Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Toni-J.J. Kinnunen' 'Matti Haukka' 'Matti Nousiainen' 'Antti Patrikka' 'Tapani A. Pakkanen' _publ_contact_author_name '?' _publ_contact_author_address ; ? ; data_compound3 _database_code_CSD 162466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'cis(Cl)-[Ru(4,4'-TBubpy)(CO)2Cl2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 Cl4 N2 O2 Ru' _chemical_formula_weight 581.31 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' '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' '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' 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 10.55850(10) _cell_length_b 11.47290(10) _cell_length_c 21.2337(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.7539(5) _cell_angle_gamma 90.00 _cell_volume 2542.22(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6773 _exptl_absorpt_correction_T_max 0.7423 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10289 _diffrn_reflns_av_R_equivalents 0.0110 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5300 _reflns_number_gt 4850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0389P)^2^+5.0049P] 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 5300 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.61298(2) 0.059560(19) 0.818681(11) 0.02904(9) Uani 1 1 d . . . Cl1 Cl 0.42204(8) -0.04966(7) 0.78023(4) 0.0432(2) Uani 1 1 d . . . Cl2 Cl 0.66080(9) -0.06798(7) 0.90946(4) 0.0451(2) Uani 1 1 d . . . C99 C 0.4843(5) 0.3275(4) 0.1856(3) 0.0841(17) Uani 1 1 d . . . Cl8A Cl 0.63940(14) 0.37141(11) 0.22200(7) 0.0718(4) Uani 0.870(2) 1 d P A 1 Cl9A Cl 0.40011(18) 0.44759(16) 0.14743(15) 0.0992(8) Uani 0.870(2) 1 d P A 1 Cl8B Cl 0.5314(10) 0.3641(7) 0.2471(5) 0.0718(4) Uani 0.130(2) 1 d P A 2 Cl9B Cl 0.4006(15) 0.4012(12) 0.1348(12) 0.0992(8) Uani 0.130(2) 1 d P A 2 O1 O 0.7608(4) -0.1084(3) 0.74828(16) 0.0765(10) Uani 1 1 d . . . O2 O 0.8444(3) 0.2047(3) 0.86564(17) 0.0746(10) Uani 1 1 d . . . N1 N 0.4925(2) 0.1709(2) 0.86101(11) 0.0288(5) Uani 1 1 d . . . N2 N 0.5478(2) 0.1728(2) 0.74531(11) 0.0269(5) Uani 1 1 d . . . C1 C 0.7107(4) -0.0446(3) 0.77358(16) 0.0427(8) Uani 1 1 d . . . C2 C 0.7575(3) 0.1497(3) 0.84754(17) 0.0455(8) Uani 1 1 d . . . C10 C 0.4754(3) 0.1672(3) 0.92226(13) 0.0368(7) Uani 1 1 d . . . H10 H 0.5234 0.1128 0.9500 0.044 Uiso 1 1 calc R . . C11 C 0.3905(3) 0.2398(3) 0.94635(14) 0.0376(7) Uani 1 1 d . . . H11 H 0.3825 0.2358 0.9903 0.045 Uiso 1 1 calc R . . C12 C 0.3164(3) 0.3186(3) 0.90708(13) 0.0322(6) Uani 1 1 d . B . C13 C 0.3343(3) 0.3212(2) 0.84294(13) 0.0299(6) Uani 1 1 d . . . H13 H 0.2853 0.3733 0.8142 0.036 Uiso 1 1 calc R . . C14 C 0.4230(3) 0.2480(2) 0.82130(12) 0.0258(5) Uani 1 1 d . . . C15 C 0.4529(3) 0.2479(2) 0.75536(12) 0.0253(5) Uani 1 1 d . . . C16 C 0.3925(3) 0.3176(2) 0.70648(13) 0.0274(5) Uani 1 1 d . . . H16 H 0.3257 0.3685 0.7144 0.033 Uiso 1 1 calc R . . C17 C 0.4280(3) 0.3142(2) 0.64566(13) 0.0281(6) Uani 1 1 d . . . C18 C 0.5286(3) 0.2410(3) 0.63803(14) 0.0334(6) Uani 1 1 d . . . H18 H 0.5594 0.2384 0.5983 0.040 Uiso 1 1 calc R . . C19 C 0.5844(3) 0.1716(3) 0.68762(14) 0.0327(6) Uani 1 1 d . . . H19 H 0.6518 0.1208 0.6806 0.039 Uiso 1 1 calc R . . C4 C 0.2218(4) 0.3993(3) 0.93268(16) 0.0446(8) Uani 1 1 d . . . C41A C 0.3054(9) 0.5041(6) 0.9662(5) 0.072(2) Uani 0.573(5) 1 d P B 3 H41A H 0.3506 0.5428 0.9350 0.107 Uiso 0.573(5) 1 calc PR B 3 H41B H 0.3678 0.4738 1.0012 0.107 Uiso 0.573(5) 1 calc PR B 3 H41C H 0.2491 0.5603 0.9830 0.107 Uiso 0.573(5) 1 calc PR B 3 C42A C 0.1563(10) 0.3398(8) 0.9855(4) 0.0610(19) Uani 0.573(5) 1 d P B 3 H42A H 0.2222 0.3124 1.0198 0.091 Uiso 0.573(5) 1 calc PR B 3 H42B H 0.1050 0.2735 0.9671 0.091 Uiso 0.573(5) 1 calc PR B 3 H42C H 0.1007 0.3962 1.0026 0.091 Uiso 0.573(5) 1 calc PR B 3 C43A C 0.1190(9) 0.4502(9) 0.8841(4) 0.077(2) Uani 0.573(5) 1 d P B 3 H43A H 0.0636 0.5006 0.9054 0.116 Uiso 0.573(5) 1 calc PR B 3 H43B H 0.0678 0.3872 0.8618 0.116 Uiso 0.573(5) 1 calc PR B 3 H43C H 0.1583 0.4961 0.8533 0.116 Uiso 0.573(5) 1 calc PR B 3 C41B C 0.2435(13) 0.5216(9) 0.9135(7) 0.072(2) Uani 0.427(5) 1 d P B 4 H41D H 0.2239 0.5285 0.8670 0.107 Uiso 0.427(5) 1 calc PR B 4 H41E H 0.3332 0.5429 0.9276 0.107 Uiso 0.427(5) 1 calc PR B 4 H41F H 0.1876 0.5740 0.9333 0.107 Uiso 0.427(5) 1 calc PR B 4 C42B C 0.2226(13) 0.3838(11) 1.0014(5) 0.0610(19) Uani 0.427(5) 1 d P B 4 H42D H 0.3042 0.4119 1.0246 0.091 Uiso 0.427(5) 1 calc PR B 4 H42E H 0.2123 0.3010 1.0106 0.091 Uiso 0.427(5) 1 calc PR B 4 H42F H 0.1520 0.4282 1.0147 0.091 Uiso 0.427(5) 1 calc PR B 4 C43B C 0.0868(12) 0.3621(12) 0.8947(6) 0.077(2) Uani 0.427(5) 1 d P B 4 H43D H 0.0194 0.4097 0.9089 0.116 Uiso 0.427(5) 1 calc PR B 4 H43E H 0.0711 0.2797 0.9029 0.116 Uiso 0.427(5) 1 calc PR B 4 H43F H 0.0865 0.3740 0.8490 0.116 Uiso 0.427(5) 1 calc PR B 4 C5 C 0.3586(3) 0.3879(3) 0.59106(13) 0.0330(6) Uani 1 1 d . . . C51 C 0.3692(4) 0.5168(3) 0.60949(18) 0.0520(9) Uani 1 1 d . . . H51A H 0.3287 0.5643 0.5736 0.078 Uiso 1 1 calc R . . H51B H 0.4597 0.5383 0.6202 0.078 Uiso 1 1 calc R . . H51C H 0.3258 0.5303 0.6465 0.078 Uiso 1 1 calc R . . C52 C 0.2171(3) 0.3540(3) 0.57902(16) 0.0457(8) Uani 1 1 d . . . H52A H 0.1797 0.3658 0.6180 0.068 Uiso 1 1 calc R . . H52B H 0.2089 0.2719 0.5664 0.068 Uiso 1 1 calc R . . H52C H 0.1718 0.4027 0.5449 0.068 Uiso 1 1 calc R . . C53 C 0.4147(4) 0.3690(4) 0.52937(16) 0.0600(11) Uani 1 1 d . . . H53A H 0.4086 0.2863 0.5177 0.090 Uiso 1 1 calc R . . H53B H 0.5049 0.3930 0.5359 0.090 Uiso 1 1 calc R . . H53C H 0.3667 0.4156 0.4951 0.090 Uiso 1 1 calc R . . 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 0.02756(15) 0.02749(13) 0.03201(13) 0.00911(8) 0.00435(9) 0.00492(8) Cl1 0.0436(5) 0.0358(4) 0.0486(4) 0.0068(3) 0.0020(4) -0.0087(3) Cl2 0.0539(5) 0.0393(4) 0.0404(4) 0.0142(3) 0.0016(4) 0.0086(3) C99 0.052(3) 0.052(3) 0.140(5) 0.007(3) -0.010(3) 0.001(2) Cl8A 0.0785(9) 0.0469(6) 0.0795(8) -0.0048(6) -0.0215(7) 0.0054(6) Cl9A 0.0487(7) 0.0682(11) 0.178(2) 0.0378(15) 0.0073(10) 0.0063(9) Cl8B 0.0785(9) 0.0469(6) 0.0795(8) -0.0048(6) -0.0215(7) 0.0054(6) Cl9B 0.0487(7) 0.0682(11) 0.178(2) 0.0378(15) 0.0073(10) 0.0063(9) O1 0.090(2) 0.074(2) 0.0696(19) 0.0088(16) 0.0272(17) 0.0464(19) O2 0.0433(16) 0.072(2) 0.100(2) 0.0215(18) -0.0173(16) -0.0139(14) N1 0.0298(13) 0.0299(11) 0.0261(11) 0.0069(9) 0.0019(9) 0.0006(9) N2 0.0244(12) 0.0266(11) 0.0305(11) 0.0064(9) 0.0072(9) 0.0022(9) C1 0.051(2) 0.0340(16) 0.0431(17) 0.0138(13) 0.0067(15) 0.0147(14) C2 0.0355(18) 0.0465(19) 0.0522(19) 0.0187(15) -0.0011(15) 0.0082(14) C10 0.0425(18) 0.0408(16) 0.0262(13) 0.0084(12) 0.0018(12) 0.0052(13) C11 0.0470(19) 0.0417(17) 0.0249(13) 0.0049(12) 0.0077(12) 0.0029(14) C12 0.0381(17) 0.0311(14) 0.0289(13) 0.0017(11) 0.0102(12) -0.0013(12) C13 0.0328(16) 0.0288(13) 0.0285(13) 0.0075(10) 0.0062(11) 0.0042(11) C14 0.0272(14) 0.0246(12) 0.0255(12) 0.0052(10) 0.0031(10) -0.0004(10) C15 0.0265(14) 0.0228(12) 0.0274(12) 0.0053(10) 0.0067(10) 0.0001(10) C16 0.0284(15) 0.0259(13) 0.0283(12) 0.0048(10) 0.0060(11) 0.0024(10) C17 0.0299(15) 0.0272(13) 0.0278(12) 0.0067(10) 0.0058(11) -0.0013(10) C18 0.0366(17) 0.0364(15) 0.0293(13) 0.0058(11) 0.0119(12) 0.0029(12) C19 0.0302(16) 0.0341(15) 0.0360(14) 0.0060(11) 0.0121(12) 0.0065(11) C4 0.058(2) 0.0408(17) 0.0396(16) 0.0071(14) 0.0219(16) 0.0115(15) C41A 0.090(6) 0.039(3) 0.098(5) -0.014(4) 0.052(5) -0.002(3) C42A 0.078(6) 0.060(5) 0.054(4) 0.006(3) 0.037(4) 0.016(3) C43A 0.077(5) 0.091(5) 0.072(4) 0.011(4) 0.039(4) 0.048(5) C41B 0.090(6) 0.039(3) 0.098(5) -0.014(4) 0.052(5) -0.002(3) C42B 0.078(6) 0.060(5) 0.054(4) 0.006(3) 0.037(4) 0.016(3) C43B 0.077(5) 0.091(5) 0.072(4) 0.011(4) 0.039(4) 0.048(5) C5 0.0381(17) 0.0341(15) 0.0272(13) 0.0100(11) 0.0061(12) 0.0042(12) C51 0.070(3) 0.0292(16) 0.053(2) 0.0152(14) -0.0046(18) -0.0023(16) C52 0.044(2) 0.0505(19) 0.0387(16) 0.0073(14) -0.0048(14) 0.0019(15) C53 0.073(3) 0.077(3) 0.0341(17) 0.0269(18) 0.0211(17) 0.029(2) _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 C2 1.868(4) . ? Ru1 C1 1.926(4) . ? Ru1 N2 2.065(2) . ? Ru1 N1 2.099(2) . ? Ru1 Cl1 2.4084(8) . ? Ru1 Cl2 2.4115(8) . ? C99 Cl8B 1.389(11) . ? C99 Cl9B 1.540(18) . ? C99 Cl9A 1.768(5) . ? C99 Cl8A 1.774(5) . ? O1 C1 1.091(4) . ? O2 C2 1.132(4) . ? N1 C10 1.341(4) . ? N1 C14 1.358(3) . ? N2 C19 1.339(4) . ? N2 C15 1.362(3) . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.403(4) . ? C12 C4 1.522(4) . ? C13 C14 1.387(4) . ? C13 H13 0.9500 . ? C14 C15 1.482(4) . ? C15 C16 1.386(4) . ? C16 C17 1.399(4) . ? C16 H16 0.9500 . ? C17 C18 1.383(4) . ? C17 C5 1.528(4) . ? C18 C19 1.378(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C4 C42B 1.468(11) . ? C4 C41B 1.489(11) . ? C4 C43A 1.498(10) . ? C4 C42A 1.560(9) . ? C4 C43B 1.585(15) . ? C4 C41A 1.594(9) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C5 C52 1.528(5) . ? C5 C51 1.529(5) . ? C5 C53 1.533(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? 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 C2 Ru1 C1 91.96(17) . . ? C2 Ru1 N2 93.50(12) . . ? C1 Ru1 N2 99.07(11) . . ? C2 Ru1 N1 92.32(14) . . ? C1 Ru1 N1 174.76(13) . . ? N2 Ru1 N1 77.65(9) . . ? C2 Ru1 Cl1 177.72(10) . . ? C1 Ru1 Cl1 89.58(12) . . ? N2 Ru1 Cl1 84.60(7) . . ? N1 Ru1 Cl1 86.06(7) . . ? C2 Ru1 Cl2 90.72(10) . . ? C1 Ru1 Cl2 87.60(9) . . ? N2 Ru1 Cl2 171.97(7) . . ? N1 Ru1 Cl2 95.37(6) . . ? Cl1 Ru1 Cl2 91.03(3) . . ? Cl8B C99 Cl9B 125.3(9) . . ? Cl8B C99 Cl9A 106.1(5) . . ? Cl9B C99 Cl9A 19.2(8) . . ? Cl8B C99 Cl8A 47.9(5) . . ? Cl9B C99 Cl8A 122.8(7) . . ? Cl9A C99 Cl8A 110.2(3) . . ? C10 N1 C14 118.8(3) . . ? C10 N1 Ru1 125.2(2) . . ? C14 N1 Ru1 115.86(18) . . ? C19 N2 C15 118.1(2) . . ? C19 N2 Ru1 125.04(19) . . ? C15 N2 Ru1 116.64(17) . . ? O1 C1 Ru1 175.8(4) . . ? O2 C2 Ru1 179.2(4) . . ? N1 C10 C11 122.2(3) . . ? N1 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 116.7(3) . . ? C11 C12 C4 121.5(3) . . ? C13 C12 C4 121.8(3) . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? N1 C14 C13 121.1(2) . . ? N1 C14 C15 114.4(2) . . ? C13 C14 C15 124.4(2) . . ? N2 C15 C16 120.9(2) . . ? N2 C15 C14 114.6(2) . . ? C16 C15 C14 124.6(2) . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 116.3(2) . . ? C18 C17 C5 122.3(2) . . ? C16 C17 C5 121.3(3) . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? N2 C19 C18 122.9(3) . . ? N2 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C42B C4 C41B 114.1(7) . . ? C42B C4 C43A 128.8(7) . . ? C41B C4 C43A 64.5(7) . . ? C42B C4 C12 112.1(5) . . ? C41B C4 C12 109.8(5) . . ? C43A C4 C12 115.9(4) . . ? C42B C4 C42A 33.9(5) . . ? C41B C4 C42A 135.4(6) . . ? C43A C4 C42A 108.2(6) . . ? C12 C4 C42A 112.1(4) . . ? C42B C4 C43B 110.0(7) . . ? C41B C4 C43B 106.2(8) . . ? C43A C4 C43B 41.7(6) . . ? C12 C4 C43B 104.1(5) . . ? C42A C4 C43B 77.6(6) . . ? C42B C4 C41A 74.3(6) . . ? C41B C4 C41A 46.6(6) . . ? C43A C4 C41A 107.9(6) . . ? C12 C4 C41A 105.6(4) . . ? C42A C4 C41A 106.6(5) . . ? C43B C4 C41A 145.5(6) . . ? C4 C41A H41A 109.5 . . ? C4 C41A H41B 109.5 . . ? C4 C41A H41C 109.5 . . ? C4 C42A H42A 109.5 . . ? C4 C42A H42B 109.5 . . ? C4 C42A H42C 109.5 . . ? C4 C43A H43A 109.5 . . ? C4 C43A H43B 109.5 . . ? C4 C43A H43C 109.5 . . ? C4 C41B H41D 109.5 . . ? C4 C41B H41E 109.5 . . ? C4 C41B H41F 109.5 . . ? C4 C42B H42D 109.5 . . ? C4 C42B H42E 109.5 . . ? C4 C42B H42F 109.5 . . ? C4 C43B H43D 109.5 . . ? C4 C43B H43E 109.5 . . ? C4 C43B H43F 109.5 . . ? C52 C5 C17 109.3(2) . . ? C52 C5 C51 108.6(3) . . ? C17 C5 C51 109.4(2) . . ? C52 C5 C53 108.5(3) . . ? C17 C5 C53 111.5(3) . . ? C51 C5 C53 109.4(3) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? 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 C2 Ru1 N1 C10 -82.9(3) . . . . ? C1 Ru1 N1 C10 132.3(13) . . . . ? N2 Ru1 N1 C10 -176.0(3) . . . . ? Cl1 Ru1 N1 C10 98.7(3) . . . . ? Cl2 Ru1 N1 C10 8.0(3) . . . . ? C2 Ru1 N1 C14 100.4(2) . . . . ? C1 Ru1 N1 C14 -44.3(14) . . . . ? N2 Ru1 N1 C14 7.33(19) . . . . ? Cl1 Ru1 N1 C14 -78.00(19) . . . . ? Cl2 Ru1 N1 C14 -168.66(19) . . . . ? C2 Ru1 N2 C19 85.5(3) . . . . ? C1 Ru1 N2 C19 -7.1(3) . . . . ? N1 Ru1 N2 C19 177.1(3) . . . . ? Cl1 Ru1 N2 C19 -95.8(2) . . . . ? Cl2 Ru1 N2 C19 -153.0(4) . . . . ? C2 Ru1 N2 C15 -99.9(2) . . . . ? C1 Ru1 N2 C15 167.5(2) . . . . ? N1 Ru1 N2 C15 -8.33(19) . . . . ? Cl1 Ru1 N2 C15 78.80(19) . . . . ? Cl2 Ru1 N2 C15 21.6(6) . . . . ? C2 Ru1 C1 O1 156(4) . . . . ? N2 Ru1 C1 O1 -110(4) . . . . ? N1 Ru1 C1 O1 -59(5) . . . . ? Cl1 Ru1 C1 O1 -26(4) . . . . ? Cl2 Ru1 C1 O1 65(4) . . . . ? C1 Ru1 C2 O2 -154(25) . . . . ? N2 Ru1 C2 O2 107(25) . . . . ? N1 Ru1 C2 O2 29(25) . . . . ? Cl1 Ru1 C2 O2 74(27) . . . . ? Cl2 Ru1 C2 O2 -66(25) . . . . ? C14 N1 C10 C11 -0.6(5) . . . . ? Ru1 N1 C10 C11 -177.1(2) . . . . ? N1 C10 C11 C12 1.5(5) . . . . ? C10 C11 C12 C13 -1.0(5) . . . . ? C10 C11 C12 C4 179.9(3) . . . . ? C11 C12 C13 C14 -0.4(4) . . . . ? C4 C12 C13 C14 178.8(3) . . . . ? C10 N1 C14 C13 -0.9(4) . . . . ? Ru1 N1 C14 C13 176.0(2) . . . . ? C10 N1 C14 C15 177.8(3) . . . . ? Ru1 N1 C14 C15 -5.3(3) . . . . ? C12 C13 C14 N1 1.4(4) . . . . ? C12 C13 C14 C15 -177.2(3) . . . . ? C19 N2 C15 C16 2.7(4) . . . . ? Ru1 N2 C15 C16 -172.3(2) . . . . ? C19 N2 C15 C14 -177.0(3) . . . . ? Ru1 N2 C15 C14 8.1(3) . . . . ? N1 C14 C15 N2 -1.7(3) . . . . ? C13 C14 C15 N2 176.9(3) . . . . ? N1 C14 C15 C16 178.7(3) . . . . ? C13 C14 C15 C16 -2.7(4) . . . . ? N2 C15 C16 C17 -0.9(4) . . . . ? C14 C15 C16 C17 178.7(3) . . . . ? C15 C16 C17 C18 -2.0(4) . . . . ? C15 C16 C17 C5 178.0(3) . . . . ? C16 C17 C18 C19 3.2(4) . . . . ? C5 C17 C18 C19 -176.7(3) . . . . ? C15 N2 C19 C18 -1.4(4) . . . . ? Ru1 N2 C19 C18 173.1(2) . . . . ? C17 C18 C19 N2 -1.6(5) . . . . ? C11 C12 C4 C42B 1.1(8) . . . . ? C13 C12 C4 C42B -178.0(7) . . . . ? C11 C12 C4 C41B 129.0(7) . . . . ? C13 C12 C4 C41B -50.1(8) . . . . ? C11 C12 C4 C43A -160.4(6) . . . . ? C13 C12 C4 C43A 20.4(7) . . . . ? C11 C12 C4 C42A -35.5(6) . . . . ? C13 C12 C4 C42A 145.3(5) . . . . ? C11 C12 C4 C43B -117.7(6) . . . . ? C13 C12 C4 C43B 63.2(6) . . . . ? C11 C12 C4 C41A 80.2(5) . . . . ? C13 C12 C4 C41A -99.0(5) . . . . ? C18 C17 C5 C52 120.0(3) . . . . ? C16 C17 C5 C52 -60.0(4) . . . . ? C18 C17 C5 C51 -121.2(3) . . . . ? C16 C17 C5 C51 58.9(4) . . . . ? C18 C17 C5 C53 0.1(4) . . . . ? C16 C17 C5 C53 -179.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.160 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.077 #===END======================================================================== data_compound4 _database_code_CSD 162467 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'trans(Cl)-[Ru(4,4'-TBubpy)(CO)2Cl2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H25 Cl5 N2 O2 Ru' _chemical_formula_weight 615.75 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' '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' '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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.11310(10) _cell_length_b 13.9583(2) _cell_length_c 15.9437(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2695.73(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.23630 _exptl_absorpt_correction_T_max 0.26723 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33328 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2542 _reflns_number_gt 2341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0631P)^2^+10.5256P] 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 2542 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.14009(3) 0.2500 0.01353(3) 0.01971(18) Uani 1 2 d S . . Cl1 Cl -0.02722(11) 0.2500 -0.06688(8) 0.0265(3) Uani 1 2 d S . . Cl2 Cl 0.29609(11) 0.2500 0.10481(9) 0.0276(3) Uani 1 2 d S . . C1 C 0.2074(3) 0.3435(3) -0.0540(2) 0.0294(9) Uani 1 1 d . . . O1 O 0.2502(3) 0.4000(3) -0.0937(2) 0.0478(9) Uani 1 1 d . . . N1 N 0.0646(2) 0.1557(2) 0.09936(18) 0.0197(6) Uani 1 1 d . . . C10 C 0.0624(3) 0.0601(3) 0.0933(2) 0.0231(8) Uani 1 1 d . . . H10 H 0.0915 0.0311 0.0442 0.028 Uiso 1 1 calc R . . C11 C 0.0197(3) 0.0017(3) 0.1552(2) 0.0226(8) Uani 1 1 d . . . H11 H 0.0195 -0.0658 0.1479 0.027 Uiso 1 1 calc R . . C12 C -0.0230(3) 0.0414(3) 0.2283(2) 0.0211(7) Uani 1 1 d . . . C13 C -0.0224(3) 0.1418(3) 0.2332(2) 0.0217(8) Uani 1 1 d . . . H13 H -0.0522 0.1723 0.2814 0.026 Uiso 1 1 calc R . . C14 C 0.0207(3) 0.1968(2) 0.1692(2) 0.0196(7) Uani 1 1 d . . . C4 C -0.0709(3) -0.0192(3) 0.2997(2) 0.0265(8) Uani 1 1 d . . . C41 C -0.0232(4) 0.0148(3) 0.3844(3) 0.0348(10) Uani 1 1 d . . . H41A H -0.0521 -0.0256 0.4296 0.052 Uiso 1 1 calc R . . H41B H -0.0449 0.0815 0.3943 0.052 Uiso 1 1 calc R . . H41C H 0.0575 0.0102 0.3830 0.052 Uiso 1 1 calc R . . C42 C -0.1970(4) -0.0054(3) 0.3005(3) 0.0349(10) Uani 1 1 d . . . H42A H -0.2278 -0.0264 0.2467 0.052 Uiso 1 1 calc R . . H42B H -0.2142 0.0624 0.3093 0.052 Uiso 1 1 calc R . . H42C H -0.2292 -0.0435 0.3460 0.052 Uiso 1 1 calc R . . C44 C -0.0444(5) -0.1254(3) 0.2881(3) 0.0452(12) Uani 1 1 d . . . H43A H -0.0784 -0.1485 0.2361 0.068 Uiso 1 1 calc R . . H43B H -0.0736 -0.1618 0.3357 0.068 Uiso 1 1 calc R . . H43C H 0.0358 -0.1340 0.2849 0.068 Uiso 1 1 calc R . . C99 C 0.2360(7) 0.2500 0.4422(5) 0.060(2) Uani 1 2 d S . . Cl5 Cl 0.0986(3) 0.2500 0.48819(17) 0.0873(9) Uani 1 2 d S . . Cl6A Cl 0.1636(15) 0.203(3) 0.5046(11) 0.126(3) Uani 0.085(2) 1 d P . 