Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name N.Connelly C.Adams S.Onganusorn _publ_contact_author_name 'Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Cyanide-bridged linkage isomers with catecholateruthenium(II) centres bound to Mn(I) or M(alkyne) units ; data_so432a _database_code_depnum_ccdc_archive 'CCDC 633387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H49 B Cl6 Mo N7 O5 P Ru' _chemical_formula_weight 1375.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 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 14.730(5) _cell_length_b 19.399(4) _cell_length_c 21.653(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.65(3) _cell_angle_gamma 90.00 _cell_volume 6157(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% none _diffrn_reflns_number 40302 _diffrn_reflns_av_R_equivalents 0.1163 _diffrn_reflns_av_sigmaI/netI 0.1655 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.47 _reflns_number_total 14071 _reflns_number_gt 6999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0568P)^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 14071 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1502 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 Mo1 Mo 0.40672(3) 0.48145(2) 0.31765(2) 0.02285(13) Uani 1 1 d . . . C30 C 0.5012(4) 0.5198(3) 0.2563(3) 0.0249(13) Uani 1 1 d . . . N7 N 0.5505(3) 0.5352(2) 0.2211(2) 0.0273(11) Uani 1 1 d . . . Ru1 Ru 0.64242(3) 0.55774(2) 0.15558(2) 0.02473(13) Uani 1 1 d . . . B1 B 0.3033(4) 0.5908(3) 0.4055(3) 0.0268(15) Uani 1 1 d . . . H1 H 0.2725 0.6236 0.4324 0.032 Uiso 1 1 calc R . . N1 N 0.4081(3) 0.5976(2) 0.4179(2) 0.0275(11) Uani 1 1 d . . . N2 N 0.4660(3) 0.5560(2) 0.38823(19) 0.0257(11) Uani 1 1 d . . . C1 C 0.4139(4) 0.6952(3) 0.4944(3) 0.0475(18) Uani 1 1 d . . . H1A H 0.3473 0.6921 0.4866 0.071 Uiso 1 1 calc R . . H1B H 0.4341 0.7408 0.4818 0.071 Uiso 1 1 calc R . . H1C H 0.4321 0.6883 0.5387 0.071 Uiso 1 1 calc R . . C2 C 0.4571(4) 0.6404(3) 0.4574(3) 0.0319(14) Uani 1 1 d . . . C3 C 0.5481(4) 0.6260(3) 0.4538(3) 0.0378(16) Uani 1 1 d . . . H3A H 0.5984 0.6479 0.4766 0.045 Uiso 1 1 calc R . . C4 C 0.5522(4) 0.5739(3) 0.4109(3) 0.0291(14) Uani 1 1 d . . . C5 C 0.6369(4) 0.5415(3) 0.3905(3) 0.0479(18) Uani 1 1 d . . . H5A H 0.6199 0.5061 0.3592 0.072 Uiso 1 1 calc R . . H5B H 0.6721 0.5203 0.4264 0.072 Uiso 1 1 calc R . . H5C H 0.6740 0.5768 0.3727 0.072 Uiso 1 1 calc R . . N3 N 0.2757(3) 0.5162(2) 0.41857(19) 0.0259(11) Uani 1 1 d . . . N4 N 0.3166(3) 0.4621(2) 