# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lahiri, Goutam' _publ_contact_author_email lahiri@chem.iitb.ac.in _publ_section_title ; Valence and spin situations in isomeric [(bpy)Ru(Q/)2]n (Q/ = 3,5-di-tert-butyl-N-aryl-1,2-benzoquinonemonoimine). An experimental and DFT analysis ; _publ_author_name G.Lahiri # Attachment '- 2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 821453' #TrackingRef '- 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Cl4 N4 O2 Ru' _chemical_formula_weight 985.84 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 8.8394(4) _cell_length_b 12.3326(5) _cell_length_c 23.5067(10) _cell_angle_alpha 103.280(4) _cell_angle_beta 96.488(4) _cell_angle_gamma 100.985(4) _cell_volume 2415.13(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2510 _cell_measurement_theta_min 3.2087 _cell_measurement_theta_max 32.6936 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_T_min 0.8526 _exptl_absorpt_correction_T_max 0.8815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17867 _diffrn_reflns_av_R_equivalents 0.1270 _diffrn_reflns_av_sigmaI/netI 0.2855 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8498 _reflns_number_gt 4097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8498 _refine_ls_number_parameters 562 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1622 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 0.776 _refine_ls_restrained_S_all 0.773 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.19825(6) 0.09581(5) 0.75142(3) 0.01238(14) Uani 1 1 d . . . Cl1 Cl 0.0496(2) 0.18833(17) 0.48517(9) 0.0608(7) Uani 1 1 d . . . Cl2 Cl 0.4772(2) 0.48170(14) 0.65964(8) 0.0463(6) Uani 1 1 d . . . Cl3 Cl 0.3660(2) 0.38224(17) 1.03212(9) 0.0739(8) Uani 1 1 d . . . Cl4 Cl -0.14638(19) 0.39692(15) 0.89137(9) 0.0476(6) Uani 1 1 d . . . O1 O 0.0965(4) -0.0699(3) 0.71745(18) 0.0192(11) Uani 1 1 d . . . O2 O 0.3857(4) 0.0374(3) 0.77853(17) 0.0184(11) Uani 1 1 d . . . N1 N 0.2563(5) 0.0741(4) 0.6713(2) 0.0167(13) Uani 1 1 d U . . N2 N 0.0132(5) 0.1586(4) 0.7245(2) 0.0218(14) Uani 1 1 d . . . N3 N 0.2848(5) 0.2671(4) 0.7822(2) 0.0168(13) Uani 1 1 d . . . N4 N 0.1612(5) 0.0903(4) 0.8330(2) 0.0163(13) Uani 1 1 d U . . C1 C 0.1613(6) -0.1160(5) 0.6727(3) 0.0161(16) Uani 1 1 d DU . . C2 C 0.1412(6) -0.2362(5) 0.6496(3) 0.0140(15) Uani 1 1 d D . . C3 C 0.2218(6) -0.2694(5) 0.6033(2) 0.0157(16) Uani 1 1 d D . . H3 H 0.2152 -0.3489 0.5888 0.019 Uiso 1 1 calc R . . C4 C 0.3121(6) -0.1954(5) 0.5762(3) 0.0155(16) Uani 1 1 d D . . C5 C 0.3233(6) -0.0800(5) 0.5970(3) 0.0157(16) Uani 1 1 d D . . H5 H 0.3789 -0.0278 0.5784 0.019 Uiso 1 1 calc R . . C6 C 0.2521(6) -0.0394(5) 0.6458(3) 0.0098(14) Uani 1 1 d DU . . C7 C 0.3976(7) -0.2451(5) 0.5275(3) 0.0240(17) Uani 1 1 d . . . C8 C 0.4596(8) -0.1602(5) 0.4952(3) 0.052(2) Uani 1 1 d . . . H8A H 0.3753 -0.1265 0.4813 0.078 Uiso 1 1 calc R . . H8B H 0.5016 -0.1984 0.4611 0.078 Uiso 1 1 calc R . . H8C H 0.5429 -0.0999 0.5218 0.078 Uiso 1 1 calc R . . C9 C 0.2823(9) -0.3416(7) 0.4795(3) 0.100(4) Uani 1 1 d . . . H9A H 0.2557 -0.4092 0.4948 0.150 Uiso 1 1 calc R . . H9B H 0.3310 -0.3611 0.4442 0.150 Uiso 1 1 calc R . . H9C H 0.1871 -0.3158 0.4691 0.150 Uiso 1 1 calc R . . C10 C 0.5275(8) -0.2899(7) 0.5528(4) 0.093(4) Uani 1 1 d . . . H10A H 0.6124 -0.2259 0.5753 0.139 Uiso 1 1 calc R . . H10B H 0.5662 -0.3371 0.5206 0.139 Uiso 1 1 calc R . . H10C H 0.4894 -0.3364 0.5791 0.139 Uiso 1 1 calc R . . C11 C 0.0333(7) -0.3202(5) 0.6732(3) 0.0197(17) Uani 1 1 d . . . C12 C 0.0258(7) -0.4436(5) 0.6415(3) 0.036(2) Uani 1 1 d . . . H12A H -0.0027 -0.4547 0.5987 0.054 Uiso 1 1 calc R . . H12B H -0.0527 -0.4943 0.6554 0.054 Uiso 1 1 calc R . . H12C H 0.1282 -0.4614 0.6499 0.054 Uiso 1 1 calc R . . C13 C 0.0862(6) -0.3047(5) 0.7398(3) 0.0302(18) Uani 1 1 d . . . H13A H 0.1925 -0.3169 0.7463 0.045 Uiso 1 1 calc R . . H13B H 0.0152 -0.3603 0.7539 0.045 Uiso 1 1 calc R . . H13C H 0.0847 -0.2271 0.7616 0.045 Uiso 1 1 calc R . . C14 C -0.1327(6) -0.3001(5) 0.6635(3) 0.036(2) Uani 1 1 d . . . H14A H -0.1332 -0.2223 0.6854 0.054 Uiso 1 1 calc R . . H14B H -0.2039 -0.3554 0.6776 0.054 Uiso 1 1 calc R . . H14C H -0.1669 -0.3097 0.6211 0.054 Uiso 1 1 calc R . . C15 C 0.2653(6) 0.1535(5) 0.6367(3) 0.0136(14) Uani 1 1 d DU . . C16 C 0.1697(6) 0.1332(5) 0.5807(3) 0.0204(16) Uani 1 1 d DU . . H16 H 0.1050 0.0594 0.5630 0.024 Uiso 1 1 calc R . . C17 C 0.1691(7) 0.2176(6) 0.5522(3) 0.0275(17) Uani 1 1 d DU . . C18 C 0.2606(6) 0.3256(5) 0.5759(3) 0.0227(16) Uani 1 1 d DU . . H18 H 0.2579 0.3841 0.5559 0.027 Uiso 1 1 calc R . . C19 C 0.3557(7) 0.3468(5) 0.6292(3) 0.0243(17) Uani 1 1 d DU . . C20 C 0.3625(6) 0.2635(5) 0.6592(3) 0.0205(16) Uani 1 1 d DU . . H20 H 0.4331 0.2804 0.6953 0.025 Uiso 1 1 calc R . . C21 C -0.1230(7) 0.0954(6) 0.6943(3) 0.0285(18) Uani 1 1 d . . . H21 H -0.1375 0.0146 0.6857 0.034 Uiso 1 1 calc R . . C22 C -0.2455(7) 0.1397(6) 0.6744(3) 0.040(2) Uani 1 1 d . . . H22 H -0.3414 0.0916 0.6527 0.048 Uiso 1 1 calc R . . C23 C -0.2209(8) 0.2570(6) 0.6878(4) 0.051(2) Uani 1 1 d . . . H23 H -0.3019 0.2910 0.6750 0.061 Uiso 1 1 calc R . . C24 C -0.0810(7) 0.3265(6) 0.7197(3) 0.035(2) Uani 1 1 d . . . H24 H -0.0643 0.4075 0.7292 0.042 Uiso 1 1 calc R . . C25 C 0.0344(7) 0.2722(6) 0.7370(3) 0.0218(17) Uani 1 1 d . . . C26 C 0.1859(7) 0.3352(6) 0.7722(3) 0.0203(17) Uani 1 1 d . . . C27 C 0.2358(8) 0.4530(5) 0.7918(3) 0.035(2) Uani 1 1 d . . . H27 H 0.1674 0.5005 0.7840 0.042 Uiso 1 1 calc R . . C28 C 0.3829(8) 0.5008(6) 0.8224(3) 0.040(2) Uani 1 1 d . . . H28 H 0.4172 0.5816 0.8359 0.048 Uiso 1 1 calc R . . C29 C 0.4800(8) 0.4330(6) 0.8336(3) 0.038(2) Uani 1 1 d . . . H29 H 0.5828 0.4654 0.8548 0.045 Uiso 1 1 calc R . . C30 C 0.4273(7) 0.3163(5) 0.8136(3) 0.0244(17) Uani 1 1 d . . . H30 H 0.4946 0.2688 0.8225 0.029 Uiso 1 1 calc R . . C31 C 0.2337(6) 0.0082(5) 0.8504(3) 0.0167(15) Uani 1 1 d U . . C32 C 0.1941(6) -0.0408(5) 0.8963(3) 0.0146(15) Uani 1 1 d . . . H32 H 0.1112 -0.0219 0.9161 0.018 Uiso 1 1 calc R . . C33 C 0.2753(7) -0.1164(5) 0.9126(3) 0.0201(17) Uani 1 1 d . . . C34 C 0.4000(6) -0.1389(5) 0.8826(3) 0.0148(15) Uani 1 1 d . . . H34 H 0.4568 -0.1908 0.8940 0.018 Uiso 1 1 calc R . . C35 C 0.4457(7) -0.0908(5) 0.8378(3) 0.0163(16) Uani 1 1 d . . . C36 C 0.3574(6) -0.0160(5) 0.8198(3) 0.0127(15) Uani 1 1 d . . . C37 C 0.5892(7) -0.1122(5) 0.8093(3) 0.0190(17) Uani 1 1 d . . . C38 C 0.7070(6) 0.0020(5) 0.8189(3) 0.0255(18) Uani 1 1 d . . . H38A H 0.7391 0.0375 0.8614 0.038 Uiso 1 1 calc R . . H38B H 0.6582 0.0531 0.8003 0.038 Uiso 1 1 calc R . . H38C H 0.7987 -0.0116 0.8010 0.038 Uiso 1 1 calc R . . C39 C 0.5399(6) -0.1662(5) 0.7424(3) 0.034(2) Uani 1 1 d . . . H39A H 0.6332 -0.1674 0.7236 0.051 Uiso 1 1 calc R . . H39B H 0.4761 -0.1210 0.7253 0.051 Uiso 1 1 calc R . . H39C H 0.4790 -0.2445 0.7356 0.051 Uiso 1 1 calc R . . C40 C 0.6743(6) -0.1895(5) 0.8359(3) 0.036(2) Uani 1 1 d . . . H40A H 0.7131 -0.1533 0.8781 0.054 Uiso 1 1 calc R . . H40B H 0.7625 -0.2019 0.8154 0.054 Uiso 1 1 calc R . . H40C H 0.6023 -0.2630 0.8315 0.054 Uiso 1 1 calc R . . C41 C 0.2329(7) -0.1769(5) 0.9606(3) 0.0227(17) Uani 1 1 d . . . C42 C 0.1745(7) -0.3043(5) 0.9341(3) 0.047(2) Uani 1 1 d . . . H42A H 0.1586 -0.3424 0.9659 0.071 Uiso 1 1 calc R . . H42B H 0.2517 -0.3341 0.9119 0.071 Uiso 1 1 calc R . . H42C H 0.0753 -0.3188 0.9073 0.071 Uiso 1 1 calc R . . C43 C 0.3774(7) -0.1549(5) 1.0075(3) 0.045(2) Uani 1 1 d . . . H43A H 0.4177 -0.0723 1.0235 0.067 Uiso 1 1 calc R . . H43B H 0.4578 -0.1889 0.9896 0.067 Uiso 1 1 calc R . . H43C H 0.3493 -0.1892 1.0396 0.067 Uiso 1 1 calc R . . C44 C 0.1073(7) -0.1306(5) 0.9913(3) 0.041(2) Uani 1 1 d . . . H44A H 0.0123 -0.1446 0.9624 0.061 Uiso 1 1 calc R . . H44B H 0.1445 -0.0483 1.0090 0.061 Uiso 1 1 calc R . . H44C H 0.0843 -0.1692 1.0225 0.061 Uiso 1 1 calc R . . C45 C 0.1363(6) 0.1798(5) 0.8768(3) 0.0158(15) Uani 1 1 d . . . C46 C 0.2433(7) 0.2264(5) 0.9285(3) 0.0230(17) Uani 1 1 d . . . H46 H 0.3270 0.1909 0.9364 0.028 Uiso 1 1 calc R . . C47 C 0.2301(7) 0.3231(6) 0.9684(3) 0.0293(18) Uani 1 1 d . . . C48 C 0.1125(7) 0.3794(5) 0.9575(3) 0.0226(17) Uani 1 1 d . . . H48 H 0.1058 0.4482 0.9843 0.027 Uiso 1 1 calc R . . C49 C 0.0050(6) 0.3309(5) 0.9057(3) 0.0182(16) Uani 1 1 d . . . C50 C 0.0130(6) 0.2327(5) 0.8664(3) 0.0147(15) Uani 1 1 d . . . H50 H -0.0647 0.2003 0.8321 0.018 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 0.0200(3) 0.0104(3) 0.0094(3) 0.0044(2) 0.0041(2) 0.0065(2) Cl1 0.0617(14) 0.0626(16) 0.0506(16) 0.0356(13) -0.0301(12) -0.0068(11) Cl2 0.0686(14) 0.0181(11) 0.0430(14) 0.0059(10) 0.0128(11) -0.0123(9) Cl3 0.0785(16) 0.0754(17) 0.0442(15) -0.0345(13) -0.0323(12) 0.0459(13) Cl4 0.0479(12) 0.0460(14) 0.0495(14) -0.0024(11) -0.0033(11) 0.0362(10) O1 0.024(3) 0.013(3) 0.020(3) 0.000(2) 0.005(2) 0.007(2) O2 0.028(3) 0.020(3) 0.011(3) 0.007(2) 0.005(2) 0.011(2) N1 0.017(3) 0.021(3) 0.014(3) 0.006(3) 0.004(3) 0.005(2) N2 0.024(3) 0.014(3) 0.023(4) 0.000(3) 0.001(3) 0.003(3) N3 0.015(3) 0.017(3) 0.014(3) 0.002(3) 0.001(3) -0.002(2) N4 0.023(3) 0.015(3) 0.012(3) 0.002(3) 0.004(3) 0.008(2) C1 0.008(3) 0.019(4) 0.023(4) 0.009(3) 0.002(3) 0.004(3) C2 0.009(3) 0.010(4) 0.018(4) 0.002(3) -0.009(3) -0.002(3) C3 0.026(4) 0.010(4) 0.010(4) -0.002(3) 0.001(3) 0.007(3) C4 0.021(4) 0.019(4) 0.009(4) 0.005(3) 0.007(3) 0.006(3) C5 0.018(4) 0.019(4) 0.011(4) 0.009(3) 0.003(3) 0.001(3) C6 0.017(4) 0.005(3) 0.004(4) -0.003(3) -0.006(3) 0.002(3) C7 0.037(4) 0.022(4) 0.023(5) 0.010(4) 0.019(4) 0.015(3) C8 0.089(6) 0.051(6) 0.040(5) 0.019(5) 0.049(5) 0.042(5) C9 0.123(8) 0.078(7) 0.058(7) -0.041(6) 0.059(6) -0.031(6) C10 0.106(7) 0.165(10) 0.078(8) 0.074(7) 0.073(6) 0.116(7) C11 0.022(4) 0.014(4) 0.024(5) 0.008(3) 0.007(4) -0.002(3) C12 0.046(5) 0.017(4) 0.043(5) 0.011(4) 0.019(4) -0.007(3) C13 0.037(4) 0.023(4) 0.035(5) 0.015(4) 0.010(4) 0.005(3) C14 0.018(4) 0.031(5) 0.061(6) 0.023(4) 0.011(4) -0.005(3) C15 0.008(3) 0.019(4) 0.013(4) 0.001(3) 0.004(3) 0.005(3) C16 0.020(4) 0.020(4) 0.015(4) -0.001(3) -0.004(3) 0.001(3) C17 0.026(4) 0.035(4) 0.026(5) 0.015(4) 0.002(3) 0.012(3) C18 0.033(4) 0.028(4) 0.018(4) 0.019(3) 0.015(3) 0.008(3) C19 0.027(4) 0.021(4) 0.029(4) 0.008(3) 0.018(3) 0.004(3) C20 0.018(4) 0.024(4) 0.017(4) 0.002(3) 0.003(3) 0.001(3) C21 0.029(4) 0.031(5) 0.020(5) 0.001(4) 0.001(4) 0.004(3) C22 0.028(5) 0.046(6) 0.045(6) 0.015(5) -0.006(4) 0.004(4) C23 0.030(5) 0.051(6) 0.077(7) 0.032(5) -0.006(5) 0.015(4) C24 0.028(4) 0.024(4) 0.063(6) 0.029(4) 0.006(4) 0.011(3) C25 0.016(4) 0.032(5) 0.021(4) 0.011(4) 0.004(3) 0.008(3) C26 0.022(4) 0.030(5) 0.014(4) 0.010(3) 0.010(3) 0.008(3) C27 0.055(5) 0.020(5) 0.036(5) 0.006(4) 0.016(4) 0.017(4) C28 0.043(5) 0.024(5) 0.043(6) -0.003(4) 0.013(5) -0.002(4) C29 0.036(5) 0.027(5) 0.036(5) -0.003(4) -0.007(4) -0.005(4) C30 0.031(4) 0.018(4) 0.023(4) 0.007(3) 0.000(4) 0.004(3) C31 0.013(3) 0.025(4) 0.012(4) 0.006(3) 0.002(3) 0.003(3) C32 0.015(4) 0.016(4) 0.015(4) 0.003(3) 0.008(3) 0.006(3) C33 0.028(4) 0.014(4) 0.013(4) -0.004(3) 0.000(3) 0.006(3) C34 0.017(4) 0.012(4) 0.013(4) -0.001(3) -0.003(3) 0.006(3) C35 0.025(4) 0.007(4) 0.010(4) -0.006(3) -0.002(3) -0.001(3) C36 0.025(4) 0.002(3) 0.006(4) -0.003(3) -0.002(3) 0.000(3) C37 0.013(4) 0.013(4) 0.030(5) 0.005(3) -0.003(3) 0.005(3) C38 0.014(4) 0.030(5) 0.036(5) 0.012(4) 0.008(3) 0.007(3) C39 0.018(4) 0.041(5) 0.039(5) -0.003(4) 0.011(4) 0.010(3) C40 0.022(4) 0.044(5) 0.048(6) 0.021(4) 0.008(4) 0.010(3) C41 0.031(4) 0.024(4) 0.024(5) 0.015(4) 0.013(4) 0.014(3) C42 0.074(6) 0.033(5) 0.040(6) 0.015(4) 0.032(5) 0.003(4) C43 0.055(5) 0.064(6) 0.028(5) 0.031(4) 0.004(4) 0.025(4) C44 0.058(5) 0.035(5) 0.042(5) 0.018(4) 0.026(4) 0.022(4) C45 0.017(4) 0.027(4) 0.004(4) 0.004(3) 0.003(3) 0.009(3) C46 0.031(4) 0.016(4) 0.023(4) -0.001(3) 0.001(3) 0.020(3) C47 0.037(4) 0.036(5) 0.011(4) -0.004(4) -0.008(3) 0.017(4) C48 0.037(4) 0.012(4) 0.019(4) -0.002(3) 0.011(4) 0.010(3) C49 0.016(4) 0.007(4) 0.028(5) -0.001(3) 0.003(3) 0.002(3) C50 0.023(4) 0.014(4) 0.011(4) 0.006(3) 0.008(3) 0.005(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 N1 1.980(5) . ? Ru1 N4 1.995(5) . ? Ru1 O1 2.003(4) . ? Ru1 O2 2.025(4) . ? Ru1 N3 2.032(5) . ? Ru1 N2 2.037(5) . ? Cl1 C17 1.716(7) . ? Cl2 C19 1.741(6) . ? Cl3 C47 1.724(6) . ? Cl4 C49 1.733(6) . ? O1 C1 1.320(6) . ? O2 C36 1.312(6) . ? N1 C6 1.382(6) . ? N1 C15 1.407(7) . ? N2 C21 1.326(6) . ? N2 C25 1.335(7) . ? N3 C30 1.339(6) . ? N3 C26 1.360(7) . ? N4 C45 1.396(7) . ? N4 C31 1.407(7) . ? C1 C2 1.426(7) . ? C1 C6 1.427(7) . ? C2 C3 1.393(7) . ? C2 C11 1.516(7) . ? C3 C4 1.407(7) . ? C3 H3 0.9500 . ? C4 C5 1.375(7) . ? C4 C7 1.518(7) . ? C5 C6 1.408(7) . ? C5 H5 0.9500 . ? C7 C10 1.489(8) . ? C7 C8 1.489(8) . ? C7 C9 1.546(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.518(8) . ? C11 