1 Cl7A Cl 0.2523(11) 0.1608(11) 0.3897(12) 0.0454(8) Uani 0.085(2) 1 d P . 1 Cl6B Cl 0.2239(2) 0.2500 0.33311(18) 0.126(3) Uani 0.830(4) 2 d SP . 2 Cl7B Cl 0.2586(2) 0.1142(2) 0.4378(2) 0.0454(8) Uani 0.415(2) 1 d P . 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 Ru1 0.0205(3) 0.0225(3) 0.0161(3) 0.000 0.00235(15) 0.000 Cl1 0.0264(7) 0.0312(7) 0.0218(6) 0.000 -0.0029(5) 0.000 Cl2 0.0248(6) 0.0283(7) 0.0297(7) 0.000 -0.0057(5) 0.000 C1 0.0255(19) 0.039(2) 0.024(2) 0.0025(18) 0.0011(16) 0.0001(17) O1 0.0473(19) 0.055(2) 0.0411(18) 0.0177(17) 0.0083(15) -0.0143(17) N1 0.0214(15) 0.0186(15) 0.0191(14) -0.0026(12) -0.0004(11) 0.0010(12) C10 0.0237(18) 0.0217(18) 0.0239(18) -0.0067(15) 0.0010(14) 0.0015(15) C11 0.0271(19) 0.0147(17) 0.0260(19) -0.0031(15) -0.0004(15) 0.0006(14) C12 0.0226(18) 0.0173(17) 0.0234(18) 0.0010(14) -0.0007(14) -0.0018(14) C13 0.0259(18) 0.0176(17) 0.0215(18) -0.0030(14) 0.0024(14) 0.0013(14) C14 0.0211(17) 0.0174(18) 0.0203(17) -0.0017(14) -0.0007(13) 0.0008(14) C4 0.039(2) 0.0168(18) 0.0240(19) 0.0020(15) 0.0049(16) -0.0018(16) C41 0.051(3) 0.029(2) 0.025(2) 0.0054(17) -0.0035(18) 0.0004(19) C42 0.037(2) 0.036(2) 0.032(2) -0.0010(18) 0.0073(18) -0.0113(19) C44 0.078(4) 0.019(2) 0.039(2) 0.0053(18) 0.018(2) 0.001(2) C99 0.058(5) 0.071(6) 0.050(5) 0.000 -0.017(4) 0.000 Cl5 0.123(3) 0.0710(16) 0.0684(16) 0.000 0.0419(17) 0.000 Cl6A 0.0405(15) 0.285(8) 0.0520(19) 0.084(5) 0.0059(13) 0.030(5) Cl7A 0.0295(12) 0.0346(15) 0.072(2) -0.0156(14) -0.0014(13) 0.0033(11) Cl6B 0.0405(15) 0.285(8) 0.0520(19) 0.084(5) 0.0059(13) 0.030(5) Cl7B 0.0295(12) 0.0346(15) 0.072(2) -0.0156(14) -0.0014(13) 0.0033(11) _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 C1 1.878(4) . ? Ru1 C1 1.878(4) 7_565 ? Ru1 N1 2.107(3) 7_565 ? Ru1 N1 2.107(3) . ? Ru1 Cl2 2.3852(13) . ? Ru1 Cl1 2.3981(13) . ? C1 O1 1.137(5) . ? N1 C10 1.339(5) . ? N1 C14 1.361(5) . ? C10 C11 1.380(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 C13 1.403(5) . ? C12 C4 1.532(5) . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C14 1.486(7) 7_565 ? C4 C44 1.529(5) . ? C4 C42 1.539(6) . ? C4 C41 1.543(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 H43A 0.9800 . ? C44 H43B 0.9800 . ? C44 H43C 0.9800 . ? C99 Cl6A 1.48(2) 7_565 ? C99 Cl6A 1.48(2) . ? C99 Cl7A 1.513(14) . ? C99 Cl7A 1.513(14) 7_565 ? C99 Cl6B 1.745(9) . ? C99 Cl5 1.818(10) . ? C99 Cl7B 1.917(3) 7_565 ? C99 Cl7B 1.917(3) . ? Cl5 Cl6A 1.06(3) 7_565 ? Cl5 Cl6A 1.06(3) . ? Cl6A Cl6A 1.32(8) 7_565 ? Cl6A Cl7A 2.20(3) . ? 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 C1 Ru1 C1 88.0(3) . 7_565 ? C1 Ru1 N1 97.29(15) . 7_565 ? C1 Ru1 N1 174.05(15) 7_565 7_565 ? C1 Ru1 N1 174.05(15) . . ? C1 Ru1 N1 97.29(15) 7_565 . ? N1 Ru1 N1 77.27(16) 7_565 . ? C1 Ru1 Cl2 90.34(12) . . ? C1 Ru1 Cl2 90.34(12) 7_565 . ? N1 Ru1 Cl2 87.00(8) 7_565 . ? N1 Ru1 Cl2 87.00(8) . . ? C1 Ru1 Cl1 93.46(12) . . ? C1 Ru1 Cl1 93.46(12) 7_565 . ? N1 Ru1 Cl1 88.87(8) 7_565 . ? N1 Ru1 Cl1 88.87(8) . . ? Cl2 Ru1 Cl1 174.71(5) . . ? O1 C1 Ru1 178.4(4) . . ? C10 N1 C14 118.1(3) . . ? C10 N1 Ru1 125.8(3) . . ? C14 N1 Ru1 116.0(2) . . ? N1 C10 C11 123.0(3) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 116.3(3) . . ? C11 C12 C4 122.9(3) . . ? C13 C12 C4 120.8(3) . . ? C14 C13 C12 121.1(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? N1 C14 C13 121.3(3) . . ? N1 C14 C14 114.9(2) . 7_565 ? C13 C14 C14 123.8(2) . 7_565 ? C44 C4 C12 111.5(3) . . ? C44 C4 C42 109.3(4) . . ? C12 C4 C42 108.3(3) . . ? C44 C4 C41 109.0(4) . . ? C12 C4 C41 109.8(3) . . ? C42 C4 C41 109.0(3) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C44 H43A 109.5 . . ? C4 C44 H43B 109.5 . . ? H43A C44 H43B 109.5 . . ? C4 C44 H43C 109.5 . . ? H43A C44 H43C 109.5 . . ? H43B C44 H43C 109.5 . . ? Cl6A C99 Cl6A 53(3) 7_565 . ? Cl6A C99 Cl7A 144.7(15) 7_565 . ? Cl6A C99 Cl7A 94.6(17) . . ? Cl6A C99 Cl7A 94.6(17) 7_565 7_565 ? Cl6A C99 Cl7A 144.7(15) . 7_565 ? Cl7A C99 Cl7A 110.8(16) . 7_565 ? Cl6A C99 Cl6B 128.3(11) 7_565 . ? Cl6A C99 Cl6B 128.3(11) . . ? Cl7A C99 Cl6B 57.3(8) . . ? Cl7A C99 Cl6B 57.3(8) 7_565 . ? Cl6A C99 Cl5 35.7(10) 7_565 . ? Cl6A C99 Cl5 35.7(10) . . ? Cl7A C99 Cl5 110.1(6) . . ? Cl7A C99 Cl5 110.1(6) 7_565 . ? Cl6B C99 Cl5 109.0(4) . . ? Cl6A C99 Cl7B 70.5(15) 7_565 7_565 ? Cl6A C99 Cl7B 123.4(16) . 7_565 ? Cl7A C99 Cl7B 140.8(9) . 7_565 ? Cl7A C99 Cl7B 31.5(7) 7_565 7_565 ? Cl6B C99 Cl7B 88.6(3) . 7_565 ? Cl5 C99 Cl7B 98.4(3) . 7_565 ? Cl6A C99 Cl7B 123.4(16) 7_565 . ? Cl6A C99 Cl7B 70.5(15) . . ? Cl7A C99 Cl7B 31.5(7) . . ? Cl7A C99 Cl7B 140.8(9) 7_565 . ? Cl6B C99 Cl7B 88.6(3) . . ? Cl5 C99 Cl7B 98.4(3) . . ? Cl7B C99 Cl7B 163.0(6) 7_565 . ? Cl6A Cl5 Cl6A 77(4) 7_565 . ? Cl6A Cl5 C99 54.6(12) 7_565 . ? Cl6A Cl5 C99 54.6(12) . . ? Cl5 Cl6A Cl6A 51.4(19) . 7_565 ? Cl5 Cl6A C99 89.7(18) . . ? Cl6A Cl6A C99 63.5(15) 7_565 . ? Cl5 Cl6A Cl7A 108.8(12) . . ? Cl6A Cl6A Cl7A 105.4(11) 7_565 . ? C99 Cl6A Cl7A 43.2(8) . . ? C99 Cl7A Cl6A 42.1(11) . . ? 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 C1 Ru1 C1 O1 -86(15) 7_565 . . . ? N1 Ru1 C1 O1 91(15) 7_565 . . . ? N1 Ru1 C1 O1 67(15) . . . . ? Cl2 Ru1 C1 O1 4(15) . . . . ? Cl1 Ru1 C1 O1 -180(100) . . . . ? C1 Ru1 N1 C10 -160.0(13) . . . . ? C1 Ru1 N1 C10 -6.4(3) 7_565 . . . ? N1 Ru1 N1 C10 176.0(3) 7_565 . . . ? Cl2 Ru1 N1 C10 -96.4(3) . . . . ? Cl1 Ru1 N1 C10 86.9(3) . . . . ? C1 Ru1 N1 C14 15.7(15) . . . . ? C1 Ru1 N1 C14 169.2(3) 7_565 . . . ? N1 Ru1 N1 C14 -8.4(3) 7_565 . . . ? Cl2 Ru1 N1 C14 79.2(2) . . . . ? Cl1 Ru1 N1 C14 -97.5(2) . . . . ? C14 N1 C10 C11 -1.2(5) . . . . ? Ru1 N1 C10 C11 174.3(3) . . . . ? N1 C10 C11 C12 -0.5(6) . . . . ? C10 C11 C12 C13 1.7(5) . . . . ? C10 C11 C12 C4 -179.6(3) . . . . ? C11 C12 C13 C14 -1.4(6) . . . . ? C4 C12 C13 C14 179.9(3) . . . . ? C10 N1 C14 C13 1.6(5) . . . . ? Ru1 N1 C14 C13 -174.4(3) . . . . ? C10 N1 C14 C14 -176.8(2) . . . 7_565 ? Ru1 N1 C14 C14 7.2(2) . . . 7_565 ? C12 C13 C14 N1 -0.3(6) . . . . ? C12 C13 C14 C14 178.0(2) . . . 7_565 ? C11 C12 C4 C44 11.6(6) . . . . ? C13 C12 C4 C44 -169.8(4) . . . . ? C11 C12 C4 C42 -108.7(4) . . . . ? C13 C12 C4 C42 69.9(4) . . . . ? C11 C12 C4 C41 132.4(4) . . . . ? C13 C12 C4 C41 -49.0(5) . . . . ? Cl6A C99 Cl5 Cl6A 100(5) . . . 7_565 ? Cl7A C99 Cl5 Cl6A 169(2) . . . 7_565 ? Cl7A C99 Cl5 Cl6A -69(2) 7_565 . . 7_565 ? Cl6B C99 Cl5 Cl6A -130(2) . . . 7_565 ? Cl7B C99 Cl5 Cl6A -39(2) 7_565 . . 7_565 ? Cl7B C99 Cl5 Cl6A 139(2) . . . 7_565 ? Cl6A C99 Cl5 Cl6A -100(5) 7_565 . . . ? Cl7A C99 Cl5 Cl6A 69(2) . . . . ? Cl7A C99 Cl5 Cl6A -169(2) 7_565 . . . ? Cl6B C99 Cl5 Cl6A 130(2) . . . . ? Cl7B C99 Cl5 Cl6A -139(2) 7_565 . . . ? Cl7B C99 Cl5 Cl6A 39(2) . . . . ? C99 Cl5 Cl6A Cl6A 55.4(19) . . . 7_565 ? Cl6A Cl5 Cl6A C99 -55.4(19) 7_565 . . . ? Cl6A Cl5 Cl6A Cl7A -95(2) 7_565 . . . ? C99 Cl5 Cl6A Cl7A -39.5(7) . . . . ? Cl6A C99 Cl6A Cl5 46(2) 7_565 . . . ? Cl7A C99 Cl6A Cl5 -118(2) . . . . ? Cl7A C99 Cl6A Cl5 18(4) 7_565 . . . ? Cl6B C99 Cl6A Cl5 -67(3) . . . . ? Cl7B C99 Cl6A Cl5 52(2) 7_565 . . . ? Cl7B C99 Cl6A Cl5 -139(2) . . . . ? Cl7A C99 Cl6A Cl6A -164.5(9) . . . 7_565 ? Cl7A C99 Cl6A Cl6A -27.5(18) 7_565 . . 7_565 ? Cl6B C99 Cl6A Cl6A -113.2(12) . . . 7_565 ? Cl5 C99 Cl6A Cl6A -46(2) . . . 7_565 ? Cl7B C99 Cl6A Cl6A 5.7(4) 7_565 . . 7_565 ? Cl7B C99 Cl6A Cl6A 174.9(3) . . . 