Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dipankar Datta' _publ_contact_author_address ; Dept. of Inorg. Chemistry IACS Jadavpur Calcutta West Bengal 700 032 INDIA ; _publ_contact_author_email ICDD@MAHENRDA.IACS.RES.IN _publ_section_title ;Use of HNO3 as the source of NO to prepare a novel nitric oxide complex of ruthenium ; loop_ _publ_author_name 'M. G. B. Drew' 'Samik Nag ' 'Dipankar Datta' # Attachment 'B714985A_Ru_NO.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 662316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H33 Cl N6 O13 Ru' _chemical_formula_weight 702.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 13.867(17) _cell_length_b 14.526(17) _cell_length_c 28.52(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5745(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Walker et al., Acta Cryst 1983 A39 158' _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2\^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25511 _diffrn_reflns_av_R_equivalents 0.1072 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.24 _reflns_number_total 4788 _reflns_number_gt 3717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1988)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; #_refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+150.2277P] 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 4788 _refine_ls_number_parameters 378 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.1253 _refine_ls_wR_factor_ref 0.2755 _refine_ls_wR_factor_gt 0.2667 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.004 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 0.01154(7) 0.19775(9) 0.35594(4) 0.0333(3) Uani 1 1 d . . . N11 N -0.0292(8) 0.0829(9) 0.3945(4) 0.044(3) Uani 1 1 d . . . C12 C -0.0492(12) -0.0171(13) 0.3887(6) 0.058(5) Uani 1 1 d . . . C121 C -0.1275(16) -0.0327(16) 0.3535(8) 0.096(7) Uani 1 1 d . . . H12A H -0.1844 0.0001 0.3629 0.115 Uiso 1 1 calc R . . H12B H -0.1417 -0.0973 0.3517 0.115 Uiso 1 1 calc R . . H12C H -0.1068 -0.0110 0.3233 0.115 Uiso 1 1 calc R . . C122 C 0.0424(15) -0.0672(14) 0.3768(11) 0.116(10) Uani 1 1 d . . . H12D H 0.0347 -0.0987 0.3474 0.139 Uiso 1 1 calc R . . H12E H 0.0567 -0.1111 0.4010 0.139 Uiso 1 1 calc R . . H12F H 0.0944 -0.0238 0.3743 0.139 Uiso 1 1 calc R . . C13 C -0.0817(15) -0.0442(14) 0.4382(7) 0.080(6) Uani 1 1 d . . . H13A H -0.1438 -0.0749 0.4373 0.096 Uiso 1 1 calc R . . H13B H -0.0350 -0.0848 0.4528 0.096 Uiso 1 1 calc R . . O14 O -0.0885(8) 0.0456(9) 0.4645(4) 0.064(3) Uani 1 1 d . . . C15 C -0.0569(11) 0.1115(13) 0.4361(5) 0.052(4) Uani 1 1 d . . . C16 C -0.0590(11) 0.2125(10) 0.4497(5) 0.044(4) Uani 1 1 d . . . O161 O -0.0906(9) 0.2330(11) 0.4886(4) 0.085(4) Uani 1 1 d . . . N17 N -0.0215(8) 0.2655(9) 0.4161(4) 0.044(3) Uani 1 1 d . . . C18 C -0.0340(13) 0.3642(12) 0.4139(6) 0.060(5) Uani 1 1 d . . . C181 C -0.0127(15) 0.4153(13) 0.4576(6) 0.073(6) Uani 1 1 d . . . H18A H -0.0668 0.4107 0.4786 0.087 Uiso 1 1 calc R . . H18B H -0.0010 0.4789 0.4504 0.087 Uiso 1 1 calc R . . H18C H 0.0433 0.3895 0.4724 0.087 Uiso 1 1 calc R . . C182 C -0.1347(12) 0.3864(12) 0.3956(6) 0.061(5) Uani 1 1 d . . . H18D H -0.1364 0.3777 0.3623 0.073 Uiso 1 1 calc R . . H18E H -0.1503 0.4492 0.4029 0.073 Uiso 1 1 calc R . . H18F H -0.1808 0.3463 0.4102 0.073 Uiso 1 1 calc R . . C19 C 0.0411(10) 0.3929(11) 0.3767(5) 0.046(4) Uani 1 1 