0.3906(2) 0.0252(11) Uani 1 1 d . . . C6 C 0.1661(4) 0.5365(3) 0.4983(3) 0.0432(17) Uani 1 1 d . . . H6A H 0.1798 0.5849 0.4901 0.065 Uiso 1 1 calc R . . H6B H 0.1836 0.5260 0.5421 0.065 Uiso 1 1 calc R . . H6C H 0.1007 0.5281 0.4885 0.065 Uiso 1 1 calc R . . C7 C 0.2185(4) 0.4913(3) 0.4588(2) 0.0297(14) Uani 1 1 d . . . C8 C 0.2212(4) 0.4204(3) 0.4550(3) 0.0360(15) Uani 1 1 d . . . H8A H 0.1872 0.3889 0.4773 0.043 Uiso 1 1 calc R . . C9 C 0.2824(4) 0.4035(3) 0.4129(2) 0.0297(14) Uani 1 1 d . . . C10 C 0.3127(4) 0.3341(3) 0.3926(3) 0.0438(18) Uani 1 1 d . . . H10A H 0.3572 0.3398 0.3622 0.066 Uiso 1 1 calc R . . H10B H 0.2598 0.3084 0.3736 0.066 Uiso 1 1 calc R . . H10C H 0.3408 0.3087 0.4286 0.066 Uiso 1 1 calc R . . N5 N 0.2771(3) 0.6078(2) 0.3356(2) 0.0253(11) Uani 1 1 d . . . N6 N 0.3148(3) 0.5708(2) 0.29063(19) 0.0224(10) Uani 1 1 d . . . C11 C 0.1812(4) 0.7130(3) 0.3478(3) 0.0376(15) Uani 1 1 d . . . H11A H 0.1890 0.6998 0.3917 0.056 Uiso 1 1 calc R . . H11B H 0.1161 0.7135 0.3332 0.056 Uiso 1 1 calc R . . H11C H 0.2070 0.7589 0.3428 0.056 Uiso 1 1 calc R . . C12 C 0.2297(4) 0.6615(3) 0.3102(3) 0.0263(13) Uani 1 1 d . . . C13 C 0.2365(4) 0.6598(3) 0.2473(3) 0.0301(14) Uani 1 1 d . . . H13A H 0.2107 0.6916 0.2172 0.036 Uiso 1 1 calc R . . C14 C 0.2889(4) 0.6021(3) 0.2367(3) 0.0253(13) Uani 1 1 d . . . C15 C 0.3158(4) 0.5777(3) 0.1753(3) 0.0380(16) Uani 1 1 d . . . H15A H 0.3522 0.5355 0.1814 0.057 Uiso 1 1 calc R . . H15B H 0.3520 0.6134 0.1572 0.057 Uiso 1 1 calc R . . H15C H 0.2608 0.5681 0.1473 0.057 Uiso 1 1 calc R . . C16 C 0.2078(4) 0.3784(3) 0.1764(3) 0.0326(14) Uani 1 1 d . . . H16A H 0.2562 0.3539 0.1604 0.039 Uiso 1 1 calc R . . C17 C 0.1191(4) 0.3716(3) 0.1482(3) 0.0414(17) Uani 1 1 d . . . H17A H 0.1070 0.3430 0.1127 0.050 Uiso 1 1 calc R . . C18 C 0.0494(4) 0.4064(3) 0.1721(3) 0.0436(17) Uani 1 1 d . . . H18A H -0.0111 0.4015 0.1530 0.052 Uiso 1 1 calc R . . C19 C 0.0660(4) 0.4482(3) 0.2235(3) 0.0417(16) Uani 1 1 d . . . H19A H 0.0170 0.4717 0.2398 0.050 Uiso 1 1 calc R . . C20 C 0.1547(4) 0.4561(3) 0.2515(3) 0.0354(15) Uani 1 1 d . . . H20A H 0.1665 0.4855 0.2864 0.043 Uiso 1 1 calc R . . C21 C 0.2259(4) 0.4208(3) 0.2279(2) 0.0259(13) Uani 1 1 d . . . C22 C 0.3197(4) 0.4267(3) 0.2586(2) 0.0231(13) Uani 1 1 d . . . C23 C 0.3977(4) 0.3937(3) 0.2638(2) 0.0244(13) Uani 1 1 d . . . C24 C 0.4462(4) 0.3343(3) 0.2427(2) 0.0256(13) Uani 1 1 d . . . C25 C 0.5356(4) 0.3417(3) 0.2262(3) 0.0351(15) Uani 1 1 d . . . H25A H 0.5655 0.3851 0.2300 0.042 Uiso 