7_565 ? Cl6A C99 Cl6A Cl7A 164.5(9) 7_565 . . . ? Cl7A C99 Cl6A Cl7A 137(3) 7_565 . . . ? Cl6B C99 Cl6A Cl7A 51.2(12) . . . . ? Cl5 C99 Cl6A Cl7A 118(2) . . . . ? Cl7B C99 Cl6A Cl7A 170.2(11) 7_565 . . . ? Cl7B C99 Cl6A Cl7A -20.6(7) . . . . ? Cl6A C99 Cl7A Cl6A -22(2) 7_565 . . . ? Cl7A C99 Cl7A Cl6A -155.0(13) 7_565 . . . ? Cl6B C99 Cl7A Cl6A -133.3(9) . . . . ? Cl5 C99 Cl7A Cl6A -33.1(7) . . . . ? Cl7B C99 Cl7A Cl6A -167.0(15) 7_565 . . . ? Cl7B C99 Cl7A Cl6A 39.5(12) . . . . ? Cl5 Cl6A Cl7A C99 68(2) . . . . ? Cl6A Cl6A Cl7A C99 14.4(8) 7_565 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.799 _refine_diff_density_min -1.722 _refine_diff_density_rms 0.118 #===END======================================================================== data_compound5 _database_code_CSD 162468 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'trans(Cl)-[Ru(4,4'-NObpy)(CO)2Cl2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H6 Cl2 N4 O6 Ru' _chemical_formula_weight 474.18 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' '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' '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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 21.6703(9) _cell_length_b 38.6235(5) _cell_length_c 7.8367(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6559.2(3) _cell_formula_units_Z 16 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 1.320 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6929 _exptl_absorpt_correction_T_max 0.8793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24184 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3176 _reflns_number_gt 3017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0139P)^2^+6.4214P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.51(2) _refine_ls_number_reflns 3176 _refine_ls_number_parameters 227 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0467 _refine_ls_wR_factor_gt 0.0458 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.725402(11) 0.084896(6) 0.58649(3) 0.02480(8) Uani 1 1 d . . . Cl1 Cl 0.74488(4) 0.028592(19) 0.69645(9) 0.03193(19) Uani 1 1 d . . . Cl2 Cl 0.71145(4) 0.13886(2) 0.44527(12) 0.0413(2) Uani 1 1 d . . . C1 C 0.77811(17) 0.10530(9) 0.7478(5) 0.0379(9) Uani 1 1 d . . . O1 O 0.80883(13) 0.11765(7) 0.8450(4) 0.0596(7) Uani 1 1 d . . . C2 C 0.66247(17) 0.09386(8) 0.7476(4) 0.0341(8) Uani 1 1 d . . . O2 O 0.62728(12) 0.09914(6) 0.8493(3) 0.0529(7) Uani 1 1 d . . . N1 N 0.67192(11) 0.06219(6) 0.3908(3) 0.0198(5) Uani 1 1 d . . . N2 N 0.79169(11) 0.07303(6) 0.3990(3) 0.0249(6) Uani 1 1 d . . . C10 C 0.60992(13) 0.05801(7) 0.3970(4) 0.0265(7) Uani 1 1 d . . . H10 H 0.5888 0.0631 0.5002 0.032 Uiso 1 1 calc R . . C11 C 0.57671(14) 0.04673(8) 0.2591(4) 0.0295(8) Uani 1 1 d . . . H11 H 0.5331 0.0446 0.2641 0.035 Uiso 1 1 calc R . . C12 C 0.60841(12) 0.03862(7) 0.1146(4) 0.0244(7) Uani 1 1 d . . . N4 N 0.57379(12) 0.02807(7) -0.0400(4) 0.0395(7) Uani 1 1 d . . . O11 O 0.51882(11) 0.03549(8) -0.0421(4) 0.0778(10) Uani 1 1 d . . . O12 O 0.60159(11) 0.01433(7) -0.1544(4) 0.0574(7) Uani 1 1 d . . . C13 C 0.67185(12) 0.04088(7) 0.1047(4) 0.0199(6) Uani 1 1 d . . . H13 H 0.6935 0.0340 0.0049 0.024 Uiso 1 1 calc R . . C14 C 0.70267(12) 0.05361(7) 0.2462(3) 0.0179(6) Uani 1 1 d . . . C15 C 0.77031(12) 0.05895(7) 0.2523(4) 0.0201(6) Uani 1 1 d . . . C16 C 0.80986(12) 0.04962(7) 0.1206(4) 0.0234(7) Uani 1 1 d . . . H16 H 0.7948 0.0398 0.0176 0.028 Uiso 1 1 calc R . . C17 C 0.87197(13) 0.05531(8) 0.1464(4) 0.0303(8) Uani 1 1 d . . . N5 N 0.91616(13) 0.04501(9) 0.0100(5) 0.0460(8) Uani 1 1 d . . . O21 O 0.97000(12) 0.05216(10) 0.0364(4) 0.0825(11) Uani 1 1 d . . . O22 O 0.89627(13) 0.03088(7) -0.1136(4) 0.0628(9) Uani 1 1 d . . . C18 C 0.89406(15) 0.06963(9) 0.2936(5) 0.0418(10) Uani 1 1 d . . . H18 H 0.9370 0.0734 0.3092 0.050 Uiso 1 1 calc R . . C19 C 0.85249(15) 0.07846(8) 0.4181(5) 0.0365(8) Uani 1 1 d . . . H19 H 0.8671 0.0887 0.5206 0.044 Uiso 1 1 calc R . . 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 0.02977(13) 0.02615(12) 0.01846(11) -0.00213(11) -0.00501(11) 0.00248(11) Cl1 0.0449(5) 0.0295(4) 0.0215(4) -0.0005(3) 0.0038(4) 0.0108(4) Cl2 0.0427(5) 0.0325(5) 0.0486(5) 0.0086(4) -0.0168(4) -0.0025(4) C1 0.053(2) 0.0325(19) 0.028(2) -0.0021(17) -0.0089(17) 0.0004(16) O1 0.0744(19) 0.0609(17) 0.0434(15) -0.0052(16) -0.0205(17) -0.0130(14) C2 0.049(2) 0.0312(18) 0.0223(18) 0.0004(15) -0.0075(17) 0.0129(16) O2 0.0721(17) 0.0598(16) 0.0268(13) 0.0021(14) 0.0072(15) 0.0323(14) N1 0.0206(13) 0.0237(12) 0.0151(12) -0.0006(10) 0.0028(10) 0.0008(10) N2 0.0186(13) 0.0310(14) 0.0251(14) 0.0058(12) -0.0071(11) -0.0033(11) C10 0.0187(16) 0.0296(17) 0.0311(18) -0.0027(14) 0.0066(13) 0.0017(13) C11 0.0148(15) 0.0301(17) 0.044(2) -0.0048(15) 0.0038(14) 0.0014(13) C12 0.0174(15) 0.0272(15) 0.0287(18) -0.0041(14) -0.0033(13) 0.0020(12) N4 0.0211(15) 0.0522(18) 0.0451(18) -0.0187(17) -0.0105(14) 0.0039(13) O11 0.0336(16) 0.104(2) 0.096(2) -0.053(2) -0.0285(16) 0.0210(15) O12 0.0372(14) 0.0849(19) 0.0500(15) -0.0337(17) -0.0083(14) -0.0036(13) C13 0.0182(14) 0.0245(14) 0.0170(15) -0.0016(14) 0.0033(13) 0.0028(11) C14 0.0160(14) 0.0196(14) 0.0183(15) 0.0016(12) 0.0031(12) 0.0015(12) C15 0.0154(15) 0.0232(15) 0.0218(15) 0.0051(14) -0.0027(12) 0.0002(12) C16 0.0187(15) 0.0282(15) 0.0232(17) 0.0059(14) 0.0049(13) 0.0004(12) C17 0.0191(17) 0.0381(18) 0.0336(18) 0.0138(14) 0.0094(14) 0.0055(14) N5 0.0242(18) 0.056(2) 0.058(2) 0.0221(17) 0.0159(15) 0.0074(15) O21 0.0162(14) 0.169(3) 0.062(2) 0.034(2) 0.0141(12) 0.0063(16) O22 0.0451(17) 0.0639(18) 0.079(2) -0.0229(16) 0.0367(17) -0.0081(14) C18 0.0166(17) 0.055(2) 0.053(3) 0.021(2) -0.0047(16) -0.0055(16) C19 0.0272(19) 0.046(2) 0.0364(19) 0.0045(17) -0.0101(16) -0.0063(15) _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 C1 1.877(4) . ? Ru1 C2 1.890(4) . ? Ru1 N2 2.106(3) . ? Ru1 N1 2.113(2) . ? Ru1 Cl1 2.3769(8) . ? Ru1 Cl2 2.3791(8) . ? C1 O1 1.118(4) . ? C2 O2 1.122(4) . ? N1 C10 1.354(4) . ? N1 C14 1.356(3) . ? N2 C19 1.343(4) . ? N2 C15 1.353(4) . ? C10 C11 1.369(4) . ? C10 H10 0.9500 . ? C11 C12 1.361(4) . ? C11 H11 0.9500 . ? C12 C13 1.380(4) . ? C12 N4 1.482(4) . ? N4 O12 1.203(3) . ? N4 O11 1.225(3) . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 C15 1.481(4) . ? C15 C16 1.389(4) . ? C16 C17 1.379(4) . ? C16 H16 0.9500 . ? C17 C18 1.366(5) . ? C17 N5 1.489(4) . ? N5 O22 1.192(4) . ? N5 O21 1.217(4) . ? C18 C19 1.371(5) . ? C18 H18 0.9500 . ? C19 H19 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 C1 Ru1 C2 84.96(15) . . ? C1 Ru1 N2 98.42(13) . . ? C2 Ru1 N2 176.55(13) . . ? C1 Ru1 N1 175.44(13) . . ? C2 Ru1 N1 99.49(12) . . ? N2 Ru1 N1 77.14(9) . . ? C1 Ru1 Cl1 91.82(11) . . ? C2 Ru1 Cl1 93.07(10) . . ? N2 Ru1 Cl1 86.14(7) . . ? N1 Ru1 Cl1 88.90(6) . . ? C1 Ru1 Cl2 91.31(11) . . ? C2 Ru1 Cl2 93.36(10) . . ? N2 Ru1 Cl2 87.29(7) . . ? N1 Ru1 Cl2 87.50(6) . . ? Cl1 Ru1 Cl2 173.07(3) . . ? O1 C1 Ru1 179.0(4) . . ? O2 C2 Ru1 176.6(3) . . ? C10 N1 C14 119.2(2) . . ? C10 N1 Ru1 124.63(19) . . ? C14 N1 Ru1 116.00(18) . . ? C19 N2 C15 119.6(3) . . ? C19 N2 Ru1 123.9(2) . . ? C15 N2 Ru1 116.53(18) . . ? N1 C10 C11 122.1(3) . . ? N1 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C12 C11 C10 117.7(3) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C11 C12 C13 122.3(3) . . ? C11 C12 N4 119.2(2) . . ? C13 C12 N4 118.4(3) . . ? O12 N4 O11 125.4(3) . . ? O12 N4 C12 118.5(2) . . ? O11 N4 C12 116.0(3) . . ? C12 C13 C14 117.3(3) . . ? C12 C13 H13 121.4 . . ? C14 C13 H13 121.4 . . ? N1 C14 C13 121.3(2) . . ? N1 C14 C15 115.2(2) . . ? C13 C14 C15 123.5(2) . . ? N2 C15 C16 121.6(2) . . ? N2 C15 C14 115.0(2) . . ? C16 C15 C14 123.4(3) . . ? C17 C16 C15 116.9(3) . . ? C17 C16 H16 121.6 . . ? C15 C16 H16 121.6 . . ? C18 C17 C16 122.0(3) . . ? C18 C17 N5 119.3(3) . . ? C16 C17 N5 118.7(3) . . ? O22 N5 O21 126.0(3) . . ? O22 N5 C17 118.2(3) . . ? O21 N5 C17 115.7(4) . . ? C17 C18 C19 118.1(3) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? N2 C19 C18 121.8(3) . . ? N2 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? 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 C2 Ru1 C1 O1 -19(22) . . . . ? N2 Ru1 C1 O1 162(100) . . . . ? N1 Ru1 C1 O1 149(100) . . . . ? Cl1 Ru1 C1 O1 -112(22) . . . . ? Cl2 Ru1 C1 O1 74(22) . . . . ? C1 Ru1 C2 O2 -26(5) . . . . ? N2 Ru1 C2 O2 143(4) . . . . ? N1 Ru1 C2 O2 155(5) . . . . ? Cl1 Ru1 C2 O2 66(5) . . . . ? Cl2 Ru1 C2 O2 -117(5) . . . . ? C1 Ru1 N1 C10 -166.3(15) . . . . ? C2 Ru1 N1 C10 1.6(2) . . . . ? N2 Ru1 N1 C10 -179.2(2) . . . . ? Cl1 Ru1 N1 C10 94.5(2) . . . . ? Cl2 Ru1 N1 C10 -91.4(2) . . . . ? C1 Ru1 N1 C14 9.1(16) . . . . ? C2 Ru1 N1 C14 177.0(2) . . . . ? N2 Ru1 N1 C14 -3.75(19) . . . . ? Cl1 Ru1 N1 C14 -90.05(18) . . . . ? Cl2 Ru1 N1 C14 84.04(19) . . . . ? C1 Ru1 N2 C19 3.6(3) . . . . ? C2 Ru1 N2 C19 -164(2) . . . . ? N1 Ru1 N2 C19 -177.4(3) . . . . ? Cl1 Ru1 N2 C19 -87.6(2) . . . . ? Cl2 Ru1 N2 C19 94.6(2) . . . . ? C1 Ru1 N2 C15 -176.7(2) . . . . ? C2 Ru1 N2 C15 15(2) . . . . ? N1 Ru1 N2 C15 2.26(19) . . . . ? Cl1 Ru1 N2 C15 92.0(2) . . . . ? Cl2 Ru1 N2 C15 -85.8(2) . . . . ? C14 N1 C10 C11 -2.8(4) . . . . ? Ru1 N1 C10 C11 172.5(2) . . . . ? N1 C10 C11 C12 2.1(5) . . . . ? C10 C11 C12 C13 1.1(5) . . . . ? C10 C11 C12 N4 -176.8(3) . . . . ? C11 C12 N4 O12 -165.1(3) . . . . ? C13 C12 N4 O12 16.9(4) . . . . ? C11 C12 N4 O11 17.7(5) . . . . ? C13 C12 N4 O11 -160.4(3) . . . . ? C11 C12 C13 C14 -3.3(4) . . . . ? N4 C12 C13 C14 174.6(3) . . . . ? C10 N1 C14 C13 0.4(4) . . . . ? Ru1 N1 C14 C13 -175.29(19) . . . . ? C10 N1 C14 C15 -179.7(2) . . . . ? Ru1 N1 C14 C15 4.6(3) . . . . ? C12 C13 C14 N1 2.6(4) . . . . ? C12 C13 C14 C15 -177.3(3) . . . . ? C19 N2 C15 C16 0.6(4) . . . . ? Ru1 N2 C15 C16 -179.1(2) . . . . ? C19 N2 C15 C14 179.1(3) . . . . ? Ru1 N2 C15 C14 -0.6(3) . . . . ? N1 C14 C15 N2 -2.7(4) . . . . ? C13 C14 C15 N2 177.2(3) . . . . ? N1 C14 C15 C16 175.8(2) . . . . ? C13 C14 C15 C16 -4.3(4) . . . . ? N2 C15 C16 C17 0.1(4) . . . . ? C14 C15 C16 C17 -178.3(3) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C15 C16 C17 N5 178.7(3) . . . . ? C18 C17 N5 O22 176.1(3) . . . . ? C16 C17 N5 O22 -3.1(5) . . . . ? C18 C17 N5 O21 -4.2(5) . . . . ? C16 C17 N5 O21 176.6(3) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? N5 C17 C18 C19 -179.1(3) . . . . ? C15 N2 C19 C18 -1.0(5) . . . . ? Ru1 N2 C19 C18 178.6(2) . . . . ? C17 C18 C19 N2 0.