Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Lahiri, Goutam Kumar' 'Laye, Rebecca H.' 'Mondal, Biplab' 'Puranik, Vedavati G.' 'Sarkar, Biprajit' 'Ward, Mike' _publ_contact_author_name 'Prof GOUTAM KUMAR LAHIRI' _publ_contact_author_address ; Chemistry Indian Institute of Technology, Bombay Powai, Mumbai-400076, India Mumbai Maharashtra 400 076 INDIA ; _publ_contact_author_email 'lahiri@ether.chem.iitb.ernet.in' _publ_contact_author_fax ' 91-022-5723480 ' _publ_contact_author_phone ' 91-022-5767159 ' _publ_section_title ; Synthesis and spectroelectrochemical properties of a dinuclear ruthenium complex exhibiting a strong electronic interaction across a 1,2,4,5-tetrazine bridging ligand ; data_C12_H16_N8 #(H2L) _database_code_CSD 170798 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12 H16 N8' _chemical_formula_sum 'C12 H16 N8' _chemical_formula_weight 272.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 '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' '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 'P21/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 11.1301(8) _cell_length_b 11.0060(9) _cell_length_c 11.4837(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.492(7) _cell_angle_gamma 90.00 _cell_volume 1383.21(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22 _cell_measurement_theta_max 30 _exptl_crystal_description 'rod like' _exptl_crystal_colour ? _exptl_crystal_size_max '0.45' _exptl_crystal_size_mid '0.35' _exptl_crystal_size_min '0.35' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q-scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% '<4%' _diffrn_reflns_number 2434 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.92 _reflns_number_total 2434 _reflns_number_gt 1955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 (MACH-3) Software' _computing_data_reduction 'NRCVAX (PC Version) Gabe, E. J. et al., 1989)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, L and Pritzkow, H, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+0.5404P] 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 SHELXL _refine_ls_extinction_coef 0.039(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2434 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.60694(16) 0.08115(17) 1.18707(15) 0.0450(5) Uani 1 d . . . N2 N 0.57494(15) 0.14521(15) 1.08247(14) 0.0392(4) Uani 1 d . . . N3 N 0.78310(15) 0.13326(17) 1.06440(15) 0.0442(5) Uani 1 d . . . H3 H 0.7931 0.0613 1.0938 0.053 Uiso 1 calc R . . N4 N 0.88327(16) 0.21134(17) 1.05280(15) 0.0449(5) Uani 1 d . . . N5 N 0.75010(16) 0.26852(17) 0.87943(15) 0.0454(5) Uani 1 d . . . H5 H 0.7440 0.2731 0.8038 0.055 Uiso 1 calc R . . N6 N 0.64606(16) 0.25608(18) 0.93624(16) 0.0458(5) Uani 1 d . . . N7 N 0.95256(15) 0.34389(16) 0.92179(14) 0.0404(4) Uani 1 d . . . N8 N 0.92349(17) 0.41162(17) 0.81932(15) 0.0460(5) Uani 1 d . . . C1 C 0.45053(19) 0.1457(2) 1.04368(19) 0.0434(5) Uani 1 d . . . C2 C 0.4031(2) 0.0819(2) 1.1270(2) 0.0490(6) Uani 1 d . . . H2 H 0.3209 0.0666 1.1265 0.059 Uiso 1 calc R . . C3 C 0.5019(2) 0.0439(2) 1.21338(19) 0.0460(5) Uani 1 d . . . C4 C 0.66903(18) 0.18316(18) 1.02432(17) 0.0380(5) Uani 1 d . . . C5 C 0.86043(18) 0.27252(18) 0.95623(17) 0.0381(5) Uani 1 d . . . C6 C 1.07399(19) 0.3548(2) 0.97221(19) 0.0472(6) Uani 1 d . . . C7 C 1.1223(2) 0.4316(2) 0.8994(2) 0.0542(6) Uani 1 d . . . H7 H 1.2030 0.4575 0.9094 0.065 Uiso 1 calc R . . C8 C 1.0277(2) 0.4641(2) 0.8070(2) 0.0491(6) Uani 1 d . . . C9 C 0.3876(2) 0.2065(2) 0.9323(2) 0.0560(6) Uani 1 d . . . H9A H 0.3900 0.2930 0.9432 0.084 Uiso 1 calc R . . H9B H 0.3041 0.1799 0.9141 0.084 Uiso 1 calc R . . H9C H 0.4283 0.1854 0.8683 