C14 1.534(7) . ? C11 C13 1.539(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.407(7) . ? C15 C16 1.423(8) . ? C16 C17 1.362(8) . ? C16 H16 0.9500 . ? C17 C18 1.373(8) . ? C18 C19 1.368(8) . ? C18 H18 0.9500 . ? C19 C20 1.380(8) . ? C20 H20 0.9500 . ? C21 C22 1.384(8) . ? C21 H21 0.9500 . ? C22 C23 1.376(8) . ? C22 H22 0.9500 . ? C23 C24 1.385(8) . ? C23 H23 0.9500 . ? C24 C25 1.395(7) . ? C24 H24 0.9500 . ? C25 C26 1.462(8) . ? C26 C27 1.386(8) . ? C27 C28 1.363(8) . ? C27 H27 0.9500 . ? C28 C29 1.352(8) . ? C28 H28 0.9500 . ? C29 C30 1.376(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.399(8) . ? C31 C36 1.417(7) . ? C32 C33 1.375(8) . ? C32 H32 0.9500 . ? C33 C34 1.412(7) . ? C33 C41 1.531(8) . ? C34 C35 1.385(8) . ? C34 H34 0.9500 . ? C35 C36 1.420(8) . ? C35 C37 1.538(7) . ? C37 C40 1.519(8) . ? C37 C39 1.536(8) . ? C37 C38 1.537(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.514(8) . ? C41 C44 1.521(7) . ? C41 C43 1.528(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.384(7) . ? C45 C50 1.399(7) . ? C46 C47 1.371(7) . ? C46 H46 0.9500 . ? C47 C48 1.388(7) . ? C48 C49 1.390(8) . ? C48 H48 0.9500 . ? C49 C50 1.364(7) . ? C50 H50 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 N1 Ru1 N4 167.9(2) . . ? N1 Ru1 O1 80.35(18) . . ? N4 Ru1 O1 92.63(18) . . ? N1 Ru1 O2 89.40(18) . . ? N4 Ru1 O2 80.08(17) . . ? O1 Ru1 O2 84.67(15) . . ? N1 Ru1 N3 98.9(2) . . ? N4 Ru1 N3 88.9(2) . . ? O1 Ru1 N3 175.0(2) . . ? O2 Ru1 N3 100.29(18) . . ? N1 Ru1 N2 90.4(2) . . ? N4 Ru1 N2 100.2(2) . . ? O1 Ru1 N2 96.73(18) . . ? O2 Ru1 N2 178.5(2) . . ? N3 Ru1 N2 78.3(2) . . ? C1 O1 Ru1 111.3(4) . . ? C36 O2 Ru1 110.8(4) . . ? C6 N1 C15 120.3(5) . . ? C6 N1 Ru1 111.5(4) . . ? C15 N1 Ru1 126.5(4) . . ? C21 N2 C25 118.3(6) . . ? C21 N2 Ru1 124.9(4) . . ? C25 N2 Ru1 116.7(4) . . ? C30 N3 C26 118.5(5) . . ? C30 N3 Ru1 125.0(4) . . ? C26 N3 Ru1 116.4(4) . . ? C45 N4 C31 118.7(5) . . ? C45 N4 Ru1 126.4(4) . . ? C31 N4 Ru1 109.1(4) . . ? O1 C1 C2 123.5(5) . . ? O1 C1 C6 116.9(5) . . ? C2 C1 C6 119.5(6) . . ? C3 C2 C1 115.6(5) . . ? C3 C2 C11 123.4(5) . . ? C1 C2 C11 120.9(5) . . ? C2 C3 C4 125.8(6) . . ? C2 C3 H3 117.1 . . ? C4 C3 H3 117.1 . . ? C5 C4 C3 117.8(5) . . ? C5 C4 C7 122.9(6) . . ? C3 C4 C7 119.3(5) . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 125.5(5) . . ? N1 C6 C1 113.1(5) . . ? C5 C6 C1 121.4(6) . . ? C10 C7 C8 109.8(6) . . ? C10 C7 C4 110.1(6) . . ? C8 C7 C4 112.4(5) . . ? C10 C7 C9 110.2(6) . . ? C8 C7 C9 104.4(6) . . ? C4 C7 C9 109.9(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 C12 112.4(5) . . ? C2 C11 C14 108.9(5) . . ? C12 C11 C14 107.4(5) . . ? C2 C11 C13 111.1(5) . . ? C12 C11 C13 107.9(6) . . ? C14 C11 C13 109.1(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C20 120.1(5) . . ? N1 C15 C16 123.4(5) . . ? C20 C15 C16 116.2(6) . . ? C17 C16 C15 121.2(6) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 121.7(6) . . ? C16 C17 Cl1 119.1(5) . . ? C18 C17 Cl1 119.2(5) . . ? C19 C18 C17 118.2(6) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? C18 C19 C20 122.2(6) . . ? C18 C19 Cl2 119.5(5) . . ? C20 C19 Cl2 118.3(5) . . ? C19 C20 C15 120.4(6) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? N2 C21 C22 124.1(7) . . ? N2 C21 H21 117.9 . . ? C22 C21 H21 117.9 . . ? C23 C22 C21 116.5(6) . . ? C23 C22 H22 121.8 . . ? C21 C22 H22 121.8 . . ? C22 C23 C24 121.5(6) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C25 116.9(6) . . ? C23 C24 H24 121.5 . . ? C25 C24 H24 121.5 . . ? N2 C25 C24 122.6(6) . . ? N2 C25 C26 114.7(6) . . ? C24 C25 C26 122.7(6) . . ? N3 C26 C27 120.1(6) . . ? N3 C26 C25 113.7(6) . . ? C27 C26 C25 126.1(6) . . ? C28 C27 C26 120.1(7) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 119.8(7) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 118.8(7) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N3 C30 C29 122.6(6) . . ? N3 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C32 C31 N4 123.3(5) . . ? C32 C31 C36 122.3(6) . . ? N4 C31 C36 114.3(5) . . ? C33 C32 C31 120.0(6) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 117.5(6) . . ? C32 C33 C41 122.4(6) . . ? C34 C33 C41 120.2(6) . . ? C35 C34 C33 124.7(6) . . ? C35 C34 H34 117.6 . . ? C33 C34 H34 117.6 . . ? C34 C35 C36 117.3(6) . . ? C34 C35 C37 122.6(6) . . ? C36 C35 C37 120.1(6) . . ? O2 C36 C31 116.6(5) . . ? O2 C36 C35 125.1(6) . . ? C31 C36 C35 118.1(6) . . ? C40 C37 C39 108.7(5) . . ? C40 C37 C38 106.9(5) . . ? C39 C37 C38 108.7(5) . . ? C40 C37 C35 113.0(5) . . ? C39 C37 C35 110.0(5) . . ? C38 C37 C35 109.4(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C44 108.8(5) . . ? C42 C41 C43 109.5(6) . . ? C44 C41 C43 107.6(6) . . ? C42 C41 C33 110.7(5) . . ? C44 C41 C33 111.1(5) . . ? C43 C41 C33 109.1(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N4 120.5(5) . . ? C46 C45 C50 118.6(6) . . ? N4 C45 C50 120.5(5) . . ? C47 C46 C45 120.8(6) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C46 C47 C48 121.2(6) . . ? C46 C47 Cl3 120.6(5) . . ? C48 C47 Cl3 118.1(5) . . ? C47 C48 C49 117.2(6) . . ? C47 C48 H48 121.4 . . ? C49 C48 H48 121.4 . . ? C50 C49 C48 122.4(6) . . ? C50 C49 Cl4 119.1(5) . . ? C48 C49 Cl4 118.5(5) . . ? C49 C50 C45 119.6(6) . . ? C49 C50 H50 120.2 . . ? C45 C50 H50 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 O1 C1 22.1(4) . . . . ? N4 Ru1 O1 C1 -148.0(4) . . . . ? O2 Ru1 O1 C1 -68.2(4) . . . . ? N3 Ru1 O1 C1 104(2) . . . . ? N2 Ru1 O1 C1 111.4(4) . . . . ? N1 Ru1 O2 C36 -148.5(4) . . . . ? N4 Ru1 O2 C36 25.5(4) . . . . ? O1 Ru1 O2 C36 -68.2(4) . . . . ? N3 Ru1 O2 C36 112.6(4) . . . . ? N2 Ru1 O2 C36 128(8) . . . . ? N4 Ru1 N1 C6 32.8(11) . . . . ? O1 Ru1 N1 C6 -22.4(3) . . . . ? O2 Ru1 N1 C6 62.3(4) . . . . ? N3 Ru1 N1 C6 162.6(4) . . . . ? N2 Ru1 N1 C6 -119.2(4) . . . . ? N4 Ru1 N1 C15 -161.8(8) . . . . ? O1 Ru1 N1 C15 143.0(5) . . . . ? O2 Ru1 N1 C15 -132.3(5) . . . . ? N3 Ru1 N1 C15 -31.9(5) . . . . ? N2 Ru1 N1 C15 46.3(5) . . . . ? N1 Ru1 N2 C21 80.4(5) . . . . ? N4 Ru1 N2 C21 -93.9(5) . . . . ? O1 Ru1 N2 C21 0.1(6) . . . . ? O2 Ru1 N2 C21 164(8) . . . . ? N3 Ru1 N2 C21 179.4(6) . . . . ? N1 Ru1 N2 C25 -97.4(5) . . . . ? N4 Ru1 N2 C25 88.3(5) . . . . ? O1 Ru1 N2 C25 -177.7(5) . . . . ? O2 Ru1 N2 C25 -14(8) . . . . ? N3 Ru1 N2 C25 1.6(5) . . . . ? N1 Ru1 N3 C30 -93.6(5) . . . . ? N4 Ru1 N3 C30 77.1(5) . . . . ? O1 Ru1 N3 C30 -174(2) . . . . ? O2 Ru1 N3 C30 -2.6(5) . . . . ? N2 Ru1 N3 C30 177.8(5) . . . . ? N1 Ru1 N3 C26 89.9(5) . . . . ? N4 Ru1 N3 C26 -99.4(5) . . . . ? O1 Ru1 N3 C26 9(3) . . . . ? O2 Ru1 N3 C26 -179.1(4) . . . . ? N2 Ru1 N3 C26 1.3(5) . . . . ? N1 Ru1 N4 C45 156.7(8) . . . . ? O1 Ru1 N4 C45 -149.2(4) . . . . ? O2 Ru1 N4 C45 126.7(5) . . . . ? N3 Ru1 N4 C45 26.1(5) . . . . ? N2 Ru1 N4 C45 -51.8(5) . . . . ? N1 Ru1 N4 C31 4.4(12) . . . . ? O1 Ru1 N4 C31 58.5(4) . . . . ? O2 Ru1 N4 C31 -25.6(3) . . . . ? N3 Ru1 N4 C31 -126.2(4) . . . . ? N2 Ru1 N4 C31 155.9(4) . . . . ? Ru1 O1 C1 C2 163.8(4) . . . . ? Ru1 O1 C1 C6 -18.0(6) . . . . ? O1 C1 C2 C3 -178.3(5) . . . . ? C6 C1 C2 C3 3.6(7) . . . . ? O1 C1 C2 C11 4.0(8) . . . . ? C6 C1 C2 C11 -174.1(5) . . . . ? C1 C2 C3 C4 -3.6(8) . . . . ? C11 C2 C3 C4 174.0(6) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C2 C3 C4 C7 177.9(5) . . . . ? C3 C4 C5 C6 3.2(9) . . . . ? C7 C4 C5 C6 -174.3(5) . . . . ? C15 N1 C6 C5 30.6(8) . . . . ? Ru1 N1 C6 C5 -162.9(4) . . . . ? C15 N1 C6 C1 -147.3(5) . . . . ? Ru1 N1 C6 C1 19.2(6) . . . . ? C4 C5 C6 N1 179.1(5) . . . . ? C4 C5 C6 C1 -3.1(8) . . . . ? O1 C1 C6 N1 -0.6(7) . . . . ? C2 C1 C6 N1 177.6(5) . . . . ? O1 C1 C6 C5 -178.6(5) . . . . ? C2 C1 C6 C5 -0.4(8) . . . . ? C5 C4 C7 C10 108.3(7) . . . . ? C3 C4 C7 C10 -69.2(8) . . . . ? C5 C4 C7 C8 -14.4(9) . . . . ? C3 C4 C7 C8 168.1(6) . . . . ? C5 C4 C7 C9 -130.2(7) . . . . ? C3 C4 C7 C9 52.3(8) . . . . ? C3 C2 C11 C12 1.1(8) . . . . ? C1 C2 C11 C12 178.6(5) . . . . ? C3 C2 C11 C14 -117.8(6) . . . . ? C1 C2 C11 C14 59.8(7) . . . . ? C3 C2 C11 C13 122.1(6) . . . . ? C1 C2 C11 C13 -60.4(7) . . . . ? C6 N1 C15 C20 -139.2(5) . . . . ? Ru1 N1 C15 C20 56.5(7) . . . . ? C6 N1 C15 C16 46.7(7) . . . . ? Ru1 N1 C15 C16 -117.6(5) . . . . ? N1 C15 C16 C17 171.9(5) . . . . ? C20 C15 C16 C17 -2.4(7) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C15 C16 C17 Cl1 -179.3(4) . . . . ? C16 C17 C18 C19 1.0(9) . . . . ? Cl1 C17 C18 C19 -179.6(5) . . . . ? C17 C18 C19 C20 0.2(9) . . . . ? C17 C18 C19 Cl2 178.2(5) . . . . ? C18 C19 C20 C15 -2.6(9) . . . . ? Cl2 C19 C20 C15 179.3(4) . . . . ? N1 C15 C20 C19 -170.9(5) . . . . ? C16 C15 C20 C19 3.6(8) . . . . ? C25 N2 C21 C22 0.3(10) . . . . ? Ru1 N2 C21 C22 -177.5(5) . . . . ? N2 C21 C22 C23 -0.3(11) . . . . ? C21 C22 C23 C24 -0.2(12) . . . . ? C22 C23 C24 C25 0.5(12) . . . . ? C21 N2 C25 C24 0.1(10) . . . . ? Ru1 N2 C25 C24 178.1(5) . . . . ? C21 N2 C25 C26 178.1(6) . . . . ? Ru1 N2 C25 C26 -4.0(7) . . . . ? C23 C24 C25 N2 -0.5(11) . . . . ? C23 C24 C25 C26 -178.3(7) . . . . ? C30 N3 C26 C27 3.1(9) . . . . ? Ru1 N3 C26 C27 179.8(5) . . . . ? C30 N3 C26 C25 179.6(5) . . . . ? Ru1 N3 C26 C25 -3.7(7) . . . . ? N2 C25 C26 N3 5.0(8) . . . . ? C24 C25 C26 N3 -177.1(6) . . . . ? N2 C25 C26 C27 -178.8(6) . . . . ? C24 C25 C26 C27 -0.9(11) . . . . ? N3 C26 C27 C28 -1.5(11) . . . . ? C25 C26 C27 C28 -177.5(6) . . . . ? C26 C27 C28 C29 -0.1(11) . . . . ? C27 C28 C29 C30 -0.1(12) . . . . ? C26 N3 C30 C29 -3.3(10) . . . . ? Ru1 N3 C30 C29 -179.8(5) . . . . ? C28 C29 C30 N3 1.8(11) . . . . ? C45 N4 C31 C32 44.6(8) . . . . ? Ru1 N4 C31 C32 -160.7(5) . . . . ? C45 N4 C31 C36 -131.9(5) . . . . ? Ru1 N4 C31 C36 22.9(6) . . . . ? N4 C31 C32 C33 -176.9(5) . . . . ? C36 C31 C32 C33 -0.7(9) . . . . ? C31 C32 C33 C34 1.7(9) . . . . ? C31 C32 C33 C41 -177.2(5) . . . . ? C32 C33 C34 C35 -0.4(9) . . . . ? C41 C33 C34 C35 178.5(5) . . . . ? C33 C34 C35 C36 -1.8(9) . . . . ? C33 C34 C35 C37 175.9(5) . . . . ? Ru1 O2 C36 C31 -20.0(6) . . . . ? Ru1 O2 C36 C35 163.4(5) . . . . ? C32 C31 C36 O2 -178.4(5) . . . . ? N4 C31 C36 O2 -1.9(8) . . . . ? C32 C31 C36 C35 -1.5(9) . . . . ? N4 C31 C36 C35 175.0(5) . . . . ? C34 C35 C36 O2 179.3(5) . . . . ? C37 C35 C36 O2 1.5(9) . . . . ? C34 C35 C36 C31 2.7(8) . . . . ? C37 C35 C36 C31 -175.1(5) . . . . ? C34 C35 C37 C40 -0.6(8) . . . . ? C36 C35 C37 C40 177.1(5) . . . . ? C34 C35 C37 C39 121.1(6) . . . . ? C36 C35 C37 C39 -61.3(7) . . . . ? C34 C35 C37 C38 -119.6(6) . . . . ? C36 C35 C37 C38 58.1(7) . . . . ? C32 C33 C41 C42 113.8(7) . . . . ? C34 C33 C41 C42 -65.0(7) . . . . ? C32 C33 C41 C44 -7.2(9) . . . . ? C34 C33 C41 C44 173.9(5) . . . . ? C32 C33 C41 C43 -125.6(6) . . . . ? C34 C33 C41 C43 55.5(7) . . . . ? C31 N4 C45 C46 35.1(8) . . . . ? Ru1 N4 C45 C46 -114.8(6) . . . . ? C31 N4 C45 C50 -152.4(5) . . . . ? Ru1 N4 C45 C50 57.6(7) . . . . ? N4 C45 C46 C47 171.9(6) . . . . ? C50 C45 C46 C47 -0.7(10) . . . . ? C45 C46 C47 C48 -2.2(10) . . . . ? C45 C46 C47 Cl3 -178.8(5) . . . . ? C46 C47 C48 C49 2.7(10) . . . . ? Cl3 C47 C48 C49 179.4(5) . . . . ? C47 C48 C49 C50 -0.4(10) . . . . ? C47 C48 C49 Cl4 178.4(5) . . . . ? C48 C49 C50 C45 -2.4(9) . . . . ? Cl4 C49 C50 C45 178.7(5) . . . . ? C46 C45 C50 C49 3.0(9) . . . . ? N4 C45 C50 C49 -169.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.755 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.097 # Attachment '- 2b.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 821454' #TrackingRef '- 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Cl4 N4 O2 Ru' _chemical_formula_weight 985.84 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 11.6914(4) _cell_length_b 17.2733(4) _cell_length_c 23.6512(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.160(3) _cell_angle_gamma 90.00 _cell_volume 4686.