# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Biprajit Sarkar' _publ_contact_author_email SARKAR@IAC.UNI-STUTTGART.DE _publ_section_title ; First Examples of Structurally Characterised Mono- and Dinuclear Ruthenium Complexes Derived from Zwitterionic Quinonoid Ligands ; loop_ _publ_author_name 'Biprajit Sarkar' 'Pierre Braunstein' 'Hari Sankar Das' 'Ralph Hubner' 'Atanu Kumar Das' 'Roberto Pattacini' # Attachment 'bipro9_revised_10_04_2009RP.cif' data_2_2ClO4 _database_code_depnum_ccdc_archive 'CCDC 727536' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C52 H48 N10 O2 Ru2, 2(C H2 Cl2), 2(Cl O4)' _chemical_formula_sum 'C54 H52 Cl6 N10 O10 Ru2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour black _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1415.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8148(5) _cell_length_b 13.9252(3) _cell_length_c 17.7605(6) _cell_angle_alpha 68.649(2) _cell_angle_beta 86.397(2) _cell_angle_gamma 88.834(2) _cell_volume 2945.97(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8954 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.103 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18481 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.50 _reflns_number_total 12203 _reflns_number_gt 8157 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. For complexnumber.2CH2Cl2, one of the dichloromethane molecules was found disordered in three positions with unequal occupancy factors, having the carbon atom in common. The chlorine atoms having the highest occupancy factors were refined anisotropically. ; _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^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12203 _refine_ls_number_parameters 754 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.72938(3) 0.25539(3) 0.34177(2) 0.02775(12) Uani 1 1 d . . . Ru2 Ru 0.84184(3) 0.23964(2) -0.10154(2) 0.02523(11) Uani 1 1 d . . . N1 N 0.6445(3) 0.2488(3) 0.2470(2) 0.0299(9) Uani 1 1 d . . . N2 N 0.7197(3) 0.2832(3) -0.0370(2) 0.0284(9) Uani 1 1 d . . . N3 N 0.6989(3) 0.4099(3) 0.3019(2) 0.0344(9) Uani 1 1 d . . . N4 N 0.6169(3) 0.2619(3) 0.4254(2) 0.0341(9) Uani 1 1 d . . . N5 N 0.8314(3) 0.2488(3) 0.4285(2) 0.0330(9) Uani 1 1 d . . . N6 N 0.7571(3) 0.1001(3) 0.3919(3) 0.0365(10) Uani 1 1 d . . . N7 N 0.8095(3) 0.0837(3) -0.0481(2) 0.0293(9) Uani 1 1 d . . . N8 N 0.9695(3) 0.1760(3) -0.1424(2) 0.0288(9) Uani 1 1 d . . . N9 N 0.7815(3) 0.2646(3) -0.2099(2) 0.0286(9) Uani 1 1 d . . . N10 N 0.8862(3) 0.3883(3) -0.1642(2) 0.0284(9) Uani 1 1 d . . . O1 O 0.8474(2) 0.2600(2) 0.25572(19) 0.0314(7) Uani 1 1 d . . . O3 O 0.8277(4) 0.6229(3) 0.5118(3) 0.0840(16) Uani 1 1 d . . . O2 O 0.9119(2) 0.2331(2) 0.00175(19) 0.0293(7) Uani 1 1 d . . . O4 O 0.8899(4) 0.5773(3) 0.4025(4) 0.0965(18) Uani 1 1 d . . . O5 O 0.7221(3) 0.5245(3) 0.4658(2) 0.0513(10) Uani 1 1 d . . . O6 O 0.7582(4) 0.6983(3) 0.3891(3) 0.0669(13) Uani 1 1 d . . . O7 O 0.5709(5) -0.1381(3) 0.2382(4) 0.121(2) Uani 1 1 d . . . O8 O 0.6212(3) 0.0341(3) 0.1802(3) 0.0773(14) Uani 1 1 d . . . O9 O 0.4673(4) -0.0140(3) 0.2638(3) 0.0757(14) Uani 1 1 d . . . O10 O 0.4789(5) -0.0244(5) 0.1382(4) 0.122(2) Uani 1 1 d . . . C1 C 0.8173(3) 0.2565(3) 0.1890(3) 0.0260(10) Uani 1 1 d . . . C2 C 0.8868(4) 0.2479(3) 0.1288(3) 0.0283(10) Uani 1 1 d . . . H2 H 0.9580 0.2425 0.1366 0.034 Uiso 1 1 calc R . . C3 C 0.8513(4) 0.2471(3) 0.0573(3) 0.0271(10) Uani 1 1 d . . . C4 C 0.7383(3) 0.2676(3) 0.0398(3) 0.0253(10) Uani 1 1 d . . . C5 C 0.6686(3) 0.2713(3) 0.1022(3) 0.0292(10) Uani 1 1 d . . . H5 H 0.5979 0.2818 0.0928 0.035 Uiso 1 1 calc R . . C6 C 0.7021(4) 0.2597(3) 0.1790(3) 0.0291(10) Uani 1 1 d . . . C7 C 0.5300(4) 0.2424(3) 0.2428(3) 0.0342(11) Uani 1 1 d . . . H7 H 0.5173 0.2081 0.2048 0.041 Uiso 1 1 calc R . . C8 C 0.4835(4) 0.3502(4) 0.2098(3) 0.0462(14) Uani 1 1 d . . . H8A H 0.4907 0.3836 0.2479 0.069 Uiso 1 1 calc R . . H8B H 0.4108 0.3454 0.2016 0.069 Uiso 1 1 calc R . . H8C H 0.5197 0.3895 0.1592 0.069 Uiso 1 1 calc R . . C9 C 0.4755(4) 0.1795(4) 0.3245(3) 0.0449(13) Uani 1 1 d . . . H9A H 0.5128 0.1163 0.3488 0.067 Uiso 1 1 calc R . . H9B H 0.4052 0.1643 0.3167 0.067 Uiso 1 1 calc R . . H9C H 0.4744 0.2184 0.3594 0.067 Uiso 1 1 calc R . . C10 C 0.6141(4) 0.3209(3) -0.0624(3) 0.0335(11) Uani 1 1 d . . . H10 H 0.5874 0.3572 -0.0271 0.040 Uiso 1 1 calc R . . C11 C 0.6152(4) 0.3985(4) -0.1490(3) 0.0470(14) Uani 1 1 d . . . H11A H 0.6712 0.4469 -0.1579 0.071 Uiso 1 1 calc R . . H11B H 0.5498 0.4346 -0.1576 0.071 Uiso 1 1 calc R . . H11C H 0.6253 0.3629 -0.1861 0.071 Uiso 1 1 calc R . . C12 C 0.5374(4) 0.2334(4) -0.0508(4) 0.0470(14) Uani 1 1 d . . . H12A H 0.5610 0.1957 -0.0844 0.070 Uiso 1 1 calc R . . H12B H 0.4694 0.2615 -0.0656 0.070 Uiso 1 1 calc R . . H12C H 0.5336 0.1879 0.0049 0.070 Uiso 1 1 calc R . . C13 C 0.7441(5) 0.4816(4) 0.2359(3) 0.0474(14) Uani 1 1 d . . . H13 H 0.7982 0.4618 0.2073 0.057 Uiso 1 1 calc R . . C14 