? B1 N3 C29 S3 1.6(5) . . . . ? Ru1 S3 C29 N3 3.6(4) . . . . ? Ru1 S3 C29 C30 -177.8(3) . . . . ? N3 C29 C30 C31 -0.2(6) . . . . ? S3 C29 C30 C31 -178.9(3) . . . . ? C29 C30 C31 C32 1.7(6) . . . . ? C30 C31 C32 C33 -0.4(6) . . . . ? C31 C32 C33 N3 -2.6(6) . . . . ? C29 N3 C33 C32 4.0(6) . . . . ? B1 N3 C33 C32 178.1(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.249 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.120 # Attachment 'Ligand_2.cif' data_hugh_36_0m _database_code_depnum_ccdc_archive 'CCDC 736095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 B2 N10 S6, Na2, C8 H16 O2' _chemical_formula_sum 'C34 H46 B2 N10 Na2 O2 S6' _chemical_formula_weight 886.76 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' Na Na 0.0362 0.0249 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.98800(10) _cell_length_b 25.7781(4) _cell_length_c 10.4744(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.8750(10) _cell_angle_gamma 90.00 _cell_volume 2136.50(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6405 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 24.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6623 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'sadabs - bruker 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42766 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.63 _reflns_number_total 4955 _reflns_number_gt 3665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0865P)^2^+0.2237P] 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 4955 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Na1 Na 0.42581(17) 0.58623(4) 0.94557(11) 0.0472(3) Uani 1 1 d . . . S1 S 0.38187(8) 0.63877(2) 0.70695(7) 0.03182(18) Uani 1 1 d . . . S2 S 1.07728(9) 0.65818(2) 0.96332(6) 0.03351(19) Uani 1 1 d . . . S3 S 0.63364(9) 0.49943(2) 0.87573(6) 0.03353(19) Uani 1 1 d . . . B1 B 0.7825(3) 0.59778(10) 0.7596(2) 0.0229(5) Uani 1 1 d . . . H100 H 0.721(3) 0.6053(9) 0.847(2) 0.015(6) Uiso 1 1 d . . . N1 N 0.6546(2) 0.58499(7) 0.63967(18) 0.0217(4) Uani 1 1 d . . . N2 N 0.8974(2) 0.54791(7) 0.78648(18) 0.0229(4) Uani 1 1 d . . . N3 N 1.0451(3) 0.71474(8) 0.7425(2) 0.0301(5) Uani 1 1 d . . . N4 N 0.4280(3) 0.58277(8) 0.4963(2) 0.0296(5) Uani 1 1 d . . . N5 N 0.8897(3) 0.64485(7) 0.72501(19) 0.0241(4) Uani 1 1 d . . . C1 C 0.4919(3) 0.60149(9) 0.6146(2) 0.0240(5) Uani 1 1 d . . . C2 C 0.6899(3) 0.55641(10) 0.5338(2) 0.0284(5) Uani 1 1 d . . . H2 H 0.7930 0.5410 0.5253 0.034 Uiso 1 1 calc R . . C3 C 0.5511(3) 0.55471(10) 0.4462(2) 0.0325(6) Uani 1 1 d . . . H3 H 0.5399 0.5379 0.3670 0.039 Uiso 1 1 calc R . . C4 C 0.2555(4) 0.59055(13) 0.4338(3) 0.0443(7) Uani 1 1 d . . . H4A H 0.1794 0.5708 0.4780 0.066 Uiso 1 1 calc R . . H4B