0.084 Uiso 1 calc R . . C10 C 0.5004(3) -0.0308(3) 1.3227(2) 0.0660(7) Uani 1 d . . . H10A H 0.5820 -0.0382 1.3668 0.099 Uiso 1 calc R . . H10B H 0.4684 -0.1101 1.3003 0.099 Uiso 1 calc R . . H10C H 0.4497 0.0082 1.3708 0.099 Uiso 1 calc R . . C11 C 1.1335(2) 0.2910(3) 1.0825(2) 0.0628(7) Uani 1 d . . . H11A H 1.0910 0.3103 1.1457 0.094 Uiso 1 calc R . . H11B H 1.2171 0.3167 1.1034 0.094 Uiso 1 calc R . . H11C H 1.1307 0.2048 1.0692 0.094 Uiso 1 calc R . . C12 C 1.0333(3) 0.5462(3) 0.7036(2) 0.0693(8) Uani 1 d . . . H12A H 1.0869 0.5116 0.6558 0.104 Uiso 1 calc R . . H12B H 1.0636 0.6244 0.7321 0.104 Uiso 1 calc R . . H12C H 0.9530 0.5549 0.6570 0.104 Uiso 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 N1 0.0503(10) 0.0524(11) 0.0334(9) 0.0013(8) 0.0101(7) -0.0055(8) N2 0.0430(9) 0.0427(9) 0.0333(9) -0.0010(7) 0.0107(7) -0.0016(7) N3 0.0436(10) 0.0452(10) 0.0452(10) 0.0098(8) 0.0118(8) 0.0011(8) N4 0.0414(10) 0.0571(11) 0.0368(10) 0.0060(8) 0.0088(7) -0.0032(8) N5 0.0445(10) 0.0621(12) 0.0308(9) 0.0038(8) 0.0095(7) -0.0021(8) N6 0.0405(9) 0.0568(11) 0.0412(10) 0.0076(8) 0.0108(8) 0.0003(8) N7 0.0443(10) 0.0436(10) 0.0350(9) -0.0004(7) 0.0117(7) -0.0024(7) N8 0.0574(11) 0.0498(11) 0.0325(9) 0.0011(8) 0.0129(8) -0.0064(8) C1 0.0408(11) 0.0449(12) 0.0462(12) -0.0085(9) 0.0127(9) 0.0017(9) C2 0.0433(12) 0.0514(13) 0.0564(13) -0.0052(10) 0.0198(10) -0.0040(9) C3 0.0530(12) 0.0460(12) 0.0435(12) -0.0041(10) 0.0208(10) -0.0065(10) C4 0.0416(11) 0.0419(11) 0.0313(10) -0.0020(8) 0.0086(8) -0.0014(8) C5 0.0416(11) 0.0441(11) 0.0308(10) -0.0024(8) 0.0123(8) 0.0006(8) C6 0.0415(12) 0.0510(13) 0.0513(13) -0.0030(10) 0.0147(9) 0.0028(9) C7 0.0458(12) 0.0567(14) 0.0644(15) -0.0024(12) 0.0213(11) -0.0056(10) C8 0.0584(14) 0.0479(12) 0.0465(12) -0.0045(10) 0.0240(11) -0.0089(10) C9 0.0446(13) 0.0678(16) 0.0551(14) 0.0041(12) 0.0078(10) 0.0097(11) C10 0.0761(18) 0.0709(17) 0.0577(16) 0.0093(13) 0.0299(13) -0.0062(14) C11 0.0438(13) 0.0730(17) 0.0712(17) 0.0138(14) 0.0088(11) 0.0075(12) C12 0.0842(19) 0.0723(17) 0.0574(15) 0.0064(13) 0.0285(14) -0.0199(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 N1 C3 1.325(3) . ? N1 N2 1.382(2) . ? N2 C1 1.375(3) . ? N2 C4 1.404(3) . ? N3 C4 1.383(3) . ? N3 N4 1.433(2) . ? N3 H3 0.8600 . ? N4 C5 1.283(3) . ? N5 C5 1.376(3) . ? N5 N6 1.435(2) . ? N5 H5 0.8600 . ? N6 C4 1.280(3) . ? N7 C6 1.375(3) . ? N7 N8 1.381(2) . ? N7 C5 1.405(3) . ? N8 C8 1.326(3) . ? C1 C2 1.368(3) . ? C1 C9 1.499(3) . ? C2 C3 1.403(3) . ? C2 H2 0.9300 . ? C3 C10 1.503(3) . ? C6 C7 1.366(3) . ? C6 C11 1.494(3) . ? C7 C8 1.398(3) . ? C7 H7 0.9300 . ? C8 C12 1.502(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 C3 N1 N2 104.92(17) . . ? C1 N2 N1 111.62(16) . . ? C1 N2 C4 129.71(17) . . ? N1 N2 C4 117.93(16) . . ? C4 N3 N4 114.43(16) . . ? C4 N3 H3 122.8 . . ? N4 N3 H3 122.8 . . ? C5 N4 N3 111.11(16) . . ? C5 N5 N6 114.29(16) . . ? C5 N5 H5 122.9 . . ? N6 N5 H5 122.9 . . ? C4 N6 N5 110.94(17) . . ? C6 N7 N8 111.81(17) . . ? C6 N7 C5 129.95(18) . . ? N8 N7 C5 118.18(17) . . ? C8 N8 N7 104.61(18) . . ? C2 C1 N2 105.37(19) . . ? C2 C1 C9 130.2(2) . . ? N2 C1 C9 124.39(19) . . ? C1 C2 C3 107.20(19) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 126.4 . . ? N1 C3 C2 110.88(19) . . ? N1 C3 C10 120.3(2) . . ? C2 C3 C10 128.8(2) . . ? N6 C4 N3 123.44(18) . . ? N6 C4 N2 120.22(18) . . ? N3 C4 N2 116.28(17) . . ? N4 C5 N5 123.41(19) . . ? N4 C5 N7 119.81(18) . . ? N5 C5 N7 116.71(17) . . ? C7 C6 N7 105.2(2) . . ? C7 C6 C11 130.3(2) . . ? N7 C6 C11 124.5(2) . . ? C6 C7 C8 107.3(2) . . ? C6 C7 H7 126.4 . . ? C8 C7 H7 126.4 . . ? N8 C8 C7 111.1(2) . . ? N8 C8 C12 120.6(2) . . ? C7 C8 C12 128.3(2) . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 C3 N1 N2 C1 -0.9(2) . . . . ? C3 N1 N2 C4 -172.03(17) . . . . ? C4 N3 N4 C5 -37.9(2) . . . . ? C5 N5 N6 C4 -39.2(3) . . . . ? C6 N7 N8 C8 0.1(2) . . . . ? C5 N7 N8 C8 -177.33(17) . . . . ? N1 N2 C1 C2 0.9(2) . . . . ? C4 N2 C1 C2 170.7(2) . . . . ? N1 N2 C1 C9 -179.35(19) . . . . ? C4 N2 C1 C9 -9.6(3) . . . . ? N2 C1 C2 C3 -0.6(2) . . . . ? C9 C1 C2 C3 179.7(2) . . . . ? N2 N1 C3 C2 0.5(2) . . . . ? N2 N1 C3 C10 179.51(19) . . . . ? C1 C2 C3 N1 0.0(3) . . . . ? C1 C2 C3 C10 -178.8(2) . . . . ? N5 N6 C4 N3 5.6(3) . . . . ? N5 N6 C4 N2 -171.36(17) . . . . ? N4 N3 C4 N6 33.9(3) . . . . ? N4 N3 C4 N2 -148.99(17) . . . . ? C1 N2 C4 N6 20.0(3) . . . . ? N1 N2 C4 N6 -170.72(18) . . . . ? C1 N2 C4 N3 -157.2(2) . . . . ? N1 N2 C4 N3 12.1(3) . . . . ? N3 N4 C5 N5 4.3(3) . . . . ? N3 N4 C5 N7 -172.68(17) . . . . ? N6 N5 C5 N4 35.4(3) . . . . ? N6 N5 C5 N7 -147.56(17) . . . . ? C6 N7 C5 N4 5.3(3) . . . . ? N8 N7 C5 N4 -177.90(18) . . . . ? C6 N7 C5 N5 -171.9(2) . . . . ? N8 N7 C5 N5 4.9(3) . . . . ? N8 N7 C6 C7 0.1(2) . . . . ? C5 N7 C6 C7 177.08(19) . . . . ? N8 N7 C6 C11 -179.0(2) . . . . ? C5 N7 C6 C11 -2.0(4) . . . . ? N7 C6 C7 C8 -0.2(2) . . . . ? C11 C6 C7 C8 178.8(2) . . . . ? N7 N8 C8 C7 -0.2(2) . . . . ? N7 N8 C8 C12 179.8(2) . . . . ? C6 C7 C8 N8 0.2(3) . . . . ? C6 C7 C8 C12 -179.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.449 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.048 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Lahiri, Goutam Kumar' 'Laye, Rebecca H.' 'Mondal, Biplab' 'Puranik, Vedavati G.' 'Sarkar, Biprajit' 'Ward, Mike' _publ_contact_author_name 'Prof Goutam Kumar Lahiri' _publ_contact_author_address ; Chemistry Indian Institute of Technology, Bombay Powai, Mumbai-400076, India Mumbai Maharashtra 400 076 INDIA ; _publ_contact_author_email 'LAHIRI@ETHER.CHEM.IITB.AC.IN' _publ_section_title ; Synthesis and spectroelectrochemical properties of a dinuclear ruthenium complex exhibiting a strong electronic interaction across a 1,2,4,5-tetrazine bridging ligand ; data_Cif_for_1 _database_code_CSD 178079 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H50 Cl4 N16 O18 Ru2' _chemical_formula_weight 1531.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 23.861(3) _cell_length_b 13.452(2) _cell_length_c 19.238(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6175.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 0.746 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19343 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 20.03 _reflns_number_total 5758 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1406P)^2^+31.1737P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.32(11) _refine_ls_number_reflns 5758 _refine_ls_number_parameters 557 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.1977 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.55545(6) 0.21953(11) 0.24675(9) 0.0471(6) Uani 1 1 d . . . Ru2 Ru 0.27953(6) 0.29573(10) 0.23609(10) 0.0370(5) Uani 1 1 d . . . Cl1 Cl 0.3065(7) 0.7880(6) 0.9992(5) 0.176(6) Uani 1 1 d . . . Cl2 Cl 0.4323(3) 0.2698(6) 0.0317(4) 0.080(2) Uani 1 1 d . . . Cl3 Cl 0.3893(4) 0.3017(6) 0.4876(4) 0.089(2) Uani 1 1 d . . . O11 O 0.2609(11) 0.7349(17) 0.9726(16) 0.162(13) Uani 1 1 d . . . O12 O 0.300(2) 0.8863(15) 0.9756(13) 0.28(3) Uani 1 1 d . . . O13 O 0.3182(19) 0.7820(15) 1.0687(14) 0.23(2) Uani 1 1 d . . . O14 O 0.3656(16) 0.732(3) 0.9585(13) 0.221(17) Uani 1 1 d . . . O21 O 0.4270(8) 0.3354(14) 0.0933(9) 0.092(6) Uani 1 1 d . . . O22 O 0.3887(8) 0.2032(14) 0.0378(10) 0.092(6) Uani 1 1 d . . . O23 O 0.4238(12) 0.3237(19) -0.0253(10) 