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18267 _cell_measurement_theta_min 3.2481 _cell_measurement_theta_max 32.7407 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_T_min 0.8486 _exptl_absorpt_correction_T_max 0.8935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32590 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8230 _reflns_number_gt 5334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8230 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.817 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.37834(2) 0.143305(13) 0.094246(10) 0.01950(7) Uani 1 1 d . . . Cl1 Cl 0.04256(8) -0.13776(5) 0.02550(4) 0.0527(3) Uani 1 1 d . . . Cl2 Cl 0.26819(10) -0.13112(5) 0.24610(4) 0.0611(3) Uani 1 1 d . . . Cl3 Cl 0.26797(8) 0.12188(6) 0.33377(4) 0.0594(3) Uani 1 1 d . . . Cl4 Cl 0.71682(8) 0.20830(5) 0.36386(4) 0.0447(2) Uani 1 1 d . . . O1 O 0.27920(17) 0.23723(9) 0.06996(8) 0.0220(5) Uani 1 1 d . . . O2 O 0.50819(17) 0.19564(10) 0.06317(8) 0.0209(5) Uani 1 1 d . . . N1 N 0.2344(2) 0.11041(12) 0.11816(9) 0.0215(6) Uani 1 1 d . . . N2 N 0.3262(2) 0.08687(12) 0.01697(10) 0.0202(6) Uani 1 1 d . . . N3 N 0.4564(2) 0.03665(12) 0.11113(10) 0.0208(6) Uani 1 1 d . . . N4 N 0.4511(2) 0.20419(12) 0.16392(10) 0.0213(6) Uani 1 1 d . . . C1 C 0.1897(3) 0.24072(15) 0.09624(12) 0.0190(7) Uani 1 1 d . . . C2 C 0.1188(3) 0.30703(15) 0.09674(12) 0.0205(7) Uani 1 1 d . . . C3 C 0.0293(3) 0.30158(15) 0.12673(12) 0.0221(7) Uani 1 1 d . . . H3 H -0.0171 0.3463 0.1285 0.027 Uiso 1 1 calc R . . C4 C 0.0018(3) 0.23456(15) 0.15495(12) 0.0215(7) Uani 1 1 d . . . C5 C 0.0664(3) 0.16906(15) 0.15094(12) 0.0218(7) Uani 1 1 d . . . H5 H 0.0471 0.1220 0.1676 0.026 Uiso 1 1 calc R . . C6 C 0.1598(3) 0.17134(15) 0.12266(12) 0.0199(7) Uani 1 1 d . . . C7 C -0.0919(3) 0.23475(16) 0.19166(14) 0.0282(8) Uani 1 1 d . . . C8 C -0.1825(3) 0.17067(16) 0.16903(15) 0.0382(9) Uani 1 1 d . . . H8A H -0.2392 0.1668 0.1945 0.057 Uiso 1 1 calc R . . H8B H -0.1424 0.1210 0.1683 0.057 Uiso 1 1 calc R . . H8C H -0.2232 0.1838 0.1300 0.057 Uiso 1 1 calc R . . C9 C -0.1549(3) 0.31146(16) 0.19038(15) 0.0376(9) Uani 1 1 d . . . H9A H -0.0982 0.3528 0.2028 0.056 Uiso 1 1 calc R . . H9B H -0.2106 0.3093 0.2165 0.056 Uiso 1 1 calc R . . H9C H -0.1968 0.3220 0.1511 0.056 Uiso 1 1 calc R . . C10 C -0.0346(3) 0.21860(18) 0.25401(13) 0.0396(9) Uani 1 1 d . . . H10A H 0.0223 0.2593 0.2678 0.059 Uiso 1 1 calc R . . H10B H 0.0050 0.1684 0.2565 0.059 Uiso 1 1 calc R . . H10C H -0.0944 0.2177 0.2779 0.059 Uiso 1 1 calc R . . C11 C 0.1420(3) 0.38113(15) 0.06532(13) 0.0246(7) Uani 1 1 d . . . C12 C 0.0588(3) 0.44626(16) 0.07353(14) 0.0387(9) Uani 1 1 d . . . H12A H -0.0214 0.4309 0.0568 0.058 Uiso 1 1 calc R . . H12B H 0.0790 0.4931 0.0543 0.058 Uiso 1 1 calc R . . H12C H 0.0651 0.4566 0.1148 0.058 Uiso 1 1 calc R . . C13 C 0.2656(3) 0.41002(16) 0.08764(14) 0.0339(8) Uani 1 1 d . . . H13A H 0.2758 0.4210 0.1290 0.051 Uiso 1 1 calc R . . H13B H 0.2790 0.4574 0.0670 0.051 Uiso 1 1 calc R . . H13C H 0.3215 0.3702 0.0813 0.051 Uiso 1 1 calc R . . C14 C 0.1256(3) 0.36417(17) 0.00087(12) 0.0414(9) Uani 1 1 d . . . H14A H 0.1839 0.3263 -0.0059 0.062 Uiso 1 1 calc R . . H14B H 0.1351 0.4121 -0.0199 0.062 Uiso 1 1 calc R . . H14C H 0.0473 0.3432 -0.0130 0.062 Uiso 1 1 calc R . . C15 C 0.1998(3) 0.03202(15) 0.12526(13) 0.0219(7) Uani 1 1 d . . . C16 C 0.1357(3) -0.00748(15) 0.07938(14) 0.0273(8) Uani 1 1 d . . . H16 H 0.1054 0.0188 0.0444 0.033 Uiso 1 1 calc R . . C17 C 0.1157(3) -0.08627(17) 0.08467(15) 0.0332(8) Uani 1 1 d . . . C18 C 0.1544(3) -0.12479(17) 0.13606(15) 0.0376(9) Uani 1 1 d . . . H18 H 0.1387 -0.1783 0.1397 0.045 Uiso 1 1 calc R . . C19 C 0.2162(3) -0.08384(17) 0.18157(15) 0.0363(9) Uani 1 1 d . . . C20 C 0.2399(3) -0.00589(16) 0.17693(13) 0.0304(8) Uani 1 1 d . . . H20 H 0.2833 0.0214 0.2089 0.036 Uiso 1 1 calc R . . C21 C 0.2610(3) 0.11960(16) -0.02911(13) 0.0272(8) Uani 1 1 d . . . H21 H 0.2397 0.1725 -0.0271 0.033 Uiso 1 1 calc R . . C22 C 0.2232(3) 0.07972(17) -0.07962(13) 0.0362(9) Uani 1 1 d . . . H22 H 0.1756 0.1041 -0.1118 0.043 Uiso 1 1 calc R . . C23 C 0.2564(3) 0.00311(18) -0.08223(14) 0.0401(9) Uani 1 1 d . . . H23 H 0.2314 -0.0259 -0.1165 0.048 Uiso 1 1 calc R . . C24 C 0.3252(3) -0.03099(16) -0.03546(13) 0.0307(8) Uani 1 1 d . . . H24 H 0.3494 -0.0833 -0.0372 0.037 Uiso 1 1 calc R . . C25 C 0.3592(3) 0.01185(15) 0.01447(13) 0.0216(7) Uani 1 1 d . . . C26 C 0.4288(3) -0.01702(15) 0.06851(13) 0.0242(7) Uani 1 1 d . . . C27 C 0.4641(3) -0.09364(16) 0.07712(14) 0.0328(8) Uani 1 1 d . . . H27 H 0.4452 -0.1301 0.0467 0.039 Uiso 1 1 calc R . . C28 C 0.5258(3) -0.11621(18) 0.12917(15) 0.0418(10) Uani 1 1 d . . . H28 H 0.5487 -0.1687 0.1359 0.050 Uiso 1 1 calc R . . C29 C 0.5545(3) -0.06155(17) 0.17204(14) 0.0382(9) Uani 1 1 d . . . H29 H 0.5982 -0.0760 0.2087 0.046 Uiso 1 1 calc R . . C30 C 0.5198(3) 0.01373(16) 0.16150(13) 0.0293(8) Uani 1 1 d . . . H30 H 0.5417 0.0510 0.1911 0.035 Uiso 1 1 calc R . . C31 C 0.5033(3) 0.26965(15) 0.14574(12) 0.0202(7) Uani 1 1 d . . . C32 C 0.5245(3) 0.33837(15) 0.17722(13) 0.0257(8) Uani 1 1 d . . . H32 H 0.5064 0.3414 0.2146 0.031 Uiso 1 1 calc R . . C33 C 0.5709(3) 0.40122(16) 0.15484(13) 0.0270(8) Uani 1 1 d . . . C34 C 0.5983(3) 0.39396(16) 0.09948(12) 0.0247(7) Uani 1 1 d . . . H34 H 0.6313 0.4375 0.0841 0.030 Uiso 1 1 calc R . . C35 C 0.5801(2) 0.32771(15) 0.06633(12) 0.0210(7) Uani 1 1 d . . . C36 C 0.5301(2) 0.26345(15) 0.08984(12) 0.0181(7) Uani 1 1 d . . . C37 C 0.6114(3) 0.32309(16) 0.00633(12) 0.0258(7) Uani 1 1 d . . . C38 C 0.6601(3) 0.40022(16) -0.01127(13) 0.0349(9) Uani 1 1 d . . . H38A H 0.6804 0.3947 -0.0494 0.052 Uiso 1 1 calc R . . H38B H 0.7299 0.4143 0.0170 0.052 Uiso 1 1 calc R . . H38C H 0.6011 0.4408 -0.0127 0.052 Uiso 1 1 calc R . . C39 C 0.7059(3) 0.26196(16) 0.00614(14) 0.0326(8) Uani 1 1 d . . . H39A H 0.6784 0.2118 0.0176 0.049 Uiso 1 1 calc R . . H39B H 0.7767 0.2770 0.0333 0.049 Uiso 1 1 calc R . . H39C H 0.7231 0.2578 -0.0327 0.049 Uiso 1 1 calc R . . C40 C 0.5018(3) 0.30457(17) -0.03810(13) 0.0324(8) Uani 1 1 d . . . H40A H 0.4682 0.2558 -0.0278 0.049 Uiso 1 1 calc R . . H40B H 0.5220 0.2996 -0.0763 0.049 Uiso 1 1 calc R . . H40C H 0.4449 0.3464 -0.0387 0.049 Uiso 1 1 calc R . . C41 C 0.5907(3) 0.47922(16) 0.18666(14) 0.0355(9) Uani 1 1 d . . . C42 C 0.5596(5) 0.4751(2) 0.24539(18) 0.108(2) Uani 1 1 d . . . H42A H 0.5773 0.5248 0.2652 0.162 Uiso 1 1 calc R . . H42B H 0.6049 0.4340 0.2679 0.162 Uiso 1 1 calc R . . H42C H 0.4762 0.4640 0.2414 0.162 Uiso 1 1 calc R . . C43 C 0.5179(3) 0.54096(18) 0.15029(16) 0.0536(11) Uani 1 1 d . . . H43A H 0.4349 0.5288 0.1468 0.080 Uiso 1 1 calc R . . H43B H 0.5376 0.5422 0.1119 0.080 Uiso 1 1 calc R . . H43C H 0.5342 0.5916 0.1688 0.080 Uiso 1 1 calc R . . C44 C 0.7171(4) 0.50467(19) 0.1923(2) 0.0733(14) Uani 1 1 d . . . H44A H 0.7364 0.5086 0.1538 0.110 Uiso 1 1 calc R . . H44B H 0.7684 0.4666 0.2152 0.110 Uiso 1 1 calc R . . H44C H 0.7279 0.5552 0.2113 0.110 Uiso 1 1 calc R . . C45 C 0.4655(3) 0.19112(14) 0.22341(12) 0.0204(7) Uani 1 1 d . . . C46 C 0.3723(3) 0.16523(15) 0.24713(12) 0.0263(7) Uani 1 1 d . . . H46 H 0.2985 0.1565 0.2230 0.032 Uiso 1 1 calc R . . C47 C 0.3872(3) 0.15219(17) 0.30574(13) 0.0306(8) Uani 1 1 d . . . C48 C 0.4915(3) 0.16439(17) 0.34263(13) 0.0320(8) Uani 1 1 d . . . H48 H 0.5002 0.1548 0.3828 0.038 Uiso 1 1 calc R . . C49 C 0.5830(3) 0.19100(16) 0.31919(13) 0.0290(8) Uani 1 1 d . . . C50 C 0.5711(3) 0.20347(16) 0.26090(13) 0.0256(7) Uani 1 1 d . . . H50 H 0.6364 0.2209 0.2459 0.031 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 0.02551(14) 0.01577(11) 0.01804(13) 0.00053(12) 0.00629(10) 0.00069(13) Cl1 0.0460(6) 0.0328(4) 0.0718(7) -0.0132(5) -0.0073(5) -0.0085(5) Cl2 0.0970(9) 0.0369(5) 0.0484(6) 0.0225(5) 0.0116(6) 0.0038(5) Cl3 0.0438(6) 0.1038(8) 0.0331(5) 0.0188(5) 0.0137(5) -0.0169(6) Cl4 0.0354(5) 0.0674(6) 0.0279(5) 0.0021(4) -0.0020(4) -0.0031(5) O1 0.0303(13) 0.0173(10) 0.0198(11) 0.0028(9) 0.0084(10) 0.0013(9) O2 0.0273(12) 0.0166(10) 0.0193(11) 0.0004(9) 0.0057(9) 0.0012(9) N1 0.0295(16) 0.0169(12) 0.0185(14) 0.0021(11) 0.0057(12) 0.0012(12) N2 0.0256(15) 0.0181(12) 0.0180(14) -0.0014(11) 0.0069(12) -0.0022(12) N3 0.0220(15) 0.0199(12) 0.0220(15) 0.0015(11) 0.0079(12) 0.0010(11) N4 0.0302(16) 0.0169(12) 0.0184(14) 0.0005(11) 0.0087(12) -0.0002(12) C1 0.0241(18) 0.0214(15) 0.0105(16) -0.0017(13) 0.0004(14) -0.0020(14) C2 0.0234(18) 0.0205(15) 0.0150(16) 0.0001(13) -0.0028(14) 0.0022(14) C3 0.0246(19) 0.0174(14) 0.0231(17) -0.0008(13) 0.0015(15) 0.0065(14) C4 0.0232(18) 0.0230(15) 0.0175(16) -0.0035(13) 0.0017(14) -0.0004(14) C5 0.0274(19) 0.0177(14) 0.0199(17) 0.0018(13) 0.0041(14) -0.0033(14) C6 0.0263(19) 0.0174(14) 0.0147(16) -0.0009(12) 0.0009(14) 0.0011(14) C7 0.030(2) 0.0217(16) 0.036(2) -0.0008(15) 0.0120(16) 0.0016(15) C8 0.028(2) 0.0286(17) 0.062(2) -0.0042(17) 0.0186(19) 0.0006(15) C9 0.034(2) 0.0328(18) 0.051(2) -0.0059(17) 0.0217(18) 0.0009(17) C10 0.043(2) 0.044(2) 0.037(2) -0.0022(17) 0.0194(19) -0.0020(18) C11 0.030(2) 0.0163(15) 0.0258(18) 0.0023(13) 0.0022(15) 0.0040(14) C12 0.044(2) 0.0249(17) 0.047(2) 0.0150(16) 0.0082(19) 0.0077(16) C13 0.041(2) 0.0198(16) 0.041(2) 0.0111(15) 0.0064(18) -0.0004(16) C14 0.067(3) 0.0319(18) 0.0234(18) 0.0067(16) 0.0039(17) 0.0062(19) C15 0.0215(19) 0.0171(15) 0.0297(19) 0.0027(14) 0.0115(15) 0.0036(14) C16 0.027(2) 0.0196(15) 0.036(2) 0.0046(15) 0.0065(16) 0.0012(15) C17 0.024(2) 0.0257(17) 0.049(2) -0.0028(17) 0.0059(17) -0.0020(16) C18 0.039(2) 0.0169(17) 0.060(3) 0.0050(17) 0.0158(19) -0.0016(15) C19 0.047(2) 0.0253(17) 0.040(2) 0.0118(17) 0.0163(19) 0.0034(17) C20 0.039(2) 0.0243(17) 0.030(2) 0.0030(15) 0.0114(17) 0.0011(16) C21 0.031(2) 0.0246(16) 0.0256(19) 0.0020(14) 0.0054(16) -0.0002(15) C22 0.050(2) 0.0306(18) 0.024(2) -0.0036(15) -0.0029(17) 0.0000(17) C23 0.056(3) 0.0349(19) 0.026(2) -0.0125(16) -0.0001(18) -0.0086(18) C24 0.043(2) 0.0188(15) 0.030(2) -0.0044(15) 0.0068(17) -0.0004(16) C25 0.0247(19) 0.0165(15) 0.0257(18) -0.0015(14) 0.0102(15) 0.0001(14) C26 0.029(2) 0.0203(15) 0.0264(19) -0.0018(14) 0.0135(15) 0.0020(15) C27 0.040(2) 0.0192(16) 0.038(2) -0.0075(15) 0.0041(18) 0.0032(16) C28 0.060(3) 0.0221(16) 0.044(2) 0.0059(17) 0.011(2) 0.0157(17) C29 0.052(3) 0.0314(18) 0.029(2) 0.0074(16) 0.0021(18) 0.0104(18) C30 0.040(2) 0.0276(17) 0.0210(19) 0.0017(14) 0.0082(16) 0.0093(16) C31 0.0240(19) 0.0178(14) 0.0179(17) 0.0018(13) 0.0017(14) 0.0035(14) C32 0.034(2) 0.0234(17) 0.0192(17) -0.0038(13) 0.0046(15) 0.0039(14) C33 0.036(2) 0.0200(16) 0.0220(18) 0.0017(14) -0.0015(16) -0.0025(15) C34 0.028(2) 0.0188(15) 0.0258(19) 0.0033(14) 0.0018(15) -0.0021(14) C35 0.0196(18) 0.0210(15) 0.0215(17) 0.0010(13) 0.0019(14) 0.0019(13) C36 0.0190(17) 0.0173(15) 0.0177(16) -0.0004(13) 0.0026(13) -0.0006(13) C37 0.034(2) 0.0228(15) 0.0210(18) 0.0041(14) 0.0059(15) -0.0048(15) C38 0.049(2) 0.0317(18) 0.0270(19) 0.0055(15) 0.0138(17) -0.0085(17) C39 0.036(2) 0.0304(17) 0.035(2) 0.0010(15) 0.0155(17) -0.0011(16) C40 0.047(2) 0.0294(17) 0.0222(18) 0.0063(15) 0.0097(17) -0.0032(16) C41 0.049(3) 0.0231(17) 0.031(2) -0.0041(15) -0.0022(18) -0.0007(17) C42 0.245(7) 0.045(2) 0.048(3) -0.029(2) 0.062(4) -0.048(3) C43 0.063(3) 0.0333(19) 0.059(3) -0.0138(19) -0.001(2) 0.012(2) C44 0.065(3) 0.037(2) 0.102(4) -0.031(2) -0.024(3) -0.001(2) C45 0.031(2) 0.0139(14) 0.0187(17) -0.0008(13) 0.0106(15) 0.0012(14) C46 0.031(2) 0.0258(16) 0.0213(18) -0.0009(13) 0.0039(15) -0.0038(15) C47 0.035(2) 0.0377(18) 0.0215(18) 0.0029(16) 0.0107(15) -0.0029(17) C48 0.040(2) 0.042(2) 0.0148(17) 0.0027(14) 0.0053(16) 0.0021(17) C49 0.032(2) 0.0300(17) 0.0240(19) 0.0008(15) 0.0029(16) 0.0061(16) C50 0.027(2) 0.0272(16) 0.0241(19) 0.0010(14) 0.0082(15) 0.0011(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 N1 1.960(2) . ? Ru1 N4 2.001(2) . ? Ru1 O1 2.0120(18) . ? Ru1 O2 2.0233(18) . ? Ru1 N2 2.057(2) . ? Ru1 N3 2.060(2) . ? Cl1 C17 1.737(3) . ? Cl2 C19 1.734(3) . ? Cl3 C47 1.737(3) . ? Cl4 C49 1.736(3) . ? O1 C1 1.318(3) . ? O2 C36 1.331(3) . ? N1 C6 1.384(3) . ? N1 C15 1.432(3) . ? N2 C21 1.329(3) . ? N2 C25 1.357(3) . ? N3 C30 1.336(4) . ? N3 C26 1.361(3) . ? N4 C31 1.391(3) . ? N4 C45 1.403(3) . ? C1 C2 1.415(4) . ? C1 C6 1.426(4) . ? C2 C3 1.376(4) . ? C2 C11 1.530(4) . ? C3 C4 1.405(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 C7 1.524(4) . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C7 C9 1.513(4) . ? C7 C10 1.523(4) . ? C7 C8 1.554(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.523(4) . ? C11 C12 1.525(4) . ? C11 C14 1.528(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.375(4) . ? C15 C20 1.386(4) . ? C16 C17 1.391(4) . ? C16 H16 0.9500 . ? C17 C18 1.383(4) . ? C18 C19 1.371(4) . ? C18 H18 0.9500 . ? C19 C20 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.376(4) . ? C21 H21 0.9500 . ? C22 C23 1.384(4) . ? C22 H22 0.9500 . ? C23 C24 1.369(4) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.464(4) . ? C26 C27 1.390(4) . ? C27 C28 1.358(4) . ? C27 H27 0.9500 . ? C28 C29 1.379(4) . ? C28 H28 0.9500 . ? C29 C30 1.371(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.398(4) . ? C31 C36 1.421(4) . ? C32 C33 1.366(4) . ? C32 H32 0.9500 . ? C33 C34 1.412(4) . ? C33 C41 1.539(4) . ? C34 C35 1.380(4) . ? C34 H34 0.9500 . ? C35 C36 1.418(4) . ? C35 C37 1.534(4) . ? C37 C40 1.525(4) . ? C37 C39 1.529(4) . ? C37 C38 1.538(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.504(5) . ? C41 C44 1.523(5) . ? C41 C43 1.523(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.390(4) . ? C45 C46 1.392(4) . ? C46 C47 1.382(4) . ? C46 H46 0.9500 . ? C47 C48 1.371(4) . ? C48 C49 1.376(4) . ? C48 H48 0.9500 . ? C49 C50 1.375(4) . ? C50 H50 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 N1 Ru1 N4 99.61(9) . . ? N1 Ru1 O1 80.61(8) . . ? N4 Ru1 O1 86.62(8) . . ? N1 Ru1 O2 168.70(8) . . ? N4 Ru1 O2 80.49(8) . . ? O1 Ru1 O2 88.12(7) . . ? N1 Ru1 N2 89.75(9) . . ? N4 Ru1 N2 170.61(9) . . ? O1 Ru1 N2 94.20(8) . . ? O2 Ru1 N2 90.18(8) . . ? N1 Ru1 N3 93.30(9) . . ? N4 Ru1 N3 102.04(9) . . ? O1 Ru1 N3 170.20(9) . . ? O2 Ru1 N3 97.74(8) . . ? N2 Ru1 N3 78.02(9) . . ? C1 O1 Ru1 111.61(16) . . ? C36 O2 Ru1 108.04(16) . . ? C6 N1 C15 120.9(2) . . ? C6 N1 Ru1 113.00(17) . . ? C15 N1 Ru1 125.84(18) . . ? C21 N2 C25 119.6(2) . . ? C21 N2 Ru1 123.45(18) . . ? C25 N2 Ru1 116.97(19) . . ? C30 N3 C26 118.0(2) . . ? C30 N3 Ru1 125.91(19) . . ? C26 N3 Ru1 115.67(19) . . ? C31 N4 C45 117.8(2) . . ? C31 N4 Ru1 108.34(17) . . ? C45 N4 Ru1 133.68(18) . . ? O1 C1 C2 124.1(2) . . ? O1 C1 C6 116.9(2) . . ? C2 C1 C6 118.9(3) . . ? C3 C2 C1 117.0(2) . . ? C3 C2 C11 122.1(3) . . ? C1 C2 C11 120.9(3) . . ? C2 C3 C4 124.6(3) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C7 120.5(2) . . ? C3 C4 C7 121.7(2) . . ? C4 C5 C6 120.3(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? N1 C6 C5 125.6(2) . . ? N1 C6 C1 113.2(2) . . ? C5 C6 C1 121.2(3) . . ? C9 C7 C10 107.5(3) . . ? C9 C7 C4 113.0(2) . . ? C10 C7 C4 108.8(3) . . ? C9 C7 C8 108.7(3) . . ? C10 C7 C8 110.2(3) . . ? C4 C7 C8 108.6(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 107.5(2) . . ? C13 C11 C14 109.6(3) . . ? C12 C11 C14 108.0(3) . . ? C13 C11 C2 110.6(2) . . ? C12 C11 C2 112.2(2) . . ? C14 C11 C2 108.9(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 120.1(3) . . ? C16 C15 N1 120.0(3) . . ? C20 C15 N1 119.7(3) . . ? C15 C16 C17 119.4(3) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 121.2(3) . . ? C18 C17 Cl1 119.2(2) . . ? C16 C17 Cl1 119.6(3) . . ? C19 C18 C17 118.4(3) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 Cl2 119.3(2) . . ? C20 C19 Cl2 119.1(3) . . ? C19 C20 C15 119.4(3) . . ? C19 C20 H20 120.3 . . ? C15 C20 H20 120.3 . . ? N2 C21 C22 122.4(3) . . ? N2 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 118.1(3) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N2 C25 C24 120.7(3) . . ? N2 C25 C26 113.7(2) . . ? C24 C25 C26 125.6(2) . . ? N3 C26 C27 121.3(3) . . ? N3 C26 C25 115.2(2) . . ? C27 C26 C25 123.5(3) . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 118.8(3) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N3 C30 C29 122.5(3) . . ? N3 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N4 C31 C32 124.7(3) . . ? N4 C31 C36 114.5(2) . . ? C32 C31 C36 120.8(3) . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 117.9(3) . . ? C32 C33 C41 122.7(3) . . ? C34 C33 C41 119.4(3) . . ? C35 C34 C33 124.2(3) . . ? C35 C34 H34 117.9 . . ? C33 C34 H34 117.9 . . ? C34 C35 C36 117.1(3) . . ? C34 C35 C37 122.0(3) . . ? C36 C35 C37 120.8(2) . . ? O2 C36 C35 124.0(2) . . ? O2 C36 C31 116.8(2) . . ? C35 C36 C31 119.2(2) . . ? C40 C37 C39 111.4(2) . . ? C40 C37 C35 109.3(2) . . ? C39 C37 C35 109.9(2) . . ? C40 C37 C38 107.5(2) . . ? C39 C37 C38 107.0(2) . . ? C35 C37 C38 111.9(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C44 109.7(4) . . ? C42 C41 C43 110.2(3) . . ? C44 C41 C43 105.9(3) . . ? C42 C41 C33 111.7(3) . . ? C44 C41 C33 110.3(3) . . ? C43 C41 C33 108.8(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 117.4(3) . . ? C50 C45 N4 122.3(3) . . ? C46 C45 N4 120.4(3) . . ? C47 C46 C45 120.0(3) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 122.5(3) . . ? C48 C47 Cl3 118.9(2) . . ? C46 C47 Cl3 118.5(3) . . ? C47 C48 C49 117.4(3) . . ? C47 C48 H48 121.3 . . ? C49 C48 H48 121.3 . . ? C50 C49 C48 121.3(3) . . ? C50 C49 Cl4 119.2(2) . . ? C48 C49 Cl4 119.5(2) . . ? C49 C50 C45 121.4(3) . . ? C49 C50 H50 119.3 . . ? C45 C50 H50 119.3 . . ? 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 Ru1 O1 C1 19.05(18) . . . . ? N4 Ru1 O1 C1 -81.27(18) . . . . ? O2 Ru1 O1 C1 -161.85(18) . . . . ? N2 Ru1 O1 C1 108.10(18) . . . . ? N3 Ru1 O1 C1 71.1(5) . . . . ? N1 Ru1 O2 C36 61.6(5) . . . . ? N4 Ru1 O2 C36 -29.83(17) . . . . ? O1 Ru1 O2 C36 57.06(17) . . . . ? N2 Ru1 O2 C36 151.25(18) . . . . ? N3 Ru1 O2 C36 -130.82(17) . . . . ? N4 Ru1 N1 C6 67.02(19) . . . . ? O1 Ru1 N1 C6 -17.90(18) . . . . ? O2 Ru1 N1 C6 -22.5(5) . . . . ? N2 Ru1 N1 C6 -112.19(19) . . . . ? N3 Ru1 N1 C6 169.83(19) . . . . ? N4 Ru1 N1 C15 -119.0(2) . . . . ? O1 Ru1 N1 C15 156.1(2) . . . . ? O2 Ru1 N1 C15 151.5(4) . . . . ? N2 Ru1 N1 C15 61.8(2) . . . . ? N3 Ru1 N1 C15 -16.2(2) . . . . ? N1 Ru1 N2 C21 88.2(2) . . . . ? N4 Ru1 N2 C21 -87.0(6) . . . . ? O1 Ru1 N2 C21 7.6(2) . . . . ? O2 Ru1 N2 C21 -80.5(2) . . . . ? N3 Ru1 N2 C21 -178.4(2) . . . . ? N1 Ru1 N2 C25 -90.3(2) . . . . ? N4 Ru1 N2 C25 94.5(6) . . . . ? O1 Ru1 N2 C25 -170.9(2) . . . . ? O2 Ru1 N2 C25 101.0(2) . . . . ? N3 Ru1 N2 C25 3.1(2) . . . . ? N1 Ru1 N3 C30 -88.8(2) . . . . ? N4 Ru1 N3 C30 11.8(3) . . . . ? O1 Ru1 N3 C30 -140.0(4) . . . . ? O2 Ru1 N3 C30 93.7(2) . . . . ? N2 Ru1 N3 C30 -177.8(3) . . . . ? N1 Ru1 N3 C26 83.5(2) . . . . ? N4 Ru1 N3 C26 -175.95(19) . . . . ? O1 Ru1 N3 C26 32.3(6) . . . . ? O2 Ru1 N3 C26 -94.1(2) . . . . ? N2 Ru1 N3 C26 -5.54(19) . . . . ? N1 Ru1 N4 C31 -140.66(18) . . . . ? O1 Ru1 N4 C31 -60.78(18) . . . . ? O2 Ru1 N4 C31 27.88(17) . . . . ? N2 Ru1 N4 C31 34.5(6) . . . . ? N3 Ru1 N4 C31 123.84(18) . . . . ? N1 Ru1 N4 C45 44.5(3) . . . . ? O1 Ru1 N4 C45 124.3(3) . . . . ? O2 Ru1 N4 C45 -147.0(3) . . . . ? N2 Ru1 N4 C45 -140.4(5) . . . . ? N3 Ru1 N4 C45 -51.0(3) . . . . ? Ru1 O1 C1 C2 166.9(2) . . . . ? Ru1 O1 C1 C6 -17.0(3) . . . . ? O1 C1 C2 C3 -179.3(3) . . . . ? C6 C1 C2 C3 4.6(4) . . . . ? O1 C1 C2 C11 0.4(4) . . . . ? C6 C1 C2 C11 -175.6(3) . . . . ? C1 C2 C3 C4 -2.2(4) . . . . ? C11 C2 C3 C4 178.1(3) . . . . ? C2 C3 C4 C5 -2.0(4) . . . . ? C2 C3 C4 C7 174.6(3) . . . . ? C3 C4 C5 C6 3.7(4) . . . . ? C7 C4 C5 C6 -173.1(3) . . . . ? C15 N1 C6 C5 21.6(4) . . . . ? Ru1 N1 C6 C5 -164.1(2) . . . . ? C15 N1 C6 C1 -160.3(3) . . . . ? Ru1 N1 C6 C1 14.1(3) . . . . ? C4 C5 C6 N1 176.8(3) . . . . ? C4 C5 C6 C1 -1.2(4) . . . . ? O1 C1 C6 N1 2.3(4) . . . . ? C2 C1 C6 N1 178.7(2) . . . . ? O1 C1 C6 C5 -179.5(3) . . . . ? C2 C1 C6 C5 -3.1(4) . . . . ? C5 C4 C7 C9 -179.4(3) . . . . ? C3 C4 C7 C9 4.0(4) . . . . ? C5 C4 C7 C10 61.3(3) . . . . ? C3 C4 C7 C10 -115.3(3) . . . . ? C5 C4 C7 C8 -58.7(4) . . . . ? C3 C4 C7 C8 124.7(3) . . . . ? C3 C2 C11 C13 122.1(3) . . . . ? C1 C2 C11 C13 -57.6(3) . . . . ? C3 C2 C11 C12 2.2(4) . . . . ? C1 C2 C11 C12 -177.6(3) . . . . ? C3 C2 C11 C14 -117.3(3) . . . . ? C1 C2 C11 C14 62.9(4) . . . . ? C6 N1 C15 C16 84.3(3) . . . . ? Ru1 N1 C15 C16 -89.3(3) . . . . ? C6 N1 C15 C20 -101.4(3) . . . . ? Ru1 N1 C15 C20 85.0(3) . . . . ? C20 C15 C16 C17 -2.6(4) . . . . ? N1 C15 C16 C17 171.7(3) . . . . ? C15 C16 C17 C18 3.0(5) . . . . ? C15 C16 C17 Cl1 -176.0(2) . . . . ? C16 C17 C18 C19 -1.7(5) . . . . ? Cl1 C17 C18 C19 177.3(3) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C17 C18 C19 Cl2 -178.8(2) . . . . ? C18 C19 C20 C15 0.4(5) . . . . ? Cl2 C19 C20 C15 179.2(2) . . . . ? C16 C15 C20 C19 0.9(4) . . . . ? N1 C15 C20 C19 -173.4(3) . . . . ? C25 N2 C21 C22 1.2(4) . . . . ? Ru1 N2 C21 C22 -177.3(2) . . . . ? N2 C21 C22 C23 -1.0(5) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C25 1.1(5) . . . . ? C21 N2 C25 C24 -0.3(4) . . . . ? Ru1 N2 C25 C24 178.3(2) . . . . ? C21 N2 C25 C26 -178.9(3) . . . . ? Ru1 N2 C25 C26 -0.3(3) . . . . ? C23 C24 C25 N2 -0.8(5) . . . . ? C23 C24 C25 C26 177.6(3) . . . . ? C30 N3 C26 C27 0.8(4) . . . . ? Ru1 N3 C26 C27 -172.1(2) . . . . ? C30 N3 C26 C25 180.0(3) . . . . ? Ru1 N3 C26 C25 7.1(3) . . . . ? N2 C25 C26 N3 -4.4(4) . . . . ? C24 C25 C26 N3 177.0(3) . . . . ? N2 C25 C26 C27 174.8(3) . . . . ? C24 C25 C26 C27 -3.8(5) . . . . ? N3 C26 C27 C28 1.0(5) . . . . ? C25 C26 C27 C28 -178.1(3) . . . . ? C26 C27 C28 C29 -1.7(5) . . . . ? C27 C28 C29 C30 0.5(5) . . . . ? C26 N3 C30 C29 -2.0(4) . . . . ? Ru1 N3 C30 C29 170.1(2) . . . . ? C28 C29 C30 N3 1.4(5) . . . . ? C45 N4 C31 C32 -28.8(4) . . . . ? Ru1 N4 C31 C32 155.3(2) . . . . ? C45 N4 C31 C36 153.9(3) . . . . ? Ru1 N4 C31 C36 -21.9(3) . . . . ? N4 C31 C32 C33 -176.8(3) . . . . ? C36 C31 C32 C33 0.3(5) . . . . ? C31 C32 C33 C34 -1.0(5) . . . . ? C31 C32 C33 C41 177.2(3) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? C41 C33 C34 C35 -177.6(3) . . . . ? C33 C34 C35 C36 0.4(4) . . . . ? C33 C34 C35 C37 179.9(3) . . . . ? Ru1 O2 C36 C35 -155.1(2) . . . . ? Ru1 O2 C36 C31 26.4(3) . . . . ? C34 C35 C36 O2 -179.5(3) . . . . ? C37 C35 C36 O2 1.0(4) . . . . ? C34 C35 C36 C31 -1.1(4) . . . . ? C37 C35 C36 C31 179.4(3) . . . . ? N4 C31 C36 O2 -3.3(4) . . . . ? C32 C31 C36 O2 179.3(3) . . . . ? N4 C31 C36 C35 178.1(2) . . . . ? C32 C31 C36 C35 0.7(4) . . . . ? C34 C35 C37 C40 -120.5(3) . . . . ? C36 C35 C37 C40 58.9(3) . . . . ? C34 C35 C37 C39 117.0(3) . . . . ? C36 C35 C37 C39 -63.5(3) . . . . ? C34 C35 C37 C38 -1.6(4) . . . . ? C36 C35 C37 C38 177.9(3) . . . . ? C32 C33 C41 C42 3.4(5) . . . . ? C34 C33 C41 C42 -178.5(4) . . . . ? C32 C33 C41 C44 125.7(3) . . . . ? C34 C33 C41 C44 -56.2(4) . . . . ? C32 C33 C41 C43 -118.5(3) . . . . ? C34 C33 C41 C43 59.6(4) . . . . ? C31 N4 C45 C50 -41.0(4) . . . . ? Ru1 N4 C45 C50 133.5(2) . . . . ? C31 N4 C45 C46 138.7(3) . . . . ? Ru1 N4 C45 C46 -46.8(4) . . . . ? C50 C45 C46 C47 -0.5(4) . . . . ? N4 C45 C46 C47 179.7(3) . . . . ? C45 C46 C47 C48 0.6(5) . . . . ? C45 C46 C47 Cl3 178.7(2) . . . . ? C46 C47 C48 C49 0.3(5) . . . . ? Cl3 C47 C48 C49 -177.8(2) . . . . ? C47 C48 C49 C50 -1.2(4) . . . . ? C47 C48 C49 Cl4 179.5(2) . . . . ? C48 C49 C50 C45 1.3(5) . . . . ? Cl4 C49 C50 C45 -179.4(2) . . . . ? C46 C45 C50 C49 -0.3(4) . . . . ? N4 C45 C50 C49 179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.062 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 821455' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 N4 O6 Ru' _chemical_formula_weight 968.18 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' 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 10.1872(3) _cell_length_b 15.1077(5) _cell_length_c 17.2960(4) _cell_angle_alpha 78.698(2) _cell_angle_beta 82.659(2) _cell_angle_gamma 71.615(3) _cell_volume 2470.86(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13180 _cell_measurement_theta_min 3.3013 _cell_measurement_theta_max 32.8051 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_T_min 0.9066 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19025 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8681 _reflns_number_gt 7219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8681 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.62972(2) 0.248312(18) 0.264727(15) 0.01198(9) Uani 1 1 d . . . O1 O 0.5483(2) 0.28994(15) 0.15910(12) 0.0158(5) Uani 1 1 d . . . O2 O 0.7107(2) 0.12103(15) 0.22950(12) 0.0135(4) Uani 1 1 d . . . O3 O 0.6931(3) 0.4511(2) 0.49992(17) 0.0468(8) Uani 1 1 d . . . O4 O 0.6410(3) 0.67252(19) 0.26089(16) 0.0363(7) Uani 1 1 d . . . O5 O 0.2920(3) 0.05967(17) 0.55137(14) 0.0270(6) Uani 1 1 d . . . O6 O 0.1340(3) 0.39229(17) 0.47076(14) 0.0282(6) Uani 1 1 d . . . N1 N 0.5357(2) 0.38417(18) 0.27118(15) 0.0143(5) Uani 1 1 d . . . N2 N 0.8111(3) 0.28360(19) 0.22699(16) 0.0170(6) Uani 1 1 d . . . N3 N 0.7414(3) 0.20049(19) 0.36493(16) 0.0170(6) Uani 1 1 d . . . N4 N 0.4743(2) 0.19357(18) 0.30423(15) 0.0141(5) Uani 1 1 d . . . C1 C 0.4468(3) 0.3699(2) 0.15632(18) 0.0142(6) Uani 1 1 d . . . C2 C 0.3557(3) 0.4068(2) 0.09361(18) 0.0152(7) Uani 1 1 d . . . C3 C 0.2531(3) 0.4913(2) 0.09936(19) 0.0178(7) Uani 1 1 d . . . H3 H 0.1903 0.5158 0.0588 0.021 Uiso 1 1 calc R . . C4 C 0.2349(3) 0.5434(2) 0.16084(19) 0.0170(7) Uani 1 1 d . . . C5 C 0.3291(3) 0.5102(2) 0.21808(19) 0.0161(7) Uani 1 1 d . . . H5 H 0.3224 0.5455 0.2590 0.019 Uiso 1 1 calc R . . C6 C 0.4352(3) 0.4241(2) 0.21616(18) 0.0154(7) Uani 1 1 d . . . C7 C 0.1122(3) 0.6339(2) 0.1634(2) 0.0227(7) Uani 1 1 d . . . C8 C 0.1156(4) 0.6831(3) 0.2324(2) 0.0326(9) Uani 1 1 d . . . H8A H 0.2014 0.7009 0.2267 0.049 Uiso 1 1 calc R . . H8B H 0.1120 0.6400 0.2824 0.049 Uiso 1 1 calc R . . H8C H 0.0356 0.7400 0.2322 0.049 Uiso 1 1 calc R . . C9 C 0.1140(4) 0.7038(3) 0.0867(2) 0.0393(10) Uani 1 1 d . . . H9A H 0.1987 0.7228 0.0808 0.059 Uiso 1 1 calc R . . H9B H 0.0328 0.7597 0.0881 0.059 Uiso 1 1 calc R . . H9C H 0.1115 0.6736 0.0418 0.059 Uiso 1 1 calc R . . C10 C -0.0230(4) 0.6071(3) 0.1741(3) 0.0373(10) Uani 1 1 d . . . H10A H -0.1023 0.6644 0.1733 0.056 Uiso 1 1 calc R . . H10B H -0.0266 0.5652 0.2248 0.056 Uiso 1 1 calc R . . H10C H -0.0265 0.5744 0.1310 0.056 Uiso 1 1 calc R . . C11 C 0.3756(3) 0.3529(2) 0.02427(19) 0.0188(7) Uani 1 1 d . . . C12 C 0.5207(3) 0.3443(3) -0.0175(2) 0.0270(8) Uani 1 1 d . . . H12A H 0.5284 0.4076 -0.0393 0.041 Uiso 1 1 calc R . . H12B H 0.5349 0.3078 -0.0605 0.041 Uiso 1 1 calc R . . H12C H 0.5912 0.3122 0.0205 0.041 Uiso 1 1 calc R . . C13 C 0.2706(4) 