1 1 calc R . . C26 C 0.5799(4) 0.2847(3) 0.2041(3) 0.0386(16) Uani 1 1 d . . . H26A H 0.6394 0.2895 0.1913 0.046 Uiso 1 1 calc R . . C27 C 0.5371(4) 0.2206(3) 0.2008(3) 0.0389(16) Uani 1 1 d . . . H27A H 0.5681 0.1818 0.1863 0.047 Uiso 1 1 calc R . . C28 C 0.4501(4) 0.2129(3) 0.2184(3) 0.0356(15) Uani 1 1 d . . . H28A H 0.4216 0.1690 0.2166 0.043 Uiso 1 1 calc R . . C29 C 0.4051(4) 0.2698(3) 0.2386(3) 0.0303(14) Uani 1 1 d . . . H29A H 0.3448 0.2648 0.2500 0.036 Uiso 1 1 calc R . . C31 C 0.5699(4) 0.6327(3) 0.1259(3) 0.0359(15) Uani 1 1 d . . . O1 O 0.5271(3) 0.6798(2) 0.1102(2) 0.0542(13) Uani 1 1 d . . . C32 C 0.5829(4) 0.4979(3) 0.0955(3) 0.0323(15) Uani 1 1 d . . . O2 O 0.5480(3) 0.4602(2) 0.0611(2) 0.0577(14) Uani 1 1 d . . . C33 C 0.7699(4) 0.5778(3) 0.2595(2) 0.0242(13) Uani 1 1 d . . . O3 O 0.7099(2) 0.61515(18) 0.22545(16) 0.0267(9) Uani 1 1 d . . . C34 C 0.7769(4) 0.5066(3) 0.2456(2) 0.0246(13) Uani 1 1 d . . . O4 O 0.7235(2) 0.48119(18) 0.19766(16) 0.0277(9) Uani 1 1 d . . . C35 C 0.8398(4) 0.4660(3) 0.2823(3) 0.0308(14) Uani 1 1 d . . . Cl1 Cl 0.84444(11) 0.37852(8) 0.26464(7) 0.0453(4) Uani 1 1 d . . . C36 C 0.8979(4) 0.4949(3) 0.3308(3) 0.0328(15) Uani 1 1 d . . . Cl2 Cl 0.97953(11) 0.44427(9) 0.37288(7) 0.0507(5) Uani 1 1 d . . . C37 C 0.8907(4) 0.5636(3) 0.3439(2) 0.0320(14) Uani 1 1 d . . . Cl3 Cl 0.96092(11) 0.60107(10) 0.40410(7) 0.0528(5) Uani 1 1 d . . . C38 C 0.8276(4) 0.6046(3) 0.3089(2) 0.0293(14) Uani 1 1 d . . . Cl4 Cl 0.81629(11) 0.69150(8) 0.32548(7) 0.0420(4) Uani 1 1 d . . . C39 C 0.5047(4) 0.4179(3) 0.3518(3) 0.0310(14) Uani 1 1 d . . . O5 O 0.5619(3) 0.3812(2) 0.3708(2) 0.0496(13) Uani 1 1 d . . . P1 P 0.75688(10) 0.58247(7) 0.09115(6) 0.0228(3) Uani 1 1 d . . . C1A C 0.8046(4) 0.5097(3) 0.0514(3) 0.0262(13) Uani 1 1 d . . . C1B C 0.8050(4) 0.4438(3) 0.0747(3) 0.0368(15) Uani 1 1 d . . . H1BA H 0.7773 0.4343 0.1115 0.044 Uiso 1 1 calc R . . C1C C 0.8461(5) 0.3914(3) 0.0443(3) 0.054(2) Uani 1 1 d . . . H1CA H 0.8466 0.3459 0.0607 0.065 Uiso 1 1 calc R . . C1D C 0.8858(5) 0.4039(3) -0.0090(3) 0.0504(19) Uani 1 1 d . . . H1DA H 0.9142 0.3675 -0.0292 0.060 Uiso 1 1 calc R . . C1E C 0.8845(5) 0.4688(3) -0.0330(3) 0.057(2) Uani 1 1 d . . . H1EA H 0.9115 0.4776 -0.0703 0.068 Uiso 1 1 calc R . . C1F C 0.8441(4) 0.5219(3) -0.0033(3) 0.0436(17) Uani 1 1 d . . . H1FA H 0.8432 0.5670 -0.0204 0.052 Uiso 1 1 calc R . . C1G C 0.8546(3) 0.6236(3) 0.1343(2) 0.0239(13) Uani 1 1 d . . . C1H C 0.9382(4) 0.5909(3) 0.1459(3) 0.0335(15) Uani 1 