C 0.7137(5) 0.5838(4) 0.2086(4) 0.0548(16) Uani 1 1 d . . . H14 H 0.7459 0.6313 0.1618 0.066 Uiso 1 1 calc R . . C15 C 0.6359(6) 0.6140(4) 0.2512(4) 0.0645(19) Uani 1 1 d . . . H15 H 0.6156 0.6828 0.2341 0.077 Uiso 1 1 calc R . . C16 C 0.5874(5) 0.5426(4) 0.3194(4) 0.0534(15) Uani 1 1 d . . . H16 H 0.5333 0.5621 0.3482 0.064 Uiso 1 1 calc R . . C17 C 0.6211(4) 0.4398(4) 0.3447(3) 0.0412(13) Uani 1 1 d . . . C18 C 0.5764(4) 0.3571(4) 0.4162(3) 0.0381(12) Uani 1 1 d . . . C19 C 0.5032(4) 0.3683(5) 0.4718(4) 0.0546(15) Uani 1 1 d . . . H19 H 0.4739 0.4328 0.4633 0.066 Uiso 1 1 calc R . . C20 C 0.4726(5) 0.2866(6) 0.5394(4) 0.0684(19) Uani 1 1 d . . . H20 H 0.4240 0.2957 0.5773 0.082 Uiso 1 1 calc R . . C21 C 0.5136(4) 0.1908(5) 0.5514(3) 0.0511(15) Uani 1 1 d . . . H21 H 0.4938 0.1341 0.5973 0.061 Uiso 1 1 calc R . . C22 C 0.5849(4) 0.1808(4) 0.4933(3) 0.0423(13) Uani 1 1 d . . . H22 H 0.6126 0.1160 0.5008 0.051 Uiso 1 1 calc R . . C23 C 0.8672(4) 0.3296(4) 0.4424(3) 0.0398(12) Uani 1 1 d . . . H23 H 0.8484 0.3954 0.4087 0.048 Uiso 1 1 calc R . . C24 C 0.9314(4) 0.3203(4) 0.5050(3) 0.0466(14) Uani 1 1 d . . . H24 H 0.9556 0.3781 0.5131 0.056 Uiso 1 1 calc R . . C25 C 0.9578(5) 0.2230(5) 0.5544(4) 0.0617(17) Uani 1 1 d . . . H25 H 1.0008 0.2142 0.5967 0.074 Uiso 1 1 calc R . . C26 C 0.9213(5) 0.1383(5) 0.5417(4) 0.0634(18) Uani 1 1 d . . . H26 H 0.9392 0.0722 0.5753 0.076 Uiso 1 1 calc R . . C27 C 0.8580(4) 0.1524(4) 0.4789(3) 0.0439(13) Uani 1 1 d . . . C28 C 0.8166(4) 0.0680(4) 0.4569(4) 0.0509(15) Uani 1 1 d . . . C29 C 0.8363(5) -0.0358(4) 0.4988(4) 0.073(2) Uani 1 1 d . . . H29 H 0.8735 -0.0568 0.5453 0.088 Uiso 1 1 calc R . . C30 C 0.7987(6) -0.1074(4) 0.4690(5) 0.084(2) Uani 1 1 d . . . H30 H 0.8109 -0.1774 0.4956 0.100 Uiso 1 1 calc R . . C31 C 0.7445(5) -0.0748(4) 0.4014(4) 0.0605(18) Uani 1 1 d . . . H31 H 0.7213 -0.1219 0.3801 0.073 Uiso 1 1 calc R . . C32 C 0.7239(4) 0.0290(4) 0.3643(4) 0.0447(14) Uani 1 1 d . . . H32 H 0.6856 0.0505 0.3183 0.054 Uiso 1 1 calc R . . C33 C 0.7237(4) 0.0401(3) 0.0002(3) 0.0346(11) Uani 1 1 d . . . H33 H 0.6752 0.0829 0.0134 0.042 Uiso 1 1 calc R . . C34 C 0.7050(4) -0.0650(4) 0.0310(3) 0.0407(13) Uani 1 1 d . . . H34 H 0.6437 -0.0917 0.0618 0.049 Uiso 1 1 calc R . . C35 C 0.7795(4) -0.1296(4) 0.0148(3) 0.0428(13) Uani 1 1 d . . . H35 H 0.7696 -0.2007 0.0353 0.051 Uiso 1 1 calc R . . C36 C 0.8688(4) -0.0864(3) -0.0325(3) 0.0382(12) Uani 1 1 d . . . H36 H 0.9201 -0.1285 -0.0434 0.046 Uiso 1 1 calc R . . C37 C 0.8816(4) 0.0189(3) -0.0634(3) 0.0300(11) Uani 1 1 d . . . C38 C 0.9727(4) 0.0717(3) -0.1159(3) 0.0297(10) Uani 1 1 d . . . C39 C 1.0556(4) 0.0200(4) -0.1369(3) 0.0430(13) Uani 1 1 d . . . H39 H 1.0562 -0.0517 -0.1174 0.052 Uiso 1 1 calc R . . C40 C 1.1372(5) 0.0744(4) -0.1866(3) 0.0497(14) Uani 1 1 d . . . H40 H 1.1938 0.0403 -0.2008 0.060 Uiso 1 1 calc R . . C41 C 1.1340(4) 0.1812(4) -0.2154(3) 0.0462(14) Uani 1 1 d . . . H41 H 1.1882 0.2198 -0.2497 0.055 Uiso 1 1 calc R . . C42 C 1.0501(4) 0.2292(4) -0.1926(3) 0.0387(12) Uani 1 1 d . . . H42 H 1.0483 0.3009 -0.2123 0.046 Uiso 1 1 calc R . . C43 C 0.9362(4) 0.4487(3) -0.1337(3) 0.0333(11) Uani 1 1 d . . . H43 H 0.9475 0.4239 -0.0787 0.040 Uiso 1 1 calc R . . C44 C 0.9713(4) 0.5460(3) -0.1814(3) 0.0403(13) Uani 1 1 d . . . H44 H 1.0060 0.5856 -0.1584 0.048 Uiso 1 1 calc R . . C45 C 0.9552(4) 0.5847(4) -0.2624(3) 0.0454(14) Uani 1 1 d . . . H45 H 0.9791 0.6502 -0.2950 0.055 Uiso 1 1 calc R . . C46 C 0.9024(4) 0.5242(4) -0.2952(3) 0.0446(13) Uani 1 1 d . . . H46 H 0.8906 0.5485 -0.3501 0.054 Uiso 1 1 calc R . . C47 C 0.8674(4) 0.4264(3) -0.2443(3) 0.0308(11) Uani 1 1 d . . . C48 C 0.8071(4) 0.3561(3) -0.2706(3) 0.0320(11) Uani 1 1 d . . . C49 C 0.7733(4) 0.3816(4) -0.3469(3) 0.0411(13) Uani 1 1 d . . . H49 H 0.7916 0.4451 -0.3865 0.049 Uiso 1 1 calc R . . C50 C 0.7119(4) 0.3134(4) -0.3655(3) 0.0487(14) Uani 1 1 d . . . H50 H 0.6884 0.3303 -0.4173 0.058 Uiso 1 1 calc R . . C51 C 0.6867(4) 0.2202(4) -0.3056(3) 0.0447(14) Uani 1 1 d . . . H51 H 0.6463 0.1723 -0.3162 0.054 Uiso 1 1 calc R . . C52 C 0.7225(4) 0.1989(4) -0.2295(3) 0.0353(12) Uani 1 1 d . . . H52 H 0.7049 0.1357 -0.1894 0.042 Uiso 1 1 calc R . . C53 C 0.7496(5) 0.5405(5) -0.0176(5) 0.072(2) Uani 1 1 d . . . H53A H 0.7568 0.5486 -0.0742 0.086 Uiso 1 1 calc R . . H53B H 0.7500 0.4671 0.0141 0.086 Uiso 1 1 calc R . . C54 C 0.7578(8) 0.8886(8) -0.2126(7) 0.126(3) Uiso 1 1 d . A 1 H54A H 0.6944 0.9146 -0.2402 0.151 Uiso 1 1 calc R A 1 H54B H 0.7432 0.8748 -0.1554 0.151 Uiso 1 1 calc R A 1 Cl1 Cl 0.80053(11) 0.60399(9) 0.44129(8) 0.0439(3) Uani 1 1 d . . . Cl2 Cl 0.53591(10) -0.03639(9) 0.20590(8) 0.0441(3) Uani 1 1 d . . . Cl3 Cl 0.63252(15) 0.58856(19) 0.00009(14) 0.0993(7) Uani 1 1 d . . . Cl4 Cl 0.85711(14) 0.59574(16) 0.00457(13) 0.0841(6) Uani 1 1 d . . . Cl5 Cl 0.7989(3) 0.7634(3) -0.2277(4) 0.1051(15) Uani 0.55 1 d P A 1 Cl5B Cl 0.7087(11) 0.8037(10) -0.1520(8) 0.113(4) Uiso 0.20 