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.569 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.060 #===END======================================================================== data_compound6 _database_code_CSD 162469 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'trans(Cl)-[Ru(4,4'-phosbpy)(CO)2Cl2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H17 Cl2 N2 O11.50 P2 Ru' _chemical_formula_weight 607.19 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' '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' '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' 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 12.9936(3) _cell_length_b 26.5886(7) _cell_length_c 12.1315(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.9532(16) _cell_angle_gamma 90.00 _cell_volume 4128.13(18) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8864 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40510 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7179 _reflns_number_gt 4889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0195P)^2^+52.9879P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7179 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.20094(5) 0.73726(3) 0.23715(6) 0.01802(18) Uani 1 1 d . . . Cl1 Cl 0.08256(16) 0.76581(8) 0.07553(18) 0.0247(5) Uani 1 1 d . . . Cl2 Cl 0.30683(16) 0.70188(8) 0.39985(18) 0.0239(5) Uani 1 1 d . . . C1 C 0.1339(7) 0.7834(3) 0.3196(8) 0.023(2) Uani 1 1 d . . . O1 O 0.0889(5) 0.8130(2) 0.3593(5) 0.0301(15) Uani 1 1 d . . . C2 C 0.3032(7) 0.7854(3) 0.2245(7) 0.0200(19) Uani 1 1 d . . . O2 O 0.3710(5) 0.8115(2) 0.2177(6) 0.0322(16) Uani 1 1 d . . . N1 N 0.2582(5) 0.6849(2) 0.1314(6) 0.0174(15) Uani 1 1 d . . . N2 N 0.1039(5) 0.6746(3) 0.2438(6) 0.0197(16) Uani 1 1 d . . . C10 C 0.3355(6) 0.6938(3) 0.0751(7) 0.021(2) Uani 1 1 d . . . H10 H 0.3755 0.7237 0.0907 0.025 Uiso 1 1 calc R . . C11 C 0.3600(6) 0.6609(3) -0.0058(7) 0.0167(18) Uani 1 1 d . . . H11 H 0.4164 0.6680 -0.0439 0.020 Uiso 1 1 calc R . . C12 C 0.3010(6) 0.6179(3) -0.0298(7) 0.0194(19) Uani 1 1 d . . . C13 C 0.2212(7) 0.6078(3) 0.0311(7) 0.0205(19) Uani 1 1 d . . . H13 H 0.1810 0.5779 0.0176 0.025 Uiso 1 1 calc R . . C14 C 0.2016(6) 0.6417(3) 0.1112(7) 0.0157(18) Uani 1 1 d . . . C15 C 0.1200(6) 0.6344(3) 0.1812(7) 0.0181(19) Uani 1 1 d . . . C16 C 0.0653(6) 0.5899(3) 0.1835(7) 0.0188(19) Uani 1 1 d . . . H16 H 0.0754 0.5628 0.1355 0.023 Uiso 1 1 calc R . . C17 C -0.0059(6) 0.5856(3) 0.2589(8) 0.0215(19) Uani 1 1 d . . . C18 C -0.0206(7) 0.6259(3) 0.3235(7) 0.023(2) Uani 1 1 d . . . H18 H -0.0688 0.6239 0.3740 0.028 Uiso 1 1 calc R . . C19 C 0.0362(7) 0.6706(3) 0.3151(8) 0.024(2) Uani 1 1 d . . . H19 H 0.0262 0.6985 0.3611 0.029 Uiso 1 1 calc R . . P4 P 0.31722(17) 0.57876(9) -0.14831(19) 0.0211(5) Uani 1 1 d . . . O11 O 0.4258(4) 0.5828(2) -0.1710(5) 0.0256(14) Uani 1 1 d . . . O12 O 0.2288(5) 0.5999(2) -0.2407(5) 0.0288(15) Uani 1 1 d . . . O13 O 0.2908(5) 0.5242(2) -0.1199(5) 0.0231(14) Uani 1 1 d . . . P5 P -0.07204(17) 0.52710(9) 0.2773(2) 0.0212(5) Uani 1 1 d . . . O21 O -0.1669(5) 0.5385(2) 0.3278(6) 0.0326(16) Uani 1 1 d . . . O22 O -0.0973(4) 0.4995(2) 0.1668(5) 0.0241(14) Uani 1 1 d . . . O23 O 0.0170(5) 0.4992(2) 0.3583(5) 0.0294(15) Uani 1 1 d . . . Ru1B Ru 0.69408(5) 0.73823(3) 0.21014(6) 0.01893(19) Uani 1 1 d . . . Cl1B Cl 0.56894(16) 0.76331(9) 0.05096(17) 0.0248(5) Uani 1 1 d . . . Cl2B Cl 0.80932(17) 0.71181(8) 0.37501(19) 0.0267(5) Uani 1 1 d . . . C1B C 0.6314(7) 0.7845(3) 0.2970(7) 0.0210(19) Uani 1 1 d . . . O1B O 0.5976(5) 0.8144(3) 0.3469(6) 0.0338(16) Uani 1 1 d . . . C2B C 0.7866(7) 0.7892(4) 0.1874(8) 0.027(2) Uani 1 1 d . . . O2B O 0.8457(6) 0.8187(3) 0.1686(7) 0.050(2) Uani 1 1 d . . . N1B N 0.7597(5) 0.6847(3) 0.1114(6) 0.0191(16) Uani 1 1 d . . . N2B N 0.6015(5) 0.6726(3) 0.2217(6) 0.0204(16) Uani 1 1 d . . . C10B C 0.8427(6) 0.6927(3) 0.0623(7) 0.0185(19) Uani 1 1 d . . . H10B H 0.8778 0.7240 0.0742 0.022 Uiso 1 1 calc R . . C11B C 0.8800(7) 0.6574(3) -0.0054(8) 0.025(2) Uani 1 1 d . . . H11B H 0.9395 0.6645 -0.0386 0.030 Uiso 1 1 calc R . . C12B C 0.8280(6) 0.6105(3) -0.0240(7) 0.0184(19) Uani 1 1 d . . . C13B C 0.7434(6) 0.6026(3) 0.0290(7) 0.0194(19) Uani 1 1 d . . . H13B H 0.7072 0.5714 0.0198 0.023 Uiso 1 1 calc R . . C14B C 0.7105(7) 0.6400(3) 0.0962(7) 0.0209(19) Uani 1 1 d . . . C15B C 0.6239(7) 0.6327(3) 0.1584(7) 0.0189(18) Uani 1 1 d . . . C16B C 0.5708(6) 0.5870(3) 0.1592(7) 0.023(2) Uani 1 1 d . . . H16B H 0.5877 0.5595 0.1156 0.027 Uiso 1 1 calc R . . C17B C 0.4936(6) 0.5823(3) 0.2239(7) 0.0215(19) Uani 1 1 d . . . C18B C 0.4724(6) 0.6231(3) 0.2881(7) 0.022(2) Uani 1 1 d . . . H18B H 0.4206 0.6203 0.3344 0.027 Uiso 1 1 calc R . . C19B C 0.5266(6) 0.6676(3) 0.2847(7) 0.021(2) Uani 1 1 d . . . H19B H 0.5104 0.6954 0.3280 0.026 Uiso 1 1 calc R . . P4B P 0.86722(17) 0.56538(8) -0.11848(19) 0.0205(5) Uani 1 1 d . . . O11B O 0.8350(5) 0.5824(2) -0.2357(5) 0.0284(15) Uani 1 1 d . . . O12B O 0.9863(4) 0.5621(2) -0.0802(5) 0.0278(15) Uani 1 1 d . . . O13B O 0.8202(4) 0.5143(2) -0.0915(5) 0.0232(14) Uani 1 1 d . . . P5B P 0.42985(17) 0.52228(9) 0.2361(2) 0.0214(5) Uani 1 1 d . . . O21B O 0.3153(4) 0.5305(2) 0.2329(5) 0.0230(14) Uani 1 1 d . . . O22B O 0.4490(5) 0.4903(2) 0.1351(5) 0.0280(15) Uani 1 1 d . . . O23B O 0.4824(5) 0.4990(2) 0.3457(5) 0.0280(15) Uani 1 1 d . . . O100 O 0.6743(5) 0.4840(3) 0.3845(5) 0.0318(16) Uani 1 1 d . . . O101 O 0.3173(5) 0.4221(3) 0.3999(5) 0.0341(16) Uani 1 1 d . . . O102 O 0.0132(5) 0.4049(3) 0.3988(6) 0.0406(18) Uani 1 1 d . . . O103 O 0.2199(5) 0.5414(3) 0.4159(5) 0.0335(16) Uani 1 1 d . . . O104 O -0.2713(5) 0.6060(2) 0.4240(6) 0.0353(16) Uani 1 1 d . . . O105 O 0.1917(6) 0.6196(3) -0.4493(6) 0.0386(17) Uani 1 1 d . . . O106 O 0.4919(6) 0.3829(3) 0.3802(6) 0.0447(19) Uani 1 1 d . . . H121 H 0.2530 0.6244 -0.2746 0.050 Uiso 1 1 d . . . H131 H 0.2237 0.5201 -0.1381 0.050 Uiso 1 1 d . . . H231 H -0.0101 0.4749 0.3905 0.050 Uiso 1 1 d . . . H122 H 1.0165 0.5661 -0.1375 0.050 Uiso 1 1 d . . . H132 H 0.7757 0.5046 -0.1488 0.050 Uiso 1 1 d . . . H221 H -0.0446 0.5012 0.1329 0.050 Uiso 1 1 d . . . H222 H 0.4674 0.4604 0.1577 0.050 Uiso 1 1 d . . . H232 H 0.5241 0.5207 0.3825 0.050 Uiso 1 1 d . . . H00A H 0.7139 0.4967 0.3417 0.050 Uiso 1 1 d . . . H00B H 0.6168 0.4764 0.3419 0.050 Uiso 1 1 d . . . H01A H 0.2808 0.4221 0.3335 0.050 Uiso 1 1 d . . . H01B H 0.3541 0.4491 0.4046 0.050 Uiso 1 1 d . . . H02A H 0.0398 0.3957 0.3417 0.050 Uiso 1 1 d . . . H02B H -0.0310 0.3819 0.4081 0.050 Uiso 1 1 d . . . H03A H 0.2453 0.5481 0.3567 0.050 Uiso 1 1 d . . . H03B H 0.1582 0.5298 0.3929 0.050 Uiso 1 1 d . . . H04A H -0.2878 0.6372 0.4266 0.050 Uiso 1 1 d . . . H04B H -0.2583 0.6009 0.3578 0.050 Uiso 1 1 d . . . H05A H 0.2221 0.6429 -0.4811 0.050 Uiso 1 1 d . . . H05B H 0.2411 0.6014 -0.4133 0.050 Uiso 1 1 d . . . H06A H 0.5051 0.3512 0.3829 0.050 Uiso 1 1 d . . . H06B H 0.4990 0.3924 0.3141 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0140(4) 0.0147(4) 0.0262(4) -0.0017(3) 0.0058(3) -0.0013(3) Cl1 0.0204(11) 0.0255(12) 0.0278(12) 0.0026(10) 0.0026(8) -0.0012(9) Cl2 0.0186(11) 0.0240(12) 0.0291(13) -0.0009(9) 0.0043(9) 0.0029(9) C1 0.019(5) 0.021(5) 0.029(5) 0.002(4) 0.007(4) 0.002(4) O1 0.024(3) 0.027(4) 0.041(4) -0.005(3) 0.013(3) 0.003(3) C2 0.018(5) 0.021(5) 0.022(5) -0.002(4) 0.006(4) 0.001(4) O2 0.026(4) 0.025(4) 0.048(4) -0.007(3) 0.014(3) -0.006(3) N1 0.017(4) 0.011(4) 0.024(4) -0.001(3) 0.005(3) -0.001(3) N2 0.011(4) 0.025(4) 0.024(4) -0.005(3) 0.006(3) 0.000(3) C10 0.015(4) 0.018(5) 0.027(5) 0.001(4) -0.002(4) -0.007(4) C11 0.015(4) 0.015(4) 0.021(5) -0.002(3) 0.006(3) -0.001(3) C12 0.021(5) 0.014(4) 0.025(5) 0.003(4) 0.008(4) 0.009(4) C13 0.019(5) 0.016(5) 0.025(5) 0.001(4) 0.000(4) -0.001(4) C14 0.011(4) 0.017(4) 0.019(5) 0.006(3) 0.004(3) 0.001(3) C15 0.012(4) 0.017(5) 0.023(5) 0.000(4) -0.003(3) 0.002(3) C16 0.022(5) 0.015(4) 0.021(5) -0.003(4) 0.008(4) 0.001(4) C17 0.015(4) 0.015(4) 0.033(5) 0.002(4) -0.001(4) 0.000(4) C18 0.020(5) 0.021(5) 0.030(5) -0.003(4) 0.011(4) -0.001(4) C19 0.018(5) 0.019(5) 