0.4050(3) -0.0377(2) 0.0284(8) Uani 1 1 d . . . H13A H 0.1765 0.4109 -0.0136 0.043 Uiso 1 1 calc R . . H13B H 0.2879 0.3694 -0.0815 0.043 Uiso 1 1 calc R . . H13C H 0.2802 0.4682 -0.0577 0.043 Uiso 1 1 calc R . . C14 C 0.3591(4) 0.2538(3) 0.0531(2) 0.0258(8) Uani 1 1 d . . . H14A H 0.4231 0.2197 0.0942 0.039 Uiso 1 1 calc R . . H14B H 0.3800 0.2189 0.0086 0.039 Uiso 1 1 calc R . . H14C H 0.2636 0.2597 0.0747 0.039 Uiso 1 1 calc R . . C15 C 0.5795(3) 0.4442(2) 0.30833(19) 0.0164(7) Uani 1 1 d . . . C16 C 0.6119(3) 0.4147(2) 0.3877(2) 0.0224(7) Uani 1 1 d . . . H16 H 0.6017 0.3565 0.4163 0.027 Uiso 1 1 calc R . . C17 C 0.6590(4) 0.4725(3) 0.4230(2) 0.0298(9) Uani 1 1 d . . . C18 C 0.6728(4) 0.5585(3) 0.3828(2) 0.0322(9) Uani 1 1 d . . . H18 H 0.7060 0.5968 0.4083 0.039 Uiso 1 1 calc R . . C19 C 0.6377(4) 0.5876(3) 0.3058(2) 0.0253(8) Uani 1 1 d . . . C20 C 0.5929(3) 0.5304(2) 0.2673(2) 0.0214(7) Uani 1 1 d . . . H20 H 0.5717 0.5501 0.2135 0.026 Uiso 1 1 calc R . . C21 C 0.8367(3) 0.3279(2) 0.1539(2) 0.0235(8) Uani 1 1 d . . . H21 H 0.7738 0.3379 0.1148 0.028 Uiso 1 1 calc R . . C22 C 0.9515(4) 0.3593(3) 0.1341(2) 0.0345(9) Uani 1 1 d . . . H22 H 0.9673 0.3905 0.0821 0.041 Uiso 1 1 calc R . . C23 C 1.0441(4) 0.3449(3) 0.1910(3) 0.0364(10) Uani 1 1 d . . . H23 H 1.1227 0.3674 0.1788 0.044 Uiso 1 1 calc R . . C24 C 1.0201(4) 0.2976(3) 0.2651(2) 0.0305(9) Uani 1 1 d . . . H24 H 1.0831 0.2861 0.3045 0.037 Uiso 1 1 calc R . . C25 C 0.9034(3) 0.2669(2) 0.2819(2) 0.0200(7) Uani 1 1 d . . . C26 C 0.8685(3) 0.2140(2) 0.3575(2) 0.0203(7) Uani 1 1 d . . . C27 C 0.9592(4) 0.1765(3) 0.4172(2) 0.0304(9) Uani 1 1 d . . . H27 H 1.0475 0.1868 0.4109 0.037 Uiso 1 1 calc R . . C28 C 0.9205(4) 0.1243(3) 0.4854(2) 0.0368(10) Uani 1 1 d . . . H28 H 0.9814 0.0983 0.5269 0.044 Uiso 1 1 calc R . . C29 C 0.7922(4) 0.1100(3) 0.4931(2) 0.0321(9) Uani 1 1 d . . . H29 H 0.7640 0.0732 0.5395 0.039 Uiso 1 1 calc R . . C30 C 0.7055(4) 0.1496(2) 0.4327(2) 0.0226(7) Uani 1 1 d . . . H30 H 0.6163 0.1406 0.4390 0.027 Uiso 1 1 calc R . . C31 C 0.4787(3) 0.1237(2) 0.26221(18) 0.0142(6) Uani 1 1 d . . . C32 C 0.3697(3) 0.0863(2) 0.25994(19) 0.0185(7) Uani 1 1 d . . . H32 H 0.2856 0.1073 0.2911 0.022 Uiso 1 1 calc R . . C33 C 0.3830(3) 0.0197(2) 0.2134(2) 0.0209(7) Uani 1 1 d . . . C34 C 0.5088(3) -0.0099(2) 0.16724(19) 0.0202(7) Uani 1 1 d . . . H34 H 0.5173 -0.0551 0.1343 0.024 Uiso 1 1 calc R . . C35 C 0.6208(3) 0.0238(2) 0.16766(18) 0.0160(7) Uani 1 1 d . . . C36 C 0.6069(3) 0.0903(2) 0.21732(18) 0.0131(6) Uani 1 1 d . . . C37 C 0.7541(3) -0.0077(2) 0.11524(19) 0.0184(7) Uani 1 1 d . . . C38 C 0.8755(3) -0.0600(3) 0.1675(2) 0.0239(8) Uani 1 1 d . . . H38A H 0.8843 -0.0184 0.2022 0.036 Uiso 1 1 calc R . . H38B H 0.9615 -0.0783 0.1340 0.036 Uiso 1 1 calc R . . H38C H 0.8582 -0.1168 0.1997 0.036 Uiso 1 1 calc R . . C39 C 0.7842(4) 0.0788(3) 0.0617(2) 0.0268(8) Uani 1 1 d . . . H39A H 0.7061 0.1126 0.0290 0.040 Uiso 1 1 calc R . . H39B H 0.8687 0.0579 0.0276 0.040 Uiso 1 1 calc R . . H39C H 0.7970 0.1211 0.0945 0.040 Uiso 1 1 calc R . . C40 C 0.7450(4) -0.0754(3) 0.0620(2) 0.0272(8) Uani 1 1 d . . . H40A H 0.7319 -0.1331 0.0948 0.041 Uiso 1 1 calc R . . H40B H 0.8308 -0.0917 0.0280 0.041 Uiso 1 1 calc R . . H40C H 0.6663 -0.0447 0.0290 0.041 Uiso 1 1 calc R . . C41 C 0.2590(4) -0.0150(3) 0.2068(2) 0.0294(9) Uani 1 1 d . . . C42 C 0.1461(4) 0.0703(3) 0.1633(3) 0.0411(10) Uani 1 1 d . . . H42A H 0.1867 0.0949 0.1124 0.062 Uiso 1 1 calc R . . H42B H 0.1126 0.1204 0.1959 0.062 Uiso 1 1 calc R . . H42C H 0.0686 0.0491 0.1545 0.062 Uiso 1 1 calc R . . C43 C 0.2945(4) -0.0941(3) 0.1592(3) 0.0403(10) Uani 1 1 d . . . H43A H 0.3662 -0.1485 0.1844 0.060 Uiso 1 1 calc R . . H43B H 0.3290 -0.0727 0.1056 0.060 Uiso 1 1 calc R . . H43C H 0.2114 -0.1127 0.1568 0.060 Uiso 1 1 calc R . . C44 C 0.1967(5) -0.0456(4) 0.2879(2) 0.0485(12) Uani 1 1 d . . . H44A H 0.1149 -0.0642 0.2825 0.073 Uiso 1 1 calc R . . H44B H 0.1696 0.0070 0.3178 0.073 Uiso 1 1 calc R . . H44C H 0.2654 -0.0995 0.3160 0.073 Uiso 1 1 calc R . . C45 C 0.3824(3) 0.2051(2) 0.37295(18) 0.0144(7) Uani 1 1 d . . . C46 C 0.3755(3) 0.1265(2) 0.42942(19) 0.0180(7) Uani 1 1 d . . . H46 H 0.4271 0.0644 0.4207 0.022 Uiso 1 1 calc R . . C47 C 0.2907(3) 0.1410(2) 0.49934(19) 0.0185(7) Uani 1 1 d . . . C48 C 0.2134(3) 0.2303(2) 0.51216(19) 0.0191(7) Uani 1 1 d . . . H48 H 0.1574 0.2393 0.5600 0.023 Uiso 1 1 calc R . . C49 C 0.2186(3) 0.3075(2) 0.45396(19) 0.0183(7) Uani 1 1 d . . . C50 C 0.3052(3) 0.2954(2) 0.38570(19) 0.0180(7) Uani 1 1 d . . . H50 H 0.3117 0.3488 0.3477 0.022 Uiso 1 1 calc R . . C51 C 0.6866(5) 0.3628(3) 0.5439(2) 0.0488(12) Uani 1 1 d . . . H51A H 0.5923 0.3585 0.5450 0.073 Uiso 1 1 calc R . . H51B H 0.7110 0.3572 0.5980 0.073 Uiso 1 1 calc R . . H51C H 0.7520 0.3115 0.5190 0.073 Uiso 1 1 calc R . . C52 C 0.6736(5) 0.7372(3) 0.2989(3) 0.0499(12) Uani 1 1 d . . . H52A H 0.6072 0.7509 0.3445 0.075 Uiso 1 1 calc R . . H52B H 0.6686 0.7959 0.2617 0.075 Uiso 1 1 calc R . . H52C H 0.7676 0.7094 0.3169 0.075 Uiso 1 1 calc R . . C53 C 0.2267(4) 0.0690(3) 0.6287(2) 0.0285(8) Uani 1 1 d . . . H53A H 0.2695 0.1047 0.6539 0.043 Uiso 1 1 calc R . . H53B H 0.2379 0.0061 0.6604 0.043 Uiso 1 1 calc R . . H53C H 0.1277 0.1027 0.6248 0.043 Uiso 1 1 calc R . . C54 C 0.1219(4) 0.4725(3) 0.4095(2) 0.0311(9) Uani 1 1 d . . . H54A H 0.2131 0.4822 0.3950 0.047 Uiso 1 1 calc R . . H54B H 0.0575 0.5287 0.4283 0.047 Uiso 1 1 calc R . . H54C H 0.0867 0.4615 0.3632 0.047 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 0.00951(14) 0.01174(15) 0.01369(15) 0.00142(9) -0.00527(9) -0.00214(10) O1 0.0145(11) 0.0150(12) 0.0167(12) 0.0010(9) -0.0068(8) -0.0026(10) O2 0.0108(10) 0.0129(11) 0.0157(12) 0.0000(9) -0.0050(8) -0.0018(9) O3 0.075(2) 0.0392(18) 0.0302(16) -0.0056(13) -0.0290(15) -0.0134(16) O4 0.0493(17) 0.0266(15) 0.0426(17) -0.0053(12) -0.0050(13) -0.0243(14) O5 0.0359(14) 0.0217(14) 0.0191(13) 0.0021(10) 0.0031(10) -0.0079(11) O6 0.0359(14) 0.0192(14) 0.0214(14) -0.0024(10) 0.0059(10) -0.0005(11) N1 0.0129(13) 0.0108(14) 0.0169(14) 0.0013(11) -0.0054(10) -0.0009(11) N2 0.0106(13) 0.0142(14) 0.0256(16) -0.0019(12) -0.0044(10) -0.0023(11) N3 0.0161(14) 0.0132(14) 0.0209(15) -0.0014(11) -0.0073(11) -0.0020(12) N4 0.0122(13) 0.0154(14) 0.0149(14) -0.0016(11) -0.0029(10) -0.0041(11) C1 0.0111(15) 0.0129(17) 0.0172(17) 0.0031(12) -0.0016(11) -0.0045(13) C2 0.0139(15) 0.0132(17) 0.0181(17) 0.0029(13) -0.0020(12) -0.0067(13) C3 0.0116(15) 0.0169(18) 0.0217(18) 0.0057(13) -0.0076(12) -0.0028(14) C4 0.0137(15) 0.0127(17) 0.0223(18) 0.0024(13) -0.0035(12) -0.0031(13) C5 0.0158(16) 0.0127(17) 0.0180(17) 0.0001(13) -0.0015(12) -0.0031(13) C6 0.0134(15) 0.0169(17) 0.0149(17) 0.0040(13) -0.0028(12) -0.0066(13) C7 0.0157(17) 0.0187(19) 0.028(2) -0.0003(15) -0.0057(13) 0.0025(14) C8 0.030(2) 0.021(2) 0.038(2) -0.0057(17) -0.0114(16) 0.0087(17) C9 0.040(2) 0.025(2) 0.034(2) 0.0038(18) -0.0031(17) 0.0106(18) C10 0.0146(18) 0.039(2) 0.054(3) -0.012(2) -0.0056(16) 0.0015(17) C11 0.0198(17) 0.0200(18) 0.0152(17) -0.0006(13) -0.0051(12) -0.0038(14) C12 0.0233(18) 0.034(2) 0.0200(19) -0.0031(16) -0.0011(14) -0.0051(17) C13 0.0290(19) 0.034(2) 0.0212(19) -0.0017(16) -0.0115(14) -0.0051(17) C14 0.0296(19) 0.025(2) 0.025(2) -0.0045(15) -0.0094(14) -0.0077(16) C15 0.0128(15) 0.0148(17) 0.0218(18) -0.0035(13) -0.0028(12) -0.0035(13) C16 0.0222(18) 0.0186(19) 0.0240(19) -0.0028(14) -0.0080(14) -0.0006(15) C17 0.032(2) 0.029(2) 0.025(2) -0.0073(16) -0.0138(15) 0.0007(17) C18 0.035(2) 0.030(2) 0.039(2) -0.0139(18) -0.0090(17) -0.0136(18) C19 0.0243(19) 0.0202(19) 0.033(2) -0.0060(15) -0.0018(15) -0.0086(16) C20 0.0193(17) 0.0229(19) 0.0228(19) -0.0037(14) -0.0046(13) -0.0062(15) C21 0.0184(17) 0.0187(19) 0.029(2) 0.0043(15) -0.0038(14) -0.0040(15) C22 0.028(2) 0.033(2) 0.039(2) 0.0046(18) 0.0044(16) -0.0133(18) C23 0.022(2) 0.036(2) 0.054(3) -0.006(2) 0.0016(17) -0.0153(18) C24 0.0181(18) 0.032(2) 0.046(2) -0.0085(18) -0.0088(15) -0.0100(17) C25 0.0138(16) 0.0203(19) 0.0265(19) -0.0059(14) -0.0043(13) -0.0036(14) C26 0.0173(17) 0.0165(18) 0.0268(19) -0.0059(14) -0.0058(13) -0.0017(14) C27 0.0227(19) 0.034(2) 0.036(2) -0.0059(18) -0.0168(15) -0.0053(17) C28 0.040(2) 0.030(2) 0.038(2) 0.0001(18) -0.0290(18) -0.0007(19) C29 0.044(2) 0.030(2) 0.022(2) 0.0067(16) -0.0174(16) -0.0116(19) C30 0.0266(18) 0.0198(19) 0.0220(19) 0.0025(14) -0.0098(14) -0.0081(15) C31 0.0155(16) 0.0130(16) 0.0126(16) 0.0035(12) -0.0052(11) -0.0039(13) C32 0.0148(16) 0.0216(19) 0.0194(18) -0.0035(14) -0.0002(12) -0.0063(14) C33 0.0209(17) 0.0232(19) 0.0215(18) -0.0030(14) -0.0048(13) -0.0097(15) C34 0.0244(18) 0.0169(18) 0.0197(18) -0.0029(14) -0.0057(13) -0.0051(15) C35 0.0160(16) 0.0155(17) 0.0142(17) 0.0031(13) -0.0063(12) -0.0028(14) C36 0.0133(15) 0.0113(16) 0.0133(16) 0.0051(12) -0.0065(11) -0.0038(13) C37 0.0169(16) 0.0184(18) 0.0177(17) -0.0034(14) -0.0027(12) -0.0014(14) C38 0.0163(17) 0.0213(19) 0.030(2) -0.0052(15) -0.0039(14) 0.0009(15) C39 0.0289(19) 0.027(2) 0.0219(19) -0.0039(15) 0.0035(14) -0.0063(16) C40 0.0260(19) 0.029(2) 0.027(2) -0.0120(16) -0.0010(14) -0.0042(16) C41 0.0248(19) 0.036(2) 0.035(2) -0.0093(17) -0.0025(15) -0.0176(18) C42 0.032(2) 0.049(3) 0.047(3) -0.007(2) -0.0120(18) -0.016(2) C43 0.038(2) 0.050(3) 0.047(3) -0.013(2) -0.0074(18) -0.029(2) C44 0.056(3) 0.074(4) 0.036(3) -0.005(2) -0.002(2) -0.051(3) C45 0.0123(15) 0.0174(17) 0.0148(16) -0.0036(13) -0.0052(11) -0.0044(13) C46 0.0169(16) 0.0137(17) 0.0217(18) -0.0025(14) -0.0035(13) -0.0015(14) C47 0.0192(17) 0.0204(18) 0.0174(17) 0.0023(13) -0.0057(12) -0.0097(15) C48 0.0194(17) 0.0240(19) 0.0144(17) -0.0032(14) -0.0007(12) -0.0074(15) C49 0.0179(16) 0.0161(18) 0.0201(18) -0.0021(13) -0.0060(12) -0.0027(14) C50 0.0174(16) 0.0207(18) 0.0163(17) -0.0010(13) -0.0016(12) -0.0074(14) C51 0.074(3) 0.042(3) 0.027(2) -0.003(2) -0.023(2) -0.007(2) C52 0.073(3) 0.041(3) 0.051(3) -0.016(2) 0.002(2) -0.037(3) C53 0.039(2) 0.029(2) 0.0166(18) 0.0033(15) -0.0017(15) -0.0130(18) C54 0.043(2) 0.0164(19) 0.024(2) -0.0021(15) -0.0008(16) 0.0037(17) _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 N1 1.991(3) . ? Ru1 N4 1.996(2) . ? Ru1 O1 2.007(2) . ? Ru1 O2 2.020(2) . ? Ru1 N2 2.073(2) . ? Ru1 N3 2.077(3) . ? O1 C1 1.317(4) . ? O2 C36 1.335(3) . ? O3 C17 1.369(4) . ? O3 C51 1.418(5) . ? O4 C19 1.371(4) . ? O4 C52 1.418(4) . ? O5 C47 1.371(4) . ? O5 C53 1.428(4) . ? O6 C49 1.361(4) . ? O6 C54 1.429(4) . ? N1 C6 1.397(4) . ? N1 C15 1.411(4) . ? N2 C21 1.345(4) . ? N2 C25 1.355(4) . ? N3 C30 1.346(4) . ? N3 C26 1.360(4) . ? N4 C31 1.381(4) . ? N4 C45 1.419(4) . ? C1 C6 1.412(4) . ? C1 C2 1.429(4) . ? C2 C3 1.384(5) . ? C2 C11 1.536(4) . ? C3 C4 1.404(5) . ? C3 H3 0.9500 . ? C4 C5 1.377(4) . ? C4 C7 1.538(5) . ? C5 C6 1.408(4) . ? C5 H5 0.9500 . ? C7 C9 1.527(5) . ? C7 C8 1.534(5) . ? C7 C10 1.534(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.531(4) . ? C11 C14 1.537(5) . ? C11 C12 1.538(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.394(5) . ? C15 C16 1.405(5) . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.389(5) . ? C18 C19 1.375(5) . ? C18 H18 0.9500 . ? C19 C20 1.397(5) . ? C20 H20 0.9500 . ? C21 C22 1.376(5) . ? C21 H21 0.9500 . ? C22 C23 1.389(6) . ? C22 H22 0.9500 . ? C23 C24 1.372(6) . ? C23 H23 0.9500 . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.458(5) . ? C26 C27 1.387(5) . ? C27 C28 1.372(6) . ? C27 H27 0.9500 . ? C28 C29 1.376(6) . ? C28 H28 0.9500 . ? C29 C30 1.374(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.404(4) . ? C31 C36 1.429(4) . ? C32 C33 1.371(5) . ? C32 H32 0.9500 . ? C33 C34 1.414(5) . ? C33 C41 1.537(4) . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.409(4) . ? C35 C37 1.530(4) . ? C37 C40 1.536(4) . ? C37 C38 1.536(4) . ? C37 C39 1.537(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.508(5) . ? C41 C44 1.513(5) . ? C41 C42 1.567(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.388(5) . ? C45 C46 1.396(4) . ? C46 C47 1.405(4) . ? C46 H46 0.9500 . ? C47 C48 1.376(5) . ? C48 C49 1.393(5) . ? C48 H48 0.9500 . ? C49 C50 1.387(4) . ? C50 H50 0.9500 . ? 