d U . . H19A H 0.0255 0.4544 0.3658 0.056 Uiso 1 1 calc R . . H19B H 0.1040 0.3956 0.3915 0.056 Uiso 1 1 calc R . . O20 O 0.0469(7) 0.3318(7) 0.3363(3) 0.049(3) Uani 1 1 d . . . N31 N 0.1580(7) 0.1729(8) 0.3763(3) 0.033(3) Uani 1 1 d . . . C32 C 0.2260(10) 0.1811(14) 0.4194(5) 0.057(5) Uani 1 1 d . . . C321 C 0.1923(18) 0.125(2) 0.4574(8) 0.161(16) Uani 1 1 d . . . H32A H 0.2355 0.1314 0.4836 0.194 Uiso 1 1 calc R . . H32B H 0.1897 0.0623 0.4477 0.194 Uiso 1 1 calc R . . H32C H 0.1290 0.1455 0.4665 0.194 Uiso 1 1 calc R . . C322 C 0.2327(18) 0.2819(18) 0.4351(8) 0.112(9) Uani 1 1 d . . . H32D H 0.2478 0.3200 0.4086 0.134 Uiso 1 1 calc R . . H32E H 0.2824 0.2880 0.4583 0.134 Uiso 1 1 calc R . . H32F H 0.1721 0.3007 0.4482 0.134 Uiso 1 1 calc R . . O34 O 0.3048(7) 0.1324(9) 0.3496(4) 0.063(3) Uani 1 1 d . . . C33 C 0.3218(13) 0.1518(17) 0.3986(5) 0.085(7) Uani 1 1 d . . . H33A H 0.3690 0.2007 0.4019 0.102 Uiso 1 1 calc R . . H33B H 0.3458 0.0974 0.4144 0.102 Uiso 1 1 calc R . . C35 C 0.2120(9) 0.1446(11) 0.3422(5) 0.038(3) Uani 1 1 d . . . C36 C 0.1679(10) 0.1321(11) 0.2972(5) 0.045(4) Uani 1 1 d . . . O37 O 0.2171(7) 0.1098(10) 0.2588(3) 0.064(3) Uani 1 1 d . . . C38 C 0.1446(11) 0.1006(14) 0.2211(5) 0.060(5) Uani 1 1 d . . . H38A H 0.1409 0.0373 0.2105 0.072 Uiso 1 1 calc R . . H38B H 0.1616 0.1392 0.1946 0.072 Uiso 1 1 calc R . . C39 C 0.0464(10) 0.1315(11) 0.2422(5) 0.044(4) Uani 1 1 d . . . C391 C -0.0275(11) 0.0585(13) 0.2351(6) 0.063(5) Uani 1 1 d . . . H39A H -0.0863 0.0761 0.2505 0.076 Uiso 1 1 calc R . . H39B H -0.0046 0.0016 0.2482 0.076 Uiso 1 1 calc R . . H39C H -0.0392 0.0506 0.2022 0.076 Uiso 1 1 calc R . . C392 C 0.0166(16) 0.2246(14) 0.2231(6) 0.083(6) Uani 1 1 d . . . H39D H -0.0055 0.2179 0.1914 0.100 Uiso 1 1 calc R . . H39E H 0.0708 0.2657 0.2239 0.100 Uiso 1 1 calc R . . H39F H -0.0345 0.2493 0.2421 0.100 Uiso 1 1 calc R . . N40 N 0.0753(7) 0.1407(8) 0.2943(3) 0.032(3) Uani 1 1 d . . . N51 N -0.1031(9) 0.2075(9) 0.3297(4) 0.044(3) Uani 1 1 d . . . O52 O -0.1720(9) 0.2137(11) 0.3099(4) 0.077(4) Uani 1 1 d . . . N21 N 0.2634(8) 0.3805(8) 0.2862(5) 0.038(3) Uani 1 1 d . . . O22 O 0.2481(14) 0.4393(16) 0.3214(7) 0.139(7) Uani 1 1 d . . . O23 O 0.3267(15) 0.3911(13) 0.2654(8) 0.139(8) Uani 1 1 d . . . O24 O 0.197(2) 0.3383(17) 0.2839(9) 0.226(16) Uani 1 1 d . . . Cl6 Cl -0.1442(4) 0.6731(3) 0.41389(18) 0.0679(13) Uani 1 1 d . . . O61 O -0.0718(13) 0.6238(12) 0.3898(6) 0.118(6) Uani 1 1 d . . . O62 O -0.2295(16) 0.661(2) 0.3934(8) 0.189(12) Uani 1 1 d . . . O63 O -0.1585(19) 0.632(2) 0.4536(8) 0.220(15) Uani 1 1 d . . . O65 O -0.118(3) 0.7519(17) 0.421(2) 0.40(3) 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 0.0260(5) 0.0469(6) 0.0271(5) -0.0018(6) 0.0003(5) -0.0015(5) N11 0.035(6) 0.056(8) 0.040(7) -0.011(6) 0.006(5) -0.011(6) C12 0.044(9) 0.074(13) 0.055(10) 0.028(9) 0.011(8) 0.012(9) C121 0.109(17) 0.089(16) 0.091(16) -0.024(14) 0.002(14) -0.036(14) C122 0.079(15) 0.041(11) 0.23(3) -0.022(16) 0.027(17) 0.008(10) C13 0.085(14) 0.070(14) 0.085(14) 0.022(12) -0.016(12) -0.045(11) O14 0.053(7) 0.088(9) 0.051(7) 0.012(7) 0.011(6) -0.017(7) C15 0.038(8) 0.091(13) 0.028(7) 0.006(8) 0.005(6) -0.014(9) C16 0.051(9) 0.042(10) 0.038(8) -0.008(7) 0.006(7) 0.001(7) O161 0.082(9) 0.128(13) 0.044(7) -0.018(7) 0.026(7) -0.021(8) N17 0.026(6) 0.061(8) 0.045(7) -0.003(6) -0.011(5) -0.011(6) C18 