0.034(6) -0.005(4) 0.004(4) 0.000(4) P4 0.0190(12) 0.0185(12) 0.0272(13) -0.0021(10) 0.0074(9) -0.0002(10) O11 0.022(3) 0.026(3) 0.031(4) -0.005(3) 0.009(3) 0.001(3) O12 0.022(3) 0.030(4) 0.033(4) 0.002(3) 0.003(3) 0.000(3) O13 0.024(3) 0.020(3) 0.025(3) -0.003(3) 0.004(3) -0.002(3) P5 0.0174(12) 0.0184(12) 0.0294(13) -0.0008(10) 0.0087(9) -0.0027(9) O21 0.025(4) 0.033(4) 0.044(4) -0.010(3) 0.019(3) -0.009(3) O22 0.013(3) 0.025(3) 0.037(4) 0.000(3) 0.009(3) -0.003(3) O23 0.024(3) 0.023(4) 0.040(4) 0.008(3) 0.002(3) -0.008(3) Ru1B 0.0145(4) 0.0147(4) 0.0284(4) -0.0015(3) 0.0059(3) -0.0002(3) Cl1B 0.0213(11) 0.0258(12) 0.0271(12) 0.0017(10) 0.0031(9) 0.0018(10) Cl2B 0.0221(11) 0.0248(12) 0.0319(13) -0.0037(10) 0.0009(9) 0.0039(10) C1B 0.024(5) 0.022(5) 0.016(5) 0.001(4) 0.001(4) -0.002(4) O1B 0.035(4) 0.030(4) 0.038(4) -0.002(3) 0.011(3) 0.003(3) C2B 0.028(5) 0.025(5) 0.032(6) -0.007(4) 0.016(4) 0.008(5) O2B 0.043(5) 0.029(4) 0.086(6) -0.015(4) 0.035(4) -0.014(4) N1B 0.016(4) 0.020(4) 0.022(4) 0.002(3) 0.004(3) -0.004(3) N2B 0.014(4) 0.018(4) 0.029(4) 0.002(3) 0.004(3) 0.000(3) C10B 0.019(5) 0.008(4) 0.030(5) 0.001(4) 0.009(4) -0.001(3) C11B 0.017(5) 0.024(5) 0.035(6) 0.000(4) 0.008(4) 0.003(4) C12B 0.018(5) 0.013(4) 0.024(5) 0.003(3) 0.002(4) -0.002(3) C13B 0.019(5) 0.015(4) 0.024(5) 0.000(4) 0.005(4) -0.003(4) C14B 0.019(5) 0.019(5) 0.026(5) 0.004(4) 0.008(4) 0.001(4) C15B 0.021(5) 0.013(4) 0.022(5) -0.002(4) 0.004(4) 0.001(4) C16B 0.018(5) 0.018(5) 0.032(5) 0.004(4) 0.007(4) -0.002(4) C17B 0.018(4) 0.017(5) 0.029(5) -0.001(4) 0.005(4) 0.002(4) C18B 0.009(4) 0.029(5) 0.029(5) 0.008(4) 0.003(4) -0.001(4) C19B 0.013(5) 0.024(5) 0.028(5) 0.000(4) 0.006(4) 0.001(4) P4B 0.0185(12) 0.0172(12) 0.0272(13) -0.0021(10) 0.0074(9) -0.0021(9) O11B 0.028(4) 0.026(4) 0.032(4) -0.001(3) 0.005(3) 0.002(3) O12B 0.019(3) 0.037(4) 0.029(4) -0.004(3) 0.008(3) -0.006(3) O13B 0.022(3) 0.021(3) 0.026(3) -0.001(3) 0.003(3) -0.002(3) P5B 0.0154(12) 0.0177(12) 0.0316(14) 0.0021(10) 0.0050(9) -0.0013(9) O21B 0.014(3) 0.024(3) 0.032(4) -0.001(3) 0.004(2) -0.002(3) O22B 0.028(4) 0.022(3) 0.034(4) -0.001(3) 0.005(3) -0.002(3) O23B 0.025(3) 0.025(4) 0.033(4) 0.002(3) 0.001(3) -0.006(3) O100 0.016(3) 0.039(4) 0.040(4) 0.005(3) 0.002(3) -0.008(3) O101 0.029(4) 0.036(4) 0.038(4) 0.005(3) 0.007(3) -0.003(3) O102 0.040(4) 0.034(4) 0.050(5) 0.005(3) 0.014(3) 0.007(3) O103 0.022(3) 0.048(4) 0.032(4) -0.008(3) 0.010(3) -0.006(3) O104 0.037(4) 0.031(4) 0.038(4) 0.000(3) 0.008(3) 0.007(3) O105 0.050(4) 0.028(4) 0.036(4) 0.010(3) 0.001(3) 0.001(3) O106 0.045(5) 0.033(4) 0.062(5) 0.004(4) 0.026(4) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.870(9) . ? Ru1 C1 1.888(9) . ? Ru1 N2 2.099(7) . ? Ru1 N1 2.113(7) . ? Ru1 Cl2 2.395(2) . ? Ru1 Cl1 2.397(2) . ? C1 O1 1.137(10) . ? C2 O2 1.136(10) . ? N1 C10 1.330(11) . ? N1 C14 1.363(10) . ? N2 C19 1.341(11) . ? N2 C15 1.348(11) . ? C10 C11 1.391(12) . ? C10 H10 0.9500 . ? C11 C12 1.380(12) . ? C11 H11 0.9500 . ? C12 C13 1.399(12) . ? C12 P4 1.816(9) . ? C13 C14 1.382(12) . ? C13 H13 0.9500 . ? C14 C15 1.480(11) . ? C15 C16 1.384(12) . ? C16 C17 1.415(12) . ? C16 H16 0.9500 . ? C17 C18 1.358(12) . ? C17 P5 1.810(9) . ? C18 C19 1.413(12) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? P4 O11 1.487(6) . ? P4 O13 1.543(6) . ? P4 O12 1.565(6) . ? O12 H121 0.8585 . ? O13 H131 0.8683 . ? P5 O21 1.500(6) . ? P5 O22 1.514(6) . ? P5 O23 1.569(7) . ? O22 H221 0.8600 . ? O23 H231 0.8601 . ? Ru1B C2B 1.864(10) . ? Ru1B C1B 1.893(9) . ? Ru1B N1B 2.130(7) . ? Ru1B N2B 2.137(7) . ? Ru1B Cl2B 2.388(2) . ? Ru1B Cl1B 2.394(2) . ? C1B O1B 1.132(10) . ? C2B O2B 1.148(11) . ? N1B C10B 1.336(10) . ? N1B C14B 1.348(11) . ? N2B C19B 1.344(11) . ? N2B C15B 1.370(11) . ? C10B C11B 1.389(12) . ? C10B H10B 0.9500 . ? C11B C12B 1.417(12) . ? C11B H11B 0.9500 . ? C12B C13B 1.383(12) . ? C12B P4B 1.793(9) . ? C13B C14B 1.399(12) . ? C13B H13B 0.9500 . ? C14B C15B 1.473(12) . ? C15B C16B 1.398(12) . ? C16B C17B 1.383(12) . ? C16B H16B 0.9500 . ? C17B C18B 1.391(12) . ? C17B P5B 1.815(9) . ? C18B C19B 1.382(12) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? P4B O11B 1.482(7) . ? P4B O12B 1.540(6) . ? P4B O13B 1.548(6) . ? O12B H122 0.8613 . ? O13B H132 0.8632 . ? P5B O21B 1.498(6) . ? P5B O23B 1.517(7) . ? P5B O22B 1.547(7) . ? O22B H222 0.8601 . ? O23B H232 0.8612 . ? O100 H00A 0.8605 . ? O100 H00B 0.8552 . ? O101 H01A 0.8613 . ? O101 H01B 0.8596 . ? O102 H02A 0.8618 . ? O102 H02B 0.8604 . ? O103 H03A 0.8590 . ? O103 H03B 0.8598 . ? O104 H04A 0.8578 . ? O104 H04B 0.8594 . ? O105 H05A 0.8606 . ? O105 H05B 0.8606 . ? O106 H06A 0.8597 . ? O106 H06B 0.8611 . ? 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 C2 Ru1 C1 89.9(4) . . ? C2 Ru1 N2 170.5(3) . . ? C1 Ru1 N2 99.2(3) . . ? C2 Ru1 N1 94.1(3) . . ? C1 Ru1 N1 172.9(3) . . ? N2 Ru1 N1 77.1(3) . . ? C2 Ru1 Cl2 91.2(3) . . ? C1 Ru1 Cl2 94.0(3) . . ? N2 Ru1 Cl2 85.4(2) . . ? N1 Ru1 Cl2 91.68(19) . . ? C2 Ru1 Cl1 94.6(3) . . ? C1 Ru1 Cl1 86.4(3) . . ? N2 Ru1 Cl1 88.7(2) . . ? N1 Ru1 Cl1 87.43(19) . . ? Cl2 Ru1 Cl1 174.13(8) . . ? O1 C1 Ru1 173.3(8) . . ? O2 C2 Ru1 174.5(8) . . ? C10 N1 C14 119.3(7) . . ? C10 N1 Ru1 124.8(6) . . ? C14 N1 Ru1 115.4(5) . . ? C19 N2 C15 118.9(8) . . ? C19 N2 Ru1 123.6(6) . . ? C15 N2 Ru1 117.0(5) . . ? N1 C10 C11 122.4(8) . . ? N1 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 118.9(8) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 118.9(8) . . ? C11 C12 P4 120.4(6) . . ? C13 C12 P4 120.4(7) . . ? C14 C13 C12 119.3(8) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? N1 C14 C13 121.1(7) . . ? N1 C14 C15 115.2(7) . . ? C13 C14 C15 123.7(8) . . ? N2 C15 C16 122.5(8) . . ? N2 C15 C14 114.5(7) . . ? C16 C15 C14 123.0(8) . . ? C15 C16 C17 118.5(8) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 118.9(8) . . ? C18 C17 P5 119.3(7) . . ? C16 C17 P5 121.7(7) . . ? C17 C18 C19 119.6(8) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? N2 C19 C18 121.5(8) . . ? N2 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? O11 P4 O13 111.4(3) . . ? O11 P4 O12 116.4(4) . . ? O13 P4 O12 109.5(3) . . ? O11 P4 C12 110.4(4) . . ? O13 P4 C12 107.5(4) . . ? O12 P4 C12 100.9(4) . . ? P4 O12 H121 109.3 . . ? P4 O13 H131 108.4 . . ? O21 P5 O22 113.1(4) . . ? O21 P5 O23 114.1(4) . . ? O22 P5 O23 110.4(4) . . ? O21 P5 C17 108.5(4) . . ? O22 P5 C17 110.1(4) . . ? O23 P5 C17 99.8(4) . . ? P5 O22 H221 109.2 . . ? P5 O23 H231 109.0 . . ? C2B Ru1B C1B 87.7(4) . . ? C2B Ru1B N1B 94.1(3) . . ? C1B Ru1B N1B 178.0(3) . . ? C2B Ru1B N2B 171.1(3) . . ? C1B Ru1B N2B 101.1(3) . . ? N1B Ru1B N2B 77.1(3) . . ? C2B Ru1B Cl2B 90.6(3) . . ? C1B Ru1B Cl2B 89.6(3) . . ? N1B Ru1B Cl2B 91.17(19) . . ? N2B Ru1B Cl2B 89.0(2) . . ? C2B Ru1B Cl1B 92.5(3) . . ? C1B Ru1B Cl1B 88.3(3) . . ? N1B Ru1B Cl1B 90.83(19) . . ? N2B Ru1B Cl1B 88.23(19) . . ? Cl2B Ru1B Cl1B 176.17(8) . . ? O1B C1B Ru1B 175.9(8) . . ? O2B C2B Ru1B 175.8(8) . . ? C10B N1B C14B 118.6(7) . . ? C10B N1B Ru1B 125.3(6) . . ? C14B N1B Ru1B 116.1(5) . . ? C19B N2B C15B 119.1(7) . . ? C19B N2B Ru1B 126.1(6) . . ? C15B N2B Ru1B 114.8(5) . . ? N1B C10B C11B 123.3(8) . . ? N1B C10B H10B 118.4 . . ? C11B C10B H10B 118.4 . . ? C10B C11B C12B 118.9(8) . . ? C10B C11B H11B 120.6 . . ? C12B C11B H11B 120.6 . . ? C13B C12B C11B 117.1(8) . . ? C13B C12B P4B 122.1(6) . . ? C11B C12B P4B 120.7(6) . . ? C12B C13B C14B 120.7(8) . . ? C12B C13B H13B 119.7 . . ? C14B C13B H13B 119.7 . . ? N1B C14B C13B 121.5(8) . . ? N1B C14B C15B 115.6(7) . . ? C13B C14B C15B 122.9(8) . . ? N2B C15B C16B 121.1(8) . . ? N2B C15B C14B 116.1(7) . . ? C16B C15B C14B 122.6(8) . . ? C17B C16B C15B 119.4(8) . . ? C17B C16B H16B 120.3 . . ? C15B C16B H16B 120.3 . . ? C16B C17B C18B 118.7(8) . . ? C16B C17B P5B 120.9(7) . . ? C18B C17B P5B 120.2(6) . . ? C19B C18B C17B 120.0(8) . . ? C19B C18B H18B 120.0 . . ? C17B C18B H18B 120.0 . . ? N2B C19B C18B 121.6(8) . . ? N2B C19B H19B 119.2 . . ? C18B C19B H19B 119.2 . . ? O11B P4B O12B 114.1(4) . . ? O11B P4B O13B 114.5(3) . . ? O12B P4B O13B 107.4(3) . . ? O11B P4B C12B 110.2(4) . . ? O12B P4B C12B 103.1(4) . . ? O13B P4B C12B 106.6(4) . . ? P4B O12B H122 108.9 . . ? P4B O13B H132 109.0 . . ? O21B P5B O23B 112.2(4) . . ? O21B P5B O22B 110.7(4) . . ? O23B P5B O22B 111.1(4) . . ? O21B P5B C17B 109.6(4) . . ? O23B P5B C17B 106.7(4) . . ? O22B P5B C17B 106.3(4) . . ? P5B O22B H222 109.2 . . ? P5B O23B H232 109.2 . . ? H00A O100 H00B 106.3 . . ? H01A O101 H01B 105.8 . . ? H02A O102 H02B 105.7 . . ? H03A O103 H03B 106.0 . . ? H04A O104 H04B 106.1 . . ? H05A O105 H05B 105.8 . . ? H06A O106 H06B 105.8 . . ? 