1 d P B 3 Cl5C Cl 0.7901(9) 0.7869(8) -0.1822(7) 0.101(3) Uiso 0.25 1 d P C 2 Cl6 Cl 0.8466(5) 0.9720(3) -0.2468(3) 0.1188(18) Uani 0.55 1 d P A 1 Cl6B Cl 0.8949(16) 0.8926(16) -0.2641(13) 0.183(7) Uiso 0.20 1 d P D 3 Cl6C Cl 0.7976(13) 0.9830(12) -0.2887(10) 0.161(6) Uiso 0.25 1 d P E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0312(2) 0.0246(2) 0.0300(2) -0.01291(15) -0.00127(17) -0.00089(15) Ru2 0.0287(2) 0.02137(19) 0.0257(2) -0.00873(15) -0.00121(16) -0.00016(14) N1 0.030(2) 0.029(2) 0.033(2) -0.0128(17) -0.0028(18) -0.0011(16) N2 0.026(2) 0.0249(19) 0.036(2) -0.0127(16) -0.0017(18) 0.0009(15) N3 0.043(2) 0.030(2) 0.034(2) -0.0150(18) -0.011(2) 0.0010(18) N4 0.028(2) 0.044(2) 0.036(2) -0.0206(19) -0.0053(19) 0.0001(18) N5 0.034(2) 0.034(2) 0.035(2) -0.0176(18) 0.0000(19) -0.0031(17) N6 0.043(2) 0.027(2) 0.040(3) -0.0127(18) 0.000(2) -0.0034(18) N7 0.033(2) 0.0262(19) 0.027(2) -0.0077(16) 0.0001(18) 0.0017(16) N8 0.035(2) 0.030(2) 0.023(2) -0.0107(16) -0.0013(17) 0.0009(16) N9 0.029(2) 0.0230(18) 0.032(2) -0.0079(16) -0.0018(18) 0.0000(15) N10 0.028(2) 0.0247(18) 0.034(2) -0.0117(16) -0.0011(17) -0.0006(15) O1 0.0294(17) 0.0350(17) 0.0316(19) -0.0135(14) -0.0051(15) -0.0037(13) O3 0.131(4) 0.072(3) 0.046(3) -0.013(2) -0.013(3) -0.046(3) O2 0.0309(18) 0.0322(16) 0.0279(18) -0.0146(14) -0.0029(15) 0.0044(13) O4 0.077(3) 0.060(3) 0.156(5) -0.049(3) 0.032(4) 0.003(2) O5 0.060(2) 0.041(2) 0.051(2) -0.0136(17) -0.009(2) -0.0142(18) O6 0.085(3) 0.037(2) 0.063(3) -0.0008(19) 0.005(2) 0.010(2) O7 0.154(5) 0.038(3) 0.142(5) -0.012(3) 0.066(4) 0.017(3) O8 0.064(3) 0.060(3) 0.112(4) -0.038(3) 0.017(3) -0.020(2) O9 0.091(3) 0.056(2) 0.079(3) -0.030(2) 0.044(3) -0.005(2) O10 0.093(4) 0.208(7) 0.087(4) -0.075(4) -0.013(4) -0.026(4) C1 0.030(2) 0.019(2) 0.030(3) -0.0095(18) -0.002(2) -0.0004(18) C2 0.028(2) 0.030(2) 0.031(3) -0.016(2) -0.003(2) -0.0008(19) C3 0.032(3) 0.016(2) 0.031(3) -0.0062(18) -0.002(2) 0.0002(17) C4 0.027(2) 0.017(2) 0.032(3) -0.0101(18) -0.004(2) 0.0004(17) C5 0.021(2) 0.032(2) 0.036(3) -0.014(2) -0.006(2) 0.0034(19) C6 0.034(3) 0.022(2) 0.033(3) -0.0131(19) -0.001(2) -0.0009(18) C7 0.030(3) 0.042(3) 0.035(3) -0.019(2) -0.003(2) 0.000(2) C8 0.034(3) 0.054(3) 0.053(4) -0.022(3) -0.007(3) 0.009(2) C9 0.032(3) 0.065(3) 0.044(3) -0.028(3) 0.007(2) -0.011(3) C10 0.032(3) 0.036(3) 0.035(3) -0.017(2) -0.005(2) 0.007(2) C11 0.041(3) 0.045(3) 0.049(3) -0.009(3) -0.008(3) 0.013(2) C12 0.033(3) 0.050(3) 0.064(4) -0.028(3) -0.011(3) 0.003(2) C13 0.067(4) 0.032(3) 0.042(3) -0.011(2) -0.007(3) -0.001(3) C14 0.077(4) 0.031(3) 0.052(4) -0.008(3) -0.017(3) -0.001(3) C15 0.092(5) 0.031(3) 0.075(5) -0.019(3) -0.045(4) 0.016(3) C16 0.059(4) 0.048(3) 0.067(4) -0.034(3) -0.028(3) 0.016(3) C17 0.042(3) 0.045(3) 0.046(3) -0.027(3) -0.017(3) 0.010(2) C18 0.031(3) 0.052(3) 0.045(3) -0.035(3) -0.004(2) 0.003(2) C19 0.042(3) 0.074(4) 0.067(4) -0.048(4) -0.007(3) 0.009(3) C20 0.047(4) 0.118(6) 0.058(4) -0.055(4) 0.016(3) -0.014(4) C21 0.039(3) 0.078(4) 0.039(3) -0.025(3) 0.002(3) -0.016(3) C22 0.037(3) 0.052(3) 0.036(3) -0.013(2) -0.001(2) -0.007(2) C23 0.040(3) 0.038(3) 0.047(3) -0.022(2) 0.002(3) -0.003(2) C24 0.038(3) 0.060(3) 0.053(4) -0.033(3) -0.010(3) -0.002(3) C25 0.055(4) 0.075(4) 0.061(4) -0.028(3) -0.024(3) 0.004(3) C26 0.066(4) 0.050(3) 0.065(4) -0.008(3) -0.033(4) 0.009(3) C27 0.045(3) 0.041(3) 0.043(3) -0.012(2) -0.012(3) 0.009(2) C28 0.052(4) 0.034(3) 0.063(4) -0.012(3) -0.009(3) -0.001(2) C29 0.076(5) 0.036(3) 0.097(6) -0.005(3) -0.038(4) 0.009(3) C30 0.083(5) 0.021(3) 0.135(7) -0.012(4) -0.020(5) 0.004(3) C31 0.050(4) 0.030(3) 0.101(6) -0.024(3) -0.002(4) -0.001(3) C32 0.047(3) 0.029(3) 0.061(4) -0.020(2) 0.003(3) -0.006(2) C33 0.038(3) 0.029(2) 0.036(3) -0.012(2) 0.006(2) -0.003(2) C34 0.043(3) 0.035(3) 0.040(3) -0.011(2) 0.007(3) -0.003(2) C35 0.057(3) 0.026(2) 0.042(3) -0.008(2) 0.001(3) -0.006(2) C36 0.049(3) 0.028(2) 0.038(3) -0.012(2) -0.001(3) 0.007(2) C37 0.041(3) 0.025(2) 0.026(3) -0.0107(19) -0.002(2) 0.002(2) C38 0.038(3) 0.026(2) 0.027(3) -0.0107(19) -0.002(2) 0.0031(19) C39 0.047(3) 0.034(3) 0.048(3) -0.017(2) 0.002(3) 0.005(2) C40 0.050(3) 0.055(3) 0.048(4) -0.025(3) 0.007(3) 0.012(3) C41 0.043(3) 0.051(3) 0.041(3) -0.013(3) 0.010(3) -0.001(2) C42 0.042(3) 0.037(3) 0.031(3) -0.006(2) 0.002(2) -0.001(2) C43 0.032(3) 0.032(2) 0.038(3) -0.015(2) -0.002(2) -0.007(2) C44 0.046(3) 0.032(3) 0.048(3) -0.019(2) -0.002(3) -0.009(2) C45 0.056(4) 0.026(3) 0.048(4) -0.006(2) 0.002(3) -0.015(2) C46 0.057(3) 0.037(3) 0.036(3) -0.008(2) -0.003(3) -0.011(2) C47 0.037(3) 0.025(2) 0.027(3) -0.0058(19) -0.002(2) -0.0035(19) C48 0.031(3) 0.030(2) 0.032(3) -0.006(2) -0.002(2) -0.0040(19) C49 0.050(3) 0.041(3) 0.029(3) -0.009(2) -0.001(2) -0.011(2) C50 0.050(3) 0.060(3) 0.038(3) -0.018(3) -0.010(3) -0.013(3) C51 0.045(3) 0.049(3) 0.040(3) -0.015(3) -0.002(3) -0.018(2) C52 0.039(3) 0.033(2) 0.035(3) -0.013(2) 0.001(2) -0.011(2) C53 