0.128(10) Uani 1 1 d . . . O24 O 0.4826(7) 0.2207(18) 0.0382(15) 0.146(11) Uani 1 1 d . . . O31 O 0.3860(18) 0.216(2) 0.5235(16) 0.24(2) Uani 1 1 d . . . O32 O 0.3475(12) 0.367(2) 0.4874(16) 0.173(12) Uani 1 1 d . . . O33 O 0.4383(11) 0.356(2) 0.5137(18) 0.177(13) Uani 1 1 d . . . O34 O 0.4063(10) 0.2729(18) 0.4196(11) 0.116(8) Uani 1 1 d . . . N1 N 0.4738(6) 0.2407(9) 0.2377(10) 0.034(4) Uani 1 1 d . . . N4 N 0.3625(5) 0.2791(8) 0.2388(10) 0.027(3) Uani 1 1 d U . . N101 N 0.5440(8) 0.3547(12) 0.3010(8) 0.045(5) Uani 1 1 d . . . N102 N 0.4891(7) 0.3814(12) 0.3048(9) 0.044(4) Uani 1 1 d . . . N111 N 0.5431(6) 0.1392(12) 0.3326(8) 0.044(4) Uani 1 1 d D . . N121 N 0.5566(6) 0.0876(11) 0.1975(11) 0.057(6) Uani 1 1 d . . . N131 N 0.6406(10) 0.1919(14) 0.2596(9) 0.081(7) Uani 1 1 d D . . N141 N 0.5823(8) 0.2963(15) 0.1627(11) 0.077(6) Uani 1 1 d D . . N201 N 0.2894(6) 0.1653(11) 0.1877(9) 0.033(4) Uani 1 1 d . . . N202 N 0.3466(6) 0.1328(10) 0.1835(8) 0.031(4) Uani 1 1 d . . . N211 N 0.2909(7) 0.3834(11) 0.1488(11) 0.050(5) Uani 1 1 d . . . N221 N 0.2831(6) 0.4347(13) 0.2848(11) 0.051(5) Uani 1 1 d . . . N231 N 0.1929(6) 0.3055(10) 0.2354(14) 0.058(5) Uani 1 1 d . . . N241 N 0.2602(7) 0.2196(11) 0.3241(8) 0.041(4) Uani 1 1 d . . . C2 C 0.4505(9) 0.3201(14) 0.2698(9) 0.037(5) Uiso 1 1 d . . . N3 N 0.3992(6) 0.3420(10) 0.2712(6) 0.026(4) Uani 1 1 d . . . C5 C 0.3850(8) 0.1974(13) 0.2112(8) 0.028(5) Uiso 1 1 d . . . N6 N 0.4389(7) 0.1767(11) 0.2061(9) 0.043(4) Uani 1 1 d . . . C103 C 0.4845(9) 0.4694(16) 0.3409(11) 0.052(6) Uiso 1 1 d . . . C104 C 0.5369(9) 0.4880(16) 0.3631(11) 0.052(6) Uiso 1 1 d . . . H104 H 0.5474 0.5409 0.3932 0.062 Uiso 1 1 calc R . . C105 C 0.5738(10) 0.4175(17) 0.3351(12) 0.056(6) Uiso 1 1 d . . . C106 C 0.4283(9) 0.5195(17) 0.3553(12) 0.060(6) Uiso 1 1 d . . . H10A H 0.4113 0.5404 0.3113 0.090 Uiso 1 1 calc R . . H10B H 0.4342 0.5777 0.3850 0.090 Uiso 1 1 calc R . . H10C H 0.4033 0.4725 0.3789 0.090 Uiso 1 1 calc R . . C107 C 0.6356(10) 0.4163(18) 0.3386(13) 0.067(7) Uiso 1 1 d . . . H10D H 0.6481 0.3555 0.3621 0.100 Uiso 1 1 calc R . . H10E H 0.6488 0.4745 0.3646 0.100 Uiso 1 1 calc R . . H10F H 0.6511 0.4179 0.2914 0.100 Uiso 1 1 calc R . . C112 C 0.5434(9) 0.0351(15) 0.3203(15) 0.087(9) Uiso 1 1 d D . . C113 C 0.5373(11) -0.035(3) 0.3748(12) 0.130(13) Uiso 1 1 d D . . H113 H 0.5347 -0.1044 0.3651 0.156 Uiso 1 1 calc R . . C114 C 0.5353(10) 0.001(2) 0.4450(14) 0.085(8) Uiso 1 1 d D . . H114 H 0.5389 -0.0449 0.4824 0.102 Uiso 1 1 calc R . . C115 C 0.5281(15) 0.103(2) 0.460(2) 0.163(16) Uiso 1 1 d D . . H115 H 0.5206 0.1264 0.5052 0.195 Uiso 1 1 calc R . . C116 C 0.5327(13) 0.170(3) 0.4019(11) 0.115(11) Uiso 1 1 d D . . H116 H 0.5284 0.2391 0.4107 0.138 Uiso 1 1 calc R . . C122 C 0.5421(11) 0.009(2) 0.2235(17) 0.098(9) Uiso 1 1 d . . . C123 C 0.5400(15) -0.083(3) 0.214(2) 0.137(13) Uiso 1 1 d . . . H123 H 0.5335 -0.1328 0.2484 0.165 Uiso 1 1 calc R . . C124 C 0.5482(10) -0.098(2) 0.1506(15) 0.082(8) Uiso 1 1 d . . . H124 H 0.5444 -0.1637 0.1340 0.099 Uiso 1 1 calc R . . C125 C 0.5625(13) -0.025(2) 0.1022(16) 0.097(10) Uiso 1 1 d . . . H125 H 0.5697 -0.0430 0.0552 0.117 Uiso 1 1 calc R . . C126 C 0.5664(11) 0.080(2) 0.1250(16) 0.082(8) Uiso 1 1 d . . . H126 H 0.5743 0.1346 0.0952 0.098 Uiso 1 1 calc R . . C132 C 0.6732(11) 0.2202(18) 0.2050(14) 0.093(10) Uiso 1 1 d D . . C133 C 0.7277(13) 0.199(2) 0.1939(19) 0.156(16) Uiso 1 1 d D . . H133 H 0.7495 0.2192 0.1550 0.188 Uiso 1 1 calc R . . C134 C 0.7458(10) 0.1441(17) 0.2485(14) 0.084(7) Uiso 1 1 d D . . H134 H 0.7842 0.1261 0.2446 0.101 Uiso 1 1 calc R . . C135 C 0.7218(11) 0.109(2) 0.3076(16) 0.117(11) Uiso 1 1 d D . . H135 H 0.7403 