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 C2 Ru1 C1 O1 83(7) . . . . ? N2 Ru1 C1 O1 -99(7) . . . . ? N1 Ru1 C1 O1 -41(8) . . . . ? Cl2 Ru1 C1 O1 175(7) . . . . ? Cl1 Ru1 C1 O1 -11(7) . . . . ? C1 Ru1 C2 O2 143(8) . . . . ? N2 Ru1 C2 O2 -20(9) . . . . ? N1 Ru1 C2 O2 -43(8) . . . . ? Cl2 Ru1 C2 O2 49(8) . . . . ? Cl1 Ru1 C2 O2 -130(8) . . . . ? C2 Ru1 N1 C10 -5.6(7) . . . . ? C1 Ru1 N1 C10 119(3) . . . . ? N2 Ru1 N1 C10 178.2(7) . . . . ? Cl2 Ru1 N1 C10 -96.9(6) . . . . ? Cl1 Ru1 N1 C10 88.9(7) . . . . ? C2 Ru1 N1 C14 -177.4(6) . . . . ? C1 Ru1 N1 C14 -53(3) . . . . ? N2 Ru1 N1 C14 6.3(5) . . . . ? Cl2 Ru1 N1 C14 91.2(5) . . . . ? Cl1 Ru1 N1 C14 -83.0(5) . . . . ? C2 Ru1 N2 C19 147.7(18) . . . . ? C1 Ru1 N2 C19 -15.3(7) . . . . ? N1 Ru1 N2 C19 170.9(7) . . . . ? Cl2 Ru1 N2 C19 78.1(7) . . . . ? Cl1 Ru1 N2 C19 -101.5(7) . . . . ? C2 Ru1 N2 C15 -25(2) . . . . ? C1 Ru1 N2 C15 172.4(6) . . . . ? N1 Ru1 N2 C15 -1.5(6) . . . . ? Cl2 Ru1 N2 C15 -94.3(6) . . . . ? Cl1 Ru1 N2 C15 86.2(6) . . . . ? C14 N1 C10 C11 1.3(12) . . . . ? Ru1 N1 C10 C11 -170.3(6) . . . . ? N1 C10 C11 C12 1.0(13) . . . . ? C10 C11 C12 C13 -2.5(12) . . . . ? C10 C11 C12 P4 170.9(6) . . . . ? C11 C12 C13 C14 1.9(12) . . . . ? P4 C12 C13 C14 -171.5(6) . . . . ? C10 N1 C14 C13 -1.9(12) . . . . ? Ru1 N1 C14 C13 170.4(6) . . . . ? C10 N1 C14 C15 177.7(7) . . . . ? Ru1 N1 C14 C15 -9.9(9) . . . . ? C12 C13 C14 N1 0.3(12) . . . . ? C12 C13 C14 C15 -179.3(8) . . . . ? C19 N2 C15 C16 3.4(12) . . . . ? Ru1 N2 C15 C16 176.1(6) . . . . ? C19 N2 C15 C14 -175.9(7) . . . . ? Ru1 N2 C15 C14 -3.2(9) . . . . ? N1 C14 C15 N2 8.6(10) . . . . ? C13 C14 C15 N2 -171.7(8) . . . . ? N1 C14 C15 C16 -170.7(7) . . . . ? C13 C14 C15 C16 9.0(13) . . . . ? N2 C15 C16 C17 -3.5(12) . . . . ? C14 C15 C16 C17 175.7(7) . . . . ? C15 C16 C17 C18 2.1(12) . . . . ? C15 C16 C17 P5 -174.2(6) . . . . ? C16 C17 C18 C19 -0.8(13) . . . . ? P5 C17 C18 C19 175.7(7) . . . . ? C15 N2 C19 C18 -1.9(12) . . . . ? Ru1 N2 C19 C18 -174.2(6) . . . . ? C17 C18 C19 N2 0.7(13) . . . . ? C11 C12 P4 O11 29.0(8) . . . . ? C13 C12 P4 O11 -157.7(7) . . . . ? C11 C12 P4 O13 150.6(7) . . . . ? C13 C12 P4 O13 -36.1(8) . . . . ? C11 C12 P4 O12 -94.7(7) . . . . ? C13 C12 P4 O12 78.6(7) . . . . ? C18 C17 P5 O21 23.7(8) . . . . ? C16 C17 P5 O21 -160.0(7) . . . . ? C18 C17 P5 O22 147.9(7) . . . . ? C16 C17 P5 O22 -35.7(8) . . . . ? C18 C17 P5 O23 -96.0(7) . . . . ? C16 C17 P5 O23 80.4(7) . . . . ? C2B Ru1B C1B O1B 7(11) . . . . ? N1B Ru1B C1B O1B -149(9) . . . . ? N2B Ru1B C1B O1B -173(11) . . . . ? Cl2B Ru1B C1B O1B 98(11) . . . . ? Cl1B Ru1B C1B O1B -85(11) . . . . ? C1B Ru1B C2B O2B -171(13) . . . . ? N1B Ru1B C2B O2B 8(13) . . . . ? N2B Ru1B C2B O2B 12(14) . . . . ? Cl2B Ru1B C2B O2B 99(13) . . . . ? Cl1B Ru1B C2B O2B -83(13) . . . . ? C2B Ru1B N1B C10B 2.7(7) . . . . ? C1B Ru1B N1B C10B 159(9) . . . . ? N2B Ru1B N1B C10B -176.7(7) . . . . ? Cl2B Ru1B N1B C10B -88.0(7) . . . . ? Cl1B Ru1B N1B C10B 95.3(7) . . . . ? C2B Ru1B N1B C14B -175.5(6) . . . . ? C1B Ru1B N1B C14B -19(9) . . . . ? N2B Ru1B N1B C14B 5.1(6) . . . . ? Cl2B Ru1B N1B C14B 93.8(6) . . . . ? Cl1B Ru1B N1B C14B -82.9(6) . . . . ? C2B Ru1B N2B C19B 172(2) . . . . ? C1B Ru1B N2B C19B -5.4(7) . . . . ? N1B Ru1B N2B C19B 175.4(7) . . . . ? Cl2B Ru1B N2B C19B 84.0(7) . . . . ? Cl1B Ru1B N2B C19B -93.3(7) . . . . ? C2B Ru1B N2B C15B -8(3) . . . . ? C1B Ru1B N2B C15B 175.2(6) . . . . ? N1B Ru1B N2B C15B -4.0(6) . . . . ? Cl2B Ru1B N2B C15B -95.4(6) . . . . ? Cl1B Ru1B N2B C15B 87.3(6) . . . . ? C14B N1B C10B C11B 1.0(13) . . . . ? Ru1B N1B C10B C11B -177.1(6) . . . . ? N1B C10B C11B C12B 0.2(13) . . . . ? C10B C11B C12B C13B -1.2(12) . . . . ? C10B C11B C12B P4B 175.5(7) . . . . ? C11B C12B C13B C14B 1.1(12) . . . . ? P4B C12B C13B C14B -175.6(7) . . . . ? C10B N1B C14B C13B -1.1(12) . . . . ? Ru1B N1B C14B C13B 177.2(6) . . . . ? C10B N1B C14B C15B 176.3(7) . . . . ? Ru1B N1B C14B C15B -5.3(9) . . . . ? C12B C13B C14B N1B 0.0(13) . . . . ? C12B C13B C14B C15B -177.2(8) . . . . ? C19B N2B C15B C16B -0.6(12) . . . . ? Ru1B N2B C15B C16B 178.9(6) . . . . ? C19B N2B C15B C14B -176.9(7) . . . . ? Ru1B N2B C15B C14B 2.6(9) . . . . ? N1B C14B C15B N2B 1.8(11) . . . . ? C13B C14B C15B N2B 179.2(8) . . . . ? N1B C14B C15B C16B -174.5(8) . . . . ? C13B C14B C15B C16B 3.0(13) . . . . ? N2B C15B C16B C17B 0.8(13) . . . . ? C14B C15B C16B C17B 176.9(8) . . . . ? C15B C16B C17B C18B -1.2(13) . . . . ? C15B C16B C17B P5B -175.1(6) . . . . ? C16B C17B C18B C19B 1.3(13) . . . . ? P5B C17B C18B C19B 175.3(6) . . . . ? C15B N2B C19B C18B 0.8(12) . . . . ? Ru1B N2B C19B C18B -178.7(6) . . . . ? C17B C18B C19B N2B -1.1(13) . . . . ? C13B C12B P4B O11B 104.1(7) . . . . ? C11B C12B P4B O11B -72.4(8) . . . . ? C13B C12B P4B O12B -133.6(7) . . . . ? C11B C12B P4B O12B 49.8(8) . . . . ? C13B C12B P4B O13B -20.6(8) . . . . ? C11B C12B P4B O13B 162.8(7) . . . . ? C16B C17B P5B O21B -139.5(7) . . . . ? C18B C17B P5B O21B 46.6(8) . . . . ? C16B C17B P5B O23B 98.8(8) . . . . ? C18B C17B P5B O23B -75.0(8) . . . . ? C16B C17B P5B O22B -19.8(8) . . . . ? C18B C17B P5B O22B 166.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O100 H00B O23B 0.86 1.85 2.488(8) 129.5 . O23B H232 O100 0.86 2.18 2.488(8) 100.8 . O22B H222 O11 0.86 1.79 2.523(8) 142.2 3_665 O22 H221 O12B 0.86 1.99 2.527(8) 119.1 3_665 O12B H122 O22 0.86 2.10 2.527(8) 110.1 3_665 O13B H132 O21B 0.86 1.70 2.533(8) 161.2 3_665 O105 H05B O12 0.86 2.13 2.548(9) 109.5 . O12 H121 O105 0.86 2.14 2.548(9) 108.9 . O101 H01A O11B 0.86 1.75 2.556(9) 154.6 3_665 O23 H231 O102 0.86 1.88 2.555(9) 133.7 . O13 H131 O22 0.87 1.70 2.558(8) 169.3 3_565 O104 H04B O21 0.86 2.11 2.639(9) 119.5 . O100 H00A O21 0.86 1.94 2.705(8) 148.1 1_655 O103 H03A O21B 0.86 1.94 2.739(8) 153.5 . O103 H03B O23 0.86 1.98 2.840(8) 173.0 . O102 H02B O105 0.86 2.23 2.907(10) 135.5 3_565 O106 H06A O2 0.86 2.42 2.986(9) 123.5 2_645 O102 H02A O11B 0.86 2.32 3.044(9) 142.4 3_665 O106 H06B O11 0.86 2.23 3.059(9) 160.4 3_665 O12 H121 O2 0.86 2.30 3.087(9) 151.9 4_575 O104 H04A Cl2B 0.86 2.49 3.095(7) 128.3 1_455 O101 H01B O23B 0.86 2.34 3.117(9) 150.8 . O102 H02A O2B 0.86 2.54 3.131(10) 126.1 2_645 O100 H00B O11 0.86 2.59 3.223(9) 132.1 3_665 C18 H18 Cl2B 0.95 2.82 3.313(9) 113.0 1_455 O105 H05B O100 0.86 2.52 3.282(9) 147.8 3_665 O105 H05A Cl2 0.86 2.51 3.364(7) 170.9 1_554 O106 H06A Cl1B 0.86 2.70 3.414(8) 141.4 2_645 C16 H16 O13B 0.95 2.56 3.422(10) 150.3 3_665 C18B H18B Cl2 0.95 2.82 3.444(9) 124.6 . C11B H11B O1 0.95 2.55 3.495(11) 175.4 4_675 C19 H19 Cl1 0.95 2.75 3.542(9) 141.7 4_576 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.020 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.159 #===END======================================================================== data_compound9 _database_code_CSD 162470 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ru(4,4'-diClbpy)(COOMe)(CO)Cl2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.50 H11 Cl3 N2 O4.50 Ru' _chemical_formula_weight 492.67 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' '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' '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8788(4) _cell_length_b 9.9646(5) _cell_length_c 10.6567(5) _cell_angle_alpha 72.402(2) _cell_angle_beta 74.689(3) _cell_angle_gamma 69.284(2) _cell_volume 920.65(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.7795 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7464 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3783 _reflns_number_gt 3523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _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^)+(0.0137P)^2^+0.9178P] 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 3783 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4216(3) 0.6098(3) 0.8386(2) 0.0278(5) Uani 1 1 d . . . C2 C 0.1678(3) 0.6396(3) 1.0009(3) 0.0275(5) Uani 1 1 d . . . C3 C 0.2020(3) 0.8865(3) 0.7909(2) 0.0250(5) Uani 1 1 d . . . C6 C 0.2556(4) 1.0677(3) 0.8507(3) 0.0504(8) Uani 1 1 d . . . H6A H 0.2897 1.1087 0.7564 0.076 Uiso 1 1 calc R . . H6B H 0.3149 1.0777 0.9061 0.076 Uiso 1 1 calc R . . H6C H 0.1522 1.1214 0.8766 0.076 Uiso 1 1 calc R . . C10 C -0.1107(3) 0.7359(3) 0.8549(2) 0.0282(5) Uani 1 1 d . . . H10 H -0.1055 0.7022 0.9475 0.034 Uiso 1 1 calc R . . C11 C -0.2467(3) 0.7851(3) 0.8174(3) 0.0314(6) Uani 1 1 d . . . H11 H -0.3336 0.7854 0.8824 0.038 Uiso 1 1 calc R . . C12 C -0.2528(3) 0.8339(3) 0.6827(3) 0.0324(6) Uani 1 1 d . . . C13 C -0.1246(3) 0.8302(3) 0.5886(3) 0.0307(5) Uani 1 1 d . . . H13 H -0.1277 0.8620 0.4956 0.037 Uiso 1 1 calc R . . C14 C 0.0072(3) 0.7791(2) 0.6336(2) 