0.064(11) 0.052(11) 0.063(11) -0.011(9) 0.011(9) 0.011(9) C181 0.096(14) 0.063(12) 0.059(11) -0.028(9) -0.002(11) -0.027(11) C182 0.056(10) 0.056(11) 0.070(12) -0.007(9) -0.004(9) 0.006(9) C19 0.048(7) 0.058(8) 0.033(6) 0.019(6) -0.026(6) 0.010(6) O20 0.057(6) 0.052(7) 0.038(5) 0.002(5) -0.002(5) -0.011(5) N31 0.031(6) 0.046(7) 0.021(5) 0.003(5) -0.003(5) 0.000(5) C32 0.039(8) 0.102(16) 0.029(8) 0.003(9) -0.006(6) 0.004(9) C321 0.085(17) 0.30(4) 0.100(19) 0.12(2) -0.049(15) -0.05(2) C322 0.108(18) 0.13(2) 0.102(17) -0.026(17) -0.061(15) 0.004(16) O34 0.036(6) 0.100(10) 0.052(7) -0.012(7) 0.000(5) 0.009(6) C33 0.062(11) 0.16(2) 0.032(9) -0.028(11) -0.019(8) 0.023(13) C35 0.022(6) 0.060(10) 0.031(7) 0.007(7) -0.002(5) 0.000(6) C36 0.032(8) 0.068(11) 0.036(8) 0.009(8) 0.004(6) 0.007(7) O37 0.038(6) 0.122(11) 0.033(6) -0.007(6) 0.005(5) 0.014(6) C38 0.048(9) 0.098(14) 0.033(8) -0.007(9) 0.004(7) -0.007(9) C39 0.038(8) 0.069(11) 0.026(7) -0.004(7) -0.006(6) 0.005(7) C391 0.052(10) 0.092(14) 0.045(9) -0.026(9) -0.003(8) 0.004(10) C392 0.113(17) 0.094(16) 0.043(10) 0.011(10) -0.012(11) 0.018(13) N40 0.031(6) 0.044(7) 0.021(5) 0.001(5) -0.002(4) 0.001(5) N51 0.044(7) 0.052(8) 0.035(7) -0.014(6) 0.010(6) 0.004(6) O52 0.057(7) 0.116(12) 0.058(8) -0.014(8) -0.006(6) -0.006(8) N21 0.018(6) 0.031(7) 0.065(9) 0.009(6) 0.011(6) -0.012(5) O22 0.095(12) 0.18(2) 0.142(16) -0.012(16) 0.013(13) -0.006(13) O23 0.117(15) 0.097(13) 0.20(2) 0.027(14) 0.031(15) 0.006(12) O24 0.30(3) 0.19(2) 0.19(2) -0.096(19) 0.15(2) -0.15(2) Cl6 0.082(3) 0.065(3) 0.057(3) -0.005(2) -0.010(2) 0.008(2) O61 0.119(14) 0.102(13) 0.133(14) 0.007(11) 0.025(12) 0.026(11) O62 0.133(18) 0.28(3) 0.157(19) -0.08(2) -0.069(15) 0.034(18) O63 0.19(2) 0.35(4) 0.120(18) 0.03(2) 0.045(17) 0.11(3) O65 0.37(5) 0.080(16) 0.73(9) -0.12(3) 0.20(5) -0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N51 1.764(13) . ? Ru1 N17 2.030(13) . ? Ru1 N11 2.075(13) . ? Ru1 O20 2.084(10) . ? Ru1 N40 2.135(10) . ? Ru1 N31 2.143(10) . ? N11 C15 1.315(18) . ? N11 C12 1.49(2) . ? C12 C121 1.50(3) . ? C12 C122 1.50(2) . ? C12 C13 1.53(2) . ? C13 O14 1.51(2) . ? O14 C15 1.329(18) . ? C15 C16 1.52(2) . ? C16 O161 1.230(17) . ? C16 N17 1.335(18) . ? N17 C18 1.44(2) . ? C18 C181 1.48(2) . ? C18 C182 1.53(2) . ? C18 C19 1.54(2) . ? C19 O20 1.458(18) . ? N31 C35 1.293(16) . ? N31 C32 1.554(17) . ? C32 C321 1.43(3) . ? C32 C33 1.52(2) . ? C32 C322 1.53(3) . ? O34 C35 1.317(15) . ? O34 C33 1.445(18) . ? C35 C36 1.434(19) . ? C36 N40 1.293(17) . ? C36 O37 1.330(16) . ? O37 C38 1.479(17) . ? C38 C39 1.55(2) . ? C39 C391 1.49(2) . ? C39 C392 1.52(2) . ? C39 N40 1.545(16) . ? N51 O52 1.112(15) . ? N21 O23 1.07(2) . ? N21 O24 1.10(2) . ? N21 O22 1.34(2) . ? Cl6 O65 1.22(2) . ? Cl6 O63 1.30(3) . ? Cl6 O62 1.33(2) . ? Cl6 O61 1.412(17) . ? 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 N51 Ru1 N17 96.7(5) . . ? N51 Ru1 N11 92.5(5) . . ? N17 Ru1 N11 83.2(5) . . ? N51 Ru1 O20 91.3(5) . . ? N17 Ru1 O20 80.1(5) . . ? N11 Ru1 O20 163.1(4) . . ? N51 Ru1 N40 93.1(4) . . ? N17 Ru1 N40 167.8(4) . . ? N11 Ru1 N40 103.7(4) . . ? O20 Ru1 N40 92.5(4) . . ? N51 Ru1 N31 169.4(5) . . ? N17 Ru1 N31 93.8(4) . . ? N11 Ru1 N31 88.8(4) . . ? O20 Ru1 N31 90.4(4) . . ? N40 Ru1 N31 76.4(4) . . ? C15 N11 C12 110.8(13) . . ? C15 N11 Ru1 107.6(11) . . ? C12 N11 Ru1 140.9(10) . . ? N11 C12 C121 111.0(14) . . ? N11 