0.0697 0.3418 0.141 Uiso 1 1 calc R . . C136 C 0.6660(11) 0.1382(19) 0.3104(15) 0.097(9) Uiso 1 1 d D . . H136 H 0.6445 0.1199 0.3500 0.117 Uiso 1 1 calc R . . C142 C 0.6372(10) 0.2917(18) 0.1501(13) 0.095(9) Uiso 1 1 d D . . C143 C 0.6583(15) 0.347(2) 0.0981(14) 0.128(12) Uiso 1 1 d D . . H143 H 0.6978 0.3500 0.0929 0.154 Uiso 1 1 calc R . . C144 C 0.6268(12) 0.400(2) 0.0531(19) 0.132(13) Uiso 1 1 d D . . H144 H 0.6425 0.4229 0.0107 0.158 Uiso 1 1 calc R . . C145 C 0.5737(12) 0.419(2) 0.0681(14) 0.105(10) Uiso 1 1 d D . . H145 H 0.5503 0.4633 0.0434 0.126 Uiso 1 1 calc R . . C146 C 0.5582(12) 0.3651(18) 0.1234(13) 0.089(8) Uiso 1 1 d D . . H146 H 0.5211 0.3800 0.1380 0.107 Uiso 1 1 calc R . . C203 C 0.3519(9) 0.0442(16) 0.1463(11) 0.052(6) Uiso 1 1 d . . . C204 C 0.2998(8) 0.0213(15) 0.1270(11) 0.050(6) Uiso 1 1 d . . . H204 H 0.2889 -0.0331 0.0985 0.060 Uiso 1 1 calc R . . C205 C 0.2631(8) 0.0944(15) 0.1573(10) 0.045(6) Uiso 1 1 d . . . C206 C 0.4062(9) -0.0011(18) 0.1324(12) 0.065(7) Uiso 1 1 d . . . H20A H 0.4278 0.0418 0.1012 0.098 Uiso 1 1 calc R . . H20B H 0.4007 -0.0662 0.1105 0.098 Uiso 1 1 calc R . . H20C H 0.4267 -0.0095 0.1762 0.098 Uiso 1 1 calc R . . C207 C 0.1999(9) 0.0949(16) 0.1455(12) 0.061(6) Uiso 1 1 d . . . H20D H 0.1809 0.1152 0.1884 0.091 Uiso 1 1 calc R . . H20E H 0.1875 0.0280 0.1324 0.091 Uiso 1 1 calc R . . H20F H 0.1907 0.1417 0.1082 0.091 Uiso 1 1 calc R . . C212 C 0.3013(10) 0.4802(18) 0.1618(13) 0.065(7) Uiso 1 1 d . . . C213 C 0.3126(11) 0.543(2) 0.1060(14) 0.078(8) Uiso 1 1 d . . . H213 H 0.3209 0.6113 0.1153 0.094 Uiso 1 1 calc R . . C214 C 0.3123(11) 0.513(2) 0.0419(17) 0.098(9) Uiso 1 1 d . . . H214 H 0.3196 0.5587 0.0052 0.118 Uiso 1 1 calc R . . C215 C 0.3017(10) 0.4172(19) 0.0278(14) 0.079(8) Uiso 1 1 d . . . H215 H 0.3013 0.3943 -0.0189 0.095 Uiso 1 1 calc R . . C216 C 0.2913(9) 0.351(2) 0.0826(13) 0.065(7) Uiso 1 1 d . . . H216 H 0.2845 0.2830 0.0730 0.078 Uiso 1 1 calc R . . C222 C 0.2936(7) 0.5078(14) 0.2306(12) 0.047(5) Uiso 1 1 d . . . C223 C 0.3002(10) 0.6045(19) 0.2649(13) 0.077(8) Uiso 1 1 d . . . H223 H 0.3105 0.6591 0.2363 0.093 Uiso 1 1 calc R . . C224 C 0.2933(10) 0.623(2) 0.3316(14) 0.075(8) Uiso 1 1 d . . . H224 H 0.2972 0.6887 0.3485 0.090 Uiso 1 1 calc R . . C225 C 0.2809(9) 0.5498(17) 0.3752(13) 0.061(7) Uiso 1 1 d . . . H225 H 0.2746 0.5632 0.4230 0.073 Uiso 1 1 calc R . . C226 C 0.2772(8) 0.4536(17) 0.3499(12) 0.050(6) Uiso 1 1 d . . . H226 H 0.2702 0.4005 0.3813 0.060 Uiso 1 1 calc R . . C232 C 0.1677(9) 0.2706(16) 0.2953(12) 0.050(6) Uiso 1 1 d . . . C233 C 0.1073(10) 0.2885(17) 0.3049(13) 0.066(7) Uiso 1 1 d . . . H233 H 0.0886 0.2717 0.3469 0.079 Uiso 1 1 calc R . . C234 C 0.0812(10) 0.3287(17) 0.2527(13) 0.075(7) Uiso 1 1 d . . . H234 H 0.0416 0.3312 0.2574 0.090 Uiso 1 1 calc R . . C235 C 0.1007(10) 0.3666(18) 0.1945(13) 0.071(7) Uiso 1 1 d . . . H235 H 0.0783 0.3999 0.1610 0.085 Uiso 1 1 calc R . . C236 C 0.1608(10) 0.3510(19) 0.1878(14) 0.073(7) Uiso 1 1 d . . . H236 H 0.1786 0.3747 0.1468 0.088 Uiso 1 1 calc R . . C242 C 0.2030(9) 0.2215(16) 0.3402(11) 0.055(6) Uiso 1 1 d . . . C243 C 0.1852(11) 0.1772(19) 0.4037(13) 0.076(7) Uiso 1 1 d . . . H243 H 0.1480 0.1862 0.4198 0.091 Uiso 1 1 calc R . . C244 C 0.2222(11) 0.122(2) 0.4408(14) 0.084(8) Uiso 1 1 d . . . H244 H 0.2102 0.0868 0.4811 0.100 Uiso 1 1 calc R . . C245 C 0.2730(12) 0.117(2) 0.4211(15) 0.086(8) Uiso 1 1 d . . . H245 H 0.2979 0.0795 0.4491 0.104 Uiso 1 1 calc R . . C246 C 0.2958(10) 0.1631(17) 0.3623(11) 0.057(6) Uiso 1 1 d . . . H246 H 0.3340 0.1549 0.3498 0.068 Uiso 1 1 calc R . . Cl4A Cl 0.3976(8) 0.891(3) 0.3261(16) 0.195(17) Uani 0.50 1 d P . . Cl4B Cl 0.402(2) 