# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'DJUKIC, Jean-Pierre' _publ_contact_author_email djukic@chimie.u-strasbg.fr _publ_section_title ; The dehydrogenation of ammonia-borane catalysed by dicarbonylruthenium(II) complexes: experimental and theoretical insights ; loop_ _publ_author_name J.-P.DJUKIC C.BOULHO # Attachment '- 7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 771514' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 Cl N2 O2 Ru' _chemical_formula_sum 'C23 H23 Cl N2 O2 Ru' _chemical_formula_weight 495.95 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' Cl Cl 0.1484 0.1585 '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' 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/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 17.6291(5) _cell_length_b 11.5208(3) _cell_length_c 24.1776(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.955(2) _cell_angle_gamma 90.00 _cell_volume 4415.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9007 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 29.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7267 _exptl_absorpt_correction_T_max 0.8828 _exptl_absorpt_process_details sadabs _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33642 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 29.02 _reflns_number_total 11736 _reflns_number_gt 9823 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0084P)^2^+5.7412P] 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 11736 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.521615(10) -0.644658(15) -0.146951(7) 0.02021(4) Uani 1 1 d . . . Cl1 Cl 0.63202(3) -0.79448(5) -0.12321(3) 0.03101(12) Uani 1 1 d . . . O1 O 0.55903(14) -0.6083(2) -0.01454(8) 0.0559(6) Uani 1 1 d . . . O2 O 0.64476(12) -0.45991(18) -0.14067(10) 0.0459(5) Uani 1 1 d . . . N1 N 0.48032(10) -0.65600(15) -0.24377(7) 0.0189(3) Uani 1 1 d . . . N2 N 0.43206(10) -0.78348(16) -0.15892(8) 0.0208(3) Uani 1 1 d . . . C1 C 0.51628(13) -0.72037(19) -0.27259(10) 0.0240(4) Uani 1 1 d . . . H1 H 0.5634 -0.7677 -0.2485 0.029 Uiso 1 1 calc R . . C2 C 0.48707(13) -0.72002(19) -0.33585(10) 0.0250(4) Uani 1 1 d . . . H2 H 0.5143 -0.7660 -0.3544 0.030 Uiso 1 1 calc R . . C3 C 0.41747(13) -0.65190(19) -0.37233(9) 0.0230(4) Uani 1 1 d . . . C4 C 0.38011(13) -0.58814(18) -0.34239(9) 0.0224(4) Uani 1 1 d . . . H4 H 0.3317 -0.5424 -0.3658 0.027 Uiso 1 1 calc R . . C5 C 0.41241(12) -0.58993(17) -0.27834(9) 0.0195(4) Uani 1 1 d . . . C6 C 0.37991(12) -0.51973(18) -0.24274(9) 0.0194(4) Uani 1 1 d . . . C7 C 0.31143(13) -0.44449(19) -0.27007(10) 0.0241(4) Uani 1 1 d . . . H7 H 0.2817 -0.4407 -0.3136 0.029 Uiso 1 1 calc R . . C8 C 0.28651(14) -0.3754(2) -0.23419(10) 0.0263(4) Uani 1 1 d . . . H8 H 0.2401 -0.3240 -0.2533 0.032 Uiso 1 1 calc R . . C9 C 0.32887(13) -0.38045(19) -0.17036(10) 0.0243(4) Uani 