C12 C122 109.9(14) . . ? C121 C12 C122 112.9(19) . . ? N11 C12 C13 101.7(14) . . ? C121 C12 C13 111.4(16) . . ? C122 C12 C13 109.4(17) . . ? O14 C13 C12 104.8(14) . . ? C15 O14 C13 107.4(12) . . ? N11 C15 O14 114.7(16) . . ? N11 C15 C16 122.8(14) . . ? O14 C15 C16 122.3(13) . . ? O161 C16 N17 130.3(16) . . ? O161 C16 C15 118.1(15) . . ? N17 C16 C15 111.5(12) . . ? C16 N17 C18 123.8(14) . . ? C16 N17 Ru1 114.5(10) . . ? C18 N17 Ru1 118.1(11) . . ? N17 C18 C181 115.9(16) . . ? N17 C18 C182 109.5(14) . . ? C181 C18 C182 111.3(15) . . ? N17 C18 C19 102.5(13) . . ? C181 C18 C19 108.0(15) . . ? C182 C18 C19 109.0(14) . . ? O20 C19 C18 114.6(13) . . ? C19 O20 Ru1 110.1(8) . . ? C35 N31 C32 105.5(10) . . ? C35 N31 Ru1 113.5(8) . . ? C32 N31 Ru1 140.9(9) . . ? C321 C32 C33 115(2) . . ? C321 C32 C322 110(2) . . ? C33 C32 C322 109.3(18) . . ? C321 C32 N31 111.0(15) . . ? C33 C32 N31 101.5(11) . . ? C322 C32 N31 109.9(14) . . ? C35 O34 C33 106.7(12) . . ? O34 C33 C32 106.9(13) . . ? N31 C35 O34 119.2(12) . . ? N31 C35 C36 117.8(12) . . ? O34 C35 C36 122.9(13) . . ? N40 C36 O37 118.8(13) . . ? N40 C36 C35 117.9(12) . . ? O37 C36 C35 123.3(12) . . ? C36 O37 C38 105.8(11) . . ? O37 C38 C39 106.7(11) . . ? C391 C39 C392 113.6(14) . . ? C391 C39 N40 111.7(12) . . ? C392 C39 N40 109.8(13) . . ? C391 C39 C38 110.2(14) . . ? C392 C39 C38 110.9(15) . . ? N40 C39 C38 99.9(10) . . ? C36 N40 C39 108.0(11) . . ? C36 N40 Ru1 113.4(9) . . ? C39 N40 Ru1 135.9(8) . . ? O52 N51 Ru1 174.7(11) . . ? O23 N21 O24 137(2) . . ? O23 N21 O22 117.0(18) . . ? O24 N21 O22 105.6(17) . . ? O65 Cl6 O63 109(3) . . ? O65 Cl6 O62 118(3) . . ? O63 Cl6 O62 100.8(18) . . ? O65 Cl6 O61 110(2) . . ? O63 Cl6 O61 107.6(14) . . ? O62 Cl6 O61 110.5(13) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.491 _refine_diff_density_min -3.517 _refine_diff_density_rms 0.174 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1997) SHELX97 program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 662317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 N6 O8 Ru ' _chemical_formula_weight 585.59 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.170(3) _cell_length_b 11.896(2) _cell_length_c 10.1839(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2443.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 1.245 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16354 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 30.15 _reflns_number_total 5647 _reflns_number_gt 3411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; #_refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0578P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 5647 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.854 _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 C12 C 0.2884(2) 0.8129(3) 0.6324(4) 0.0199(9) Uani 1 1 d . . . C13 C 0.3123(2) 0.7952(4) 0.4893(5) 0.0257(10) Uani 1 1 d . . . H13A H 0.3163 0.8666 0.4441 0.031 Uiso 1 1 calc R . . H13B H 0.3551 0.7578 0.4879 0.031 Uiso 1 1 calc R . . O14 O 0.26088(18) 0.7239(3) 0.4265(4) 0.0263(9) Uani 1 1 d . . . C15 C 0.2139(2) 0.7153(4) 0.5165(5) 0.0197(9) Uani 1 1 d . . . C16 C 0.1532(2) 0.6537(4) 0.4893(5) 0.0195(9) Uani 1 1 d . . . O17 O 0.14860(16) 0.5897(3) 0.3835(3) 0.0248(7) Uani 1 1 d . . . C18 C 0.0799(2) 0.5507(4) 0.3855(5) 0.0320(12) Uani 1 1 d . . . H18A H 0.0777 0.4707 0.3675 0.038 Uiso 1 1 calc R . . H18B H 0.0538 0.5903 0.3203 0.038 Uiso 1 1 calc R . . C19 C 0.0545(2) 0.5762(4) 0.5242(5) 0.0242(10) Uani 1 1 d . . . C32 C 0.0751(2) 0.9815(4) 0.5777(4) 0.0241(10) Uani 1 1 d . . . C33 C 0.0847(2) 1.1050(4) 0.6182(5) 0.0318(11) Uani 1 1 d . . . H33A H 0.1188 1.1405 0.5653 0.038 Uiso 1 1 calc R . . H33B H 0.0437 1.1468 0.6086 0.038 Uiso 1 1 calc R . . O34 O 0.10504(15) 1.0996(2) 0.7574(4) 0.0291(7) Uani 1 1 d . . . C35 C 0.1204(2) 0.9913(3) 0.7771(4) 0.0193(10) Uani 1 1 d . . . C36 C 0.1472(2) 0.9494(3) 0.9001(4) 0.0194(9) Uani 1 1 d . . . O37 O 0.15866(16) 1.0167(3) 1.0018(3) 0.0277(7) Uani 1 1 d . . . C39 C 0.1808(2) 0.8242(4) 1.0480(4) 0.0226(9) Uani 1 1 d . . . C121 C 0.33048(18) 0.7449(4) 0.7310(7) 0.0321(11) Uani 1 1 d . . . H12A H 0.3319 0.6676 0.7042 0.048 Uiso 1 1 calc R . . H12B H 0.3110 0.7501 0.8168 0.048 Uiso 1 1 calc R . . H12C H 0.3747 0.7748 0.7334 0.048 Uiso 1 1 calc R . . C122 C 0.2850(2) 0.9357(4) 0.6693(5) 0.0332(12) Uani 1 1 d . . . H12D H 0.2587 0.9754 0.6059 0.050 Uiso 1 1 calc R . . H12E H 0.3289 0.9667 0.6708 0.050 Uiso 1 1 calc R . . H12F H 0.2652 0.9432 0.7546 0.050 Uiso 1 1 calc R . . C191 C 0.0578(2) 0.4736(4) 0.6128(5) 0.0310(11) Uani 1 1 d . . . H19A H 0.0421 0.4931 0.6988 0.046 Uiso 1 1 calc R . . H19B H 0.1028 0.4478 0.6185 0.046 Uiso 1 1 calc R . . H19C H 0.0305 0.4150 0.5770 0.046 Uiso 1 1 calc R . . C192 C -0.0157(2) 0.6259(4) 0.5185(6) 0.0361(13) Uani 1 1 d . . . H19D H -0.0160 0.6898 0.4610 0.054 Uiso 1 1 calc R . . H19E H -0.0292 0.6487 0.6049 0.054 Uiso 1 1 calc R . . H19F H -0.0460 0.5701 0.4859 0.054 Uiso 1 1 calc R . . C321 C 0.0027(2) 0.9478(4) 0.5773(6) 0.0359(12) Uani 1 1 d . . . H32A H -0.0163 0.9627 0.6620 0.054 Uiso 1 1 calc R . . H32B H -0.0010 0.8691 0.5580 0.054 Uiso 1 1 calc R . . H32C H -0.0205 0.9903 0.5117 0.054 Uiso 1 1 calc R . . C381 C 0.1956(2) 0.9448(4) 1.0941(5) 0.0341(12) Uani 1 1 d . . . H38A H 0.1804 0.9563 1.1834 0.041 Uiso 1 1 calc R . . H38B H 0.2427 0.9604 1.0900 0.041 Uiso 1 1 calc R . . C391 C 0.1211(2) 0.7727(4) 1.1203(5) 0.0283(12) Uani 1 1 d . . . H39A H 0.1125 0.6989 1.0862 0.042 Uiso 1 1 calc R . . H39B H 0.0829 0.8194 1.1074 0.042 Uiso 1 1 calc R . . H39C H 0.1308 0.7677 1.2124 0.042 Uiso 1 1 calc R . . C392 C 0.2419(3) 0.7493(4) 1.0611(5) 0.0309(13) Uani 1 1 d . . . H39D H 0.2784 0.7827 1.0147 0.046 Uiso 1 1 calc R . . H39E H 0.2326 0.6765 1.0247 0.046 Uiso 1 1 calc R . . H39F H 0.2533 0.7414 1.1522 0.046 Uiso 1 1 calc R . . O42 O 0.01574(14) 0.8307(3) 0.8818(3) 0.0297(8) Uani 1 1 d . . . O43 O 0.00623(15) 0.6570(3) 0.8306(4) 0.0325(8) Uani 1 1 d . . . O52 O 0.13442(17) 0.5630(3) 0.9250(4) 0.0309(8) Uani 1 1 d . . . O53 O 0.20036(15) 0.5420(2) 0.7636(4) 0.0360(9) Uani 1 1 d . . . N11 N 0.22065(15) 0.7611(3) 0.6294(3) 0.0172(7) Uani 1 1 d . . . Ru1 Ru 0.130540(10) 0.75042(3) 0.74515(11) 0.01294(7) Uani 1 1 d . . . N20 N 0.10537(16) 0.6607(3) 0.5726(4) 0.0171(7) Uani 1 1 d . . . N41 N 0.04015(16) 0.7443(3) 0.8305(4) 0.0194(7) Uani 1 1 d . . . N51 N 0.15753(18) 0.6005(3) 0.8199(4) 0.0210(8) Uani 1 1 d . . . N31 N 0.10882(16) 0.9201(3) 0.6854(4) 0.0189(8) Uani 1 1 d . . . N40 N 0.16121(17) 0.8450(3) 0.9074(3) 0.0186(8) Uani 1 1 d . . . C322 C 0.1086(3) 0.9591(5) 0.4468(6) 0.0426(14) Uani 1 1 d . . . H32D H 0.1542 0.9819 0.4515 0.064 Uiso 1 1 calc R . . H32E H 0.0865 1.0009 0.3791 0.064 Uiso 1 1 calc R . . H32F H 0.1063 0.8803 