0.053(4) 0.067(4) 0.100(6) -0.038(4) 0.008(4) 0.002(3) Cl1 0.0533(8) 0.0327(6) 0.0427(8) -0.0087(5) -0.0101(6) -0.0034(6) Cl2 0.0482(8) 0.0383(7) 0.0471(8) -0.0187(6) 0.0100(7) -0.0083(6) Cl3 0.0545(11) 0.157(2) 0.1087(17) -0.0755(15) -0.0122(11) 0.0265(12) Cl4 0.0568(10) 0.1234(16) 0.0954(15) -0.0656(13) -0.0202(10) 0.0102(10) Cl5 0.079(3) 0.077(2) 0.174(5) -0.061(3) -0.023(3) 0.0140(19) Cl6 0.206(6) 0.088(3) 0.072(3) -0.039(2) -0.010(3) -0.036(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 N4 2.029(4) . ? Ru1 N3 2.044(4) . ? Ru1 N6 2.050(4) . ? Ru1 N5 2.058(4) . ? Ru1 O1 2.066(3) . ? Ru1 N1 2.091(4) . ? Ru2 N9 2.028(4) . ? Ru2 N10 2.034(3) . ? Ru2 N8 2.061(4) . ? Ru2 O2 2.065(3) . ? Ru2 N7 2.067(3) . ? Ru2 N2 2.091(4) . ? N1 C6 1.336(6) . ? N1 C7 1.479(6) . ? N2 C4 1.337(6) . ? N2 C10 1.479(6) . ? N3 C13 1.338(6) . ? N3 C17 1.364(6) . ? N4 C22 1.365(6) . ? N4 C18 1.370(6) . ? N5 C23 1.333(6) . ? N5 C27 1.365(6) . ? N6 C32 1.341(6) . ? N6 C28 1.354(7) . ? N7 C33 1.358(6) . ? N7 C37 1.362(6) . ? N8 C38 1.355(5) . ? N8 C42 1.359(6) . ? N9 C52 1.350(6) . ? N9 C48 1.365(5) . ? N10 C43 1.345(6) . ? N10 C47 1.361(6) . ? O1 C1 1.287(5) . ? O3 Cl1 1.435(5) . ? O2 C3 1.286(5) . ? O4 Cl1 1.412(5) . ? O5 Cl1 1.437(3) . ? O6 Cl1 1.424(4) . ? O7 Cl2 1.396(5) . ? O8 Cl2 1.422(4) . ? O9 Cl2 1.427(4) . ? O10 Cl2 1.403(6) . ? C1 C2 1.386(6) . ? C1 C6 1.495(6) . ? C2 C3 1.378(6) . ? C2 H2 0.9300 . ? C3 C4 1.500(6) . ? C4 C5 1.394(6) . ? C5 C6 1.408(6) . ? C5 H5 0.9300 . ? C7 C8 1.523(7) . ? C7 C9 1.528(7) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.524(7) . ? C10 C12 1.528(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.382(7) . ? C13 H13 0.9300 . ? C14 C15 1.366(9) . ? C14 H14 0.9300 . ? C15 C16 1.378(9) . ? C15 H15 0.9300 . ? C16 C17 1.403(7) . ? C16 H16 0.9300 . ? C17 C18 1.463(7) . ? C18 C19 1.367(7) . ? C19 C20 1.362(9) . ? C19 H19 0.9300 . ? C20 C21 1.372(9) . ? C20 H20 0.9300 . ? C21 C22 1.377(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.392(7) . ? C23 H23 0.9300 . ? C24 C25 1.367(8) . ? C24 H24 0.9300 . ? C25 C26 1.375(8) . ? C25 H25 0.9300 . ? C26 C27 1.375(8) . ? C26 H26 0.9300 . ? C27 C28 1.484(8) . ? C28 C29 1.389(7) . ? C29 C30 1.393(9) . ? C29 H29 0.9300 . ? C30 C31 1.351(10) . ? C30 H30 0.9300 . ? C31 C32 1.381(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.382(6) . ? C33 H33 0.9300 . ? C34 C35 1.387(7) . ? C34 H34 0.9300 . ? C35 C36 1.385(7) . ? C35 H35 0.9300 . ? C36 C37 1.375(6) . ? C36 H36 0.9300 . ? C37 C38 1.474(6) . ? C38 C39 1.378(7) . ? C39 C40 1.370(7) . ? C39 H39 0.9300 . ? C40 C41 1.386(7) . ? C40 H40 0.9300 . ? C41 C42 1.371(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.377(6) . ? C43 H43 0.9300 . ? C44 C45 1.368(7) . ? C44 H44 0.9300 . ? C45 C46 1.391(7) . ? C45 H45 0.9300 . ? C46 C47 1.396(6) . ? C46 H46 0.9300 . ? C47 C48 1.477(6) . ? C48 C49 1.367(7) . ? C49 C50 1.387(7) . ? C49 H49 0.9300 . ? C50 C51 1.375(7) . ? C50 H50 0.9300 . ? C51 C52 1.380(7) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 Cl3 1.688(6) . ? C53 Cl4 1.725(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 Cl6 1.570(11) . ? C54 Cl5 1.916(11) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? 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 N4 Ru1 N3 78.73(16) . . ? N4 Ru1 N6 97.02(16) . . ? N3 Ru1 N6 174.97(17) . . ? N4 Ru1 N5 84.68(15) . . ? N3 Ru1 N5 98.30(15) . . ? N6 Ru1 N5 78.50(16) . . ? N4 Ru1 O1 175.58(13) . . ? N3 Ru1 O1 97.45(14) . . ? N6 Ru1 O1 86.69(14) . . ? N5 Ru1 O1 93.73(14) . . ? N4 Ru1 N1 103.57(15) . . ? N3 Ru1 N1 87.74(14) . . ? N6 Ru1 N1 95.93(15) . . ? N5 Ru1 N1 170.66(15) . . ? O1 Ru1 N1 78.35(14) . . ? N9 Ru2 N10 78.99(14) . . ? N9 Ru2 N8 87.02(15) . . ? N10 Ru2 N8 95.00(14) . . ? N9 Ru2 O2 172.52(12) . . ? N10 Ru2 O2 93.56(13) . . ? N8 Ru2 O2 92.97(13) . . ? N9 Ru2 N7 97.99(14) . . ? N10 Ru2 N7 172.69(15) . . ? N8 Ru2 N7 78.13(14) . . ? O2 Ru2 N7 89.32(13) . . ? N9 Ru2 N2 102.99(15) . . ? N10 Ru2 N2 92.73(14) . . ? N8 Ru2 N2 168.38(14) . . ? O2 Ru2 N2 77.88(13) . . ? N7 Ru2 N2 94.45(14) . . ? C6 N1 C7 116.1(4) . . ? C6 N1 Ru1 114.6(3) . . ? C7 N1 Ru1 129.1(3) . . ? C4 N2 C10 116.1(4) . . ? C4 N2 Ru2 114.6(3) . . ? C10 N2 Ru2 129.2(3) . . ? C13 N3 C17 118.4(4) . . ? C13 N3 Ru1 125.7(4) . . ? C17 N3 Ru1 115.8(3) . . ? C22 N4 C18 117.6(4) . . ? C22 N4 Ru1 125.2(3) . . ? C18 N4 Ru1 117.0(3) . . ? C23 N5 C27 118.3(4) . . ? C23 N5 Ru1 125.5(3) . . ? C27 N5 Ru1 116.0(3) . . ? C32 N6 C28 117.9(4) . . ? C32 N6 Ru1 125.5(4) . . ? C28 N6 Ru1 116.6(3) . . ? C33 N7 C37 117.2(4) . . ? C33 N7 Ru2 126.4(3) . . ? C37 N7 Ru2 116.4(3) . . ? C38 N8 C42 117.7(4) . . ? C38 N8 Ru2 116.5(3) . . ? C42 N8 Ru2 125.9(3) . . ? C52 N9 C48 116.5(4) . . ? C52 N9 Ru2 127.1(3) . . ? C48 N9 Ru2 116.3(3) . . ? C43 N10 C47 118.4(4) . . ? C43 N10 Ru2 125.3(3) . . ? C47 N10 Ru2 116.2(3) . . ? C1 O1 Ru1 115.5(3) . . ? C3 O2 Ru2 116.0(3) . . ? O1 C1 C2 122.6(4) . . ? O1 C1 C6 117.1(4) . . ? C2 C1 C6 120.3(4) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? O2 C3 C2 122.9(4) . . ? O2 C3 C4 116.8(4) . . ? C2 C3 C4 120.2(4) . . ? N2 C4 C5 128.9(4) . . ? N2 C4 C3 113.1(4) . . ? C5 C4 C3 118.0(4) . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? N1 C6 C5 128.8(4) . . ? N1 C6 C1 113.6(4) . . ? C5 C6 C1 117.7(4) . . ? N1 C7 C8 110.1(4) . . ? N1 C7 C9 112.6(4) . . ? C8 C7 C9 110.3(4) . . ? N1 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? 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 . . ? N2 C10 C11 112.8(4) . . ? N2 C10 C12 112.6(4) . . ? C11 C10 C12 110.4(4) . . ? N2 C10 H10 106.9 . . ? C11 C10 H10 106.9 . . ? C12 C10 H10 106.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 122.7(6) . . ? N3 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 119.1(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 118.8(6) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? N3 C17 C16 121.1(5) . . ? N3 C17 C18 115.0(4) . . ? C16 C17 C18 123.9(5) . . ? C19 C18 N4 120.5(5) . . ? C19 C18 C17 126.1(5) . . ? N4 C18 C17 113.3(4) . . ? C20 C19 C18 121.0(6) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.8(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 118.0(5) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? N4 C22 C21 123.0(5) . . ? N4 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? N5 C23 C24 123.0(5) . . ? N5 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C25 C24 C23 117.7(5) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 119.3(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N5 C27 C26 121.3(5) . . ? N5 C27 C28 114.0(5) . . ? C26 C27 C28 124.7(5) . . ? N6 C28 C29 122.0(5) . . ? N6 C28 C27 114.4(4) . . ? C29 C28 C27 123.6(6) . . ? C28 C29 C30 118.1(6) . . ? C28 C29 H29 120.9 . . ? C30 C29 H29 120.9 . . ? C31 C30 C29 119.7(5) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.4(6) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? N6 C32 C31 122.6(6) . . ? N6 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? N7 C33 C34 123.2(5) . . ? N7 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C33 C34 C35 118.6(5) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? C36 C35 C34 118.8(4) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? N7 C37 C36 122.2(4) . . ? N7 C37 C38 114.2(4) . . ? C36 C37 C38 123.6(4) . . ? N8 C38 C39 121.9(4) . . ? N8 C38 C37 114.8(4) . . ? C39 C38 C37 123.3(4) . . ? C40 C39 C38 119.9(5) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 118.9(5) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? C42 C41 C40 119.1(5) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? N8 C42 C41 122.5(4) . . ? N8 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? N10 C43 C44 122.1(5) . . ? N10 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C45 C44 C43 120.2(5) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 118.7(4) . . ? C44 C45 H45 120.6 . . ? C46 C45 H45 120.6 . . ? C45 C46 C47 119.0(5) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? N10 C47 C46 121.5(4) . . ? N10 C47 C48 114.0(4) . . ? C46 C47 C48 124.5(4) . . ? N9 C48 C49 122.2(4) . . ? N9 C48 C47 113.9(4) . . ? C49 C48 C47 123.8(4) . . ? C48 C49 C50 120.3(5) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 118.3(5) . . ? C51 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C50 C51 C52 118.8(5) . . ? C50 C51 H51 120.6 . . ? C52 C51 H51 120.6 . . ? N9 C52 C51 123.8(4) . . ? N9 C52 H52 118.1 . . ? C51 C52 H52 118.1 . . ? Cl3 C53 Cl4 115.6(4) . . ? Cl3 C53 H53A 108.4 . . ? Cl4 C53 H53A 108.4 . . ? Cl3 C53 H53B 108.4 . . ? Cl4 C53 H53B 108.4 . . ? H53A C53 H53B 107.4 . . ? Cl6 C54 Cl5 110.6(6) . . ? Cl6 C54 H54A 109.5 . . ? Cl5 C54 H54A 109.5 . . ? Cl6 C54 H54B 109.5 . . ? Cl5 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? O4 Cl1 O6 109.9(3) . . ? O4 Cl1 O3 110.8(4) . . ? O6 Cl1 O3 105.6(3) . . ? O4 Cl1 O5 112.1(3) . . ? O6 Cl1 O5 110.0(3) . . ? O3 Cl1 O5 108.1(2) . . ? O7 Cl2 O10 109.0(4) . . ? O7 Cl2 O8 111.2(3) . . ? O10 Cl2 O8 108.0(3) . . ? O7 Cl2 O9 110.1(3) . . ? O10 Cl2 O9 107.6(3) . . ? O8 Cl2 O9 110.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.354 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.117 # Attachment 'bsokt08_revised_10_04_2009RP.cif' data_1_ClO4 _database_code_depnum_ccdc_archive 'CCDC 727537' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C32 H33 Cl N6 O6 Ru, (C H2 Cl2)' _chemical_formula_sum 'C33 H35 Cl3 N6 O6 Ru' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour red _diffrn_ambient_temperature 100(2) _chemical_formula_weight 819.