1 1 d . . . C10 C 0.39551(13) -0.45858(18) -0.14317(10) 0.0223(4) Uani 1 1 d . . . H10 H 0.4229 -0.4645 -0.0996 0.027 Uiso 1 1 calc R . . C11 C 0.42329(12) -0.52841(18) -0.17789(9) 0.0203(4) Uani 1 1 d . . . C12 C 0.38739(15) -0.6467(2) -0.44201(10) 0.0292(5) Uani 1 1 d . . . C13 C 0.3731(2) -0.7699(3) -0.46815(12) 0.0534(8) Uani 1 1 d . . . H13A H 0.4267 -0.8123 -0.4510 0.080 Uiso 1 1 calc R . . H13B H 0.3509 -0.7664 -0.5130 0.080 Uiso 1 1 calc R . . H13C H 0.3326 -0.8100 -0.4572 0.080 Uiso 1 1 calc R . . C14 C 0.4549(2) -0.5854(4) -0.45479(13) 0.0621(10) Uani 1 1 d . . . H14A H 0.4631 -0.5065 -0.4381 0.093 Uiso 1 1 calc R . . H14B H 0.4368 -0.5819 -0.4993 0.093 Uiso 1 1 calc R . . H14C H 0.5080 -0.6286 -0.4352 0.093 Uiso 1 1 calc R . . C15 C 0.30464(19) -0.5795(3) -0.47447(11) 0.0500(8) Uani 1 1 d . . . H15A H 0.2612 -0.6155 -0.4651 0.075 Uiso 1 1 calc R . . H15B H 0.2865 -0.5811 -0.5190 0.075 Uiso 1 1 calc R . . H15C H 0.3132 -0.4989 -0.4601 0.075 Uiso 1 1 calc R . . C16 C 0.30488(16) -0.2992(2) -0.13163(12) 0.0347(5) Uani 1 1 d . . . H16A H 0.3319 -0.2237 -0.1289 0.052 Uiso 1 1 calc R . . H16B H 0.3237 -0.3318 -0.0903 0.052 Uiso 1 1 calc R . . H16C H 0.2435 -0.2894 -0.1506 0.052 Uiso 1 1 calc R . . C17 C 0.37519(14) -0.7754(2) -0.13612(10) 0.0290(5) Uani 1 1 d . . . H17 H 0.3749 -0.7077 -0.1137 0.035 Uiso 1 1 calc R . . C18 C 0.31710(15) -0.8618(2) -0.14405(11) 0.0357(6) Uani 1 1 d . . . H18 H 0.2778 -0.8538 -0.1272 0.043 Uiso 1 1 calc R . . C19 C 0.31680(16) -0.9598(2) -0.17676(13) 0.0380(6) Uani 1 1 d . . . H19 H 0.2773 -1.0203 -0.1829 0.046 Uiso 1 1 calc R . . C20 C 0.37512(16) -0.9683(2) -0.20043(12) 0.0356(5) Uani 1 1 d . . . H20 H 0.3759 -1.0345 -0.2236 0.043 Uiso 1 1 calc R . . C21 C 0.43219(14) -0.8794(2) -0.18992(11) 0.0289(5) Uani 1 1 d . . . H21 H 0.4732 -0.8866 -0.2053 0.035 Uiso 1 1 calc R . . C22 C 0.54644(15) -0.6243(2) -0.06371(11) 0.0324(5) Uani 1 1 d . . . C23 C 0.59799(14) -0.5279(2) -0.14209(10) 0.0278(5) Uani 1 1 d . . . Ru2 Ru 0.033023(10) -0.929850(15) -0.139715(7) 0.01975(4) Uani 1 1 d . . . Cl2 Cl 0.13685(3) -0.77306(5) -0.12274(3) 0.02872(11) Uani 1 1 d . . . O3 O 0.09266(12) -0.9770(2) -0.00484(8) 0.0474(5) Uani 1 1 d . . . O4 O 0.15497(13) -1.10167(18) -0.14767(11) 0.0510(5) Uani 1 1 d . . . N3 N -0.01950(11) -0.91734(15) -0.23726(8) 0.0211(3) Uani 1 1 d . . . N4 N -0.05661(11) -0.79628(16) -0.14417(8) 0.0242(4) Uani 1 1 d . . . C24 C 0.00996(14) -0.8500(2) -0.26916(10) 0.0276(5) Uani 1 1 d . . . H24 H 0.0572 -0.8015 -0.2471 0.033 Uiso 1 1 calc R . . C25 C -0.02575(15) -0.8489(2) -0.33243(11) 0.0318(5) Uani 1 1 d . . . H25 H -0.0030 -0.8003 -0.3532 0.038 Uiso 1 1 calc R . . C26 C -0.09538(15) -0.9191(2) -0.36628(10) 0.0275(5) Uani 1 1 d . . . C27 C -0.12520(14) -0.98757(19) -0.33298(10) 0.0257(4) Uani 1 1 d . . . H27 H -0.1729 -1.0359 -0.3543 0.031 Uiso 