0.851(4) 0.303(2) 0.31(4) Uani 0.50 1 d P . . O42 O 0.3772(19) 0.803(3) 0.239(4) 0.140(15) Uiso 0.50 1 d P . . O41 O 0.3711(18) 0.836(3) 0.365(2) 0.236(16) Uiso 1 1 d . . . O45 O 0.3880(16) 0.968(3) 0.309(2) 0.210(15) Uiso 1 1 d . . . O44 O 0.457(3) 0.870(5) 0.296(3) 0.33(3) Uiso 1 1 d . . . O43 O 0.400(3) 0.926(5) 0.408(4) 0.18(2) Uiso 0.50 1 d P . . O50 O 0.4615(14) 0.528(2) 0.1660(18) 0.197(12) Uiso 1 1 d . . . O51 O 0.6780(16) 0.100(3) 0.015(2) 0.235(16) 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 0.0362(10) 0.0415(10) 0.0636(13) 0.0095(13) -0.0004(10) -0.0011(7) Ru2 0.0351(9) 0.0293(8) 0.0467(10) 0.0065(11) -0.0033(10) 0.0010(6) Cl1 0.396(19) 0.066(6) 0.066(7) 0.007(5) -0.036(9) -0.087(9) Cl2 0.083(6) 0.088(5) 0.069(5) -0.009(5) -0.010(4) -0.013(5) Cl3 0.138(7) 0.064(5) 0.065(5) 0.011(4) -0.022(4) 0.003(5) O11 0.15(2) 0.114(17) 0.23(3) -0.12(2) 0.027(19) -0.057(17) O12 0.74(8) 0.035(13) 0.073(16) 0.010(12) -0.12(3) -0.04(2) O13 0.53(6) 0.053(15) 0.10(2) 0.010(14) 0.01(3) -0.05(2) O14 0.31(4) 0.27(4) 0.091(19) -0.03(2) 0.11(2) 0.04(3) O21 0.109(15) 0.081(13) 0.086(14) -0.015(11) -0.029(10) 0.002(11) O22 0.085(14) 0.087(15) 0.103(15) -0.018(12) -0.015(11) -0.007(12) O23 0.21(3) 0.14(2) 0.031(12) 0.005(13) 0.010(12) -0.101(19) O24 0.026(11) 0.16(2) 0.25(3) -0.10(2) -0.005(13) -0.009(12) O31 0.45(6) 0.15(3) 0.13(2) 0.11(2) 0.04(3) -0.07(3) O32 0.16(2) 0.14(2) 0.21(3) -0.01(2) 0.01(2) 0.09(2) O33 0.14(2) 0.16(3) 0.24(3) -0.08(2) -0.06(2) -0.025(19) O34 0.14(2) 0.128(19) 0.078(16) -0.007(14) 0.024(13) -0.018(16) N1 0.048(9) 0.019(7) 0.037(9) 0.010(10) 0.019(10) 0.010(7) N4 0.018(6) 0.025(6) 0.038(7) 0.021(7) -0.002(7) -0.001(5) N101 0.062(14) 0.043(11) 0.031(10) -0.019(9) 0.015(9) 0.000(10) N102 0.030(11) 0.046(11) 0.058(12) -0.001(9) -0.011(8) -0.005(9) N111 0.064(12) 0.047(11) 0.021(10) 0.013(8) -0.005(8) 0.001(9) N121 0.030(11) 0.015(9) 0.125(18) 0.002(10) 0.007(10) -0.015(7) N131 0.122(18) 0.066(13) 0.056(15) -0.009(12) 0.009(12) 0.020(12) N141 0.049(13) 0.096(16) 0.086(16) 0.026(13) 0.005(11) 0.020(11) N201 0.036(11) 0.014(8) 0.050(11) -0.008(8) -0.006(8) -0.008(7) N202 0.025(10) 0.021(9) 0.049(10) 0.000(8) -0.004(7) 0.001(7) N211 0.059(12) 0.009(9) 0.083(15) 0.001(9) -0.024(10) -0.012(8) N221 0.019(10) 0.036(11) 0.098(16) 0.002(10) 0.006(8) -0.007(8) N231 0.048(10) 0.032(8) 0.092(14) -0.008(12) -0.037(15) -0.001(7) N241 0.055(12) 0.023(9) 0.046(10) 0.001(8) 0.004(9) 0.015(8) N3 0.041(11) 0.019(8) 0.020(8) 0.011(6) -0.004(7) -0.011(7) N6 0.040(11) 0.020(9) 0.069(12) 0.005(8) -0.004(8) -0.014(8) Cl4A 0.055(11) 0.33(4) 0.20(3) 0.21(3) -0.087(14) -0.086(16) Cl4B 0.37(7) 0.32(6) 0.23(4) -0.08(4) 0.16(4) 0.15(5) _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 1.976(14) . ? Ru1 N111 1.995(15) . ? Ru1 N121 2.012(17) . ? Ru1 N141 2.02(2) . ? Ru1 N131 2.08(2) . ? Ru1 N101 2.114(16) . ? Ru2 N4 1.993(11) . ? Ru2 N201 2.000(14) . ? Ru2 N241 2.031(16) . ? Ru2 N211 2.070(18) . ? Ru2 N231 2.072(14) . ? Ru2 N221 2.093(18) . ? Cl1 O13 1.37(3) . ? Cl1 O11 1.40(2) . ? Cl1 O12 1.41(2) . ? Cl1 O14 1.78(3) . ? Cl2 O23 1.33(2) . ? Cl2 O24 1.37(2) . ? Cl2 O22 1.379(19) . ? Cl2 O21 1.483(19) . ? Cl3 O32 1.32(2) . ? Cl3 O31 1.35(2) . ? Cl3 O34 1.42(2) . ? Cl3 O33 1.47(2) . ? N1 N6 1.34(2) . ? N1 C2 1.35(2) . ? N4 C5 1.33(2) . ? N4 N3 1.369(19) . ? N101 C105 1.28(3) . ? N101 N102 1.36(2) . ? N102 C103 1.38(3) . ? N102 C2 1.41(2) . ? N111 C112 1.419(17) . ? N111 C116 1.420(17) . ? N121 C122 1.22(3) . ? N121 C126 1.42(3) . ? N131 C136 1.358(17) . ? N131 C132 1.363(17) . ? N141 C146 1.326(16) . ? N141 C142 1.335(16) . ? N201 C205 1.28(2) . ? N201 N202 1.437(19) . ? N202 C5 1.37(2) . ? N202 C203 