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru1 Ru1 -1.2594 0.8363 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 9.8944(2) _cell_length_b 18.0252(2) _cell_length_c 19.8545(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.2600(10) _cell_angle_gamma 90.00 _cell_volume 3494.87(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7212 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.56 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15946 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.87 _reflns_number_total 8319 _reflns_number_gt 6724 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. the dichloromethane molecule was found disordered in two very close positions having equal occupancy factors ; _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^)+(0.0779P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8319 _refine_ls_number_parameters 479 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.191 _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 0.58640(2) 0.602393(11) 0.163281(11) 0.00872(9) Uani 1 1 d . . . N1 N 0.6987(2) 0.69983(12) 0.17527(11) 0.0114(5) Uani 1 1 d . . . N2 N 0.6914(3) 0.94826(13) 0.08047(13) 0.0156(5) Uani 1 1 d . . . N3 N 0.6949(2) 0.55811(12) 0.09226(11) 0.0107(5) Uani 1 1 d . . . N4 N 0.4819(2) 0.50424(12) 0.13796(11) 0.0107(5) Uani 1 1 d . . . N5 N 0.6609(2) 0.54307(12) 0.24947(12) 0.0116(5) Uani 1 1 d . . . N6 N 0.4701(2) 0.64285(12) 0.23157(12) 0.0118(5) Uani 1 1 d . . . O1 O 0.48724(19) 0.66686(10) 0.08409(10) 0.0120(4) Uani 1 1 d . . . O2 O 0.4541(2) 0.91303(11) 0.00370(10) 0.0169(4) Uani 1 1 d . . . O3 O 1.0154(2) 0.33308(12) 0.10218(11) 0.0249(5) Uani 1 1 d . . . O4 O 0.8008(2) 0.35508(12) 0.13566(13) 0.0306(6) Uani 1 1 d . . . O5 O 0.9999(2) 0.35214(12) 0.21808(11) 0.0268(5) Uani 1 1 d . . . O6 O 0.9635(2) 0.45103(11) 0.14032(11) 0.0213(5) Uani 1 1 d . . . C1 C 0.5283(3) 0.73484(14) 0.08384(14) 0.0106(5) Uani 1 1 d . . . C2 C 0.4629(3) 0.78827(15) 0.04011(14) 0.0134(6) Uani 1 1 d . . . H2 H 0.3852 0.7752 0.0095 0.016 Uiso 1 1 calc R . . C3 C 0.5112(3) 0.86203(15) 0.04077(14) 0.0136(6) Uani 1 1 d . . . C4 C 0.6418(3) 0.87965(15) 0.08802(15) 0.0136(6) Uani 1 1 d . . . C5 C 0.7046(3) 0.82822(14) 0.13389(15) 0.0143(6) Uani 1 1 d . . . H5 H 0.7821 0.8414 0.1646 0.017 Uiso 1 1 calc R . . C6 C 0.6513(3) 0.75458(14) 0.13454(14) 0.0112(5) Uani 1 1 d . . . C7 C 0.8194(3) 0.71295(15) 0.22843(15) 0.0159(6) Uani 1 1 d . . . H7 H 0.8592 0.7607 0.2186 0.019 Uiso 1 1 calc R . . C8 C 0.7737(4) 0.71921(18) 0.29791(16) 0.0260(7) Uani 1 1 d . . . H8A H 0.6935 0.7499 0.2941 0.039 Uiso 1 1 calc R . . H8B H 0.8458 0.7409 0.3300 0.039 Uiso 1 1 calc R . . H8C H 0.7529 0.6707 0.3134 0.039 Uiso 1 1 calc R . . C9 C 0.9301(3) 0.65387(18) 0.22886(18) 0.0254(7) Uani 1 1 d . . . H9A H 0.8915 0.6057 0.2339 0.038 Uiso 1 1 calc R . . H9B H 1.0028 0.6629 0.2662 0.038 Uiso 1 1 calc R . . H9C H 0.9658 0.6559 0.1867 0.038 Uiso 1 1 calc R . . C10 C 0.8246(3) 0.97377(16) 0.11506(15) 0.0170(6) Uani 1 1 d . . . H10 H 0.8894 0.9325 0.1159 0.020 Uiso 1 1 calc R . . C11 C 0.8205(3) 0.99690(16) 0.18865(16) 0.0213(7) Uani 1 1 d . . . H11A H 0.7721 1.0430 0.1890 0.032 Uiso 1 1 calc R . . H11B H 0.9123 1.0028 0.2125 0.032 Uiso 1 1 calc R . . H11C H 0.7745 0.9594 0.2108 0.032 Uiso 1 1 calc R . . C12 C 0.8741(4) 1.03665(17) 0.07410(18) 0.0274(8) Uani 1 1 d . . . H12A H 0.8818 1.0192 0.0292 0.041 Uiso 1 1 calc R . . H12B H 0.9620 1.0535 0.0965 0.041 Uiso 1 1 calc R . . H12C H 0.8098 1.0769 0.0707 0.041 Uiso 1 1 calc R . . C13 C 0.7942(3) 0.59284(15) 0.06496(15) 0.0133(6) Uani 1 1 d . . . H13 H 0.8247 0.6387 0.0827 0.016 Uiso 1 1 calc R . . C14 C 0.8528(3) 0.56405(16) 0.01239(15) 0.0158(6) Uani 1 1 d . . . H14 H 0.9213 0.5898 -0.0047 0.019 Uiso 1 1 calc R . . C15 C 0.8076(3) 0.49569(16) -0.01471(15) 0.0162(6) Uani 1 1 d . . . H15 H 0.8462 0.4747 -0.0499 0.019 Uiso 1 1 calc R . . C16 C 0.7046(3) 0.45947(16) 0.01128(14) 0.0135(6) Uani 1 1 d . . . H16 H 0.6726 0.4139 -0.0065 0.016 Uiso 1 1 calc R . . C17 C 0.6487(3) 0.49173(14) 0.06464(13) 0.0102(5) Uani 1 1 d . . . C18 C 0.5359(3) 0.45911(14) 0.09409(13) 0.0094(5) Uani 1 1 d . . . C19 C 0.4852(3) 0.38803(15) 0.07924(15) 0.0136(6) Uani 1 1 d . . . H19 H 0.5226 0.3581 0.0488 0.016 Uiso 1 1 calc R . . C20 C 0.3789(3) 0.36231(15) 0.11001(15) 0.0165(6) Uani 1 1 d . . . H20 H 0.3437 0.3150 0.1003 0.020 Uiso 1 1 calc R . . C21 C 0.3249(3) 0.40747(15) 0.15547(16) 0.0168(6) Uani 1 1 d . . . H21 H 0.2541 0.3909 0.1773 0.020 Uiso 1 1 calc R . . C22 C 0.3787(3) 0.47772(15) 0.16759(14) 0.0132(6) Uani 1 1 d . . . H22 H 0.3419 0.5083 0.1977 0.016 Uiso 1 1 calc R . . C23 C 0.7525(3) 0.48691(15) 0.25265(15) 0.0144(6) Uani 1 1 d . . . H23 H 0.7959 0.4784 0.2152 0.017 Uiso 1 1 calc R . . C24 C 0.7843(3) 0.44170(16) 0.30902(16) 0.0186(6) Uani 1 1 d . . . H24 H 0.8480 0.4037 0.3094 0.022 Uiso 1 1 calc R . . C25 C 0.7199(3) 0.45394(16) 0.36506(16) 0.0202(7) Uani 1 1 d . . . H25 H 0.7395 0.4240 0.4035 0.024 Uiso 1 1 calc R . . C26 C 0.6263(3) 0.51111(16) 0.36321(15) 0.0173(6) Uani 1 1 d . . . H26 H 0.5832 0.5205 0.4006 0.021 Uiso 1 1 calc R . . C27 C 0.5975(3) 0.55445(15) 0.30454(14) 0.0123(6) Uani 1 1 d . . . C28 C 0.4976(3) 0.61566(15) 0.29637(14) 0.0124(6) Uani 1 1 d . . . C29 C 0.4378(3) 0.64522(16) 0.34904(15) 0.0180(6) Uani 1 1 d . . . H29 H 0.4587 0.6261 0.3930 