H 0.2464 0.5793 0.3457 0.066 Uiso 1 1 calc R . . H4C H 0.2271 0.6267 0.4365 0.066 Uiso 1 1 calc R . . C5 C 1.0004(3) 0.67270(9) 0.8089(2) 0.0257(5) Uani 1 1 d . . . C6 C 0.8717(3) 0.67024(10) 0.6064(2) 0.0327(6) Uani 1 1 d . . . H6 H 0.8043 0.6592 0.5319 0.039 Uiso 1 1 calc R . . C7 C 0.9672(3) 0.71306(10) 0.6172(3) 0.0354(6) Uani 1 1 d . . . H7 H 0.9786 0.7370 0.5526 0.043 Uiso 1 1 calc R . . C8 C 1.1661(4) 0.75425(10) 0.7952(3) 0.0425(7) Uani 1 1 d . . . H8A H 1.1339 0.7676 0.8739 0.064 Uiso 1 1 calc R . . H8B H 1.1672 0.7820 0.7341 0.064 Uiso 1 1 calc R . . H8C H 1.2768 0.7392 0.8124 0.064 Uiso 1 1 calc R . . C9 C 0.8376(3) 0.50435(9) 0.8406(2) 0.0278(5) Uani 1 1 d . . . C10 C 0.9494(4) 0.46208(10) 0.8673(3) 0.0394(7) Uani 1 1 d . . . H10 H 0.9127 0.4329 0.9078 0.047 Uiso 1 1 calc R . . C11 C 1.1068(4) 0.46259(11) 0.8360(3) 0.0430(7) Uani 1 1 d . . . H11 H 1.1782 0.4343 0.8545 0.052 Uiso 1 1 calc R . . C12 C 1.1614(4) 0.50629(10) 0.7753(3) 0.0356(6) Uani 1 1 d . . . H12 H 1.2681 0.5070 0.7494 0.043 Uiso 1 1 calc R . . C13 C 1.0571(3) 0.54788(9) 0.7543(2) 0.0290(5) Uani 1 1 d . . . H13 H 1.0960 0.5774 0.7167 0.035 Uiso 1 1 calc R . . O1 O 0.5775(3) 0.64235(7) 1.08700(19) 0.0407(5) Uani 1 1 d . . . C14 C 0.6077(7) 0.69201(17) 1.0229(5) 0.0367(12) Uani 0.712(9) 1 d P A 1 H14A H 0.5441 0.6937 0.9372 0.044 Uiso 0.712(9) 1 calc PR A 1 H14B H 0.7268 0.6967 1.0167 0.044 Uiso 0.712(9) 1 calc PR A 1 C15 C 0.5459(6) 0.73195(16) 1.1108(5) 0.0449(14) Uani 0.712(9) 1 d P A 1 H15A H 0.4236 0.7346 1.0975 0.054 Uiso 0.712(9) 1 calc PR A 1 H15B H 0.5948 0.7658 1.0995 0.054 Uiso 0.712(9) 1 calc PR A 1 C16 C 0.6109(8) 0.7088(3) 1.2420(7) 0.047(2) Uani 0.712(9) 1 d P A 1 H16A H 0.5478 0.7217 1.3082 0.057 Uiso 0.712(9) 1 calc PR A 1 H16B H 0.7301 0.7161 1.2667 0.057 Uiso 0.712(9) 1 calc PR A 1 C17 C 0.5795(13) 0.6511(2) 1.2171(5) 0.079(3) Uani 0.712(9) 1 d P A 1 H17A H 0.6684 0.6308 1.2661 0.095 Uiso 0.712(9) 1 calc PR A 1 H17B H 0.4723 0.6410 1.2433 0.095 Uiso 0.712(9) 1 calc PR A 1 C18 C 0.647(3) 0.6887(9) 1.092(2) 0.112(10) Uani 0.288(9) 1 d P A 2 H18A H 0.5774 0.7122 1.0352 0.135 Uiso 0.288(9) 1 calc PR A 2 H18B H 0.7575 0.6868 1.0632 0.135 Uiso 0.288(9) 1 calc PR A 2 C19 C 0.665(5) 0.7086(15) 1.226(3) 0.19(2) Uani 0.288(9) 1 d P A 2 H19A H 0.7830 0.7070 1.2642 0.226 Uiso 0.288(9) 1 calc PR A 2 H19B H 0.6293 0.7446 1.2259 0.226 Uiso 0.288(9) 1 calc PR A 2 C20 C 0.5653(16) 0.6782(6) 1.2987(14) 0.057(4) Uani 0.288(9) 1 d P A 2 H20A H 0.4993 0.7001 1.3482 0.069 Uiso 0.288(9) 1 calc PR A 2 H20B H 0.6356 0.6555 1.3573 0.069 Uiso 0.288(9) 1 calc PR A 2 C21 C 0.447(2) 0.6459(6) 1.1964(12) 0.056(4) Uani 0.288(9) 1 d P A 2 H21A H 0.3434 0.6642 1.1648 0.067 Uiso 0.288(9) 1 calc PR A 