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 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 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 N1 Ru1 N4 100.57(10) . . ? N1 Ru1 O1 80.71(9) . . ? N4 Ru1 O1 88.22(9) . . ? N1 Ru1 O2 165.33(9) . . ? N4 Ru1 O2 80.73(9) . . ? O1 Ru1 O2 84.74(8) . . ? N1 Ru1 N2 88.03(10) . . ? N4 Ru1 N2 171.05(10) . . ? O1 Ru1 N2 95.67(10) . . ? O2 Ru1 N2 91.58(9) . . ? N1 Ru1 N3 103.12(10) . . ? N4 Ru1 N3 98.10(10) . . ? O1 Ru1 N3 171.79(9) . . ? O2 Ru1 N3 91.08(9) . . ? N2 Ru1 N3 77.35(10) . . ? C1 O1 Ru1 112.06(18) . . ? C36 O2 Ru1 108.68(18) . . ? C17 O3 C51 117.8(3) . . ? C19 O4 C52 117.1(3) . . ? C47 O5 C53 117.6(3) . . ? C49 O6 C54 117.1(3) . . ? C6 N1 C15 119.2(3) . . ? C6 N1 Ru1 111.1(2) . . ? C15 N1 Ru1 127.9(2) . . ? C21 N2 C25 118.8(3) . . ? C21 N2 Ru1 124.1(2) . . ? C25 N2 Ru1 116.9(2) . . ? C30 N3 C26 117.7(3) . . ? C30 N3 Ru1 125.9(2) . . ? C26 N3 Ru1 116.0(2) . . ? C31 N4 C45 119.1(2) . . ? C31 N4 Ru1 110.12(19) . . ? C45 N4 Ru1 129.89(19) . . ? O1 C1 C6 117.2(3) . . ? O1 C1 C2 123.4(3) . . ? C6 C1 C2 119.2(3) . . ? C3 C2 C1 116.7(3) . . ? C3 C2 C11 123.5(3) . . ? C1 C2 C11 119.8(3) . . ? C2 C3 C4 124.8(3) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C7 121.9(3) . . ? C3 C4 C7 120.2(3) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 124.8(3) . . ? N1 C6 C1 114.2(3) . . ? C5 C6 C1 121.0(3) . . ? C9 C7 C8 108.2(3) . . ? C9 C7 C10 109.5(3) . . ? C8 C7 C10 108.2(3) . . ? C9 C7 C4 110.4(3) . . ? C8 C7 C4 112.0(3) . . ? C10 C7 C4 108.5(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C2 111.8(3) . . ? C13 C11 C14 107.9(3) . . ? C2 C11 C14 111.0(3) . . ? C13 C11 C12 106.9(3) . . ? C2 C11 C12 109.4(3) . . ? C14 C11 C12 109.7(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 120.3(3) . . ? C20 C15 N1 121.1(3) . . ? C16 C15 N1 118.6(3) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? O3 C17 C16 123.4(4) . . ? O3 C17 C18 114.6(3) . . ? C16 C17 C18 122.0(3) . . ? C19 C18 C17 119.1(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? O4 C19 C18 124.8(3) . . ? O4 C19 C20 114.5(3) . . ? C18 C19 C20 120.7(3) . . ? C15 C20 C19 119.6(3) . . ? C15 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? N2 C21 C22 122.0(3) . . ? N2 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C23 119.3(4) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 119.0(3) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 119.6(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N2 C25 C24 121.4(3) . . ? N2 C25 C26 114.0(3) . . ? C24 C25 C26 124.7(3) . . ? N3 C26 C27 121.6(3) . . ? N3 C26 C25 115.2(3) . . ? C27 C26 C25 123.2(3) . . ? C28 C27 C26 119.5(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 119.2(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 119.1(4) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? N3 C30 C29 122.9(3) . . ? N3 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N4 C31 C32 125.6(3) . . ? N4 C31 C36 114.6(3) . . ? C32 C31 C36 119.8(3) . . ? C33 C32 C31 120.9(3) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 118.4(3) . . ? C32 C33 C41 120.2(3) . . ? C34 C33 C41 121.2(3) . . ? C35 C34 C33 123.3(3) . . ? C35 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? C34 C35 C36 117.6(3) . . ? C34 C35 C37 122.0(3) . . ? C36 C35 C37 120.4(3) . . ? O2 C36 C35 123.7(3) . . ? O2 C36 C31 116.3(3) . . ? C35 C36 C31 119.9(3) . . ? C35 C37 C40 112.2(3) . . ? C35 C37 C38 109.4(3) . . ? C40 C37 C38 107.5(3) . . ? C35 C37 C39 110.0(3) . . ? C40 C37 C39 107.9(3) . . ? C38 C37 C39 109.6(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 109.6(3) . . ? C43 C41 C33 113.4(3) . . ? C44 C41 C33 110.7(3) . . ? C43 C41 C42 107.3(3) . . ? C44 C41 C42 108.1(3) . . ? C33 C41 C42 107.6(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 120.2(3) . . ? C50 C45 N4 119.5(3) . . ? C46 C45 N4 120.2(3) . . ? C45 C46 C47 118.7(3) . . ? C45 C46 H46 120.7 . . ? C47 C46 H46 120.7 . . ? O5 C47 C48 124.3(3) . . ? O5 C47 C46 114.3(3) . . ? C48 C47 C46 121.4(3) . . ? C47 C48 C49 119.0(3) . . ? C47 C48 H48 120.5 . . ? C49 C48 H48 120.5 . . ? O6 C49 C50 124.7(3) . . ? O6 C49 C48 114.5(3) . . ? C50 C49 C48 120.7(3) . . ? C49 C50 C45 119.9(3) . . ? C49 C50 H50 120.1 . . ? C45 C50 H50 120.1 . . ? O3 C51 H51A 109.5 . . ? O3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O5 C53 H53A 109.5 . . ? O5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O6 C54 H54A 109.5 . . ? O6 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O6 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 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 Ru1 O1 C1 -18.80(19) . . . . ? N4 Ru1 O1 C1 82.22(19) . . . . ? O2 Ru1 O1 C1 163.07(19) . . . . ? N2 Ru1 O1 C1 -105.86(19) . . . . ? N3 Ru1 O1 C1 -137.3(6) . . . . ? N1 Ru1 O2 C36 -68.6(4) . . . . ? N4 Ru1 O2 C36 27.71(18) . . . . ? O1 Ru1 O2 C36 -61.33(18) . . . . ? N2 Ru1 O2 C36 -156.88(19) . . . . ? N3 Ru1 O2 C36 125.74(19) . . . . ? N4 Ru1 N1 C6 -68.0(2) . . . . ? O1 Ru1 N1 C6 18.45(19) . . . . ? O2 Ru1 N1 C6 25.8(5) . . . . ? N2 Ru1 N1 C6 114.5(2) . . . . ? N3 Ru1 N1 C6 -168.96(19) . . . . ? N4 Ru1 N1 C15 127.9(3) . . . . ? O1 Ru1 N1 C15 -145.7(3) . . . . ? O2 Ru1 N1 C15 -138.3(3) . . . . ? N2 Ru1 N1 C15 -49.6(3) . . . . ? N3 Ru1 N1 C15 26.9(3) . . . . ? N1 Ru1 N2 C21 -75.3(3) . . . . ? N4 Ru1 N2 C21 120.6(6) . . . . ? O1 Ru1 N2 C21 5.2(3) . . . . ? O2 Ru1 N2 C21 90.0(3) . . . . ? N3 Ru1 N2 C21 -179.2(3) . . . . ? N1 Ru1 N2 C25 99.5(2) . . . . ? N4 Ru1 N2 C25 -64.6(7) . . . . ? O1 Ru1 N2 C25 179.9(2) . . . . ? O2 Ru1 N2 C25 -95.2(2) . . . . ? N3 Ru1 N2 C25 -4.4(2) . . . . ? N1 Ru1 N3 C30 102.0(3) . . . . ? N4 Ru1 N3 C30 -0.9(3) . . . . ? O1 Ru1 N3 C30 -140.9(6) . . . . ? O2 Ru1 N3 C30 -81.7(3) . . . . ? N2 Ru1 N3 C30 -173.1(3) . . . . ? N1 Ru1 N3 C26 -85.2(2) . . . . ? N4 Ru1 N3 C26 171.9(2) . . . . ? O1 Ru1 N3 C26 31.9(8) . . . . ? O2 Ru1 N3 C26 91.1(2) . . . . ? N2 Ru1 N3 C26 -0.3(2) . . . . ? N1 Ru1 N4 C31 141.8(2) . . . . ? O1 Ru1 N4 C31 61.6(2) . . . . ? O2 Ru1 N4 C31 -23.37(19) . . . . ? N2 Ru1 N4 C31 -54.4(7) . . . . ? N3 Ru1 N4 C31 -113.1(2) . . . . ? N1 Ru1 N4 C45 -49.5(3) . . . . ? O1 Ru1 N4 C45 -129.7(3) . . . . ? O2 Ru1 N4 C45 145.3(3) . . . . ? N2 Ru1 N4 C45 114.3(7) . . . . ? N3 Ru1 N4 C45 55.5(3) . . . . ? Ru1 O1 C1 C6 15.6(3) . . . . ? Ru1 O1 C1 C2 -168.9(2) . . . . ? O1 C1 C2 C3 179.4(3) . . . . ? C6 C1 C2 C3 -5.1(4) . . . . ? O1 C1 C2 C11 -1.0(4) . . . . ? C6 C1 C2 C11 174.5(3) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C11 C2 C3 C4 -178.1(3) . . . . ? C2 C3 C4 C5 2.6(5) . . . . ? C2 C3 C4 C7 -176.8(3) . . . . ? C3 C4 C5 C6 -3.2(4) . . . . ? C7 C4 C5 C6 176.2(3) . . . . ? C15 N1 C6 C5 -30.5(4) . . . . ? Ru1 N1 C6 C5 163.9(2) . . . . ? C15 N1 C6 C1 150.0(3) . . . . ? Ru1 N1 C6 C1 -15.7(3) . . . . ? C4 C5 C6 N1 180.0(3) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? O1 C1 C6 N1 0.1(4) . . . . ? C2 C1 C6 N1 -175.7(3) . . . . ? O1 C1 C6 C5 -179.5(3) . . . . ? C2 C1 C6 C5 4.7(4) . . . . ? C5 C4 C7 C9 124.5(4) . . . . ? C3 C4 C7 C9 -56.1(4) . . . . ? C5 C4 C7 C8 3.8(4) . . . . ? C3 C4 C7 C8 -176.8(3) . . . . ? C5 C4 C7 C10 -115.5(3) . . . . ? C3 C4 C7 C10 63.8(4) . . . . ? C3 C2 C11 C13 1.1(4) . . . . ? C1 C2 C11 C13 -178.5(3) . . . . ? C3 C2 C11 C14 -119.4(3) . . . . ? C1 C2 C11 C14 61.0(4) . . . . ? C3 C2 C11 C12 119.4(3) . . . . ? C1 C2 C11 C12 -60.2(4) . . . . ? C6 N1 C15 C20 -36.8(4) . . . . ? Ru1 N1 C15 C20 126.2(3) . . . . ? C6 N1 C15 C16 144.3(3) . . . . ? Ru1 N1 C15 C16 -52.7(4) . . . . ? C20 C15 C16 C17 -1.0(5) . . . . ? N1 C15 C16 C17 178.0(3) . . . . ? C51 O3 C17 C16 3.5(6) . . . . ? C51 O3 C17 C18 -177.7(4) . . . . ? C15 C16 C17 O3 179.7(3) . . . . ? C15 C16 C17 C18 1.0(5) . . . . ? O3 C17 C18 C19 -178.4(3) . . . . ? C16 C17 C18 C19 0.4(6) . . . . ? C52 O4 C19 C18 -4.6(5) . . . . ? C52 O4 C19 C20 174.5(3) . . . . ? C17 C18 C19 O4 177.1(3) . . . . ? C17 C18 C19 C20 -2.0(5) . . . . ? C16 C15 C20 C19 -0.5(5) . . . . ? N1 C15 C20 C19 -179.4(3) . . . . ? O4 C19 C20 C15 -177.1(3) . . . . ? C18 C19 C20 C15 2.0(5) . . . . ? C25 N2 C21 C22 -2.1(5) . . . . ? Ru1 N2 C21 C22 172.6(3) . . . . ? N2 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 1.5(6) . . . . ? C22 C23 C24 C25 -1.1(6) . . . . ? C21 N2 C25 C24 2.5(5) . . . . ? Ru1 N2 C25 C24 -172.6(3) . . . . ? C21 N2 C25 C26 -176.9(3) . . . . ? Ru1 N2 C25 C26 8.1(4) . . . . ? C23 C24 C25 N2 -0.9(6) . . . . ? C23 C24 C25 C26 178.4(3) . . . . ? C30 N3 C26 C27 0.4(5) . . . . ? Ru1 N3 C26 C27 -173.0(3) . . . . ? C30 N3 C26 C25 178.0(3) . . . . ? Ru1 N3 C26 C25 4.6(4) . . . . ? N2 C25 C26 N3 -8.2(4) . . . . ? C24 C25 C26 N3 172.5(3) . . . . ? N2 C25 C26 C27 169.3(3) . . . . ? C24 C25 C26 C27 -10.0(6) . . . . ? N3 C26 C27 C28 0.1(6) . . . . ? C25 C26 C27 C28 -177.3(3) . . . . ? C26 C27 C28 C29 0.2(6) . . . . ? C27 C28 C29 C30 -1.0(6) . . . . ? C26 N3 C30 C29 -1.2(5) . . . . ? Ru1 N3 C30 C29 171.5(3) . . . . ? C28 C29 C30 N3 1.5(6) . . . . ? C45 N4 C31 C32 26.4(4) . . . . ? Ru1 N4 C31 C32 -163.5(3) . . . . ? C45 N4 C31 C36 -154.6(3) . . . . ? Ru1 N4 C31 C36 15.5(3) . . . . ? N4 C31 C32 C33 177.1(3) . . . . ? C36 C31 C32 C33 -1.8(5) . . . . ? C31 C32 C33 C34 -0.4(5) . . . . ? C31 C32 C33 C41 -175.4(3) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C41 C33 C34 C35 176.0(3) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C33 C34 C35 C37 -178.3(3) . . . . ? Ru1 O2 C36 C35 156.8(2) . . . . ? Ru1 O2 C36 C31 -27.4(3) . . . . ? C34 C35 C36 O2 172.9(3) . . . . ? C37 C35 C36 O2 -8.4(4) . . . . ? C34 C35 C36 C31 -2.7(4) . . . . ? C37 C35 C36 C31 176.0(3) . . . . ? N4 C31 C36 O2 8.4(4) . . . . ? C32 C31 C36 O2 -172.5(3) . . . . ? N4 C31 C36 C35 -175.6(3) . . . . ? C32 C31 C36 C35 3.5(4) . . . . ? C34 C35 C37 C40 2.3(4) . . . . ? C36 C35 C37 C40 -176.4(3) . . . . ? C34 C35 C37 C38 -117.0(3) . . . . ? C36 C35 C37 C38 64.4(4) . . . . ? C34 C35 C37 C39 122.5(3) . . . . ? C36 C35 C37 C39 -56.2(4) . . . . ? C32 C33 C41 C43 -174.9(3) . . . . ? C34 C33 C41 C43 10.4(5) . . . . ? C32 C33 C41 C44 -51.2(5) . . . . ? C34 C33 C41 C44 134.0(4) . . . . ? C32 C33 C41 C42 66.6(4) . . . . ? C34 C33 C41 C42 -108.1(4) . . . . ? C31 N4 C45 C50 -136.8(3) . . . . ? Ru1 N4 C45 C50 55.4(4) . . . . ? C31 N4 C45 C46 46.8(4) . . . . ? Ru1 N4 C45 C46 -121.0(3) . . . . ? C50 C45 C46 C47 -0.9(4) . . . . ? N4 C45 C46 C47 175.6(3) . . . . ? C53 O5 C47 C48 -10.4(4) . . . . ? C53 O5 C47 C46 170.2(3) . . . . ? C45 C46 C47 O5 -179.3(3) . . . . ? C45 C46 C47 C48 1.2(4) . . . . ? O5 C47 C48 C49 -178.7(3) . . . . ? C46 C47 C48 C49 0.8(5) . . . . ? C54 O6 C49 C50 7.8(5) . . . . ? C54 O6 C49 C48 -172.6(3) . . . . ? C47 C48 C49 O6 177.3(3) . . . . ? C47 C48 C49 C50 -3.1(5) . . . . ? O6 C49 C50 C45 -177.0(3) . . . . ? C48 C49 C50 C45 3.4(5) . . . . ? C46 C45 C50 C49 -1.4(4) . . . . ? N4 C45 C50 C49 -177.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.939 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.100 # Attachment '- [3](ClO4)2.cif' data_[3](ClO4)2 _database_code_depnum_ccdc_archive 'CCDC 821456' #TrackingRef '- [3](ClO4)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Cl2 N4 O14 Ru' _chemical_formula_weight 1167.08 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/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 24.2408(3) _cell_length_b 11.46730(10) _cell_length_c 20.0408(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.3590(10) _cell_angle_gamma 90.00 _cell_volume 5566.15(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16459 _cell_measurement_theta_min 3.2997 _cell_measurement_theta_max 32.7682 _exptl_crystal_description block _exptl_crystal_colour dark-blue _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_T_min 0.8671 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44303 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9789 _reflns_number_gt 6975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9789 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.221138(10) 0.21757(2) 0.069225(12) 0.01781(8) Uani 1 1 d . . . O1 O 0.29310(9) 0.23306(17) 0.01976(10) 0.0208(5) Uani 1 1 d . . . O2 O 0.16345(8) 0.19998(16) -0.00596(9) 0.0180(5) Uani 1 1 d . . . O3 O 0.24211(10) 0.3907(2) 0.36776(11) 0.0377(6) Uani 1 1 d . . . O4 O 0.22940(12) -0.0071(2) 0.32960(13) 0.0506(7) Uani 1 1 d . . . O5 O 0.29998(10) 0.6074(2) 0.20914(11) 0.0408(6) Uani 1 1 d . . . O6 O 0.34406(10) 0.6448(2) -0.02346(12) 0.0412(6) Uani 1 1 d . . . N1 N 0.27678(10) 0.2400(2) 0.14395(12) 0.0185(6) Uani 1 1 d . . . N2 N 0.22112(11) 0.0393(2) 0.07113(12) 0.0195(6) Uani 1 1 d . . . N3 N 0.15646(10) 0.1864(2) 0.12814(12) 0.0204(6) Uani 1 1 d . . . N4 N 0.20415(10) 0.3845(2) 0.04336(12) 0.0182(6) Uani 1 1 d . . . C1 C 0.33522(13) 0.2606(2) 0.05630(15) 0.0201(7) Uani 1 1 d . . . C2 C 0.38946(12) 0.2789(3) 0.03102(14) 0.0212(7) Uani 1 1 d . . . C3 C 0.42920(14) 0.3099(3) 0.07772(15) 0.0251(8) Uani 1 1 d . . . H3 H 0.4651 0.3248 0.0623 0.030 Uiso 1 1 calc R . . C4 C 0.42183(14) 0.3223(3) 0.14859(15) 0.0237(7) Uani 1 1 d . . . C5 C 0.37215(13) 0.2997(3) 0.17288(15) 0.0213(7) Uani 1 1 d . . . H5 H 0.3669 0.3040 0.2195 0.026 Uiso 1 1 calc R . . C6 C 0.32730(13) 0.2691(3) 0.12804(15) 0.0196(7) Uani 1 1 d . . . C7 C 0.47239(13) 0.3577(3) 0.19245(16) 0.0289(8) Uani 1 1 d . . . C8 C 0.49667(16) 0.4714(3) 0.16667(18) 0.0426(10) Uani 1 1 d . . . H8A H 0.5094 0.4594 0.1214 0.064 Uiso 1 1 calc R . . H8B H 0.5278 0.4954 0.1962 0.064 Uiso 1 1 calc R . . H8C H 0.4683 0.5323 0.1659 0.064 Uiso 1 1 calc R . . C9 C 0.51555(15) 