data_dra22 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Cl2 N2 Ru' _chemical_formula_weight 594.56 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' '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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.4420(10) _cell_length_b 16.5926(10) _cell_length_c 22.4396(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6121.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15425 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.65 _exptl_crystal_description Blade _exptl_crystal_colour Green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 5 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86972 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7436 _reflns_number_gt 3704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT v6.45A' _computing_data_reduction 'Bruker SAINT v6.45A' _computing_structure_solution 'Bruker XS v6.12' _computing_structure_refinement 'Bruker XL v6.12' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF v6.12' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7436 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.507 _refine_ls_restrained_S_all 1.507 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.764873(14) 0.797973(15) 0.606595(12) 0.03629(8) Uani 1 1 d . . . Cl1 Cl 0.66607(6) 0.69488(6) 0.62439(5) 0.0767(3) Uani 1 1 d . . . Cl2 Cl 0.76708(5) 0.74461(5) 0.50864(4) 0.0504(2) Uani 1 1 d . . . N1 N 0.74557(16) 0.95274(15) 0.54553(11) 0.0414(7) Uani 1 1 d . . . N2 N 0.87472(16) 0.93666(15) 0.55901(12) 0.0412(8) Uani 1 1 d . . . C1 C 0.8018(2) 0.90425(18) 0.56962(14) 0.0342(8) Uani 1 1 d . . . C2 C 0.77948(19) 1.0246(2) 0.51616(18) 0.0603(12) Uani 1 1 d . . . H2A H 0.7609 1.0738 0.5352 0.072 Uiso 1 1 calc R . . H2B H 0.7653 1.0262 0.4742 0.072 Uiso 1 1 calc R . . C3 C 0.86959(19) 1.0127(2) 0.52472(17) 0.0536(11) Uani 1 1 d . . . H3A H 0.8972 1.0078 0.4867 0.064 Uiso 1 1 calc R . . H3B H 0.8932 1.0572 0.5468 0.064 Uiso 1 1 calc R . . C4 C 0.6591(2) 0.94034(19) 0.55152(17) 0.0388(9) Uani 1 1 d . . . C5 C 0.6202(2) 0.96867(18) 0.60216(17) 0.0416(9) Uani 1 1 d . . . C6 C 0.5377(2) 0.95345(19) 0.60820(17) 0.0482(9) Uani 1 1 d . . . H6 H 0.5110 0.9710 0.6423 0.058 Uiso 1 1 calc R . . C7 C 0.4942(2) 0.9130(2) 0.56494(19) 0.0457(10) Uani 1 1 d . . . C8 C 0.5335(2) 0.8915(2) 0.51330(17) 0.0483(10) Uani 1 1 d . . . H8 H 0.5041 0.8666 0.4831 0.058 Uiso 1 1 calc R . . C9 C 0.6156(2) 0.9059(2) 0.50490(17) 0.0426(9) Uani 1 1 d . . . C10 C 0.6633(2) 1.0197(2) 0.64883(17) 0.0627(12) Uani 1 1 d . . . H10A H 0.7190 1.0027 0.6521 0.094 Uiso 1 1 calc R . . H10B H 0.6368 1.0132 0.6866 