2 H21B H 0.4205 0.6120 1.2286 0.067 Uiso 0.288(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0718(9) 0.0389(6) 0.0328(6) -0.0042(5) 0.0135(6) -0.0232(6) S1 0.0246(3) 0.0338(3) 0.0390(4) -0.0067(3) 0.0112(3) 0.0039(2) S2 0.0405(4) 0.0290(3) 0.0309(3) -0.0051(2) 0.0045(3) -0.0070(3) S3 0.0420(4) 0.0334(3) 0.0255(3) 0.0032(2) 0.0058(3) -0.0151(3) B1 0.0237(14) 0.0222(12) 0.0237(12) 0.0016(10) 0.0060(11) 0.0008(10) N1 0.0212(10) 0.0241(9) 0.0209(9) -0.0020(7) 0.0074(8) 0.0010(7) N2 0.0239(11) 0.0244(9) 0.0199(9) -0.0026(7) 0.0012(8) 0.0004(8) N3 0.0269(11) 0.0232(10) 0.0432(13) 0.0011(9) 0.0148(10) -0.0005(8) N4 0.0225(11) 0.0360(11) 0.0297(11) -0.0040(9) 0.0019(8) 0.0025(8) N5 0.0248(11) 0.0234(9) 0.0258(10) 0.0022(7) 0.0089(8) 0.0003(8) C1 0.0217(12) 0.0244(11) 0.0264(11) 0.0003(9) 0.0055(9) -0.0014(9) C2 0.0263(13) 0.0346(13) 0.0257(12) -0.0053(10) 0.0089(10) 0.0046(10) C3 0.0318(15) 0.0402(14) 0.0261(12) -0.0076(10) 0.0060(11) 0.0056(11) C4 0.0294(15) 0.0575(18) 0.0434(16) -0.0075(14) -0.0041(12) 0.0054(13) C5 0.0237(12) 0.0211(10) 0.0344(13) -0.0023(9) 0.0118(10) 0.0014(9) C6 0.0360(15) 0.0343(13) 0.0290(13) 0.0065(10) 0.0087(11) 0.0010(11) C7 0.0351(15) 0.0323(13) 0.0418(15) 0.0109(11) 0.0159(12) 0.0033(11) C8 0.0411(17) 0.0287(13) 0.0613(19) -0.0037(12) 0.0198(14) -0.0120(11) C9 0.0364(15) 0.0243(11) 0.0206(11) -0.0020(9) -0.0039(10) -0.0033(10) C10 0.0529(19) 0.0259(12) 0.0346(14) -0.0015(10) -0.0109(13) 0.0014(12) C11 0.0432(18) 0.0334(14) 0.0475(17) -0.0109(12) -0.0111(14) 0.0079(12) C12 0.0263(14) 0.0363(14) 0.0432(15) -0.0129(11) 0.0015(11) 0.0046(11) C13 0.0255(13) 0.0268(12) 0.0341(13) -0.0064(10) 0.0020(10) -0.0015(9) O1 0.0538(13) 0.0313(10) 0.0365(11) -0.0055(8) 0.0045(9) -0.0008(9) C14 0.042(3) 0.0257(19) 0.044(3) -0.0074(19) 0.011(2) -0.0088(17) C15 0.048(3) 0.037(2) 0.053(3) -0.0136(19) 0.017(2) -0.0010(18) C16 0.046(3) 0.057(4) 0.039(4) -0.025(3) 0.005(3) 0.004(3) C17 0.149(8) 0.060(3) 0.028(3) -0.001(2) 0.008(4) 0.021(4) C18 0.15(2) 0.114(16) 0.091(15) -0.048(13) 0.071(15) -0.104(16) C19 0.28(4) 0.22(3) 0.089(18) -0.09(2) 0.11(3) -0.20(3) C20 0.046(7) 0.072(9) 0.049(7) -0.016(7) -0.011(6) -0.005(6) C21 0.068(10) 0.069(8) 0.029(6) -0.010(5) -0.002(6) -0.006(7) _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 Na1 O1 2.294(2) . ? Na1 H100 2.75(2) . ? Na1 S1 2.8221(13) . ? Na1 S3 2.9377(15) . ? Na1 S3 2.9746(12) 3_667 ? Na1 S2 3.3717(16) 1_455 ? S1 C1 1.692(2) . ? S2 C5 1.691(3) . ? S2 Na1 3.3716(16) 1_655 ? S3 C9 1.723(3) . ? S3 Na1 2.9746(12) 3_667 ? B1 N1 1.542(3) . ? B1 N5 1.556(3) . ? B1 N2 1.582(3) . ? B1 H100 1.12(2) . ? N1 C1 1.358(3) . ? N1 C2 1.392(3) . ? N2 C13 1.364(3) . ? N2 C9 1.373(3) . ? N3 C5 1.361(3) . ? N3 C7 