1 d . . . H1HA H 0.9473 0.5463 0.1295 0.040 Uiso 1 1 calc R . . C1I C 1.0086(4) 0.6239(4) 0.1817(3) 0.0496(19) Uani 1 1 d . . . H1IA H 1.0656 0.6011 0.1902 0.059 Uiso 1 1 calc R . . C1J C 0.9971(4) 0.6891(3) 0.2051(3) 0.0461(18) Uani 1 1 d . . . H1JA H 1.0461 0.7113 0.2290 0.055 Uiso 1 1 calc R . . C1K C 0.9151(4) 0.7214(3) 0.1936(3) 0.0365(15) Uani 1 1 d . . . H1KA H 0.9073 0.7666 0.2091 0.044 Uiso 1 1 calc R . . C1L C 0.8429(4) 0.6886(3) 0.1594(2) 0.0271(13) Uani 1 1 d . . . H1LA H 0.7851 0.7107 0.1530 0.033 Uiso 1 1 calc R . . C1M C 0.7244(4) 0.6420(3) 0.0282(2) 0.0276(13) Uani 1 1 d . . . C1N C 0.7834(4) 0.6942(3) 0.0120(2) 0.0303(14) Uani 1 1 d . . . H1NA H 0.8412 0.6998 0.0351 0.036 Uiso 1 1 calc R . . C1O C 0.7581(5) 0.7378(3) -0.0373(3) 0.0373(16) Uani 1 1 d . . . H1OA H 0.7981 0.7736 -0.0474 0.045 Uiso 1 1 calc R . . C1P C 0.6750(5) 0.7295(3) -0.0719(3) 0.0400(17) Uani 1 1 d . . . H1PA H 0.6581 0.7596 -0.1057 0.048 Uiso 1 1 calc R . . C1Q C 0.6166(4) 0.6779(4) -0.0576(3) 0.0459(18) Uani 1 1 d . . . H1QA H 0.5597 0.6721 -0.0817 0.055 Uiso 1 1 calc R . . C1R C 0.6409(4) 0.6345(3) -0.0082(3) 0.0378(16) Uani 1 1 d . . . H1RA H 0.6002 0.5989 0.0014 0.045 Uiso 1 1 calc R . . C100 C 0.1022(7) 0.7787(5) 0.0863(4) 0.093(3) Uani 1 1 d . . . H10D H 0.0974 0.8232 0.1082 0.112 Uiso 1 1 calc R . . H10E H 0.0796 0.7421 0.1127 0.112 Uiso 1 1 calc R . . Cl1A Cl 0.2113(2) 0.76369(16) 0.07807(15) 0.1286(11) Uani 1 1 d . . . Cl1B Cl 0.0317(2) 0.78178(12) 0.01639(12) 0.1112(10) 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 Mo1 0.0233(3) 0.0232(3) 0.0225(3) 0.0007(2) 0.0045(2) -0.0012(2) C30 0.029(3) 0.023(3) 0.022(3) 0.001(3) -0.001(3) 0.002(3) N7 0.024(3) 0.035(3) 0.022(3) -0.001(2) 0.000(2) -0.004(2) Ru1 0.0208(2) 0.0311(3) 0.0223(3) 0.0024(2) 0.00221(18) -0.0018(2) B1 0.034(4) 0.024(4) 0.022(4) -0.002(3) 0.001(3) 0.002(3) N1 0.030(3) 0.028(3) 0.024(3) -0.004(2) 0.000(2) -0.008(2) N2 0.027(3) 0.026(3) 0.024(3) -0.001(2) 0.005(2) -0.005(2) C1 0.056(5) 0.048(4) 0.036(4) -0.012(3) -0.009(3) -0.004(3) C2 0.039(4) 0.030(3) 0.025(3) 0.002(3) -0.002(3) -0.003(3) C3 0.046(4) 0.041(4) 0.025(4) 0.000(3) -0.008(3) -0.020(3) C4 0.024(3) 0.037(4) 0.026(3) 0.002(3) -0.001(3) -0.010(3) C5 0.033(4) 0.068(5) 0.041(4) -0.004(4) -0.001(3) -0.004(3) N3 0.028(3) 0.029(3) 0.021(3) 0.004(2) 0.008(2) 0.000(2) N4 0.025(3) 0.025(3) 0.026(3) -0.002(2) 0.004(2) -0.007(2) C6 0.039(4) 0.055(5) 0.039(4) 0.003(3) 0.016(3) 0.010(3) C7 0.026(3) 0.040(4) 0.024(3) 0.005(3) 0.003(3) 0.001(3) C8 