0.022 Uiso 1 1 calc R . . C30 C 0.3471(3) 0.70342(17) 0.33535(16) 0.0208(7) Uani 1 1 d . . . H30 H 0.3073 0.7246 0.3702 0.025 Uiso 1 1 calc R . . C31 C 0.3157(3) 0.73007(16) 0.26921(16) 0.0201(7) Uani 1 1 d . . . H31 H 0.2533 0.7686 0.2590 0.024 Uiso 1 1 calc R . . C32 C 0.3782(3) 0.69875(15) 0.21872(15) 0.0163(6) Uani 1 1 d . . . H32 H 0.3564 0.7166 0.1744 0.020 Uiso 1 1 calc R . . Cl1 Cl 0.94453(7) 0.37294(4) 0.14891(4) 0.01588(16) Uani 1 1 d . . . Cl3A Cl 1.1076(6) 0.1697(2) 0.0141(3) 0.0340(7) Uani 0.50 1 d PU A 2 Cl2B Cl 0.9201(9) 0.2483(4) -0.0909(3) 0.0776(19) Uani 0.50 1 d PU A 2 Cl3B Cl 1.1364(7) 0.1735(4) 0.0173(3) 0.082(2) Uani 0.50 1 d PU B 1 Cl2A Cl 0.9359(9) 0.2326(4) -0.0934(3) 0.0531(13) Uani 0.50 1 d PU B 1 C33A C 0.960(3) 0.2073(15) -0.0036(8) 0.032(2) Uani 0.50 1 d PU B 1 H33A H 0.8958 0.1689 0.0043 0.038 Uiso 0.50 1 calc PR B 1 H33B H 0.9463 0.2501 0.0242 0.038 Uiso 0.50 1 calc PR B 1 C33B C 0.946(3) 0.2107(18) -0.0163(10) 0.044(2) Uani 0.50 1 d PU A 2 H33C H 0.8770 0.1727 -0.0156 0.053 Uiso 0.50 1 calc PR A 2 H33D H 0.9300 0.2483 0.0164 0.053 Uiso 0.50 1 calc PR A 2 H1N H 0.647(3) 0.9726(18) 0.0500(17) 0.017(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01148(13) 0.00757(13) 0.00691(13) -0.00002(8) 0.00085(8) -0.00071(7) N1 0.0146(12) 0.0087(10) 0.0103(11) -0.0010(9) 0.0000(9) -0.0015(9) N2 0.0169(13) 0.0112(11) 0.0176(13) 0.0041(10) -0.0007(10) -0.0002(10) N3 0.0102(11) 0.0115(11) 0.0097(11) 0.0023(9) -0.0008(9) 0.0016(9) N4 0.0115(11) 0.0116(11) 0.0087(11) 0.0010(9) 0.0005(9) -0.0002(9) N5 0.0118(12) 0.0111(11) 0.0113(11) -0.0007(9) 0.0006(9) -0.0020(9) N6 0.0138(12) 0.0097(11) 0.0118(11) -0.0019(9) 0.0023(9) -0.0019(9) O1 0.0154(10) 0.0104(9) 0.0094(9) 0.0009(7) -0.0001(8) -0.0007(7) O2 0.0262(12) 0.0119(9) 0.0114(10) 0.0020(8) -0.0002(9) 0.0044(8) O3 0.0329(13) 0.0236(11) 0.0196(12) -0.0003(9) 0.0088(10) 0.0055(10) O4 0.0163(12) 0.0276(12) 0.0470(16) 0.0172(11) 0.0023(11) -0.0031(9) O5 0.0344(14) 0.0285(12) 0.0167(11) 0.0063(9) 0.0016(10) 0.0154(10) O6 0.0223(12) 0.0139(10) 0.0271(12) 0.0050(9) 0.0020(10) 0.0001(8) C1 0.0141(14) 0.0102(13) 0.0078(13) -0.0023(10) 0.0023(11) -0.0005(10) C2 0.0162(14) 0.0143(13) 0.0088(13) -0.0012(11) -0.0009(11) 0.0001(11) C3 0.0200(15) 0.0130(14) 0.0083(13) -0.0001(11) 0.0042(11) 0.0032(11) C4 0.0181(15) 0.0103(13) 0.0129(14) 0.0008(11) 0.0044(12) 0.0022(11) C5 0.0165(15) 0.0120(13) 0.0135(14) 0.0004(11) -0.0004(11) -0.0023(11) C6 0.0137(14) 0.0106(12) 0.0096(13) -0.0011(10) 0.0023(11) 0.0000(10) C7 0.0180(15) 0.0102(13) 0.0166(15) 0.0008(11) -0.0060(12) -0.0057(11) C8 0.0310(19) 0.0286(17) 0.0163(16) -0.0055(14) -0.0019(14) -0.0092(14) C9 0.0185(16) 0.0252(17) 0.0291(18) 0.0027(14) -0.0070(14) -0.0006(13) C10 0.0172(15) 0.0136(14) 0.0203(16) 0.0039(12) 0.0033(12) -0.0019(11) C11 0.0260(17) 0.0132(14) 0.0243(17) -0.0010(12) 0.0027(13) -0.0003(12) C12 0.0282(19) 0.0189(15) 0.036(2) 0.0075(14) 0.0083(16) -0.0035(13) C13 0.0127(14) 0.0129(13) 0.0139(14) 0.0037(11) 0.0011(11) -0.0012(10) C14 0.0135(14) 0.0181(14) 0.0164(14) 0.0062(12) 0.0039(11) 0.0016(11) C15 0.0135(15) 0.0228(15) 0.0126(14) 0.0027(12) 0.0029(11) 0.0070(11) C16 0.0134(14) 0.0160(13) 0.0101(13) -0.0006(11) -0.0004(11) 0.0032(11) C17 0.0125(13) 0.0093(12) 0.0079(12) 0.0025(10) -0.0008(10) 0.0019(10) C18 0.0104(13) 0.0102(12) 0.0065(12) 0.0012(10) -0.0021(10) 0.0015(10) C19 0.0171(15) 0.0105(13) 0.0120(14) -0.0008(11) -0.0009(11) 0.0015(10) C20 0.0197(15) 0.0131(14) 0.0157(15) -0.0002(11) -0.0003(12) -0.0043(11) C21 0.0176(15) 0.0178(15) 0.0155(15) 0.0027(11) 0.0039(12) -0.0057(11) C22 0.0152(14) 0.0152(14) 0.0098(13) -0.0007(11) 0.0040(11) -0.0023(10) C23 0.0147(14) 0.0139(13) 0.0146(14) 0.0023(11) 0.0026(11) 0.0001(11) C24 0.0167(15) 0.0177(15) 0.0202(16) 0.0018(12) -0.0006(12) 0.0039(11) C25 0.0239(17) 0.0196(15) 0.0165(15) 0.0089(12) 0.0010(13) 0.0015(12) C26 0.0200(16) 0.0202(15) 0.0122(14) 0.0015(12) 0.0039(12) -0.0003(12) C27 0.0151(14) 0.0120(13) 0.0095(13) -0.0017(11) 0.0011(11) -0.0029(10) C28 0.0144(14) 0.0116(13) 0.0110(13) -0.0016(10) 0.0013(11) -0.0029(10) C29 0.0249(16) 0.0181(15) 0.0111(14) -0.0012(12) 0.0035(12) -0.0016(12) C30 0.0277(18) 0.0181(15) 0.0176(15) -0.0052(12) 0.0066(13) 0.0034(13) C31 0.0219(16) 0.0166(15) 0.0227(17) -0.0032(12) 0.0066(13) 0.0061(12) C32 0.0194(15) 0.0140(14) 0.0153(14) 0.0013(11) 0.0026(12) 0.0032(11) Cl1 0.0152(3) 0.0155(3) 0.0172(4) 0.0052(3) 0.0031(3) 0.0029(3) Cl3A 0.0335(17) 0.0386(13) 0.0318(15) 0.0025(11) 0.0111(11) 0.0021(10) Cl2B 0.070(3) 0.099(4) 0.054(3) 0.051(3) -0.021(2) -0.035(3) Cl3B 0.062(4) 0.144(4) 0.047(2) -0.042(2) 0.028(2) -0.016(2) Cl2A 0.061(2) 0.052(2) 0.050(2) -0.0114(19) 0.020(2) -0.0070(16) C33A 0.050(5) 0.033(3) 0.013(5) -0.001(4) 0.007(4) -0.007(3) C33B 0.053(5) 0.043(4) 0.036(5) 0.003(5) 0.005(5) -0.010(4) _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 N6 2.048(2) . ? Ru1 N5 2.052(2) . ? Ru1 N3 2.065(2) . ? Ru1 N4 2.070(2) . ? Ru1 