1 1 calc R . . C28 C -0.08667(13) -0.98707(18) -0.26874(9) 0.0214(4) Uani 1 1 d . . . C29 C -0.11149(13) -1.05988(18) -0.22951(10) 0.0215(4) Uani 1 1 d . . . C30 C -0.17957(14) -1.1368(2) -0.25315(10) 0.0269(4) Uani 1 1 d . . . H30 H -0.2123 -1.1428 -0.2964 0.032 Uiso 1 1 calc R . . C31 C -0.19961(14) -1.2043(2) -0.21405(11) 0.0301(5) Uani 1 1 d . . . H31 H -0.2461 -1.2562 -0.2307 0.036 Uiso 1 1 calc R . . C32 C -0.15217(15) -1.1969(2) -0.15051(11) 0.0284(5) Uani 1 1 d . . . C33 C -0.08442(14) -1.11962(19) -0.12718(10) 0.0250(4) Uani 1 1 d . . . H33 H -0.0522 -1.1139 -0.0839 0.030 Uiso 1 1 calc R . . C34 C -0.06232(13) -1.05057(18) -0.16516(10) 0.0213(4) Uani 1 1 d . . . C35 C -0.13376(17) -0.9190(2) -0.43684(11) 0.0364(6) Uani 1 1 d . . . C36 C -0.1590(2) -0.7942(3) -0.46002(12) 0.0505(8) Uani 1 1 d . . . H36A H -0.1972 -0.7634 -0.4439 0.076 Uiso 1 1 calc R . . H36B H -0.1875 -0.7940 -0.5051 0.076 Uiso 1 1 calc R . . H36C H -0.1084 -0.7456 -0.4458 0.076 Uiso 1 1 calc R . . C37 C -0.0674(2) -0.9649(4) -0.45625(14) 0.0636(10) Uani 1 1 d . . . H37A H -0.0167 -0.9166 -0.4379 0.095 Uiso 1 1 calc R . . H37B H -0.0901 -0.9624 -0.5012 0.095 Uiso 1 1 calc R . . H37C H -0.0531 -1.0452 -0.4421 0.095 Uiso 1 1 calc R . . C38 C -0.21235(19) -0.9948(3) -0.46583(12) 0.0489(7) Uani 1 1 d . . . H38A H -0.1970 -1.0759 -0.4540 0.073 Uiso 1 1 calc R . . H38B H -0.2369 -0.9878 -0.5107 0.073 Uiso 1 1 calc R . . H38C H -0.2537 -0.9695 -0.4514 0.073 Uiso 1 1 calc R . . C39 C -0.17293(18) -1.2719(2) -0.10772(13) 0.0412(6) Uani 1 1 d . . . H39A H -0.1493 -1.3497 -0.1056 0.062 Uiso 1 1 calc R . . H39B H -0.2343 -1.2775 -0.1232 0.062 Uiso 1 1 calc R . . H39C H -0.1487 -1.2372 -0.0666 0.062 Uiso 1 1 calc R . . C40 C -0.11052(14) -0.8116(2) -0.11892(11) 0.0309(5) Uani 1 1 d . . . H40 H -0.1078 -0.8816 -0.0974 0.037 Uiso 1 1 calc R . . C41 C -0.16966(15) -0.7289(3) -0.12329(12) 0.0404(6) Uani 1 1 d . . . H41 H -0.2073 -0.7425 -0.1054 0.048 Uiso 1 1 calc R . . C42 C -0.17342(16) -0.6268(3) -0.15379(14) 0.0469(7) Uani 1 1 d . . . H42 H -0.2134 -0.5687 -0.1571 0.056 Uiso 1 1 calc R . . C43 C -0.11816(16) -0.6101(2) -0.17945(14) 0.0433(7) Uani 1 1 d . . . H43 H -0.1197 -0.5405 -0.2010 0.052 Uiso 1 1 calc R . . C44 C -0.06048(15) -0.6962(2) -0.17334(12) 0.0321(5) Uani 1 1 d . . . H44 H -0.0219 -0.6838 -0.1906 0.039 Uiso 1 1 calc R . . C45 C 0.07098(14) -0.9557(2) -0.05497(11) 0.0296(5) Uani 1 1 d . . . C46 C 0.10886(15) -1.0393(2) -0.14267(11) 0.0292(5) 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 0.01879(7) 0.02368(9) 0.01814(8) 0.00113(6) 0.00806(6) 0.00362(6) Cl1 0.0248(2) 0.0340(3) 0.0337(3) 0.0035(2) 0.0123(2) 0.0095(2) O1 0.0583(13) 0.0827(17) 0.0225(9) -0.0024(10) 0.0137(9) 0.0134(12) O2 0.0385(10) 0.0446(12) 0.0550(12) -0.0104(9) 0.0207(9) -0.0135(9) N1 0.0183(7) 0.0199(8) 0.0196(8) 0.0001(6) 0.0092(6) 