0.032(4) 0.048(4) 0.029(4) 0.006(3) 0.008(3) -0.011(3) C9 0.039(4) 0.028(3) 0.023(3) 0.002(3) 0.004(3) -0.012(3) C10 0.068(5) 0.026(4) 0.040(4) 0.001(3) 0.015(3) -0.020(3) N5 0.030(3) 0.023(3) 0.023(3) -0.001(2) 0.005(2) 0.000(2) N6 0.026(3) 0.023(3) 0.018(3) -0.001(2) 0.001(2) -0.003(2) C11 0.043(4) 0.035(4) 0.035(4) 0.001(3) 0.006(3) 0.009(3) C12 0.023(3) 0.022(3) 0.034(4) 0.004(3) 0.004(3) -0.003(2) C13 0.023(3) 0.035(4) 0.031(4) 0.008(3) -0.002(3) -0.001(3) C14 0.022(3) 0.027(3) 0.026(3) 0.005(3) 0.000(2) -0.003(2) C15 0.041(4) 0.046(4) 0.027(4) 0.006(3) 0.003(3) -0.002(3) C16 0.039(4) 0.031(3) 0.028(4) -0.003(3) 0.001(3) 0.003(3) C17 0.042(4) 0.047(4) 0.033(4) -0.005(3) -0.004(3) -0.001(3) C18 0.033(4) 0.053(4) 0.044(4) 0.001(4) -0.006(3) -0.008(3) C19 0.024(3) 0.052(4) 0.051(4) -0.001(4) 0.011(3) 0.007(3) C20 0.036(4) 0.036(4) 0.036(4) -0.002(3) 0.008(3) 0.001(3) C21 0.026(3) 0.025(3) 0.026(3) 0.001(3) 0.000(3) 0.000(2) C22 0.027(3) 0.019(3) 0.024(3) 0.004(2) 0.008(2) 0.002(2) C23 0.025(3) 0.025(3) 0.023(3) 0.004(2) 0.001(2) -0.004(2) C24 0.029(3) 0.024(3) 0.024(3) 0.001(3) 0.001(2) 0.005(3) C25 0.034(4) 0.033(4) 0.038(4) -0.002(3) 0.006(3) -0.001(3) C26 0.023(3) 0.044(4) 0.050(4) 0.000(3) 0.008(3) 0.006(3) C27 0.045(4) 0.032(4) 0.038(4) -0.007(3) -0.003(3) 0.017(3) C28 0.042(4) 0.024(3) 0.040(4) -0.003(3) -0.003(3) 0.001(3) C29 0.026(3) 0.031(3) 0.033(4) -0.002(3) 0.000(3) 0.000(3) C31 0.031(4) 0.055(4) 0.021(3) 0.008(3) 0.002(3) 0.005(3) O1 0.048(3) 0.061(3) 0.054(3) 0.016(3) 0.009(2) 0.023(3) C32 0.029(4) 0.040(4) 0.029(4) 0.009(3) 0.004(3) -0.004(3) O2 0.059(3) 0.059(3) 0.053(3) -0.010(3) -0.012(3) -0.024(3) C33 0.019(3) 0.035(3) 0.019(3) 0.000(3) 0.005(2) 0.000(2) O3 0.023(2) 0.032(2) 0.024(2) -0.0012(18) -0.0010(17) 0.0030(17) C34 0.019(3) 0.038(4) 0.017(3) 0.009(3) 0.005(2) 0.003(2) O4 0.026(2) 0.029(2) 0.027(2) 0.0004(18) -0.0026(17) 0.0005(17) C35 0.033(4) 0.031(3) 0.030(3) 0.006(3) 0.009(3) 0.004(3) Cl1 0.0534(11) 0.0362(9) 0.0454(11) 0.0053(8) 0.0007(8) 0.0099(8) C36 0.030(3) 0.048(4) 0.020(3) 0.013(3) 0.000(3) 0.006(3) Cl2 0.0430(10) 0.0714(12) 0.0357(10) 0.0113(9) -0.0063(8) 0.0157(9) C37 0.029(3) 0.045(4) 0.021(3) -0.001(3) -0.002(3) -0.006(3) Cl3 0.0466(11) 0.0750(13) 0.0334(10) -0.0041(9) -0.0129(8) -0.0116(9) C38 0.031(3) 0.037(4) 0.021(3) 0.000(3) 0.009(3) -0.001(3) Cl4 0.0481(10) 0.0436(10) 0.0339(9) -0.0129(7) 0.0025(7) -0.0015(8) C39 0.037(4) 0.034(4) 0.022(3) 0.002(3) 0.003(3) -0.006(3) O5 0.050(3) 0.046(3) 0.050(3) 0.005(2) -0.012(2) 