1.40(2) . ? N211 C216 1.35(3) . ? N211 C212 1.35(3) . ? N221 C226 1.28(3) . ? N221 C222 1.46(3) . ? N231 C236 1.34(3) . ? N231 C232 1.38(3) . ? N241 C246 1.36(3) . ? N241 C242 1.40(3) . ? C2 N3 1.26(2) . ? C5 N6 1.32(2) . ? C103 C104 1.35(3) . ? C103 C106 1.53(3) . ? C104 C105 1.40(3) . ? C105 C107 1.48(3) . ? C112 C113 1.421(18) . ? C112 C122 1.89(4) . ? C113 C114 1.435(18) . ? C114 C115 1.417(18) . ? C115 C116 1.430(18) . ? C122 C123 1.25(4) . ? C122 C124 2.01(4) . ? C123 C124 1.25(4) . ? C124 C125 1.39(4) . ? C125 C126 1.49(4) . ? C132 C133 1.348(18) . ? C132 C142 1.67(4) . ? C133 C134 1.356(19) . ? C134 C135 1.360(18) . ? C135 C136 1.390(18) . ? C142 C143 1.348(17) . ? C143 C144 1.344(17) . ? C144 C145 1.323(17) . ? C145 C146 1.336(17) . ? C203 C204 1.33(3) . ? C203 C206 1.46(3) . ? C204 C205 1.44(3) . ? C205 C207 1.53(3) . ? C212 C222 1.39(3) . ? C212 C213 1.40(3) . ? C213 C214 1.30(3) . ? C214 C215 1.34(3) . ? C215 C216 1.40(3) . ? C222 C223 1.47(3) . ? C223 C224 1.32(3) . ? C224 C225 1.33(3) . ? C225 C226 1.38(3) . ? C232 C242 1.38(3) . ? C232 C233 1.47(3) . ? C233 C234 1.30(3) . ? C234 C235 1.31(3) . ? C235 C236 1.46(3) . ? C242 C243 1.42(3) . ? C243 C244 1.36(3) . ? C244 C245 1.27(3) . ? C245 C246 1.40(3) . ? Cl4A Cl4B 0.71(6) . ? Cl4A O45 1.11(4) . ? Cl4A O41 1.22(5) . ? Cl4A O44 1.56(7) . ? Cl4A O43 1.64(7) . ? Cl4A O42 2.10(8) . ? Cl4B O44 1.34(7) . ? Cl4B O41 1.42(6) . ? Cl4B O42 1.51(7) . ? Cl4B O45 1.61(6) . ? O41 O43 1.63(7) . ? 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 N111 90.3(7) . . ? N1 Ru1 N121 95.7(6) . . ? N111 Ru1 N121 85.0(8) . . ? N1 Ru1 N141 99.6(7) . . ? N111 Ru1 N141 170.0(7) . . ? N121 Ru1 N141 94.0(8) . . ? N1 Ru1 N131 177.3(7) . . ? N111 Ru1 N131 87.1(7) . . ? N121 Ru1 N131 83.4(7) . . ? N141 Ru1 N131 83.0(7) . . ? N1 Ru1 N101 78.0(7) . . ? N111 Ru1 N101 92.2(6) . . ? N121 Ru1 N101 173.1(7) . . ? N141 Ru1 N101 89.9(7) . . ? N131 Ru1 N101 102.8(7) . . ? N4 Ru2 N201 78.3(6) . . ? N4 Ru2 N241 98.4(7) . . ? N201 Ru2 N241 88.4(7) . . ? N4 Ru2 N211 87.4(6) . . ? N201 Ru2 N211 96.1(7) . . ? N241 Ru2 N211 173.2(7) . . ? N4 Ru2 N231 177.0(6) . . ? N201 Ru2 N231 99.8(6) . . ? N241 Ru2 N231 79.1(8) . . ? N211 Ru2 N231 95.1(8) . . ? N4 Ru2 N221 92.7(6) . . ? N201 Ru2 N221 170.8(6) . . ? N241 Ru2 N221 95.0(7) . . ? N211 Ru2 N221 81.3(8) . . ? N231 Ru2 N221 89.3(6) . . ? O13 Cl1 O11 119(2) . . ? O13 Cl1 O12 113.1(14) . . ? O11 Cl1 O12 106(2) . . ? O13 Cl1 O14 104(2) . . ? O11 Cl1 O14 103.7(17) . . ? O12 Cl1 O14 110(2) . . ? O23 Cl2 O24 118.1(18) . . ? O23 Cl2 O22 108.0(13) . . ? O24 Cl2 O22 109.8(14) . . ? O23 Cl2 O21 108.7(14) . . ? O24 Cl2 O21 106.7(12) . . ? O22 Cl2 O21 104.6(12) . . ? O32 Cl3 O31 121(2) . . ? O32 Cl3 O34 113.0(18) . . ? O31 Cl3 O34 104.8(19) . . ? O32 Cl3 O33 105.9(19) . . ? O31 Cl3 O33 107(2) . . ? O34 Cl3 O33 102.9(18) . . ? N6 N1 C2 117.2(15) . . ? N6 N1 Ru1 124.0(11) . . ? C2 N1 Ru1 118.6(13) . . ? C5 N4 N3 115.6(13) . . ? C5 N4 Ru2 118.9(11) . . ? N3 N4 Ru2 125.4(11) . . ? C105 N101 N102 109.4(16) . . ? C105 N101 Ru1 138.3(16) . . ? N102 N101 Ru1 112.2(12) . . ? N101 N102 C103 109.3(15) . . ? N101 N102 C2 116.7(16) . . ? C103 N102 C2 133.9(18) . . ? C112 N111 C116 116(2) . . ? C112 N111 Ru1 113.3(15) . . ? C116 N111 Ru1 130.2(17) . . ? C122 N121 C126 113(2) . . ? C122 N121 Ru1 125(2) . . ? C126 N121 Ru1 121.9(16) . . ? C136 N131 C132 117(3) . . ? C136 N131 Ru1 128.1(18) . . ? C132 N131 Ru1 114.6(17) . . ? C146 N141 C142 111(2) . . ? C146 N141 Ru1 132.5(18) . . ? C142 N141 Ru1 115.6(16) . . ? C205 N201 N202 102.2(15) . . ? C205 N201 Ru2 143.9(14) . . ? N202 N201 Ru2 113.9(9) . . ? C5 N202 C203 132.8(16) . . ? C5 N202 N201 114.9(13) . . ? C203 