1.374(4) . ? N3 C8 1.460(3) . ? N4 C1 1.362(3) . ? N4 C3 1.381(3) . ? N4 C4 1.456(3) . ? N5 C5 1.363(3) . ? N5 C6 1.394(3) . ? C2 C3 1.339(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C7 1.338(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.412(4) . ? C10 C11 1.342(4) . ? C10 H10 0.9300 . ? C11 C12 1.393(4) . ? C11 H11 0.9300 . ? C12 C13 1.357(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? O1 C18 1.317(17) . ? O1 C17 1.379(5) . ? O1 C14 1.481(5) . ? O1 C21 1.654(14) . ? C14 C15 1.509(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.522(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.526(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.48(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.42(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.568(17) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? 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 H100 Na1 140.9(16) . . ? O1 Na1 H100 74.0(5) . . ? O1 Na1 S1 105.06(6) . . ? H100 Na1 S1 65.9(5) . . ? O1 Na1 S3 112.00(7) . . ? H100 Na1 S3 59.9(5) . . ? S1 Na1 S3 98.68(4) . . ? O1 Na1 S3 100.22(6) . 3_667 ? H100 Na1 S3 126.1(5) . 3_667 ? S1 Na1 S3 154.47(5) . 3_667 ? S3 Na1 S3 74.68(3) . 3_667 ? O1 Na1 S2 89.11(6) . 1_455 ? H100 Na1 S2 132.9(5) . 1_455 ? S1 Na1 S2 77.37(4) . 1_455 ? S3 Na1 S2 158.72(4) . 1_455 ? S3 Na1 S2 99.75(4) 3_667 1_455 ? C1 S1 Na1 102.84(9) . . ? C5 S2 Na1 105.27(8) . 1_655 ? C9 S3 Na1 125.46(8) . . ? C9 S3 Na1 115.21(9) . 3_667 ? Na1 S3 Na1 105.32(3) . 3_667 ? N1 B1 N5 107.56(18) . . ? N1 B1 N2 105.95(18) . . ? N5 B1 N2 110.53(19) . . ? N1 B1 H100 113.1(12) . . ? N5 B1 H100 111.9(12) . . ? N2 B1 H100 107.7(12) . . ? C1 N1 C2 107.75(19) . . ? C1 N1 B1 126.87(19) . . ? C2 N1 B1 125.29(19) . . ? C13 N2 C9 119.5(2) . . ? C13 N2 B1 119.72(19) . . ? C9 N2 B1 120.8(2) . . ? C5 N3 C7 110.3(2) . . ? C5 N3 C8 124.7(2) . . ? C7 N3 C8 125.0(2) . . ? C1 N4 C3 109.5(2) . . ? C1 N4 C4 125.0(2) . . ? C3 N4 C4 125.5(2) . . ? C5 N5 C6 107.8(2) . . ? C5 N5 B1 126.1(2) . . ? C6 N5 B1 125.5(2) . . ? N1 C1 N4 107.10(19) . . ? N1 C1 S1 128.72(18) . . ? N4 C1 S1 124.17(18) . . ? C3 C2 N1 108.9(2) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N4 106.7(2) . . ? C2 C3 H3 126.6 . . ? N4 C3 H3 126.6 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N5 106.4(2) . . ? N3 C5 S2 125.34(19) . . ? N5 C5 S2 128.22(18) . . ? C7 C6 N5 108.9(2) . . ? C7 C6 H6 125.6 . . ? N5 C6 H6 125.6 . . ? C6 C7 N3 106.6(2) . . ? C6 C7 H7 126.7 . . ? N3 C7 H7 126.7 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 117.8(2) . . ? N2 C9 S3 122.73(18) . . ? C10 C9 S3 119.5(2) . . ? C11 C10 C9 122.2(3) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 