0.2592(3) 0.18994(19) 0.0451(10) Uani 1 1 d . . . H9A H 0.5000 0.1872 0.2075 0.068 Uiso 1 1 calc R . . H9B H 0.5485 0.2811 0.2171 0.068 Uiso 1 1 calc R . . H9C H 0.5257 0.2468 0.1436 0.068 Uiso 1 1 calc R . . C10 C 0.45683(15) 0.3754(3) 0.26526(16) 0.0417(10) Uani 1 1 d . . . H10A H 0.4297 0.4384 0.2675 0.063 Uiso 1 1 calc R . . H10B H 0.4899 0.3958 0.2925 0.063 Uiso 1 1 calc R . . H10C H 0.4410 0.3031 0.2822 0.063 Uiso 1 1 calc R . . C11 C 0.40125(13) 0.2605(3) -0.04299(15) 0.0262(8) Uani 1 1 d . . . C12 C 0.38294(16) 0.1375(3) -0.06497(17) 0.0386(9) Uani 1 1 d . . . H12A H 0.4007 0.0796 -0.0353 0.058 Uiso 1 1 calc R . . H12B H 0.3936 0.1236 -0.1109 0.058 Uiso 1 1 calc R . . H12C H 0.3428 0.1309 -0.0627 0.058 Uiso 1 1 calc R . . C13 C 0.37019(15) 0.3532(3) -0.08573(17) 0.0392(9) Uani 1 1 d . . . H13A H 0.3305 0.3476 -0.0786 0.059 Uiso 1 1 calc R . . H13B H 0.3769 0.3400 -0.1330 0.059 Uiso 1 1 calc R . . H13C H 0.3834 0.4311 -0.0727 0.059 Uiso 1 1 calc R . . C14 C 0.46313(14) 0.2716(3) -0.05447(17) 0.0369(9) Uani 1 1 d . . . H14A H 0.4760 0.3491 -0.0404 0.055 Uiso 1 1 calc R . . H14B H 0.4696 0.2607 -0.1020 0.055 Uiso 1 1 calc R . . H14C H 0.4834 0.2120 -0.0284 0.055 Uiso 1 1 calc R . . C15 C 0.26415(12) 0.2265(3) 0.21389(15) 0.0223(7) Uani 1 1 d . . . C16 C 0.26113(13) 0.3224(3) 0.25577(15) 0.0255(8) Uani 1 1 d . . . H16 H 0.2691 0.3986 0.2403 0.031 Uiso 1 1 calc R . . C17 C 0.24602(14) 0.3036(3) 0.32142(16) 0.0300(8) Uani 1 1 d . . . C18 C 0.23474(15) 0.1935(3) 0.34332(18) 0.0370(9) Uani 1 1 d . . . H18 H 0.2235 0.1822 0.3877 0.044 Uiso 1 1 calc R . . C19 C 0.23955(14) 0.0985(3) 0.30146(17) 0.0337(9) Uani 1 1 d . . . C20 C 0.25386(13) 0.1140(3) 0.23574(16) 0.0267(8) Uani 1 1 d . . . H20 H 0.2565 0.0493 0.2064 0.032 Uiso 1 1 calc R . . C21 C 0.25416(14) -0.0268(3) 0.03475(16) 0.0280(8) Uani 1 1 d . . . H21 H 0.2831 0.0092 0.0117 0.034 Uiso 1 1 calc R . . C22 C 0.24711(15) -0.1459(3) 0.02999(18) 0.0342(9) Uani 1 1 d . . . H22 H 0.2701 -0.1910 0.0027 0.041 Uiso 1 1 calc R . . C23 C 0.20655(16) -0.1985(3) 0.06503(18) 0.0352(9) Uani 1 1 d . . . H23 H 0.2024 -0.2809 0.0640 0.042 Uiso 1 1 calc R . . C24 C 0.17182(15) -0.1306(3) 0.10186(17) 0.0321(8) Uani 1 1 d . . . H24 H 0.1430 -0.1657 0.1256 0.039 Uiso 1 1 calc R . . C25 C 0.17940(14) -0.0112(3) 0.10377(16) 0.0243(8) Uani 1 1 d . . . C26 C 0.14388(13) 0.0715(3) 0.13806(15) 0.0238(7) Uani 1 1 d . . . C27 C 0.10086(14) 0.0401(3) 0.17728(16) 0.0307(8) Uani 1 1 d . . . H27 H 0.0932 -0.0399 0.1850 0.037 Uiso 1 1 calc R . . C28 C 0.06890(14) 0.1259(3) 0.20535(17) 0.0334(9) Uani 1 1 d . . . H28 H 0.0383 0.1053 0.2311 0.040 Uiso 1 1 calc R . . C29 C 0.08198(14) 0.2413(3) 0.19556(16) 0.0292(8) Uani 1 1 d . . . H29 H 0.0611 0.3014 0.2152 0.035 Uiso 1 1 calc R . . C30 C 0.12602(13) 0.2682(3) 0.15658(15) 0.0227(7) Uani 1 1 d . . . H30 H 0.1350 0.3479 0.1498 0.027 Uiso 1 1 calc R . . C31 C 0.16198(12) 0.4010(2) 0.00004(14) 0.0175(7) Uani 1 1 d . . . C32 C 0.14028(13) 0.5098(2) -0.02363(15) 0.0206(7) Uani 1 1 d . . . H32 H 0.1571 0.5810 -0.0096 0.025 Uiso 1 1 calc R . . C33 C 0.09579(13) 0.5105(3) -0.06601(14) 0.0208(7) Uani 1 1 d . . . C34 C 0.07111(13) 0.4005(3) -0.08799(14) 0.0203(7) Uani 1 1 d . . . H34 H 0.0395 0.4040 -0.1175 0.024 Uiso 1 1 calc R . . C35 C 0.09005(12) 0.2923(3) -0.06926(14) 0.0189(7) Uani 1 1 d . . . C36 C 0.13763(12) 0.2916(3) -0.02446(14) 0.0189(7) Uani 1 1 d . . . C37 C 0.06383(13) 0.1771(3) -0.09307(15) 0.0226(7) Uani 1 1 d . . . C38 C 0.04832(15) 0.1030(3) -0.03280(16) 0.0307(8) Uani 1 1 d . . . H38A H 0.0816 0.0862 -0.0050 0.046 Uiso 1 1 calc R . . H38B H 0.0316 0.0296 -0.0485 0.046 Uiso 1 1 calc R . . H38C H 0.0219 0.1459 -0.0064 0.046 Uiso 1 1 calc R . . C39 C 0.10478(14) 0.1096(3) -0.13493(16) 0.0292(8) Uani 1 1 d . . . H39A H 0.1156 0.1581 -0.1725 0.044 Uiso 1 1 calc R . . H39B H 0.0873 0.0379 -0.1520 0.044 Uiso 1 1 calc R . . H39C H 0.1376 0.0898 -0.1070 0.044 Uiso 1 1 calc R . . C40 C 0.01112(14) 0.1985(3) -0.13526(17) 0.0305(8) Uani 1 1 d . . . H40A H -0.0158 0.2391 -0.1084 0.046 Uiso 1 1 calc R . . H40B H -0.0043 0.1236 -0.1505 0.046 Uiso 1 1 calc R . . H40C H 0.0195 0.2464 -0.1740 0.046 Uiso 1 1 calc R . . C41 C 0.06808(14) 0.6226(3) -0.09066(15) 0.0248(7) Uani 1 1 d . . . C42 C 0.06642(15) 0.6252(3) -0.16714(16) 0.0320(8) Uani 1 1 d . . . H42A H 0.1039 0.6157 -0.1829 0.048 Uiso 1 1 calc R . . H42B H 0.0513 0.7000 -0.1829 0.048 Uiso 1 1 calc R . . H42C H 0.0430 0.5615 -0.1846 0.048 Uiso 1 1 calc R . . C43 C 0.00904(14) 0.6264(3) -0.06568(17) 0.0330(8) Uani 1 1 d . . . H43A H -0.0089 0.6991 -0.0804 0.049 Uiso 1 1 calc R . . H43B H 0.0103 0.6226 -0.0168 0.049 Uiso 1 1 calc R . . H43C H -0.0120 0.5598 -0.0839 0.049 Uiso 1 1 calc R . . C44 C 0.09890(16) 0.7304(3) -0.06460(19) 0.0389(9) Uani 1 1 d . . . H44A H 0.1004 0.7296 -0.0157 0.058 Uiso 1 1 calc R . . H44B H 0.0796 0.8007 -0.0806 0.058 Uiso 1 1 calc R . . H44C H 0.1365 0.7301 -0.0807 0.058 Uiso 1 1 calc R . . C45 C 0.24203(13) 0.4782(2) 0.05955(15) 0.0197(7) Uani 1 1 d . . . C46 C 0.25029(13) 0.5095(3) 0.12538(15) 0.0239(7) Uani 1 1 d . . . H46 H 0.2268 0.4805 0.1584 0.029 Uiso 1 1 calc R . . C47 C 0.29358(14) 0.5845(3) 0.14290(16) 0.0272(8) Uani 1 1 d . . . C48 C 0.32740(14) 0.6304(3) 0.09454(17) 0.0275(8) Uani 1 1 d . . . H48 H 0.3574 0.6803 0.1067 0.033 Uiso 1 1 calc R . . C49 C 0.31593(14) 0.6011(3) 0.02835(17) 0.0277(8) Uani 1 1 d . . . C50 C 0.27309(13) 0.5247(3) 0.00999(16) 0.0249(7) Uani 1 1 d . . . H50 H 0.2655 0.5051 -0.0355 0.030 Uiso 1 1 calc R . . C51 C 0.24916(18) 0.5070(3) 0.34579(19) 0.0490(11) Uani 1 1 d . . . H51A H 0.2871 0.5179 0.3320 0.074 Uiso 1 1 calc R . . H51B H 0.2418 0.5609 0.3823 0.074 Uiso 1 1 calc R . . H51C H 0.2234 0.5228 0.3079 0.074 Uiso 1 1 calc R . . C52 C 0.2378(2) -0.1088(4) 0.2895(2) 0.0705(15) Uani 1 1 d . . . H52A H 0.2120 -0.1076 0.2506 0.106 Uiso 1 1 calc R . . H52B H 0.2314 -0.1789 0.3161 0.106 Uiso 1 1 calc R . . H52C H 0.2758 -0.1093 0.2746 0.106 Uiso 1 1 calc R . . C53 C 0.34873(17) 0.6683(3) 0.2324(2) 0.0496(11) Uani 1 1 d . . . H53A H 0.3815 0.6245 0.2199 0.074 Uiso 1 1 calc R . . H53B H 0.3487 0.6760 0.2811 0.074 Uiso 1 1 calc R . . H53C H 0.3493 0.7460 0.2120 0.074 Uiso 1 1 calc R . . C54 C 0.39316(19) 0.7107(4) -0.0068(2) 0.0736(16) Uani 1 1 d . . . H54A H 0.3834 0.7801 0.0187 0.110 Uiso 1 1 calc R . . H54B H 0.4106 0.7345 -0.0479 0.110 Uiso 1 1 calc R . . H54C H 0.4189 0.6624 0.0202 0.110 Uiso 1 1 calc R . . Cl1 Cl 0.38540(5) -0.04046(9) 0.14595(6) 0.0594(3) Uani 1 1 d . . . Cl2 Cl 0.10164(3) 0.59580(7) 0.19242(4) 0.02720(19) Uani 1 1 d . . . O111 O 0.32670(14) -0.0803(3) 0.15862(19) 0.0891(11) Uani 1 1 d . . . O222 O 0.40248(19) 0.0218(3) 0.2022(2) 0.1141(16) Uani 1 1 d . . . O333 O 0.41671(11) -0.1438(2) 0.13747(15) 0.0539(8) Uani 1 1 d . . . O444 O 0.37762(18) 0.0233(3) 0.08920(18) 0.1001(13) Uani 1 1 d . . . O555 O 0.14262(10) 0.5222(2) 0.22407(12) 0.0410(6) Uani 1 1 d . . . O666 O 0.10583(11) 0.5889(2) 0.12133(12) 0.0483(7) Uani 1 1 d . . . O777 O 0.10941(12) 0.7140(2) 0.21276(13) 0.0485(7) Uani 1 1 d . . . O888 O 0.04796(10) 0.5571(2) 0.21085(14) 0.0501(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01525(15) 0.01827(13) 0.01979(14) 0.00111(11) -0.00063(9) -0.00070(11) O1 0.0189(13) 0.0249(12) 0.0184(11) 0.0001(9) -0.0012(9) -0.0011(9) O2 0.0191(12) 0.0166(11) 0.0184(11) 0.0005(8) 0.0011(9) 0.0010(9) O3 0.0309(16) 0.0592(18) 0.0231(13) -0.0060(12) 0.0029(10) 0.0068(12) O4 0.061(2) 0.0506(17) 0.0408(16) 0.0234(14) 0.0157(14) 0.0029(14) O5 0.0422(17) 0.0478(16) 0.0315(14) -0.0068(12) -0.0080(12) -0.0201(12) O6 0.0352(16) 0.0463(16) 0.0431(15) -0.0043(12) 0.0134(12) -0.0217(12) N1 0.0157(15) 0.0206(14) 0.0194(14) 0.0008(10) 0.0031(11) 0.0011(10) N2 0.0153(15) 0.0205(13) 0.0225(14) 0.0016(11) -0.0028(11) 0.0014(12) N3 0.0165(15) 0.0239(15) 0.0204(14) 0.0008(11) -0.0044(11) -0.0014(11) N4 0.0151(15) 0.0207(14) 0.0190(13) -0.0029(11) 0.0035(11) -0.0025(11) C1 0.0186(19) 0.0209(16) 0.0207(17) -0.0003(13) -0.0002(13) 0.0015(13) C2 0.0155(18) 0.0269(17) 0.0212(16) 0.0035(14) 0.0022(13) -0.0009(14) C3 0.019(2) 0.0304(19) 0.0260(18) 0.0020(14) 0.0039(14) -0.0023(14) C4 0.022(2) 0.0262(17) 0.0227(18) 0.0033(14) -0.0021(14) -0.0009(14) C5 0.0189(19) 0.0278(18) 0.0171(16) 0.0015(13) -0.0009(13) 0.0006(14) C6 0.0161(18) 0.0202(16) 0.0224(17) 0.0010(13) 0.0006(13) 0.0006(13) C7 0.016(2) 0.047(2) 0.0233(18) 0.0010(16) -0.0004(14) -0.0069(16) C8 0.040(3) 0.052(2) 0.036(2) -0.0023(18) -0.0038(18) -0.0204(19) C9 0.025(2) 0.070(3) 0.039(2) 0.0045(19) -0.0057(17) 0.0033(19) C10 0.029(2) 0.072(3) 0.024(2) 0.0023(18) -0.0048(16) -0.0144(19) C11 0.0174(19) 0.042(2) 0.0194(17) -0.0018(14) 0.0023(13) -0.0038(15) C12 0.036(2) 0.050(2) 0.031(2) -0.0136(17) 0.0119(17) -0.0060(18) C13 0.034(2) 0.062(3) 0.0221(19) 0.0026(17) 0.0020(16) 0.0062(19) C14 0.026(2) 0.061(2) 0.0245(19) -0.0051(18) 0.0086(15) -0.0038(18) C15 0.0103(17) 0.0364(19) 0.0202(16) 0.0063(15) 0.0001(12) 0.0003(14) C16 0.020(2) 0.0371(19) 0.0195(18) 0.0028(14) -0.0018(14) 0.0019(14) C17 0.017(2) 0.051(2) 0.0224(18) -0.0016(16) 0.0013(14) 0.0061(16) C18 0.025(2) 0.063(3) 0.0231(19) 0.0081(18) 0.0029(15) 0.0078(18) C19 0.022(2) 0.044(2) 0.034(2) 0.0191(18) 0.0027(16) 0.0017(16) C20 0.020(2) 0.037(2) 0.0229(18) 0.0065(15) -0.0004(14) -0.0006(15) C21 0.027(2) 0.0278(18) 0.0288(19) 0.0012(15) 0.0002(15) 0.0068(15) C22 0.038(2) 0.0236(19) 0.041(2) -0.0041(16) -0.0053(18) 0.0096(16) C23 0.045(3) 0.0174(18) 0.042(2) 0.0000(16) -0.0130(19) -0.0013(16) C24 0.031(2) 0.0276(19) 0.037(2) 0.0069(16) -0.0079(16) -0.0064(16) C25 0.023(2) 0.0225(17) 0.0270(18) 0.0035(14) -0.0064(14) -0.0044(14) C26 0.021(2) 0.0257(18) 0.0241(18) 0.0044(14) -0.0054(14) -0.0028(14) C27 0.026(2) 0.0322(19) 0.034(2) 0.0085(16) -0.0019(16) -0.0090(16) C28 0.018(2) 0.052(2) 0.030(2) 0.0111(17) 0.0057(15) -0.0037(17) C29 0.023(2) 0.042(2) 0.0230(18) 0.0001(15) 0.0031(14) 0.0030(15) C30 0.0223(19) 0.0237(17) 0.0217(17) 0.0037(14) -0.0031(13) 0.0001(14) C31 0.0144(18) 0.0194(16) 0.0189(16) 0.0005(13) 0.0026(13) -0.0005(12) C32 0.023(2) 0.0160(16) 0.0230(17) -0.0008(13) 0.0042(14) -0.0017(13) C33 0.0209(19) 0.0221(17) 0.0195(17) 0.0003(13) 0.0024(13) 0.0003(13) C34 0.0168(19) 0.0245(17) 0.0196(17) -0.0002(13) 0.0021(13) -0.0027(13) C35 0.0162(18) 0.0209(16) 0.0198(16) 0.0008(13) 0.0020(12) -0.0020(13) C36 0.0183(18) 0.0205(16) 0.0183(16) 0.0007(13) 0.0050(13) -0.0025(14) C37 0.022(2) 0.0213(17) 0.0240(18) -0.0014(13) -0.0002(14) -0.0031(13) C38 0.031(2) 0.0262(18) 0.035(2) -0.0003(15) 0.0041(16) -0.0091(15) C39 0.028(2) 0.0291(19) 0.0298(19) -0.0080(15) -0.0043(15) -0.0023(15) C40 0.022(2) 0.0262(19) 0.043(2) -0.0006(15) -0.0059(16) -0.0053(14) C41 0.027(2) 0.0190(17) 0.0280(18) 0.0033(14) -0.0040(14) 0.0034(14) C42 0.031(2) 0.0307(19) 0.034(2) 0.0083(16) 0.0019(16) 0.0017(16) C43 0.036(2) 0.0302(19) 0.033(2) 0.0007(16) 0.0001(16) 0.0130(16) C44 0.041(2) 0.0202(18) 0.054(2) 0.0030(17) -0.0142(19) 0.0030(17) C45 0.0162(18) 0.0163(15) 0.0262(18) -0.0010(13) -0.0029(13) 0.0011(13) C46 0.021(2) 0.0240(17) 0.0268(18) 0.0045(14) -0.0034(14) -0.0010(14) C47 0.025(2) 0.0246(18) 0.031(2) -0.0049(15) -0.0078(15) 0.0006(14) C48 0.022(2) 0.0217(17) 0.038(2) -0.0020(15) -0.0038(15) -0.0052(14) C49 0.023(2) 0.0249(18) 0.035(2) 0.0016(15) 0.0081(15) -0.0032(14) C50 0.025(2) 0.0236(17) 0.0259(18) -0.0041(14) 0.0013(14) -0.0006(14) C51 0.056(3) 0.057(3) 0.034(2) -0.013(2) -0.0001(19) 0.003(2) C52 0.097(4) 0.046(3) 0.070(3) 0.033(2) 0.027(3) 0.005(3) C53 0.049(3) 0.052(3) 0.046(2) -0.010(2) -0.018(2) -0.020(2) C54 0.053(3) 0.101(4) 0.068(3) -0.009(3) 0.020(2) -0.056(3) Cl1 0.0815(9) 0.0334(6) 0.0602(7) 0.0025(5) -0.0328(6) 0.0071(5) Cl2 0.0243(5) 0.0285(4) 0.0290(5) -0.0009(3) 0.0040(3) 0.0015(3) O111 0.052(2) 0.098(3) 0.116(3) 0.001(2) -0.006(2) 0.008(2) O222 0.142(4) 0.081(3) 0.112(3) -0.033(2) -0.081(3) 0.022(2) O333 0.0359(18) 0.0374(16) 0.088(2) 0.0000(15) -0.0065(15) -0.0011(13) O444 0.129(4) 0.086(3) 0.083(3) 0.041(2) -0.021(2) 0.006(2) O555 0.0288(16) 0.0470(16) 0.0473(16) 0.0093(12) 0.0012(12) 0.0113(12) O666 0.058(2) 0.0621(18) 0.0245(14) -0.0050(12) 0.0019(12) 0.0037(14) O777 0.063(2) 0.0305(14) 0.0524(17) -0.0098(13) 0.0096(14) -0.0039(13) O888 0.0245(16) 0.0590(18) 0.0672(19) 0.0170(14) 0.0070(13) -0.0032(13) _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 N1 1.990(2) . ? Ru1 N4 2.021(2) . ? Ru1 O2 2.0233(19) . ? Ru1 N3 2.033(3) . ? Ru1 N2 2.045(2) . ? Ru1 O1 2.049(2) . ? O1 C1 1.272(3) . ? O2 C36 1.270(3) . ? O3 C17 1.369(4) . ? O3 C51 1.418(4) . ? O4 C19 1.362(4) . ? O4 C52 1.435(5) . ? O5 C47 1.356(4) . ? O5 C53 1.434(4) . ? O6 C49 1.361(4) . ? O6 C54 1.438(4) . ? N1 C6 1.321(4) . ? N1 C15 1.455(4) . ? N2 C21 1.340(4) . ? N2 C25 1.356(4) . ? N3 C30 1.335(4) . ? N3 C26 1.368(4) . ? N4 C31 1.327(4) . ? N4 C45 1.442(4) . ? C1 C2 1.444(4) . ? C1 C6 1.462(4) . ? C2 C3 1.362(4) . ? C2 C11 1.536(4) . ? C3 C4 1.446(4) . ? C3 H3 0.9500 . ? C4 C5 1.343(4) . ? C4 C7 1.533(4) . ? C5 C6 1.425(4) . ? C5 H5 0.9500 . ? C7 C8 1.529(5) . ? C7 C10 1.535(5) . ? C7 C9 1.542(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.532(5) . ? C11 C12 1.538(5) . ? C11 C13 1.542(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.387(4) . ? C15 C20 1.389(4) . ? C16 C17 1.397(4) . ? C16 H16 0.9500 . ? C17 C18 1.368(5) . ? C18 C19 1.383(5) . ? C18 H18 0.9500 . ? C19 C20 1.387(5) . ? C20 H20 0.9500 . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.371(5) . ? C22 H22 0.9500 . ? C23 C24 1.382(5) . ? C23 H23 0.9500 . ? C24 C25 1.383(4) . ? C24 H24 0.9500 . ? C25 C26 1.470(5) . ? C26 C27 1.379(4) . ? C27 C28 1.386(5) . ? C27 H27 0.9500 . ? C28 C29 1.377(5) . ? C28 H28 0.9500 . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.428(4) . ? C31 C36 1.462(4) . ? C32 C33 1.345(4) . ? C32 H32 0.9500 . ? C33 C34 1.457(4) . ? C33 C41 1.523(4) . ? C34 C35 1.370(4) . ? C34 H34 0.9500 . ? C35 C36 1.432(4) . ? C35 C37 1.533(4) . ? C37 C40 1.523(4) . ? C37 C39 1.535(4) . ? C37 C38 1.536(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.525(4) . ? C41 C42 1.532(4) . ? C41 C43 1.536(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.374(4) . ? C45 C50 1.378(4) . ? C46 C47 1.390(4) . ? C46 H46 0.9500 . ? C47 C48 1.398(5) . ? C48 C49 1.385(4) . ? C48 H48 0.9500 . ? C49 C50 1.397(4) . ? C50 H50 0.9500 . ? 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 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Cl1 O444 1.359(3) . ? Cl1 O222 1.384(3) . ? Cl1 O333 1.422(3) . ? Cl1 O111 1.526(4) . ? Cl2 O777 1.426(2) . ? Cl2 O555 1.431(2) . ? Cl2 O666 1.435(2) . ? Cl2 O888 1.437(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 N1 Ru1 N4 101.27(9) . . ? N1 Ru1 O2 178.09(9) . . ? N4 Ru1 O2 77.06(9) . . ? N1 Ru1 N3 95.78(10) . . ? N4 Ru1 N3 99.29(10) . . ? O2 Ru1 N3 83.63(9) . . ? N1 Ru1 N2 96.64(9) . . ? N4 Ru1 N2 162.09(10) . . ? O2 Ru1 N2 85.04(9) . . ? N3 Ru1 N2 79.21(10) . . ? N1 Ru1 O1 77.81(9) . . ? N4 Ru1 O1 87.84(9) . . ? O2 Ru1 O1 102.97(8) . . ? N3 Ru1 O1 171.28(9) . . ? N2 Ru1 O1 95.54(9) . . ? C1 O1 Ru1 114.99(19) . . ? C36 O2 Ru1 116.87(18) . . ? C17 O3 C51 117.6(3) . . ? C19 O4 C52 117.3(3) . . ? C47 O5 C53 118.2(3) . . ? C49 O6 C54 116.9(3) . . ? C6 N1 C15 119.6(3) . . ? C6 N1 Ru1 117.21(19) . . ? C15 N1 Ru1 123.2(2) . . ? C21 N2 C25 119.7(3) . . ? C21 N2 Ru1 123.7(2) . . ? C25 N2 Ru1 115.8(2) . . ? C30 N3 C26 118.9(3) . . ? C30 N3 Ru1 125.3(2) . . ? C26 N3 Ru1 115.8(2) . . ? C31 N4 C45 120.5(2) . . ? C31 N4 Ru1 116.50(19) . . ? C45 N4 Ru1 121.81(19) . . ? O1 C1 C2 123.7(3) . . ? O1 C1 C6 116.6(3) . . ? C2 C1 C6 119.6(3) . . ? C3 C2 C1 115.2(3) . . ? C3 C2 C11 123.0(3) . . ? C1 C2 C11 121.8(3) . . ? C2 C3 C4 126.0(3) . . ? C2 C3 H3 117.0 . . ? C4 C3 H3 117.0 . . ? C5 C4 C3 119.1(3) . . ? C5 C4 C7 123.4(3) . . ? C3 C4 C7 117.4(3) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? N1 C6 C5 126.9(3) . . ? N1 C6 C1 112.4(3) . . ? C5 C6 C1 120.6(3) . . ? C8 C7 C4 110.0(3) . . ? C8 C7 C10 108.8(3) . . ? C4 C7 C10 111.0(3) . . ? C8 C7 C9 110.0(3) . . ? C4 C7 C9 108.4(3) . . ? C10 C7 C9 108.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C2 110.8(3) . . ? C14 C11 C12 107.8(3) . . ? C2 C11 C12 109.8(3) . . ? C14 C11 C13 108.6(3) . . ? C2 C11 C13 109.6(3) . . ? C12 C11 C13 110.2(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 122.1(3) . . ? C16 C15 N1 121.1(3) . . ? C20 C15 N1 116.7(3) . . ? C15 C16 C17 118.0(3) . . ? C15 C16 H16 121.0 . . ? C17 C16 H16 121.0 . . ? C18 C17 O3 115.8(3) . . ? C18 C17 C16 120.6(3) . . ? O3 C17 C16 123.7(3) . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? O4 C19 C18 115.3(3) . . ? O4 C19 C20 124.3(3) . . ? C18 C19 C20 120.4(3) . . ? C19 C20 C15 118.3(3) . . ? C19 C20 H20 120.9 . . ? C15 C20 H20 120.9 . . ? N2 C21 C22 121.5(3) . . ? N2 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 119.3(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.4(3) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 119.3(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N2 C25 C24 120.7(3) . . ? N2 C25 C26 114.4(3) . . ? C24 C25 C26 124.9(3) . . ? N3 C26 C27 120.8(3) . . ? N3 C26 C25 114.5(3) . . ? C27 C26 C25 124.7(3) . . ? C26 C27 C28 119.6(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 118.8(3) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N3 C30 C29 122.5(3) . . ? N3 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N4 C31 C32 127.2(3) . . ? N4 C31 C36 112.8(3) . . ? C32 C31 C36 120.0(3) . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 C41 122.8(3) . . ? C34 C33 C41 117.6(3) . . ? C35 C34 C33 124.9(3) . . ? C35 C34 H34 117.5 . . ? C33 C34 H34 117.5 . . ? C34 C35 C36 115.4(3) . . ? C34 C35 C37 124.4(3) . . ? C36 C35 C37 120.2(3) . . ? O2 C36 C35 124.2(3) . . ? O2 C36 C31 115.1(3) . . ? C35 C36 C31 120.6(3) . . ? C40 C37 C35 111.2(2) . . ? C40 C37 C39 108.9(3) . . ? C35 C37 C39 109.6(3) . . ? C40 C37 C38 107.4(3) . . ? C35 C37 C38 110.1(2) . . ? C39 C37 C38 109.6(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C33 C41 C44 111.7(3) . . ? C33 C41 C42 109.5(3) . . ? C44 C41 C42 108.6(3) . . ? C33 C41 C43 108.8(3) . . ? C44 C41 C43 108.4(3) . . ? C42 C41 C43 109.8(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 121.9(3) . . ? C46 C45 N4 118.5(3) . . ? C50 C45 N4 119.2(3) . . ? C45 C46 C47 118.9(3) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? O5 C47 C46 115.0(3) . . ? O5 C47 C48 124.0(3) . . ? C46 C47 C48 121.0(3) . . ? C49 C48 C47 118.2(3) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? O6 C49 C48 123.7(3) . . ? O6 C49 C50 114.9(3) . . ? C48 C49 C50 121.5(3) . . ? C45 C50 C49 118.4(3) . . ? C45 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? O3 C51 H51A 109.5 . . ? O3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O5 C53 H53A 109.5 . . ? O5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O6 C54 H54A 109.5 . . ? O6 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O6 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O444 Cl1 O222 115.6(3) . . ? O444 Cl1 O333 113.9(2) . . ? O222 Cl1 O333 112.6(2) . . ? O444 Cl1 O111 101.7(2) . . ? O222 Cl1 O111 105.6(3) . . ? O333 Cl1 O111 106.04(19) . . ? O777 Cl2 O555 110.64(16) . . ? O777 Cl2 O666 108.82(16) . . ? O555 Cl2 O666 109.35(16) . . ? O777 Cl2 O888 109.27(17) . . ? O555 Cl2 O888 108.87(15) . . ? O666 Cl2 O888 109.87(17) . . ? 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 Ru1 O1 C1 -7.05(19) . . . . ? N4 Ru1 O1 C1 95.0(2) . . . . ? O2 Ru1 O1 C1 171.16(19) . . . . ? N3 Ru1 O1 C1 -50.2(6) . . . . ? N2 Ru1 O1 C1 -102.7(2) . . . . ? N1 Ru1 O2 C36 17(3) . . . . ? N4 Ru1 O2 C36 -12.2(2) . . . . ? N3 Ru1 O2 C36 88.9(2) . . . . ? N2 Ru1 O2 C36 168.5(2) . . . . ? O1 Ru1 O2 C36 -96.9(2) . . . . ? N4 Ru1 N1 C6 -76.1(2) . . . . ? O2 Ru1 N1 C6 -105(3) . . . . ? N3 Ru1 N1 C6 -176.8(2) . . . . ? N2 Ru1 N1 C6 103.5(2) . . . . ? O1 Ru1 N1 C6 9.2(2) . . . . ? N4 Ru1 N1 C15 103.5(2) . . . . ? O2 Ru1 N1 C15 75(3) . . . . ? N3 Ru1 N1 C15 2.8(2) . . . . ? N2 Ru1 N1 C15 -76.9(2) . . . . ? O1 Ru1 N1 C15 -171.2(2) . . . . ? N1 Ru1 N2 C21 -91.2(3) . . . . ? N4 Ru1 N2 C21 87.4(4) . . . . ? O2 Ru1 N2 C21 89.8(2) . . . . ? N3 Ru1 N2 C21 174.2(3) . . . . ? O1 Ru1 N2 C21 -12.8(3) . . . . ? N1 Ru1 N2 C25 98.8(2) . . . . ? N4 Ru1 N2 C25 -82.6(4) . . . . ? O2 Ru1 N2 C25 -80.2(2) . . . . ? N3 Ru1 N2 C25 4.2(2) . . . . ? O1 Ru1 N2 C25 177.2(2) . . . . ? N1 Ru1 N3 C30 82.9(2) . . . . ? N4 Ru1 N3 C30 -19.6(3) . . . . ? O2 Ru1 N3 C30 -95.3(2) . . . . ? N2 Ru1 N3 C30 178.6(3) . . . . ? O1 Ru1 N3 C30 125.1(5) . . . . ? N1 Ru1 N3 C26 -97.7(2) . . . . ? N4 Ru1 N3 C26 159.9(2) . . . . ? O2 Ru1 N3 C26 84.2(2) . . . . ? N2 Ru1 N3 C26 -2.0(2) . . . . ? O1 Ru1 N3 C26 -55.5(7) . . . . ? N1 Ru1 N4 C31 -170.8(2) . . . . ? O2 Ru1 N4 C31 8.2(2) . . . . ? N3 Ru1 N4 C31 -73.0(2) . . . . ? N2 Ru1 N4 C31 10.7(5) . . . . ? O1 Ru1 N4 C31 112.1(2) . . . . ? N1 Ru1 N4 C45 21.8(2) . . . . ? O2 Ru1 N4 C45 -159.2(2) . . . . ? N3 Ru1 N4 C45 119.6(2) . . . . ? N2 Ru1 N4 C45 -156.7(3) . . . . ? O1 Ru1 N4 C45 -55.4(2) . . . . ? Ru1 O1 C1 C2 -178.3(2) . . . . ? Ru1 O1 C1 C6 4.2(3) . . . . ? O1 C1 C2 C3 178.9(3) . . . . ? C6 C1 C2 C3 -3.6(4) . . . . ? O1 C1 C2 C11 -2.9(5) . . . . ? C6 C1 C2 C11 174.5(3) . . . . ? C1 C2 C3 C4 1.8(5) . . . . ? C11 C2 C3 C4 -176.3(3) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C2 C3 C4 C7 179.8(3) . . . . ? C3 C4 C5 C6 -2.8(4) . . . . ? C7 C4 C5 C6 179.0(3) . . . . ? C15 N1 C6 C5 -5.7(4) . . . . ? Ru1 N1 C6 C5 173.9(2) . . . . ? C15 N1 C6 C1 170.8(3) . . . . ? Ru1 N1 C6 C1 -9.6(3) . . . . ? C4 C5 C6 N1 177.1(3) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? O1 C1 C6 N1 3.4(4) . . . . ? C2 C1 C6 N1 -174.3(3) . . . . ? O1 C1 C6 C5 -179.9(3) . . . . ? C2 C1 C6 C5 2.4(4) . . . . ? C5 C4 C7 C8 -126.1(3) . . . . ? C3 C4 C7 C8 55.6(4) . . . . ? C5 C4 C7 C10 -5.7(4) . . . . ? C3 C4 C7 C10 176.0(3) . . . . ? C5 C4 C7 C9 113.6(3) . . . . ? C3 C4 C7 C9 -64.7(4) . . . . ? C3 C2 C11 C14 4.8(4) . . . . ? C1 C2 C11 C14 -173.2(3) . . . . ? C3 C2 C11 C12 123.8(3) . . . . ? C1 C2 C11 C12 -54.2(4) . . . . ? C3 C2 C11 C13 -115.0(3) . . . . ? C1 C2 C11 C13 67.0(4) . . . . ? C6 N1 C15 C16 71.4(4) . . . . ? Ru1 N1 C15 C16 -108.2(3) . . . . ? C6 N1 C15 C20 -110.3(3) . . . . ? Ru1 N1 C15 C20 70.1(3) . . . . ? C20 C15 C16 C17 -1.4(5) . . . . ? N1 C15 C16 C17 176.8(3) . . . . ? C51 O3 C17 C18 -175.1(3) . . . . ? C51 O3 C17 C16 5.7(5) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C15 C16 C17 O3 179.3(3) . . . . ? O3 C17 C18 C19 -177.4(3) . . . . ? C16 C17 C18 C19 1.8(5) . . . . ? C52 O4 C19 C18 -175.6(4) . . . . ? C52 O4 C19 C20 4.4(5) . . . . ? C17 C18 C19 O4 177.5(3) . . . . ? C17 C18 C19 C20 -2.5(5) . . . . ? O4 C19 C20 C15 -178.7(3) . . . . ? C18 C19 C20 C15 1.2(5) . . . . ? C16 C15 C20 C19 0.7(5) . . . . ? N1 C15 C20 C19 -177.5(3) . . . . ? C25 N2 C21 C22 -0.6(5) . . . . ? Ru1 N2 C21 C22 -170.2(2) . . . . ? N2 C21 C22 C23 -2.2(5) . . . . ? C21 C22 C23 C24 3.1(5) . . . . ? C22 C23 C24 C25 -1.4(5) . . . . ? C21 N2 C25 C24 2.4(4) . . . . ? Ru1 N2 C25 C24 172.8(2) . . . . ? C21 N2 C25 C26 -176.0(3) . . . . ? Ru1 N2 C25 C26 -5.6(3) . . . . ? C23 C24 C25 N2 -1.4(5) . . . . ? C23 C24 C25 C26 176.8(3) . . . . ? C30 N3 C26 C27 -0.6(4) . . . . ? Ru1 N3 C26 C27 179.9(2) . . . . ? C30 N3 C26 C25 179.2(3) . . . . ? Ru1 N3 C26 C25 -0.3(3) . . . . ? N2 C25 C26 N3 3.9(4) . . . . ? C24 C25 C26 N3 -174.4(3) . . . . ? N2 C25 C26 C27 -176.3(3) . . . . ? C24 C25 C26 C27 5.4(5) . . . . ? N3 C26 C27 C28 2.0(5) . . . . ? C25 C26 C27 C28 -177.8(3) . . . . ? C26 C27 C28 C29 -2.4(5) . . . . ? C27 C28 C29 C30 1.5(5) . . . . ? C26 N3 C30 C29 -0.3(4) . . . . ? Ru1 N3 C30 C29 179.2(2) . . . . ? C28 C29 C30 N3 -0.1(5) . . . . ? C45 N4 C31 C32 -15.5(5) . . . . ? Ru1 N4 C31 C32 176.9(2) . . . . ? C45 N4 C31 C36 163.8(3) . . . . ? Ru1 N4 C31 C36 -3.8(3) . . . . ? N4 C31 C32 C33 -177.6(3) . . . . ? C36 C31 C32 C33 3.1(4) . . . . ? C31 C32 C33 C34 -1.1(4) . . . . ? C31 C32 C33 C41 176.5(3) . . . . ? C32 C33 C34 C35 -0.7(5) . . . . ? C41 C33 C34 C35 -178.4(3) . . . . ? C33 C34 C35 C36 0.3(4) . . . . ? C33 C34 C35 C37 -179.7(3) . . . . ? Ru1 O2 C36 C35 -169.9(2) . . . . ? Ru1 O2 C36 C31 13.9(3) . . . . ? C34 C35 C36 O2 -174.2(3) . . . . ? C37 C35 C36 O2 5.7(4) . . . . ? C34 C35 C36 C31 1.8(4) . . . . ? C37 C35 C36 C31 -178.2(3) . . . . ? N4 C31 C36 O2 -6.5(4) . . . . ? C32 C31 C36 O2 172.8(3) . . . . ? N4 C31 C36 C35 177.1(3) . . . . ? C32 C31 C36 C35 -3.6(4) . . . . ? C34 C35 C37 C40 -5.0(4) . . . . ? C36 C35 C37 C40 175.0(3) . . . . ? C34 C35 C37 C39 115.5(3) . . . . ? C36 C35 C37 C39 -64.5(4) . . . . ? C34 C35 C37 C38 -123.9(3) . . . . ? C36 C35 C37 C38 56.1(4) . . . . ? C32 C33 C41 C44 3.2(4) . . . . ? C34 C33 C41 C44 -179.1(3) . . . . ? C32 C33 C41 C42 123.6(3) . . . . ? C34 C33 C41 C42 -58.7(4) . . . . ? C32 C33 C41 C43 -116.4(3) . . . . ? C34 C33 C41 C43 61.3(3) . . . . ? C31 N4 C45 C46 124.3(3) . . . . ? Ru1 N4 C45 C46 -68.8(3) . . . . ? C31 N4 C45 C50 -62.7(4) . . . . ? Ru1 N4 C45 C50 104.2(3) . . . . ? C50 C45 C46 C47 -4.2(5) . . . . ? N4 C45 C46 C47 168.5(3) . . . . ? C53 O5 C47 C46 170.1(3) . . . . ? C53 O5 C47 C48 -9.4(5) . . . . ? C45 C46 C47 O5 -177.7(3) . . . . ? C45 C46 C47 C48 1.8(5) . . . . ? O5 C47 C48 C49 -179.2(3) . . . . ? C46 C47 C48 C49 1.3(5) . . . . ? C54 O6 C49 C48 9.5(5) . . . . ? C54 O6 C49 C50 -171.6(3) . . . . ? C47 C48 C49 O6 176.6(3) . . . . ? C47 C48 C49 C50 -2.2(5) . . . . ? C46 C45 C50 C49 3.3(5) . . . . ? N4 C45 C50 C49 -169.4(3) . . . . ? O6 C49 C50 C45 -178.9(3) . . . . ? C48 C49 C50 C45 0.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.993 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.072