0.0009(6) N2 0.0213(8) 0.0224(9) 0.0207(8) 0.0078(7) 0.0109(7) 0.0077(7) C1 0.0239(10) 0.0236(11) 0.0257(10) 0.0001(8) 0.0121(8) 0.0037(8) C2 0.0269(10) 0.0237(11) 0.0281(11) -0.0044(9) 0.0154(9) 0.0007(8) C3 0.0266(10) 0.0222(10) 0.0197(9) -0.0024(8) 0.0097(8) -0.0047(8) C4 0.0235(10) 0.0213(10) 0.0202(9) -0.0005(8) 0.0076(8) 0.0002(8) C5 0.0210(9) 0.0168(9) 0.0206(9) 0.0009(7) 0.0090(8) -0.0011(7) C6 0.0193(9) 0.0187(10) 0.0218(9) 0.0015(7) 0.0103(8) -0.0004(7) C7 0.0234(10) 0.0250(11) 0.0240(10) 0.0052(8) 0.0104(8) 0.0038(8) C8 0.0250(10) 0.0248(11) 0.0322(11) 0.0076(9) 0.0154(9) 0.0074(8) C9 0.0247(10) 0.0211(10) 0.0325(11) 0.0023(8) 0.0176(9) 0.0024(8) C10 0.0233(10) 0.0228(10) 0.0225(10) 0.0018(8) 0.0117(8) 0.0018(8) C11 0.0179(9) 0.0223(10) 0.0210(9) 0.0017(8) 0.0088(8) -0.0010(7) C12 0.0361(12) 0.0311(12) 0.0198(10) -0.0037(9) 0.0118(9) -0.0036(10) C13 0.087(2) 0.0402(16) 0.0262(13) -0.0106(12) 0.0180(14) -0.0023(16) C14 0.0559(18) 0.103(3) 0.0276(13) 0.0054(16) 0.0188(13) -0.0290(19) C15 0.0545(17) 0.065(2) 0.0203(12) -0.0014(12) 0.0066(11) 0.0109(15) C16 0.0388(13) 0.0338(13) 0.0386(13) -0.0005(11) 0.0234(11) 0.0105(11) C17 0.0273(11) 0.0364(13) 0.0271(11) 0.0079(9) 0.0154(9) 0.0077(9) C18 0.0279(11) 0.0474(16) 0.0368(13) 0.0150(12) 0.0187(10) 0.0057(11) C19 0.0285(12) 0.0349(14) 0.0473(15) 0.0141(11) 0.0135(11) -0.0002(10) C20 0.0340(12) 0.0255(12) 0.0464(15) 0.0026(10) 0.0167(11) 0.0013(10) C21 0.0275(11) 0.0271(12) 0.0364(12) 0.0036(9) 0.0178(10) 0.0051(9) C22 0.0273(11) 0.0403(14) 0.0273(11) -0.0022(10) 0.0098(9) 0.0055(10) C23 0.0243(10) 0.0310(12) 0.0265(11) -0.0048(9) 0.0096(9) 0.0047(9) Ru2 0.01969(8) 0.02131(8) 0.02040(8) -0.00200(6) 0.01076(6) -0.00284(6) Cl2 0.0233(2) 0.0289(3) 0.0336(3) -0.0011(2) 0.0121(2) -0.0056(2) O3 0.0468(11) 0.0701(14) 0.0249(9) 0.0001(9) 0.0151(8) -0.0095(10) O4 0.0523(12) 0.0416(11) 0.0758(15) 0.0123(10) 0.0435(11) 0.0182(9) N3 0.0226(8) 0.0210(9) 0.0227(8) -0.0012(7) 0.0127(7) -0.0021(7) N4 0.0197(8) 0.0257(9) 0.0299(9) -0.0117(8) 0.0133(7) -0.0091(7) C24 0.0301(11) 0.0271(11) 0.0277(11) -0.0003(9) 0.0145(9) -0.0039(9) C25 0.0393(13) 0.0282(12) 0.0297(11) 0.0055(10) 0.0168(10) -0.0034(10) C26 0.0345(11) 0.0255(11) 0.0217(10) 0.0000(8) 0.0115(9) 0.0049(9) C27 0.0279(10) 0.0231(11) 0.0225(10) -0.0034(8) 0.0078(8) -0.0003(8) C28 0.0222(9) 0.0198(10) 0.0234(10) -0.0027(8) 0.0110(8) 0.0008(8) C29 0.0225(9) 0.0173(10) 0.0273(10) -0.0039(8) 0.0132(8) -0.0004(8) C30 0.0255(10) 0.0258(11) 0.0299(11) -0.0073(9) 0.0127(9) -0.0049(9) C31 0.0288(11) 0.0252(11) 0.0398(13) -0.0081(10) 0.0182(10) -0.0090(9) C32 0.0326(11) 0.0226(11) 0.0395(13) -0.0022(9) 0.0246(10) -0.0029(9) C33 0.0296(11) 0.0242(11) 0.0270(10) -0.0027(8) 0.0179(9) -0.0036(9) C34 0.0223(9) 0.0200(10) 0.0251(10) -0.0060(8) 0.0135(8) -0.0004(8) C35 0.0488(15) 0.0360(14) 0.0200(10) -0.0007(10) 