119.3(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 N2 122.3(2) . . ? C12 C13 H13 118.8 . . ? N2 C13 H13 118.8 . . ? C18 O1 C17 82.2(9) . . ? C18 O1 C14 30.6(11) . . ? C17 O1 C14 109.1(3) . . ? C18 O1 C21 103.1(10) . . ? C17 O1 C21 39.6(5) . . ? C14 O1 C21 115.1(6) . . ? C18 O1 Na1 141.4(12) . . ? C17 O1 Na1 132.4(4) . . ? C14 O1 Na1 110.9(2) . . ? C21 O1 Na1 98.9(5) . . ? O1 C14 C15 103.1(4) . . ? O1 C14 H14A 111.2 . . ? C15 C14 H14A 111.2 . . ? O1 C14 H14B 111.2 . . ? C15 C14 H14B 111.2 . . ? H14A C14 H14B 109.1 . . ? C14 C15 C16 100.6(4) . . ? C14 C15 H15A 111.6 . . ? C16 C15 H15A 111.6 . . ? C14 C15 H15B 111.6 . . ? C16 C15 H15B 111.6 . . ? H15A C15 H15B 109.4 . . ? C15 C16 C17 101.5(5) . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16B 111.5 . . ? C17 C16 H16B 111.5 . . ? H16A C16 H16B 109.3 . . ? O1 C17 C16 107.9(5) . . ? O1 C17 H17A 110.1 . . ? C16 C17 H17A 110.1 . . ? O1 C17 H17B 110.1 . . ? C16 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? O1 C18 C19 109.7(18) . . ? O1 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? O1 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C18 109(2) . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? C19 C20 C21 105.0(17) . . ? C19 C20 H20A 110.7 . . ? C21 C20 H20A 110.7 . . ? C19 C20 H20B 110.7 . . ? C21 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C20 C21 O1 97.1(10) . . ? C20 C21 H21A 112.3 . . ? O1 C21 H21A 112.3 . . ? C20 C21 H21B 112.3 . . ? O1 C21 H21B 112.3 . . ? H21A C21 H21B 109.9 . . ? 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 O1 Na1 S1 C1 115.11(11) . . . . ? H100 Na1 S1 C1 50.8(5) . . . . ? S3 Na1 S1 C1 -0.58(9) . . . . ? S3 Na1 S1 C1 -73.09(15) 3_667 . . . ? S2 Na1 S1 C1 -159.29(9) 1_455 . . . ? O1 Na1 S3 C9 -42.48(13) . . . . ? H100 Na1 S3 C9 12.2(6) . . . . ? S1 Na1 S3 C9 67.71(11) . . . . ? S3 Na1 S3 C9 -137.51(11) 3_667 . . . ? S2 Na1 S3 C9 145.16(14) 1_455 . . . ? O1 Na1 S3 Na1 95.03(7) . . . 3_667 ? H100 Na1 S3 Na1 149.7(6) . . . 3_667 ? S1 Na1 S3 Na1 -154.77(5) . . . 3_667 ? S3 Na1 S3 Na1 0.0 3_667 . . 3_667 ? S2 Na1 S3 Na1 -77.32(11) 1_455 . . 3_667 ? N5 B1 N1 C1 -95.5(2) . . . . ? N2 B1 N1 C1 146.3(2) . . . . ? N5 B1 N1 C2 80.8(3) . . . . ? N2 B1 N1 C2 -37.5(3) . . . . ? N1 B1 N2 C13 103.9(2) . . . . ? N5 B1 N2 C13 -12.3(3) . . . . ? N1 B1 N2 C9 -75.4(2) . . . . ? N5 B1 N2 C9 168.38(19) . . . . ? N1 B1 N5 C5 170.3(2) . . . . ? N2 B1 N5 C5 -74.4(3) . . . . ? N1 B1 N5 C6 -0.2(3) . . . . ? N2 B1 N5 C6 115.1(2) . . . . ? C2 N1 C1 N4 0.8(3) . . . . ? B1 N1 C1 N4 177.5(2) . . . . ? C2 N1 C1 S1 -178.54(18) . . . . ? B1 N1 C1 S1 -1.8(3) . . . . ? C3 N4 C1 N1 -0.4(3) . . . . ? C4 N4 C1 N1 178.6(2) . . . . ? C3 N4 C1 S1 178.92(18) . . . . ? C4 N4 C1 S1 -2.1(4) . . . . ? Na1 S1 C1 