0.4271 0.064 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 C12 0.020(2) 0.022(2) 0.018(2) 0.0004(17) 0.0018(17) -0.0080(17) C13 0.022(2) 0.028(2) 0.027(3) -0.007(2) -0.0039(19) -0.0072(19) O14 0.0217(19) 0.035(2) 0.0223(18) -0.0007(16) 0.0054(15) -0.0067(15) C15 0.0142(18) 0.0196(19) 0.025(2) 0.0036(18) 0.0008(18) -0.0025(16) C16 0.019(2) 0.019(2) 0.020(2) 0.0005(19) -0.0001(19) -0.0030(18) O17 0.0244(16) 0.0302(18) 0.0199(17) -0.0052(14) 0.0040(14) -0.0070(15) C18 0.025(2) 0.046(3) 0.025(3) -0.013(2) 0.003(2) -0.014(2) C19 0.018(2) 0.025(2) 0.029(3) -0.008(2) 0.002(2) -0.0068(18) C32 0.027(2) 0.027(2) 0.018(2) 0.008(2) -0.004(2) 0.005(2) C33 0.036(3) 0.026(2) 0.033(3) 0.005(2) -0.010(2) 0.004(2) O34 0.0375(15) 0.0179(13) 0.032(2) 0.0007(17) -0.0071(18) 0.0038(12) C35 0.021(2) 0.0122(18) 0.025(3) 0.0019(15) 0.0041(16) 0.0021(15) C36 0.027(2) 0.014(2) 0.017(2) -0.0014(18) -0.0047(19) -0.0003(17) O37 0.0340(18) 0.0274(17) 0.0216(17) -0.0036(15) -0.0063(15) 0.0013(15) C39 0.027(2) 0.024(2) 0.016(2) 0.0013(19) -0.0034(19) -0.0003(19) C121 0.0151(14) 0.043(2) 0.038(3) 0.003(3) -0.001(2) -0.006(2) C122 0.026(2) 0.030(3) 0.044(3) -0.012(2) 0.014(2) -0.016(2) C191 0.035(3) 0.023(2) 0.034(3) -0.003(2) 0.006(2) -0.012(2) C192 0.020(2) 0.043(3) 0.045(3) -0.011(3) -0.003(2) -0.004(2) C321 0.025(2) 0.040(3) 0.042(3) 0.007(3) -0.009(2) 0.000(2) C381 0.043(3) 0.035(3) 0.025(3) -0.003(2) -0.011(2) -0.006(2) C391 0.037(3) 0.037(3) 0.011(2) 0.0020(18) 0.0061(18) -0.001(2) C392 0.040(3) 0.036(3) 0.017(2) 0.002(2) -0.006(2) 0.000(3) O42 0.0235(17) 0.0307(18) 0.035(2) -0.0100(17) 0.0120(15) 0.0010(14) O43 0.0243(16) 0.0323(19) 0.041(2) -0.0037(16) 0.0122(16) -0.0122(15) O52 0.046(2) 0.0185(16) 0.028(2) 0.0090(15) 0.0086(16) 0.0066(15) O53 0.0374(17) 0.0230(15) 0.047(2) 0.0037(17) 0.0183(19) 0.0126(13) N11 0.0132(15) 0.0181(19) 0.0202(18) -0.0007(16) -0.0011(13) -0.0022(14) Ru1 0.01491(11) 0.01193(10) 0.01198(11) -0.00048(16) 0.0008(3) -0.00093(15) N20 0.0144(16) 0.0171(17) 0.0200(19) -0.0017(15) -0.0007(14) -0.0019(14) N41 0.0167(15) 0.0235(19) 0.0178(17) 0.0009(18) 0.0003(13) -0.0011(18) N51 0.0238(19) 0.0166(18) 0.023(2) 0.0000(16) 0.0015(17) -0.0043(16) N31 0.0158(17) 0.023(2) 0.018(2) 0.0043(16) -0.0009(14) 0.0009(15) N40 0.0171(17) 0.0229(19) 0.0157(19) 0.0036(16) -0.0013(15) 0.0012(15) C322 0.044(3) 0.051(4) 0.033(3) 0.001(3) 0.001(3) 0.013(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 C12 N11 1.500(5) . ? C12 C122 1.510(6) . ? C12 C121 1.544(7) . ? C12 C13 1.549(6) . ? C13 O14 1.485(5) . ? O14 C15 1.322(5) . ? C15 N11 1.280(6) . ? C15 C16 1.454(6) . ? C16 N20 1.288(6) . ? C16 O17 1.322(5) . ? O17 C18 1.461(5) . ? C18 C19 1.533(6) . ? C19 N20 1.518(5) . ? C19 C191 1.519(6) . ? C19 C192 1.536(6) . ? C32 N31 1.483(5) . ? C32 C322 1.517(7) . ? C32 C321 1.514(6) . ? C32 C33 1.539(6) . ? C33 O34 1.477(6) . ? O34 C35 1.341(5) . ? C35 N31 1.283(5) . ? C35 C36 1.452(6) . ? C36 N40 1.276(5) . ? C36 O37 1.329(5) . ? O37 C381 1.473(6) . ? C39 N40 1.506(5) . ? C39 C381 1.538(6) . ? C39 C392 1.527(6) . ? C39 C391 1.538(6) . ? O42 N41 1.254(4) . ? O43 N41 1.244(4) . ? O52 N51 1.250(5) . ? O53 N51 1.248(4) . ? N11 Ru1 2.170(3) . ? Ru1 N51 2.014(4) . ? Ru1 N41 2.021(3) . ? Ru1 N40 2.092(4) . ? Ru1 N20 2.118(4) . ? Ru1 N31 2.153(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 N11 C12 C122 111.2(3) . . ? N11 C12 C121 