0.094 Uiso 1 1 calc R . . H10C H 0.6615 1.0754 0.6372 0.094 Uiso 1 1 calc R . . C11 C 0.40476(19) 0.8946(2) 0.57314(17) 0.0699(12) Uani 1 1 d . . . H11A H 0.3768 0.9024 0.5360 0.105 Uiso 1 1 calc R . . H11B H 0.3824 0.9300 0.6027 0.105 Uiso 1 1 calc R . . H11C H 0.3984 0.8397 0.5859 0.105 Uiso 1 1 calc R . . C12 C 0.6535(2) 0.8872(2) 0.44482(15) 0.0600(11) Uani 1 1 d . . . H12A H 0.6565 0.9357 0.4216 0.090 Uiso 1 1 calc R . . H12B H 0.6207 0.8482 0.4243 0.090 Uiso 1 1 calc R . . H12C H 0.7072 0.8660 0.4506 0.090 Uiso 1 1 calc R . . C13 C 0.95340(19) 0.9096(2) 0.57932(17) 0.0378(9) Uani 1 1 d . . . C14 C 0.9870(2) 0.9412(2) 0.62997(16) 0.0427(10) Uani 1 1 d . . . C15 C 1.0628(2) 0.9138(2) 0.64825(16) 0.0518(10) Uani 1 1 d . . . H15 H 1.0851 0.9331 0.6836 0.062 Uiso 1 1 calc R . . C16 C 1.1058(2) 0.8581(2) 0.61451(17) 0.0445(9) Uani 1 1 d . . . C17 C 1.0719(2) 0.83134(19) 0.56215(16) 0.0417(9) Uani 1 1 d . . . H17 H 1.1010 0.7951 0.5388 0.050 Uiso 1 1 calc R . . C18 C 0.9963(2) 0.8562(2) 0.54291(15) 0.0367(9) Uani 1 1 d . . . C19 C 0.9468(2) 1.0078(2) 0.66631(17) 0.0691(12) Uani 1 1 d . . . H19A H 0.9797 1.0555 0.6648 0.104 Uiso 1 1 calc R . . H19B H 0.9412 0.9906 0.7069 0.104 Uiso 1 1 calc R . . H19C H 0.8940 1.0193 0.6501 0.104 Uiso 1 1 calc R . . C20 C 1.1880(2) 0.8295(2) 0.63553(16) 0.0729(13) Uani 1 1 d . . . H20A H 1.1926 0.7725 0.6290 0.109 Uiso 1 1 calc R . . H20B H 1.1938 0.8409 0.6773 0.109 Uiso 1 1 calc R . . H20C H 1.2298 0.8570 0.6137 0.109 Uiso 1 1 calc R . . C21 C 0.96497(19) 0.8285(2) 0.48320(15) 0.0530(10) Uani 1 1 d . . . H21A H 0.9178 0.7953 0.4889 0.080 Uiso 1 1 calc R . . H21B H 1.0064 0.7979 0.4632 0.080 Uiso 1 1 calc R . . H21C H 0.9508 0.8745 0.4595 0.080 Uiso 1 1 calc R . . C22 C 0.86412(18) 0.75165(18) 0.61967(15) 0.0409(9) Uani 1 1 d . . . H22 H 0.8875 0.7224 0.5887 0.049 Uiso 1 1 calc R . . C23 C 0.9084(2) 0.7575(2) 0.67472(17) 0.0462(10) Uani 1 1 d . . . C24 C 0.9778(2) 0.7154(2) 0.69087(18) 0.0593(11) Uani 1 1 d . . . H24 H 1.0002 0.6781 0.6646 0.071 Uiso 1 1 calc R . . C25 C 1.0135(2) 0.7281(3) 0.7448(2) 0.0734(13) Uani 1 1 d . . . H25 H 1.0591 0.6985 0.7559 0.088 Uiso 1 1 calc R . . C26 C 0.9814(3) 0.7850(3) 0.7830(2) 0.0894(15) Uani 1 1 d . . . H26 H 1.0055 0.7935 0.8200 0.107 Uiso 1 1 calc R . . C27 C 0.9143(3) 0.8293(3) 0.76699(19) 0.0817(14) Uani 1 1 d . . . H27 H 0.8945 0.8691 0.7923 0.098 Uiso 1 1 calc R . . C28 C 0.8765(2) 0.8147(2) 0.71343(18) 0.0573(11) Uani 1 1 d . . . C29 C 0.8016(3) 0.8581(2) 0.69121(16) 0.0602(11) Uani 1 1 d . . . H29 H 0.8047 0.9170 0.6902 0.072 Uiso 1 1 calc R . . C30 C 0.7276(2) 0.8267(2) 0.69759(15) 0.0707(12) Uani 