0.0112(10) 0.0050(11) C36 0.074(2) 0.0448(17) 0.0266(13) 0.0072(12) 0.0162(13) 0.0036(15) C37 0.069(2) 0.091(3) 0.0323(15) -0.0082(16) 0.0244(15) 0.018(2) C38 0.0597(18) 0.0458(16) 0.0242(12) -0.0022(11) 0.0025(12) -0.0009(14) C39 0.0497(15) 0.0364(14) 0.0495(16) 0.0000(12) 0.0328(13) -0.0131(12) C40 0.0266(11) 0.0402(14) 0.0286(11) -0.0122(10) 0.0145(9) -0.0066(10) C41 0.0282(12) 0.0580(18) 0.0393(14) -0.0239(13) 0.0189(11) -0.0062(12) C42 0.0279(12) 0.0486(17) 0.0585(18) -0.0236(14) 0.0137(12) 0.0034(12) C43 0.0325(13) 0.0318(14) 0.0596(18) -0.0063(12) 0.0146(12) 0.0040(11) C44 0.0273(11) 0.0266(12) 0.0432(14) -0.0026(10) 0.0162(10) -0.0035(9) C45 0.0230(10) 0.0357(13) 0.0301(12) 0.0002(10) 0.0116(9) -0.0059(9) C46 0.0295(11) 0.0269(12) 0.0341(12) 0.0022(9) 0.0167(10) -0.0029(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 C23 1.870(2) . ? Ru1 C22 1.878(2) . ? Ru1 C11 2.055(2) . ? Ru1 N1 2.1295(16) . ? Ru1 N2 2.1758(18) . ? Ru1 Cl1 2.4737(6) . ? O1 C22 1.125(3) . ? O2 C23 1.126(3) . ? N1 C1 1.351(3) . ? N1 C5 1.355(2) . ? N2 C21 1.335(3) . ? N2 C17 1.342(3) . ? C1 C2 1.384(3) . ? C1 H1 0.9500 . ? C2 C3 1.397(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 C12 1.530(3) . ? C4 C5 1.397(3) . ? C4 H4 0.9500 . ? C5 C6 1.468(3) . ? C6 C7 1.395(3) . ? C6 C11 1.416(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.395(3) . ? C9 C16 1.509(3) . ? C10 C11 1.397(3) . ? C10 H10 0.9500 . ? C12 C14 1.527(4) . ? C12 C13 1.529(4) . ? C12 C15 1.530(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.380(3) . ? C17 H17 0.9500 . ? C18 C19 1.377(4) . ? C18 H18 0.9500 . ? C19 C20 1.382(4) . ? C19 H19 0.9500 . ? C20 C21 1.380(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? Ru2 C46 1.862(2) . ? Ru2 C45 1.880(2) . ? Ru2 C34 2.057(2) . ? Ru2 N3 2.1281(17) . ? Ru2 N4 2.1742(18) . ? Ru2 Cl2 2.4747(6) . ? O3 C45 1.127(3) . ? O4 C46 1.130(3) . ? N3 C24 1.348(3) . ? N3 C28 1.356(3) . ? N4 C44 1.338(3) . ? N4 C40 1.347(3) . ? C24 C25 1.376(3) . ? C24 H24 0.9500 . ? C25 C26 1.397(3) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 C35 1.535(3) . ? C27 C28 1.396(3) . ? C27 H27 0.9500 . ? C28 C29 1.469(3) . ? C29 C30 1.397(3) . ? C29 C34 1.415(3) . ? C30 C31 1.384(3) . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 H31 0.9500 . ? C32 C33 1.396(3) . ? C32 C39 1.511(3) . ? C33 C34 1.393(3) . ? C33 H33 0.9500 . ? C35 C38 1.525(4) . ? C35 C37 1.532(4) . ? C35 C36 1.537(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.382(4) . ? C40 H40 0.9500 . ? C41 C42 1.374(4) . ? C41 H41 0.9500 . ? C42 C43 1.378(4) . ? C42 H42 0.9500 . ? C43 C44 1.381(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 C23 Ru1 C22 91.10(11) . . ? C23 Ru1 C11 91.34(9) . . ? C22 Ru1 C11 94.16(9) . . ? C23 Ru1 N1 90.21(8) . . ? C22 Ru1 N1 173.22(8) . . ? C11 Ru1 N1 79.15(7) . . ? C23 Ru1 N2 176.02(8) . . ? C22 Ru1 N2 