O1 2.0709(18) . ? Ru1 N1 2.071(2) . ? N1 C6 1.314(3) . ? N1 C7 1.480(3) . ? N2 C4 1.348(4) . ? N2 C10 1.459(4) . ? N2 H1N 0.82(3) . ? N3 C13 1.350(4) . ? N3 C17 1.364(3) . ? N4 C22 1.345(4) . ? N4 C18 1.362(3) . ? N5 C23 1.353(4) . ? N5 C27 1.361(4) . ? N6 C32 1.354(4) . ? N6 C28 1.363(4) . ? O1 C1 1.291(3) . ? O2 C3 1.254(3) . ? O3 Cl1 1.442(2) . ? O4 Cl1 1.440(2) . ? O5 Cl1 1.444(2) . ? O6 Cl1 1.434(2) . ? C1 C2 1.385(4) . ? C1 C6 1.492(4) . ? C2 C3 1.412(4) . ? C2 H2 0.9300 . ? C3 C4 1.503(4) . ? C4 C5 1.376(4) . ? C5 C6 1.429(4) . ? C5 H5 0.9300 . ? C7 C8 1.523(4) . ? C7 C9 1.527(4) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.521(4) . ? C10 C11 1.526(4) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.374(4) . ? C13 H13 0.9300 . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.378(4) . ? C15 H15 0.9300 . ? C16 C17 1.398(4) . ? C16 H16 0.9300 . ? C17 C18 1.464(4) . ? C18 C19 1.390(4) . ? C19 C20 1.379(4) . ? C19 H19 0.9300 . ? C20 C21 1.385(4) . ? C20 H20 0.9300 . ? C21 C22 1.380(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.379(4) . ? C23 H23 0.9300 . ? C24 C25 1.386(4) . ? C24 H24 0.9300 . ? C25 C26 1.382(4) . ? C25 H25 0.9300 . ? C26 C27 1.394(4) . ? C26 H26 0.9300 . ? C27 C28 1.473(4) . ? C28 C29 1.388(4) . ? C29 C30 1.379(4) . ? C29 H29 0.9300 . ? C30 C31 1.386(4) . ? C30 H30 0.9300 . ? C31 C32 1.380(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? Cl3A C33B 1.77(3) . ? Cl2B C33B 1.61(2) . ? Cl3B C33A 1.83(3) . ? Cl2A C33A 1.818(17) . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C33B H33C 0.9700 . ? C33B H33D 0.9700 . ? 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 N6 Ru1 N5 78.36(9) . . ? N6 Ru1 N3 176.96(9) . . ? N5 Ru1 N3 102.21(9) . . ? N6 Ru1 N4 98.82(9) . . ? N5 Ru1 N4 81.69(9) . . ? N3 Ru1 N4 78.36(9) . . ? N6 Ru1 O1 93.14(8) . . ? N5 Ru1 O1 171.30(9) . . ? N3 Ru1 O1 86.18(8) . . ? N4 Ru1 O1 97.94(8) . . ? N6 Ru1 N1 88.27(9) . . ? N5 Ru1 N1 103.42(9) . . ? N3 Ru1 N1 94.48(9) . . ? N4 Ru1 N1 172.04(9) . . ? O1 Ru1 N1 77.95(8) . . ? C6 N1 C7 119.1(2) . . ? C6 N1 Ru1 115.77(18) . . ? C7 N1 Ru1 125.01(17) . . ? C4 N2 C10 123.7(2) . . ? C4 N2 H1N 114(2) . . ? C10 N2 H1N 121(2) . . ? C13 N3 C17 117.6(2) . . ? C13 N3 Ru1 125.94(18) . . ? C17 N3 Ru1 115.84(18) . . ? C22 N4 C18 118.1(2) . . ? C22 N4 Ru1 125.59(19) . . ? C18 N4 Ru1 115.70(18) . . ? C23 N5 C27 117.8(2) . . ? C23 N5 Ru1 125.2(2) . . ? C27 N5 Ru1 116.18(18) . . ? C32 N6 C28 118.1(2) . . ? C32 N6 Ru1 124.90(19) . . ? C28 N6 Ru1 116.70(18) . . ? C1 O1 Ru1 115.12(16) . . ? O1 C1 C2 123.1(2) . . ? O1 C1 C6 116.5(2) . . ? C2 C1 C6 120.3(2) . . ? C1 C2 C3 121.7(3) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? O2 C3 C2 124.4(3) . . ? O2 C3 C4 118.2(2) . . ? C2 C3 C4 117.4(2) . . ? N2 C4 C5 123.9(3) . . ? N2 C4 C3 114.6(2) . . ? C5 C4 C3 121.5(2) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 127.4(3) . . ? N1 C6 C1 114.0(2) . . ? C5 C6 C1 118.5(2) . . ? N1 C7 C8 109.5(2) . . ? N1 C7 C9 112.9(2) . . ? C8 C7 C9 111.3(3) . . ? N1 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? 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 . . ? N2 C10 C12 109.1(2) . . ? N2 C10 C11 112.1(3) . . ? C12 C10 C11 111.6(3) . . ? N2 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 123.6(3) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N3 C17 C16 121.4(3) . . ? N3 C17 C18 114.8(2) . . ? C16 C17 C18 123.8(2) . . ? N4 C18 C19 121.4(3) . . ? N4 C18 C17 114.7(2) . . ? C19 C18 C17 123.9(3) . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 118.3(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N4 C22 C21 123.3(3) . . ? N4 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N5 C23 C24 122.9(3) . . ? N5 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C23 C24 C25 118.9(3) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 119.3(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 119.1(3) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N5 C27 C26 121.9(3) . . ? N5 C27 C28 114.4(2) . . ? C26 C27 C28 123.8(3) . . ? N6 C28 C29 122.0(3) . . ? N6 C28 C27 113.7(2) . . ? C29 C28 C27 124.4(3) . . ? C30 C29 C28 119.1(3) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 119.2(3) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? N6 C32 C31 122.2(3) . . ? N6 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? O6 Cl1 O4 110.00(13) . . ? O6 Cl1 O3 109.03(13) . . ? O4 Cl1 O3 109.83(15) . . ? O6 Cl1 O5 109.35(13) . . ? O4 Cl1 O5 109.14(15) . . ? O3 Cl1 O5 109.48(13) . . ? Cl2A C33A Cl3B 106.0(13) . . ? Cl2A C33A H33A 110.5 . . ? Cl3B C33A H33A 110.5 . . ? Cl2A C33A H33B 110.5 . . ? Cl3B C33A H33B 110.5 . . ? H33A C33A H33B 108.7 . . ? Cl2B C33B Cl3A 119.3(18) . . ? Cl2B C33B H33C 107.5 . . ? Cl3A C33B H33C 107.5 . . ? Cl2B C33B H33D 107.5 . . ? Cl3A C33B H33D 107.5 . . ? H33C C33B H33D 107.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.088 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.257