1 1 d . . . H30A H 0.7211 0.7770 0.7161 0.085 Uiso 1 1 calc R . . H30B H 0.6824 0.8546 0.6835 0.085 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 0.03177(14) 0.02933(13) 0.04776(16) 0.00072(16) 0.00365(15) -0.00277(14) Cl1 0.0721(7) 0.0569(7) 0.1011(9) -0.0068(7) 0.0332(6) -0.0325(6) Cl2 0.0519(5) 0.0460(5) 0.0533(6) -0.0106(4) -0.0023(5) -0.0078(5) N1 0.0270(18) 0.0309(14) 0.0662(19) 0.0100(15) -0.0035(16) -0.0048(13) N2 0.0311(18) 0.0276(17) 0.065(2) 0.0090(15) -0.0018(16) -0.0010(14) C1 0.029(2) 0.030(2) 0.044(2) 0.0027(17) -0.0020(17) 0.0026(17) C2 0.040(3) 0.040(2) 0.101(3) 0.020(2) -0.006(2) -0.0084(18) C3 0.034(2) 0.039(2) 0.088(3) 0.013(2) 0.001(2) -0.0086(18) C4 0.030(2) 0.028(2) 0.059(3) 0.0098(19) -0.006(2) -0.0010(17) C5 0.031(2) 0.033(2) 0.061(3) -0.002(2) -0.008(2) 0.0013(15) C6 0.044(2) 0.043(2) 0.058(3) -0.001(2) 0.009(2) 0.0098(17) C7 0.031(2) 0.037(2) 0.069(3) 0.008(2) -0.003(2) 0.0026(18) C8 0.042(3) 0.040(2) 0.063(3) 0.003(2) -0.016(2) -0.0030(19) C9 0.040(2) 0.034(2) 0.054(3) 0.0036(19) -0.012(2) 0.0005(18) C10 0.045(3) 0.054(3) 0.089(3) -0.020(2) -0.012(2) 0.012(2) C11 0.034(2) 0.077(3) 0.098(3) 0.010(3) -0.004(2) -0.007(2) C12 0.064(3) 0.057(3) 0.059(3) 0.006(2) -0.003(2) -0.002(2) C13 0.024(2) 0.035(2) 0.055(3) 0.006(2) 0.0046(18) -0.0054(17) C14 0.036(2) 0.037(2) 0.056(3) -0.009(2) 0.004(2) -0.0029(18) C15 0.038(2) 0.063(3) 0.054(3) -0.008(2) -0.010(2) 0.001(2) C16 0.035(2) 0.046(2) 0.052(3) 0.009(2) -0.001(2) -0.0018(17) C17 0.038(2) 0.036(2) 0.051(3) 0.0029(19) 0.0067(19) 0.0047(17) C18 0.033(2) 0.034(2) 0.044(2) 0.0071(18) 0.0012(18) -0.0061(17) C19 0.051(3) 0.059(3) 0.097(4) -0.025(3) -0.003(2) 0.004(2) C20 0.045(3) 0.098(3) 0.075(3) -0.003(2) -0.017(2) 0.014(2) C21 0.042(2) 0.059(3) 0.058(3) 0.005(2) 0.001(2) -0.0024(19) C22 0.046(2) 0.031(2) 0.046(2) 0.0079(19) 0.0066(18) -0.0043(17) C23 0.044(2) 0.041(2) 0.054(3) 0.002(2) -0.001(2) 0.0007(19) C24 0.050(2) 0.062(3) 0.066(3) 0.008(2) -0.002(2) 0.006(2) C25 0.053(3) 0.080(3) 0.087(4) 0.017(3) -0.023(3) 0.011(2) C26 0.086(4) 0.115(5) 0.067(3) 0.001(3) -0.034(3) 0.008(3) C27 0.091(4) 0.088(4) 0.066(3) -0.010(3) -0.017(3) 0.018(3) C28 0.055(3) 0.066(3) 0.051(3) 0.001(2) -0.013(2) 0.003(2) C29 0.079(3) 0.057(3) 0.046(3) -0.016(2) -0.001(2) 0.000(3) C30 0.073(3) 0.090(3) 0.049(3) -0.008(2) 0.006(2) -0.011(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 C22 1.827(3) . yes Ru1 C1 2.041(3) . yes Ru1 C30 2.185(3) . yes Ru1 C29 2.228(4) . yes Ru1 Cl2 2.3701(9) . yes Ru1 Cl1 2.3926(9) . yes N1 C1 1.340(3) . ? N1 C4 1.443(4) . ? N1 C2 1.472(4) . ? N2 C1 1.335(3) . ? N2 C13 1.443(4) . ? N2 C3 