92.83(9) . . ? C11 Ru1 N2 89.04(7) . . ? N1 Ru1 N2 85.97(6) . . ? C23 Ru1 Cl1 90.90(7) . . ? C22 Ru1 Cl1 92.73(7) . . ? C11 Ru1 Cl1 172.71(6) . . ? N1 Ru1 Cl1 93.90(5) . . ? N2 Ru1 Cl1 88.25(5) . . ? C1 N1 C5 118.54(17) . . ? C1 N1 Ru1 126.08(14) . . ? C5 N1 Ru1 115.37(13) . . ? C21 N2 C17 118.2(2) . . ? C21 N2 Ru1 120.21(14) . . ? C17 N2 Ru1 121.55(16) . . ? N1 C1 C2 122.48(19) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 117.10(19) . . ? C4 C3 C12 122.7(2) . . ? C2 C3 C12 120.16(19) . . ? C3 C4 C5 121.04(19) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 120.92(19) . . ? N1 C5 C6 114.46(17) . . ? C4 C5 C6 124.58(18) . . ? C7 C6 C11 120.28(19) . . ? C7 C6 C5 122.92(19) . . ? C11 C6 C5 116.77(18) . . ? C8 C7 C6 120.5(2) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.8(2) . . ? C8 C9 C16 120.1(2) . . ? C10 C9 C16 121.0(2) . . ? C9 C10 C11 122.2(2) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C6 117.61(18) . . ? C10 C11 Ru1 128.20(15) . . ? C6 C11 Ru1 114.19(15) . . ? C14 C12 C13 110.3(3) . . ? C14 C12 C3 108.40(19) . . ? C13 C12 C3 109.5(2) . . ? C14 C12 C15 108.3(2) . . ? C13 C12 C15 108.1(2) . . ? C3 C12 C15 112.2(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 122.3(2) . . ? N2 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 119.2(2) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C21 C20 C19 119.1(2) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N2 C21 C20 122.5(2) . . ? N2 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? O1 C22 Ru1 177.1(2) . . ? O2 C23 Ru1 177.4(2) . . ? C46 Ru2 C45 90.88(10) . . ? C46 Ru2 C34 92.12(9) . . ? C45 Ru2 C34 94.20(9) . . ? C46 Ru2 N3 88.56(9) . . ? C45 Ru2 N3 173.32(8) . . ? C34 Ru2 N3 79.17(7) . . ? C46 Ru2 N4 174.85(9) . . ? C45 Ru2 N4 94.05(9) . . ? C34 Ru2 N4 89.01(7) . . ? N3 Ru2 N4 86.72(7) . . ? C46 Ru2 Cl2 90.54(7) . . ? C45 Ru2 Cl2 92.88(7) . . ? C34 Ru2 Cl2 172.39(6) . . ? N3 Ru2 Cl2 93.77(5) . . ? N4 Ru2 Cl2 87.73(5) . . ? C24 N3 C28 118.71(18) . . ? C24 N3 Ru2 125.69(14) . . ? C28 N3 Ru2 115.56(14) . . ? C44 N4 C40 117.9(2) . . ? C44 N4 Ru2 120.30(15) . . ? C40 N4 Ru2 121.78(17) . . ? N3 C24 C25 122.6(2) . . ? N3 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C24 C25 C26 120.2(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 116.7(2) . . ? C27 C26 C35 123.5(2) . . ? C25 C26 C35 119.8(2) . . ? C26 C27 C28 121.4(2) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? N3 C28 C27 120.5(2) . . ? N3 C28 C29 114.19(18) . . ? C27 C28 C29 125.34(19) . . ? C30 C29 C34 120.1(2) . . ? C30 C29 C28 122.91(19) . . ? C34 C29 C28 117.02(18) . . ? C31 C30 C29 120.5(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.6(2) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C33 118.6(2) . . ? C31 C32 C39 120.8(2) . . ? C33 C32 C39 120.6(2) . . ? C34 C33 C32 122.3(2) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C29 