N1 -52.8(2) . . . . ? Na1 S1 C1 N4 128.0(2) . . . . ? C1 N1 C2 C3 -0.9(3) . . . . ? B1 N1 C2 C3 -177.7(2) . . . . ? N1 C2 C3 N4 0.6(3) . . . . ? C1 N4 C3 C2 -0.1(3) . . . . ? C4 N4 C3 C2 -179.1(3) . . . . ? C7 N3 C5 N5 -1.4(3) . . . . ? C8 N3 C5 N5 -178.1(2) . . . . ? C7 N3 C5 S2 176.16(18) . . . . ? C8 N3 C5 S2 -0.5(3) . . . . ? C6 N5 C5 N3 1.3(3) . . . . ? B1 N5 C5 N3 -170.5(2) . . . . ? C6 N5 C5 S2 -176.18(19) . . . . ? B1 N5 C5 S2 11.9(3) . . . . ? Na1 S2 C5 N3 -88.6(2) 1_655 . . . ? Na1 S2 C5 N5 88.4(2) 1_655 . . . ? C5 N5 C6 C7 -0.8(3) . . . . ? B1 N5 C6 C7 171.2(2) . . . . ? N5 C6 C7 N3 -0.1(3) . . . . ? C5 N3 C7 C6 1.0(3) . . . . ? C8 N3 C7 C6 177.7(2) . . . . ? C13 N2 C9 C10 3.5(3) . . . . ? B1 N2 C9 C10 -177.2(2) . . . . ? C13 N2 C9 S3 -176.12(17) . . . . ? B1 N2 C9 S3 3.2(3) . . . . ? Na1 S3 C9 N2 -30.0(2) . . . . ? Na1 S3 C9 N2 -163.92(16) 3_667 . . . ? Na1 S3 C9 C10 150.42(17) . . . . ? Na1 S3 C9 C10 16.5(2) 3_667 . . . ? N2 C9 C10 C11 -3.1(4) . . . . ? S3 C9 C10 C11 176.5(2) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C13 2.8(4) . . . . ? C11 C12 C13 N2 -2.4(4) . . . . ? C9 N2 C13 C12 -0.8(3) . . . . ? B1 N2 C13 C12 179.9(2) . . . . ? H100 Na1 O1 C18 59(2) . . . . ? S1 Na1 O1 C18 -0.3(19) . . . . ? S3 Na1 O1 C18 105.8(19) . . . . ? S3 Na1 O1 C18 -176.7(19) 3_667 . . . ? S2 Na1 O1 C18 -76.9(19) 1_455 . . . ? H100 Na1 O1 C17 -153.2(7) . . . . ? S1 Na1 O1 C17 148.0(5) . . . . ? S3 Na1 O1 C17 -105.9(5) . . . . ? S3 Na1 O1 C17 -28.4(5) 3_667 . . . ? S2 Na1 O1 C17 71.4(5) 1_455 . . . ? H100 Na1 O1 C14 61.5(5) . . . . ? S1 Na1 O1 C14 2.7(3) . . . . ? S3 Na1 O1 C14 108.8(2) . . . . ? S3 Na1 O1 C14 -173.7(2) 3_667 . . . ? S2 Na1 O1 C14 -74.0(2) 1_455 . . . ? H100 Na1 O1 C21 -177.2(8) . . . . ? S1 Na1 O1 C21 124.0(6) . . . . ? S3 Na1 O1 C21 -129.9(6) . . . . ? S3 Na1 O1 C21 -52.4(6) 3_667 . . . ? S2 Na1 O1 C21 47.3(6) 1_455 . . . ? C18 O1 C14 C15 -56(2) . . . . ? C17 O1 C14 C15 -26.0(6) . . . . ? C21 O1 C14 C15 16.5(7) . . . . ? Na1 O1 C14 C15 127.6(3) . . . . ? O1 C14 C15 C16 40.1(5) . . . . ? C14 C15 C16 C17 -39.1(6) . . . . ? C18 O1 C17 C16 15.3(14) . . . . ? C14 O1 C17 C16 0.5(8) . . . . ? C21 O1 C17 C16 -106.2(11) . . . . ? Na1 O1 C17 C16 -145.3(4) . . . . ? C15 C16 C17 O1 24.8(8) . . . . ? C17 O1 C18 C19 0(2) . . . . ? C14 O1 C18 C19 151(4) . . . . ? C21 O1 C18 C19 34(3) . . . . ? Na1 O1 C18 C19 157(2) . . . . ? O1 C18 C19 C20 -15(4) . . . . ? C18 C19 C20 C21 -13(4) . . . . ? C19 C20 C21 O1 30(2) . . . . ? C18 O1 C21 C20 -39.1(16) . . . . ? C17 O1 C21 C20 21.0(8) . . . . ? C14 O1 C21 C20 -69.0(11) . . . . ? Na1 O1 C21 C20 172.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.702 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.160