0.0246(5) Uani 1 1 d . . . C15 C 0.1508(3) 0.7648(2) 0.5425(2) 0.0248(5) Uani 1 1 d . . . C16 C 0.1628(3) 0.8038(3) 0.4039(2) 0.0303(5) Uani 1 1 d . . . H16 H 0.0779 0.8448 0.3632 0.036 Uiso 1 1 calc R . . C17 C 0.3025(3) 0.7810(3) 0.3275(2) 0.0316(6) Uani 1 1 d . . . C18 C 0.4252(3) 0.7202(3) 0.3870(3) 0.0321(6) Uani 1 1 d . . . H18 H 0.5213 0.7023 0.3350 0.039 Uiso 1 1 calc R . . C19 C 0.4037(3) 0.6860(3) 0.5251(2) 0.0281(5) Uani 1 1 d . . . H19 H 0.4876 0.6455 0.5674 0.034 Uiso 1 1 calc R . . N1 N 0.0147(2) 0.7337(2) 0.76580(19) 0.0239(4) Uani 1 1 d . . . N2 N 0.2701(2) 0.7074(2) 0.60223(19) 0.0235(4) Uani 1 1 d . . . O1 O 0.5400(2) 0.5762(2) 0.8517(2) 0.0417(5) Uani 1 1 d . . . O2 O 0.1317(2) 0.6246(2) 1.11355(18) 0.0394(4) Uani 1 1 d . . . O3 O 0.1376(2) 0.98107(19) 0.7112(2) 0.0415(5) Uani 1 1 d . . . O4 O 0.2707(2) 0.91252(19) 0.86987(19) 0.0396(5) Uani 1 1 d . . . Cl2 Cl 0.23436(7) 0.41352(6) 0.81417(6) 0.03214(14) Uani 1 1 d . . . Cl5 Cl 0.32186(9) 0.82836(8) 0.15504(6) 0.04431(18) Uani 1 1 d . . . Cl4 Cl -0.41927(8) 0.89994(8) 0.62863(8) 0.0481(2) Uani 1 1 d . . . Ru1 Ru 0.22625(2) 0.665543(18) 0.813422(17) 0.02146(7) Uani 1 1 d . . . O99 O 0.2120(11) 0.4212(9) 0.4972(9) 0.129(3) Uani 0.50 1 d P . . C99 C 0.0512(13) 0.4345(12) 0.5874(12) 0.107(4) Uani 0.50 1 d P . . H99A H 0.0277 0.5076 0.6402 0.160 Uiso 0.50 1 calc PR . . H99B H 0.0496 0.3386 0.6475 0.160 Uiso 0.50 1 calc PR . . H99C H -0.0218 0.4656 0.5293 0.160 Uiso 0.50 1 calc PR . . H99 H 0.2499 0.4722 0.5305 0.050 Uiso 0.50 1 d P . . 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 C1 0.0322(15) 0.0221(11) 0.0262(12) 0.0044(9) -0.0077(11) -0.0111(10) C2 0.0254(13) 0.0242(11) 0.0336(13) 0.0007(9) -0.0108(11) -0.0103(9) C3 0.0229(12) 0.0360(13) 0.0172(10) -0.0007(9) -0.0039(9) -0.0143(10) C6 0.082(2) 0.0283(14) 0.0510(18) -0.0062(13) -0.0242(17) -0.0220(15) C10 0.0298(13) 0.0253(11) 0.0294(12) -0.0011(9) -0.0062(11) -0.0117(10) C11 0.0252(13) 0.0271(12) 0.0400(14) -0.0027(10) -0.0041(11) -0.0109(10) C12 0.0271(13) 0.0257(12) 0.0447(15) 0.0038(11) -0.0166(12) -0.0108(10) C13 0.0328(14) 0.0272(12) 0.0309(13) 0.0047(10) -0.0117(11) -0.0127(10) C14 0.0278(13) 0.0193(10) 0.0267(11) 0.0010(9) -0.0081(10) -0.0100(9) C15 0.0302(13) 0.0193(10) 0.0258(11) 0.0003(9) -0.0078(10) -0.0110(9) C16 0.0381(15) 0.0261(12) 0.0284(12) -0.0007(9) -0.0111(11) -0.0125(10) C17 0.0463(16) 0.0245(12) 0.0243(12) -0.0027(9) -0.0033(11) -0.0156(11) C18 0.0358(14) 0.0275(12) 0.0304(13) -0.0061(10) 0.0023(11) -0.0128(10) C19 0.0285(13) 0.0250(11) 0.0289(12) -0.0034(9) -0.0034(10) -0.0093(9) N1 0.0272(11) 0.0194(9) 0.0257(10) -0.0018(7) -0.0052(8) -0.0101(8) N2 0.0266(11) 0.0195(9) 0.0241(9) -0.0006(7) -0.0054(8) -0.0095(8) O1 0.0309(11) 0.0408(11) 0.0478(12) 0.0064(9) -0.0146(9) -0.0125(8) O2 0.0391(11) 0.0517(12) 0.0250(10) -0.0005(8) -0.0062(8) -0.0173(9) O3 0.0558(13) 0.0243(9) 0.0465(11) 0.0018(8) -0.0239(10) -0.0121(8) O4 0.0599(13) 0.0260(9) 0.0384(10) -0.0003(8) -0.0225(10) -0.0153(9) Cl2 0.0363(3) 0.0218(3) 0.0343(3) -0.0032(2) 0.0019(3) -0.0125(2) Cl5 0.0629(5) 0.0458(4) 0.0227(3) -0.0039(3) -0.0035(3) -0.0207(3) Cl4 0.0308(4) 0.0479(4) 0.0611(5) 0.0122(3) -0.0230(4) -0.0164(3) Ru1 0.02252(11) 0.01863(10) 0.02207(10) 0.00106(7) -0.00618(8) -0.00800(7) O99 0.170(8) 0.101(5) 0.131(7) -0.072(5) 0.037(6) -0.065(5) C99 0.108(9) 0.099(8) 0.123(9) -0.041(7) -0.058(8) -0.003(6) _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 C1 O1 1.131(3) . ? C1 Ru1 1.879(3) . ? C2 O2 1.138(3) . ? C2 Ru1 1.891(3) . ? C3 O3 1.180(3) . ? C3 O4 1.340(3) . ? C3 Ru1 2.073(2) . ? C6 O4 1.455(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C10 N1 1.345(3) . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 C13 1.389(4) . ? C12 Cl4 1.725(3) . ? C13 C14 1.377(4) . ? C13 H13 0.9500 . ? C14 N1 1.357(3) . ? C14 C15 1.480(3) . ? C15 N2 1.349(3) . ? C15 C16 1.392(3) . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.375(4) . ? C17 Cl5 1.729(2) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 N2 1.340(3) . ? C19 H19 0.9500 . ? N1 Ru1 2.106(2) . ? N2 Ru1 2.1147(19) . ? Cl2 Ru1 2.4818(6) . ? O99 C99 1.608(14) . ? O99 H99 0.9156 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? 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 O1 C1 Ru1 178.9(2) . . ? O2 C2 Ru1 179.5(3) . . ? O3 C3 O4 122.7(2) . . ? O3 C3 Ru1 122.56(19) . . ? O4 C3 Ru1 114.66(16) . . ? O4 C6 H6A 109.5 . . ? O4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C10 C11 122.7(2) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 118.0(2) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 Cl4 120.6(2) . . ? C13 C12 Cl4 119.1(2) . . ? C14 C13 C12 118.3(2) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N1 C14 C13 122.1(2) . . ? N1 C14 C15 115.0(2) . . ? C13 C14 C15 122.9(2) . . ? N2 C15 C16 122.0(2) . . ? N2 C15 C14 115.7(2) . . ? C16 C15 C14 122.3(2) . . ? C17 C16 C15 117.9(2) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? C18 C17 C16 120.8(2) . . ? C18 C17 Cl5 119.9(2) . . ? C16 C17 Cl5 119.2(2) . . ? C17 C18 C19 117.7(2) . . ? C17 C18 H18 121.2 . . ? C19 C18 H18 121.2 . . ? N2 C19 C18 123.1(2) . . ? N2 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C10 N1 C14 118.6(2) . . ? C10 N1 Ru1 125.42(17) . . ? C14 N1 Ru1 116.02(16) . . ? C19 N2 C15 118.6(2) . . ? C19 N2 Ru1 125.78(17) . . ? C15 N2 Ru1 115.59(15) . . ? C3 O4 C6 114.0(2) . . ? C1 Ru1 C2 88.01(10) . . ? C1 Ru1 C3 91.76(10) . . ? C2 Ru1 C3 91.16(9) . . ? C1 Ru1 N1 174.63(9) . . ? C2 Ru1 N1 97.29(9) . . ? C3 Ru1 N1 87.24(8) . . ? C1 Ru1 N2 97.30(9) . . ? C2 Ru1 N2 174.37(9) . . ? C3 Ru1 N2 86.81(8) . . ? N1 Ru1 N2 77.38(8) . . ? C1 Ru1 Cl2 94.60(7) . . ? C2 Ru1 Cl2 94.29(7) . . ? C3 Ru1 Cl2 171.75(7) . . ? N1 Ru1 Cl2 85.94(5) . . ? N2 Ru1 Cl2 87.18(5) . . ? C99 O99 H99 103.6 . . ? O99 C99 H99A 109.5 . . ? O99 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O99 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? 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 N1 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 1.3(4) . . . . ? C10 C11 C12 Cl4 -178.87(19) . . . . ? C11 C12 C13 C14 -1.1(4) . . . . ? Cl4 C12 C13 C14 179.10(18) . . . . ? C12 C13 C14 N1 -0.4(4) . . . . ? C12 C13 C14 C15 177.6(2) . . . . ? N1 C14 C15 N2 0.7(3) . . . . ? C13 C14 C15 N2 -177.4(2) . . . . ? N1 C14 C15 C16 178.8(2) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? N2 C15 C16 C17 0.4(3) . . . . ? C14 C15 C16 C17 -177.6(2) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C15 C16 C17 Cl5 -179.90(17) . . . . ? C16 C17 C18 C19 -1.4(4) . . . . ? Cl5 C17 C18 C19 179.20(18) . . . . ? C17 C18 C19 N2 1.1(4) . . . . ? C11 C10 N1 C14 -1.3(3) . . . . ? C11 C10 N1 Ru1 178.47(17) . . . . ? C13 C14 N1 C10 1.6(3) . . . . ? C15 C14 N1 C10 -176.56(19) . . . . ? C13 C14 N1 Ru1 -178.25(18) . . . . ? C15 C14 N1 Ru1 3.6(2) . . . . ? C18 C19 N2 C15 0.1(3) . . . . ? C18 C19 N2 Ru1 -177.79(17) . . . . ? C16 C15 N2 C19 -0.8(3) . . . . ? C14 C15 N2 C19 177.29(19) . . . . ? C16 C15 N2 Ru1 177.24(17) . . . . ? C14 C15 N2 Ru1 -4.6(2) . . . . ? O3 C3 O4 C6 1.4(4) . . . . ? Ru1 C3 O4 C6 178.6(2) . . . . ? O1 C1 Ru1 C2 173(100) . . . . ? O1 C1 Ru1 C3 -96(11) . . . . ? O1 C1 Ru1 N1 -17(11) . . . . ? O1 C1 Ru1 N2 -9(11) . . . . ? O1 C1 Ru1 Cl2 79(11) . . . . ? O2 C2 Ru1 C1 156(29) . . . . ? O2 C2 Ru1 C3 64(29) . . . . ? O2 C2 Ru1 N1 -23(29) . . . . ? O2 C2 Ru1 N2 -5(29) . . . . ? O2 C2 Ru1 Cl2 -109(29) . . . . ? O3 C3 Ru1 C1 140.1(2) . . . . ? O4 C3 Ru1 C1 -37.06(19) . . . . ? O3 C3 Ru1 C2 -131.9(2) . . . . ? O4 C3 Ru1 C2 50.99(19) . . . . ? O3 C3 Ru1 N1 -34.6(2) . . . . ? O4 C3 Ru1 N1 148.23(18) . . . . ? O3 C3 Ru1 N2 42.9(2) . . . . ? O4 C3 Ru1 N2 -134.27(18) . . . . ? O3 C3 Ru1 Cl2 -0.4(6) . . . . ? O4 C3 Ru1 Cl2 -177.6(3) . . . . ? C10 N1 Ru1 C1 -176.4(9) . . . . ? C14 N1 Ru1 C1 3.4(10) . . . . ? C10 N1 Ru1 C2 -6.2(2) . . . . ? C14 N1 Ru1 C2 173.57(16) . . . . ? C10 N1 Ru1 C3 -97.05(19) . . . . ? C14 N1 Ru1 C3 82.75(16) . . . . ? C10 N1 Ru1 N2 175.60(19) . . . . ? C14 N1 Ru1 N2 -4.60(15) . . . . ? C10 N1 Ru1 Cl2 87.59(18) . . . . ? C14 N1 Ru1 Cl2 -92.61(15) . . . . ? C19 N2 Ru1 C1 3.6(2) . . . . ? C15 N2 Ru1 C1 -174.29(16) . . . . ? C19 N2 Ru1 C2 164.0(8) . . . . ? C15 N2 Ru1 C2 -13.9(9) . . . . ? C19 N2 Ru1 C3 95.00(19) . . . . ? C15 N2 Ru1 C3 -82.92(16) . . . . ? C19 N2 Ru1 N1 -177.12(19) . . . . ? C15 N2 Ru1 N1 4.96(15) . . . . ? C19 N2 Ru1 Cl2 -90.65(18) . . . . ? C15 N2 Ru1 Cl2 91.43(15) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.583 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.071 #===END========================================================================