1.481(4) . ? C2 C3 1.507(4) . ? C4 C5 1.386(4) . ? C4 C9 1.390(4) . ? C5 C6 1.385(4) . ? C5 C10 1.523(4) . ? C6 C7 1.380(5) . ? C7 C8 1.374(4) . ? C7 C11 1.513(4) . ? C8 C9 1.383(4) . ? C9 C12 1.517(4) . ? C13 C14 1.368(4) . ? C13 C18 1.397(4) . ? C14 C15 1.389(4) . ? C14 C19 1.525(4) . ? C15 C16 1.388(4) . ? C16 C17 1.374(4) . ? C16 C20 1.507(4) . ? C17 C18 1.379(4) . ? C18 C21 1.507(4) . ? C22 C23 1.437(4) . ? C23 C24 1.387(4) . ? C23 C28 1.389(4) . ? C24 C25 1.362(5) . ? C25 C26 1.380(5) . ? C26 C27 1.374(5) . ? C27 C28 1.374(5) . ? C28 C29 1.511(5) . ? C29 C30 1.331(4) . ? 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 C22 Ru1 C1 99.36(12) . . yes C22 Ru1 C30 101.10(15) . . yes C1 Ru1 C30 105.94(14) . . yes C22 Ru1 C29 79.02(15) . . yes C1 Ru1 C29 83.05(14) . . yes C30 Ru1 C29 35.10(11) . . yes C22 Ru1 Cl2 88.74(11) . . yes C1 Ru1 Cl2 86.63(9) . . yes C30 Ru1 Cl2 162.31(11) . . yes C29 Ru1 Cl2 162.45(11) . . yes C22 Ru1 Cl1 106.19(9) . . yes C1 Ru1 Cl1 152.57(9) . . yes C30 Ru1 Cl1 79.02(11) . . yes C29 Ru1 Cl1 111.21(11) . . yes Cl2 Ru1 Cl1 84.15(3) . . yes C1 N1 C4 123.9(3) . . ? C1 N1 C2 113.9(3) . . ? C4 N1 C2 122.0(3) . . ? C1 N2 C13 128.5(3) . . ? C1 N2 C3 112.6(3) . . ? C13 N2 C3 118.7(3) . . ? N2 C1 N1 107.8(3) . . ? N2 C1 Ru1 133.4(2) . . ? N1 C1 Ru1 118.5(2) . . ? N1 C2 C3 102.1(3) . . ? N2 C3 C2 103.5(3) . . ? C5 C4 C9 121.3(3) . . ? C5 C4 N1 118.9(3) . . ? C9 C4 N1 119.7(3) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C10 119.4(3) . . ? C4 C5 C10 122.5(3) . . ? C7 C6 C5 121.8(4) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 C11 120.5(4) . . ? C6 C7 C11 121.1(4) . . ? C7 C8 C9 122.0(3) . . ? C8 C9 C4 118.0(3) . . ? C8 C9 C12 119.1(3) . . ? C4 C9 C12 122.8(3) . . ? C14 C13 C18 121.7(3) . . ? C14 C13 N2 120.3(3) . . ? C18 C13 N2 117.7(3) . . ? C13 C14 C15 118.8(3) . . ? C13 C14 C19 123.2(3) . . ? C15 C14 C19 118.0(3) . . ? C16 C15 C14 120.9(3) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 C20 122.0(3) . . ? C15 C16 C20 119.7(3) . . ? C16 C17 C18 122.5(3) . . ? C17 C18 C13 117.5(3) . . ? C17 C18 C21 119.7(3) . . ? C13 C18 C21 122.8(3) . . ? C23 C22 Ru1 124.2(3) . . ? C24 C23 C28 119.5(4) . . ? C24 C23 C22 127.4(4) . . ? C28 C23 C22 113.1(3) . . ? C25 C24 C23 120.6(4) . . ? C24 C25 C26 119.6(4) . . ? C27 C26 C25 120.7(4) . . ? C26 C27 C28 119.8(4) . . ? C27 C28 C23 119.8(4) . . ? C27 C28 C29 125.0(4) . . ? C23 C28 C29 115.2(3) . . ? C30 C29 C28 121.6(4) . . ? C30 C29 Ru1 70.7(2) . . ? C28 C29 Ru1 106.8(2) . . ? C29 C30 Ru1 74.2(2) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.676 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.085