0.014(2) P1 0.0221(8) 0.0244(8) 0.0221(8) 0.0021(6) 0.0030(6) -0.0009(6) C1A 0.027(3) 0.023(3) 0.028(3) -0.004(3) 0.001(3) -0.005(2) C1B 0.044(4) 0.036(4) 0.031(4) 0.000(3) 0.011(3) 0.000(3) C1C 0.076(6) 0.036(4) 0.054(5) -0.003(4) 0.022(4) 0.009(4) C1D 0.063(5) 0.029(4) 0.061(5) -0.020(4) 0.019(4) 0.007(3) C1E 0.078(6) 0.040(4) 0.058(5) -0.006(4) 0.037(4) 0.008(4) C1F 0.055(4) 0.026(4) 0.055(5) -0.003(3) 0.027(3) -0.002(3) C1G 0.021(3) 0.034(3) 0.018(3) 0.000(3) 0.005(2) -0.003(2) C1H 0.032(4) 0.031(3) 0.037(4) -0.009(3) 0.000(3) 0.005(3) C1I 0.023(4) 0.070(5) 0.053(5) -0.012(4) -0.007(3) 0.007(3) C1J 0.024(4) 0.057(5) 0.056(5) -0.020(4) -0.001(3) -0.010(3) C1K 0.040(4) 0.033(4) 0.037(4) -0.007(3) 0.005(3) -0.003(3) C1L 0.025(3) 0.032(3) 0.025(3) 0.000(3) 0.004(2) 0.003(3) C1M 0.029(3) 0.035(4) 0.020(3) -0.003(3) 0.005(2) 0.010(3) C1N 0.038(4) 0.033(4) 0.020(3) -0.001(3) 0.005(3) 0.004(3) C1O 0.063(5) 0.028(4) 0.023(4) 0.001(3) 0.011(3) 0.001(3) C1P 0.063(5) 0.034(4) 0.024(4) 0.006(3) 0.009(3) 0.020(3) C1Q 0.041(4) 0.073(5) 0.022(4) 0.009(4) -0.003(3) 0.020(4) C1R 0.039(4) 0.048(4) 0.027(4) 0.002(3) 0.005(3) 0.001(3) C100 0.133(9) 0.087(7) 0.060(6) -0.012(5) 0.016(6) 0.009(6) Cl1A 0.103(2) 0.142(3) 0.143(3) -0.009(2) 0.0225(19) -0.027(2) Cl1B 0.148(3) 0.0680(16) 0.109(2) 0.0212(14) -0.0304(18) 0.0002(16) _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 Mo1 C39 1.985(6) . ? Mo1 C22 2.020(5) . ? Mo1 C23 2.060(5) . ? Mo1 C30 2.149(6) . ? Mo1 N4 2.193(5) . ? Mo1 N2 2.219(4) . ? Mo1 N6 2.242(4) . ? C30 N7 1.144(7) . ? N7 Ru1 2.101(5) . ? Ru1 C31 1.880(6) . ? Ru1 C32 1.893(6) . ? Ru1 O3 2.055(3) . ? Ru1 O4 2.061(3) . ? Ru1 P1 2.3414(17) . ? B1 N3 1.538(7) . ? B1 N1 1.546(7) . ? B1 N5 1.559(7) . ? N1 C2 1.349(7) . ? N1 N2 1.378(6) . ? N2 C4 1.361(6) . ? C1 C2 1.509(8) . ? C2 C3 1.378(8) . ? C3 C4 1.377(8) . ? C4 C5 1.502(8) . ? N3 C7 1.359(7) . ? N3 N4 1.379(6) . ? N4 C9 1.352(6) . ? C6 C7 1.491(8) . ? C7 C8 1.379(8) . ? C8 C9 1.383(8) . ? C9 C10 1.499(8) . ? N5 C12 1.343(6) . ? N5 N6 1.371(6) . ? N6 C14 1.337(6) . ? C11 C12 1.510(7) . ? C12 C13 1.377(7) . ? C13 C14 1.390(7) . ? C14 C15 1.501(8) . ? C16 C21 1.390(7) . ? C16 C17 1.392(8) . ? C17 C18 1.372(8) . ? C18 C19 1.379(8) . ? C19 C20 1.393(8) . ? C20 C21 1.392(8) . ? C21 C22 1.477(7) . ? C22 C23 1.311(7) . ? C23 C24 1.453(7) . ? C24 C29 1.389(7) . ? C24 C25 1.405(8) . ? C25 C26 1.393(8) . ? C26 C27 1.392(8) . ? C27 C28 1.380(8) . ? C28 C29 1.382(7) . ? C31 O1 1.142(6) . ? C32 O2 1.130(6) . ? C33 