117.90(19) . . ? C33 C34 Ru2 128.05(16) . . ? C29 C34 Ru2 114.02(15) . . ? C38 C35 C37 108.8(2) . . ? C38 C35 C26 112.3(2) . . ? C37 C35 C26 108.4(2) . . ? C38 C35 C36 108.0(2) . . ? C37 C35 C36 110.5(3) . . ? C26 C35 C36 108.8(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C32 C39 H39A 109.5 . . ? C32 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C32 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 C41 122.3(3) . . ? N4 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 119.2(2) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C41 C42 C43 118.9(3) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C42 C43 C44 119.0(3) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? N4 C44 C43 122.7(2) . . ? N4 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? O3 C45 Ru2 176.5(2) . . ? O4 C46 Ru2 175.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 Ru1 N1 C1 85.59(18) . . . . ? C11 Ru1 N1 C1 176.91(18) . . . . ? N2 Ru1 N1 C1 -93.29(17) . . . . ? Cl1 Ru1 N1 C1 -5.33(17) . . . . ? C23 Ru1 N1 C5 -93.20(15) . . . . ? C11 Ru1 N1 C5 -1.88(14) . . . . ? N2 Ru1 N1 C5 87.92(14) . . . . ? Cl1 Ru1 N1 C5 175.88(13) . . . . ? C22 Ru1 N2 C21 -136.21(17) . . . . ? C11 Ru1 N2 C21 129.67(16) . . . . ? N1 Ru1 N2 C21 50.48(16) . . . . ? Cl1 Ru1 N2 C21 -43.56(15) . . . . ? C22 Ru1 N2 C17 44.31(17) . . . . ? C11 Ru1 N2 C17 -49.81(16) . . . . ? N1 Ru1 N2 C17 -129.00(16) . . . . ? Cl1 Ru1 N2 C17 136.96(16) . . . . ? C5 N1 C1 C2 0.9(3) . . . . ? Ru1 N1 C1 C2 -177.85(16) . . . . ? N1 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C1 C2 C3 C12 177.1(2) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C12 C3 C4 C5 -176.2(2) . . . . ? C1 N1 C5 C4 0.0(3) . . . . ? Ru1 N1 C5 C4 178.87(15) . . . . ? C1 N1 C5 C6 -177.71(18) . . . . ? Ru1 N1 C5 C6 1.2(2) . . . . ? C3 C4 C5 N1 -1.3(3) . . . . ? C3 C4 C5 C6 176.14(19) . . . . ? N1 C5 C6 C7 178.72(19) . . . . ? C4 C5 C6 C7 1.1(3) . . . . ? N1 C5 C6 C11 0.7(3) . . . . ? C4 C5 C6 C11 -176.86(19) . . . . ? C11 C6 C7 C8 1.7(3) . . . . ? C5 C6 C7 C8 -176.2(2) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C7 C8 C9 C10 -1.6(3) . . . . ? C7 C8 C9 C16 176.0(2) . . . . ? C8 C9 C10 C11 2.7(3) . . . . ? C16 C9 C10 C11 -175.0(2) . . . . ? C9 C10 C11 C6 -1.5(3) . . . . ? C9 C10 C11 Ru1 178.12(16) . . . . ? C7 C6 C11 C10 -0.7(3) . . . . ? C5 C6 C11 C10 177.35(18) . . . . ? C7 C6 C11 Ru1 179.64(15) . . . . ? C5 C6 C11 Ru1 -2.3(2) . . . . ? C23 Ru1 C11 C10 -87.5(2) . . . . ? C22 Ru1 C11 C10 3.7(2) . . . . ? N1 Ru1 C11 C10 -177.4(2) . . . . ? N2 Ru1 C11 C10 96.49(19) . . . . ? C23 Ru1 C11 C6 92.15(16) . . . . ? C22 Ru1 C11 C6 -176.65(16) . . . . ? N1 Ru1 C11 C6 2.20(14) . . . . ? N2 Ru1 C11 C6 -83.88(15) . . . . ? C4 C3 C12 C14 110.6(3) . . . . ? C2 C3 C12 C14 -67.2(3) . . . . ? C4 C3 C12 C13 -129.0(3) . . . . ? C2 C3 C12 C13 