N202 N201 112.1(14) . . ? C216 N211 C212 119(2) . . ? C216 N211 Ru2 125.8(14) . . ? C212 N211 Ru2 115.1(17) . . ? C226 N221 C222 125.7(19) . . ? C226 N221 Ru2 127.5(16) . . ? C222 N221 Ru2 106.8(14) . . ? C236 N231 C232 118.5(19) . . ? C236 N231 Ru2 127.0(19) . . ? C232 N231 Ru2 114.0(15) . . ? C246 N241 C242 120.0(18) . . ? C246 N241 Ru2 126.4(15) . . ? C242 N241 Ru2 113.3(12) . . ? N3 C2 N1 126.4(17) . . ? N3 C2 N102 119.3(18) . . ? N1 C2 N102 114.3(18) . . ? C2 N3 N4 118.0(14) . . ? N6 C5 N4 126.6(15) . . ? N6 C5 N202 119.3(16) . . ? N4 C5 N202 114.0(15) . . ? C5 N6 N1 115.9(15) . . ? C104 C103 N102 104.3(18) . . ? C104 C103 C106 133(2) . . ? N102 C103 C106 122.8(19) . . ? C103 C104 C105 110(2) . . ? N101 C105 C104 107(2) . . ? N101 C105 C107 125(2) . . ? C104 C105 C107 128(2) . . ? N111 C112 C113 122(2) . . ? N111 C112 C122 110(2) . . ? C113 C112 C122 127(2) . . ? C112 C113 C114 118(3) . . ? C115 C114 C113 121(3) . . ? C114 C115 C116 117(3) . . ? N111 C116 C115 124(3) . . ? N121 C122 C123 144(4) . . ? N121 C122 C112 104(2) . . ? C123 C122 C112 109(3) . . ? N121 C122 C124 108(2) . . ? C123 C122 C124 37(2) . . ? C112 C122 C124 145(2) . . ? C124 C123 C122 107(4) . . ? C123 C124 C125 126(3) . . ? C123 C124 C122 37(2) . . ? C125 C124 C122 89(2) . . ? C124 C125 C126 119(3) . . ? N121 C126 C125 110(2) . . ? C133 C132 N131 128(3) . . ? C133 C132 C142 121(2) . . ? N131 C132 C142 111(2) . . ? C132 C133 C134 107(3) . . ? C133 C134 C135 135(3) . . ? C134 C135 C136 110(3) . . ? N131 C136 C135 123(3) . . ? N141 C142 C143 118(3) . . ? N141 C142 C132 115(2) . . ? C143 C142 C132 127(2) . . ? C144 C143 C142 124(3) . . ? C145 C144 C143 120(4) . . ? C144 C145 C146 110(3) . . ? N141 C146 C145 135(3) . . ? C204 C203 N202 104.8(18) . . ? C204 C203 C206 133(2) . . ? N202 C203 C206 122.2(18) . . ? C203 C204 C205 107.2(19) . . ? N201 C205 C204 113.4(18) . . ? N201 C205 C207 123.2(18) . . ? C204 C205 C207 122.9(19) . . ? N211 C212 C222 114(2) . . ? N211 C212 C213 119(2) . . ? C222 C212 C213 127(2) . . ? C214 C213 C212 123(3) . . ? C213 C214 C215 120(3) . . ? C214 C215 C216 119(3) . . ? N211 C216 C215 121(2) . . ? C212 C222 N221 121.7(19) . . ? C212 C222 C223 131(2) . . ? N221 C222 C223 107.1(19) . . ? C224 C223 C222 126(3) . . ? C223 C224 C225 120(3) . . ? C224 C225 C226 119(2) . . ? N221 C226 C225 121(2) . . ? C242 C232 N231 114.9(19) . . ? C242 C232 C233 127(2) . . ? N231 C232 C233 118.4(19) . . ? C234 C233 C232 116(2) . . ? C233 C234 C235 130(3) . . ? C234 C235 C236 112(2) . . ? N231 C236 C235 125(2) . . ? C232 C242 N241 118(2) . . ? C232 C242 C243 124(2) . . ? N241 C242 C243 118(2) . . ? C244 C243 C242 119(3) . . ? C245 C244 C243 119(3) . . ? C244 C245 C246 126(3) . . ? N241 C246 C245 116(2) . . ? Cl4B Cl4A O45 123(6) . . ? Cl4B Cl4A O41 90(6) . . ? O45 Cl4A O41 130(5) . . ? Cl4B Cl4A O44 59(7) . . ? O45 Cl4A O44 104(3) . . ? O41 Cl4A O44 126(4) . . ? Cl4B Cl4A O43 145(6) . . ? O45 Cl4A O43 92(5) . . ? O41 Cl4A O43 67(3) . . ? O44 Cl4A O43 112(3) . . ? Cl4B Cl4A O42 27(6) . . ? O45 Cl4A O42 104(3) . . ? O41 Cl4A O42 91(3) . . ? O44 Cl4A O42 79(3) . . ? O43 Cl4A O42 158(3) . . ? Cl4A Cl4B O44 94(9) . . ? Cl4A Cl4B O41 60(4) . . ? O44 Cl4B O41 128(6) . . ? Cl4A Cl4B O42 141(8) . . ? O44 Cl4B O42 113(4) . . ? O41 Cl4B O42 114(6) . . ? Cl4A Cl4B O45 35(4) . . ? O44 Cl4B O45 92(6) . . ? O41 Cl4B O45 89(3) . . ? O42 Cl4B O45 113(5) . . ? Cl4B O42 Cl4A 12(2) . . ? Cl4A O41 Cl4B 30(3) . . ? Cl4A O41 O43 69(4) . . ? Cl4B O41 O43 95(4) . . ? Cl4A O45 Cl4B 22(3) . . ? Cl4B O44 Cl4A 27(3) . . ? O41 O43 Cl4A 44(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.834 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.135