O3 1.311(6) . ? C33 C38 1.399(7) . ? C33 C34 1.421(7) . ? C34 O4 1.333(6) . ? C34 C35 1.401(7) . ? C35 C36 1.404(8) . ? C35 Cl1 1.743(6) . ? C36 C37 1.370(8) . ? C36 Cl2 1.739(5) . ? C37 C38 1.392(7) . ? C37 Cl3 1.740(5) . ? C38 Cl4 1.735(6) . ? C39 O5 1.148(6) . ? P1 C1M 1.815(5) . ? P1 C1G 1.821(5) . ? P1 C1A 1.829(6) . ? C1A C1B 1.374(7) . ? C1A C1F 1.391(8) . ? C1B C1C 1.383(8) . ? C1C C1D 1.365(9) . ? C1D C1E 1.362(9) . ? C1E C1F 1.379(8) . ? C1G C1H 1.385(7) . ? C1G C1L 1.391(7) . ? C1H C1I 1.387(8) . ? C1I C1J 1.379(8) . ? C1J C1K 1.362(8) . ? C1K C1L 1.390(7) . ? C1M C1R 1.401(7) . ? C1M C1N 1.402(8) . ? C1N C1O 1.384(7) . ? C1O C1P 1.380(8) . ? C1P C1Q 1.375(9) . ? C1Q C1R 1.380(8) . ? C100 Cl1A 1.659(9) . ? C100 Cl1B 1.750(8) . ? 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 C39 Mo1 C22 107.6(2) . . ? C39 Mo1 C23 72.6(2) . . ? C22 Mo1 C23 37.46(19) . . ? C39 Mo1 C30 87.4(2) . . ? C22 Mo1 C30 101.6(2) . . ? C23 Mo1 C30 87.0(2) . . ? C39 Mo1 N4 95.5(2) . . ? C22 Mo1 N4 88.52(18) . . ? C23 Mo1 N4 104.82(18) . . ? C30 Mo1 N4 168.21(18) . . ? C39 Mo1 N2 85.8(2) . . ? C22 Mo1 N2 163.74(19) . . ? C23 Mo1 N2 157.99(19) . . ? C30 Mo1 N2 88.00(18) . . ? N4 Mo1 N2 80.81(16) . . ? C39 Mo1 N6 167.41(19) . . ? C22 Mo1 N6 84.94(18) . . ? C23 Mo1 N6 119.20(18) . . ? C30 Mo1 N6 88.96(18) . . ? N4 Mo1 N6 85.83(16) . . ? N2 Mo1 N6 82.08(15) . . ? N7 C30 Mo1 174.3(5) . . ? C30 N7 Ru1 176.9(5) . . ? C31 Ru1 C32 91.7(3) . . ? C31 Ru1 O3 92.8(2) . . ? C32 Ru1 O3 175.00(19) . . ? C31 Ru1 O4 173.5(2) . . ? C32 Ru1 O4 94.1(2) . . ? O3 Ru1 O4 81.24(14) . . ? C31 Ru1 N7 90.5(2) . . ? C32 Ru1 N7 92.9(2) . . ? O3 Ru1 N7 84.99(15) . . ? O4 Ru1 N7 86.31(16) . . ? C31 Ru1 P1 93.20(19) . . ? C32 Ru1 P1 91.61(18) . . ? O3 Ru1 P1 90.17(11) . . ? O4 Ru1 P1 89.49(11) . . ? N7 Ru1 P1 174.03(12) . . ? N3 B1 N1 109.0(4) . . ? N3 B1 N5 109.4(4) . . ? N1 B1 N5 107.3(5) . . ? C2 N1 N2 109.8(4) . . ? C2 N1 B1 128.7(5) . . ? N2 N1 B1 121.5(4) . . ? C4 N2 N1 106.3(4) . . ? C4 N2 Mo1 134.8(4) . . ? N1 N2 Mo1 118.9(3) . . ? N1 C2 C3 107.6(5) . . ? N1 C2 C1 122.8(5) . . ? C3 C2 C1 129.5(5) . . ? C4 C3 C2 107.2(5) . . ? N2 C4 C3 109.2(5) . . ? N2 C4 C5 124.0(5) . . ? C3 C4 C5 126.8(5) . . ? C7 N3 N4 109.6(4) . . ? C7 N3 B1 130.2(5) . . ? N4 N3 B1 120.0(4) . . ? C9 N4 N3 106.7(5) . . ? C9 N4 Mo1 132.4(4) . . ? N3 N4 Mo1 120.5(3) . . ? N3 C7 C8 107.1(5) . . ? N3 C7 C6 123.1(5) . . ? C8 C7 C6 129.8(5) . . ? C7 C8 C9 107.4(5) . . ? N4 C9 C8 109.1(5) . . ? N4 C9 C10 121.2(5) . . ? C8 C9 