53.2(3) . . . . ? C4 C3 C12 C15 -9.0(3) . . . . ? C2 C3 C12 C15 173.2(2) . . . . ? C21 N2 C17 C18 -0.5(3) . . . . ? Ru1 N2 C17 C18 179.01(17) . . . . ? N2 C17 C18 C19 -0.4(3) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C18 C19 C20 C21 0.8(4) . . . . ? C17 N2 C21 C20 1.5(3) . . . . ? Ru1 N2 C21 C20 -177.97(18) . . . . ? C19 C20 C21 N2 -1.7(4) . . . . ? C46 Ru2 N3 C24 -84.31(19) . . . . ? C34 Ru2 N3 C24 -176.74(19) . . . . ? N4 Ru2 N3 C24 93.64(18) . . . . ? Cl2 Ru2 N3 C24 6.14(18) . . . . ? C46 Ru2 N3 C28 93.39(16) . . . . ? C34 Ru2 N3 C28 0.96(15) . . . . ? N4 Ru2 N3 C28 -88.66(15) . . . . ? Cl2 Ru2 N3 C28 -176.16(14) . . . . ? C45 Ru2 N4 C44 132.99(18) . . . . ? C34 Ru2 N4 C44 -132.87(17) . . . . ? N3 Ru2 N4 C44 -53.66(17) . . . . ? Cl2 Ru2 N4 C44 40.25(16) . . . . ? C45 Ru2 N4 C40 -48.08(17) . . . . ? C34 Ru2 N4 C40 46.07(17) . . . . ? N3 Ru2 N4 C40 125.28(17) . . . . ? Cl2 Ru2 N4 C40 -140.81(16) . . . . ? C28 N3 C24 C25 0.3(3) . . . . ? Ru2 N3 C24 C25 177.96(18) . . . . ? N3 C24 C25 C26 0.1(4) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C24 C25 C26 C35 -178.9(2) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? C35 C26 C27 C28 178.2(2) . . . . ? C24 N3 C28 C27 -1.0(3) . . . . ? Ru2 N3 C28 C27 -178.83(16) . . . . ? C24 N3 C28 C29 177.76(18) . . . . ? Ru2 N3 C28 C29 -0.1(2) . . . . ? C26 C27 C28 N3 1.2(3) . . . . ? C26 C27 C28 C29 -177.4(2) . . . . ? N3 C28 C29 C30 179.44(19) . . . . ? C27 C28 C29 C30 -1.9(3) . . . . ? N3 C28 C29 C34 -1.3(3) . . . . ? C27 C28 C29 C34 177.3(2) . . . . ? C34 C29 C30 C31 0.1(3) . . . . ? C28 C29 C30 C31 179.3(2) . . . . ? C29 C30 C31 C32 -0.1(3) . . . . ? C30 C31 C32 C33 0.4(3) . . . . ? C30 C31 C32 C39 -179.0(2) . . . . ? C31 C32 C33 C34 -0.5(3) . . . . ? C39 C32 C33 C34 178.8(2) . . . . ? C32 C33 C34 C29 0.5(3) . . . . ? C32 C33 C34 Ru2 178.59(16) . . . . ? C30 C29 C34 C33 -0.2(3) . . . . ? C28 C29 C34 C33 -179.48(19) . . . . ? C30 C29 C34 Ru2 -178.61(16) . . . . ? C28 C29 C34 Ru2 2.1(2) . . . . ? C46 Ru2 C34 C33 92.1(2) . . . . ? C45 Ru2 C34 C33 1.0(2) . . . . ? N3 Ru2 C34 C33 -179.8(2) . . . . ? N4 Ru2 C34 C33 -92.96(19) . . . . ? C46 Ru2 C34 C29 -89.75(16) . . . . ? C45 Ru2 C34 C29 179.21(16) . . . . ? N3 Ru2 C34 C29 -1.63(14) . . . . ? N4 Ru2 C34 C29 85.23(15) . . . . ? C27 C26 C35 C38 4.7(3) . . . . ? C25 C26 C35 C38 -176.4(2) . . . . ? C27 C26 C35 C37 -115.6(3) . . . . ? C25 C26 C35 C37 63.3(3) . . . . ? C27 C26 C35 C36 124.2(3) . . . . ? C25 C26 C35 C36 -56.9(3) . . . . ? C44 N4 C40 C41 1.2(3) . . . . ? Ru2 N4 C40 C41 -177.75(17) . . . . ? N4 C40 C41 C42 -0.7(4) . . . . ? C40 C41 C42 C43 0.3(4) . . . . ? C41 C42 C43 C44 -0.4(4) . . . . ? C40 N4 C44 C43 -1.3(3) . . . . ? Ru2 N4 C44 C43 177.64(19) . . . . ? C42 C43 C44 N4 1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.694 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.074