C10 129.6(5) . . ? C12 N5 N6 110.2(4) . . ? C12 N5 B1 129.1(5) . . ? N6 N5 B1 120.1(4) . . ? C14 N6 N5 106.4(4) . . ? C14 N6 Mo1 133.8(4) . . ? N5 N6 Mo1 119.7(3) . . ? N5 C12 C13 107.5(5) . . ? N5 C12 C11 123.2(5) . . ? C13 C12 C11 129.3(5) . . ? C12 C13 C14 106.2(5) . . ? N6 C14 C13 109.7(5) . . ? N6 C14 C15 123.5(5) . . ? C13 C14 C15 126.8(5) . . ? C21 C16 C17 120.4(6) . . ? C18 C17 C16 119.5(6) . . ? C17 C18 C19 121.0(6) . . ? C18 C19 C20 119.9(6) . . ? C21 C20 C19 119.7(6) . . ? C16 C21 C20 119.5(5) . . ? C16 C21 C22 120.3(5) . . ? C20 C21 C22 120.1(5) . . ? C23 C22 C21 140.6(5) . . ? C23 C22 Mo1 73.0(3) . . ? C21 C22 Mo1 146.4(4) . . ? C22 C23 C24 144.6(5) . . ? C22 C23 Mo1 69.6(3) . . ? C24 C23 Mo1 145.7(4) . . ? C29 C24 C25 119.3(5) . . ? C29 C24 C23 120.5(5) . . ? C25 C24 C23 120.1(5) . . ? C26 C25 C24 119.2(6) . . ? C27 C26 C25 120.2(6) . . ? C28 C27 C26 120.6(6) . . ? C27 C28 C29 119.3(6) . . ? C28 C29 C24 121.3(6) . . ? O1 C31 Ru1 177.0(6) . . ? O2 C32 Ru1 177.4(5) . . ? O3 C33 C38 123.3(5) . . ? O3 C33 C34 118.5(5) . . ? C38 C33 C34 118.2(5) . . ? C33 O3 Ru1 111.4(3) . . ? O4 C34 C35 122.7(5) . . ? O4 C34 C33 118.3(4) . . ? C35 C34 C33 118.9(5) . . ? C34 O4 Ru1 110.5(3) . . ? C34 C35 C36 121.4(5) . . ? C34 C35 Cl1 117.4(4) . . ? C36 C35 Cl1 121.2(4) . . ? C37 C36 C35 119.3(5) . . ? C37 C36 Cl2 120.2(4) . . ? C35 C36 Cl2 120.4(5) . . ? C36 C37 C38 120.3(5) . . ? C36 C37 Cl3 120.7(4) . . ? C38 C37 Cl3 119.1(5) . . ? C37 C38 C33 121.9(5) . . ? C37 C38 Cl4 121.0(4) . . ? C33 C38 Cl4 117.1(4) . . ? O5 C39 Mo1 179.1(5) . . ? C1M P1 C1G 104.1(3) . . ? C1M P1 C1A 102.9(2) . . ? C1G P1 C1A 105.0(2) . . ? C1M P1 Ru1 115.21(19) . . ? C1G P1 Ru1 111.31(18) . . ? C1A P1 Ru1 117.06(19) . . ? C1B C1A C1F 118.9(5) . . ? C1B C1A P1 122.2(5) . . ? C1F C1A P1 118.8(4) . . ? C1A C1B C1C 119.7(6) . . ? C1D C1C C1B 121.0(6) . . ? C1E C1D C1C 119.8(6) . . ? C1D C1E C1F 120.2(7) . . ? C1E C1F C1A 120.4(6) . . ? C1H C1G C1L 119.1(5) . . ? C1H C1G P1 122.5(4) . . ? C1L C1G P1 118.3(4) . . ? C1G C1H C1I 119.5(5) . . ? C1J C1I C1H 121.0(6) . . ? C1K C1J C1I 119.6(6) . . ? C1J C1K C1L 120.3(6) . . ? C1K C1L C1G 120.3(5) . . ? C1R C1M C1N 117.9(5) . . ? C1R C1M P1 120.5(5) . . ? C1N C1M P1 121.5(4) . . ? C1O C1N C1M 120.4(5) . . ? C1P C1O C1N 120.4(6) . . ? C1Q C1P C1O 120.2(6) . . ? C1P C1Q C1R 119.9(6) . . ? C1Q C1R C1M 121.2(6) . . ? Cl1A C100 Cl1B 114.3(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.683 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.119