107.4(3) . . ? C122 C12 C121 111.7(4) . . ? N11 C12 C13 102.1(3) . . ? C122 C12 C13 112.3(4) . . ? C121 C12 C13 111.7(4) . . ? O14 C13 C12 105.4(3) . . ? C15 O14 C13 104.3(4) . . ? N11 C15 O14 120.9(4) . . ? N11 C15 C16 118.4(4) . . ? O14 C15 C16 120.7(4) . . ? N20 C16 O17 121.4(4) . . ? N20 C16 C15 118.2(4) . . ? O17 C16 C15 120.3(4) . . ? C16 O17 C18 103.8(3) . . ? O17 C18 C19 105.5(3) . . ? N20 C19 C191 108.1(4) . . ? N20 C19 C18 101.8(3) . . ? C191 C19 C18 111.9(4) . . ? N20 C19 C192 112.4(4) . . ? C191 C19 C192 111.8(4) . . ? C18 C19 C192 110.4(4) . . ? N31 C32 C322 111.0(4) . . ? N31 C32 C321 108.3(4) . . ? C322 C32 C321 112.4(4) . . ? N31 C32 C33 102.4(3) . . ? C322 C32 C33 110.3(4) . . ? C321 C32 C33 112.0(4) . . ? O34 C33 C32 104.5(3) . . ? C35 O34 C33 104.5(3) . . ? N31 C35 O34 118.9(4) . . ? N31 C35 C36 118.0(4) . . ? O34 C35 C36 123.1(4) . . ? N40 C36 O37 120.2(4) . . ? N40 C36 C35 117.8(4) . . ? O37 C36 C35 122.0(4) . . ? C36 O37 C381 103.6(3) . . ? N40 C39 C381 100.8(4) . . ? N40 C39 C392 113.0(4) . . ? C381 C39 C392 111.2(4) . . ? N40 C39 C391 108.4(4) . . ? C381 C39 C391 112.1(4) . . ? C392 C39 C391 111.0(4) . . ? O37 C381 C39 104.4(4) . . ? C15 N11 C12 106.8(3) . . ? C15 N11 Ru1 112.0(3) . . ? C12 N11 Ru1 141.0(3) . . ? N51 Ru1 N41 92.84(16) . . ? N51 Ru1 N40 95.63(15) . . ? N41 Ru1 N40 86.92(15) . . ? N51 Ru1 N20 86.09(14) . . ? N41 Ru1 N20 97.05(14) . . ? N40 Ru1 N20 175.61(14) . . ? N51 Ru1 N31 172.71(15) . . ? N41 Ru1 N31 88.37(14) . . ? N40 Ru1 N31 77.25(13) . . ? N20 Ru1 N31 100.91(14) . . ? N51 Ru1 N11 91.75(14) . . ? N41 Ru1 N11 172.44(15) . . ? N40 Ru1 N11 98.61(13) . . ? N20 Ru1 N11 77.27(13) . . ? N31 Ru1 N11 87.83(13) . . ? C16 N20 C19 104.5(4) . . ? C16 N20 Ru1 113.6(3) . . ? C19 N20 Ru1 139.9(3) . . ? O43 N41 O42 118.0(3) . . ? O43 N41 Ru1 121.7(3) . . ? O42 N41 Ru1 120.3(3) . . ? O53 N51 O52 116.9(4) . . ? O53 N51 Ru1 120.5(3) . . ? O52 N51 Ru1 122.6(3) . . ? C35 N31 C32 107.3(3) . . ? C35 N31 Ru1 112.1(3) . . ? C32 N31 Ru1 139.8(3) . . ? C36 N40 C39 105.9(4) . . ? C36 N40 Ru1 114.3(3) . . ? C39 N40 Ru1 137.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.837 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.114 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 662318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H32 Cl2 N6 O15 Ru' _chemical_formula_weight 768.48 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.054(5) _cell_length_b 14.903(4) _cell_length_c 15.135(2) _cell_angle_alpha 75.339(16) _cell_angle_beta 85.209(18) _cell_angle_gamma 82.35(3) _cell_volume 3035.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 1.336 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20091 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.1649 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.00 _reflns_number_total 16088 _reflns_number_gt 9120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; #_refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+11.2613P] 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 16088 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1880 _refine_ls_R_factor_gt 0.1153 _refine_ls_wR_factor_ref 0.2890 _refine_ls_wR_factor_gt 0.2580 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C12 C 0.1775(7) 0.3835(7) -0.0325(6) 0.027(2) Uani 1 1 d . . . C13 C 0.1839(9) 0.4849(8) -0.0317(7) 0.040(3) Uani 1 1 d . . . H13A H 0.2354 0.5097 -0.0738 0.048 Uiso 1 1 calc R . . H13B H 0.1240 0.5234 -0.0493 0.048 Uiso 1 1 calc R . . O62 O -0.0189(5) 0.7719(6) 0.5019(5) 0.045(2) Uani 1 1 d . . . O14 O 0.2037(5) 0.4828(5) 0.0641(5) 0.0350(17) Uani 1 1 d . . . C15 C 0.2329(7) 0.3931(7) 0.0981(6) 0.029(2) Uani 1 1 d . . . C16 C 0.2671(7) 0.3598(7) 0.1941(6) 0.028(2) Uani 1 1 d . . . O17 O 0.2542(5) 0.4143(5) 0.2497(5) 0.0320(16) Uani 1 1 d . . . C18 C 0.2895(8) 0.3536(9) 0.3380(7) 0.038(3) Uani 1 1 d . . . H18A H 0.2418 0.3568 0.3876 0.045 Uiso 1 1 calc R . . H18B H 0.3486 0.3726 0.3523 0.045 Uiso 1 1 calc R . . C19 C 0.3068(8) 0.2545(8) 0.3227(6) 0.033(2) Uani 1 1 d . . . C22 C 0.2475(9) 0.0557(8) -0.0101(6) 0.036(3) Uani 1 1 d . . . C23 C 0.3084(11) 0.0432(10) -0.0970(8) 0.059(4) Uani 1 1 d . . . H23A H 0.3266 -0.0226 -0.0940 0.070 Uiso 1 1 calc R . . H23B H 0.2722 0.0707 -0.1511 0.070 Uiso 1 1 calc R . . C25 C 0.3777(8) 0.1405(9) -0.0377(7) 0.039(3) Uani 1 1 d . . . C26 C 0.4448(8) 0.1955(8) -0.0169(7) 0.036(3) Uani 1 1 d . . . C28 C 0.5734(9) 0.2759(10) -0.0288(8) 0.047(3) Uani 1 1 d . . . H28A H 0.5736 0.3352 -0.0738 0.056 Uiso 1 1 calc R . . H28B H 0.6390 0.2518 -0.0130 0.056 Uiso 1 1 calc R . . C29 C 0.5095(8) 0.2865(8) 0.0570(7) 0.036(2) Uani 1 1 d . . . O42 O 0.1153(5) 0.1281(6) 0.2065(5) 0.0397(18) Uani 1 1 d . . . C52 C 0.1988(8) 0.8873(7) 0.6041(6) 0.032(2) Uani 1 1 d . . . C53 C 0.2582(9) 0.8519(8) 0.6894(7) 0.038(3) Uani 1 1 d . . . H53A H 0.3210 0.8741 0.6782 0.046 Uiso 1 1 calc R . . H53B H 0.2255 0.8725 0.7411 0.046 Uiso 1 1 calc R . . C55 C 0.2476(6) 0.7320(7) 0.6285(5) 0.026(2) Uani 1 1 d . . . C56 C 0.2508(6) 0.6393(7) 0.6152(6) 0.023(2) Uani 1 1 d . . . C58 C 0.2465(8) 0.4851(7) 0.6446(7) 0.033(2) Uani 1 1 d . . . H58A H 0.1873 0.4622 0.6736 0.040 Uiso 1 1 calc R . . H58B H 0.2979 0.4338 0.6544 0.040 Uiso 1 1 calc R . . C59 C 0.2352(6) 0.5296(7) 0.5395(6) 0.0242(19) Uani 1 1 d . . . C62 C 0.4287(6) 0.7749(7) 0.4046(6) 0.024(2) Uani 1 1 d . . . C63 C 0.4764(7) 0.7857(10) 0.3061(7) 0.042(3) Uani 1 1 d . . . H63A H 0.4834 0.8507 0.2776 0.050 Uiso 1 1 calc R . . H63B H 0.5394 0.7498 0.3079 0.050 Uiso 1 1 calc R . . C65 C 0.3303(7) 0.7436(8) 0.3063(6) 0.031(2) Uani 1 1 d . . . C66 C 0.2438(7) 0.7194(8) 0.2747(5) 0.027(2) Uani 1 1 d . . . C68 C 0.1436(8) 0.6744(9) 0.1945(7) 0.037(3) Uani 1 1 d . . . H68A H 0.1475 0.6068 0.2095 0.045 Uiso 1 1 calc R . . H68B H 0.1148 0.6994 0.1360 0.045 Uiso 1 1 calc R . . C69 C 0.0850(7) 0.7139(8) 0.2700(6) 0.029(2) Uani 1 1 d . . . O721 O 0.2096(6) 0.9199(6) 0.2937(5) 0.0424(19) Uani 1 1 d . . . O731 O 0.0915(6) 0.9499(6) 0.3867(5) 0.049(2) Uani 1 1 d . . . C121 C 0.2261(8) 0.3584(9) -0.1167(7) 0.041(3) Uani 1 1 d . . . H12A H 0.2200 0.2944 -0.1141 0.062 Uiso 1 1 calc R . . H12B H 0.2930 0.3668 -0.1198 0.062 Uiso 1 1 calc R . . H12C H 0.1965 0.3980 -0.1700 0.062 Uiso 1 1 calc R . . C122 C 0.0744(8) 0.3566(8) -0.0155(7) 0.040(3) Uani 1 1 d . . . H12D H 0.0454 0.3740 0.0383 0.060 Uiso 1 1 calc R . . H12E H 0.0760 0.2904 -0.0072 0.060 Uiso 1 1 calc R . . H12F H 0.0373 0.3885 -0.0671 0.060 Uiso 1 1 calc R . . C191 C 0.4027(8) 0.2057(9) 0.3580(7) 0.044(3) Uani 1 1 d . . . H19A H 0.4527 0.2433 0.3301 0.066 Uiso 1 1 calc R . . H19B H 0.4150 0.1462 0.3431 0.066 Uiso 1 1 calc R . . H19C H 0.4013 0.1967 0.4231 0.066 Uiso 1 1 calc R . . C192 C 0.2245(8) 0.1959(8) 0.3673(7) 0.036(2) Uani 1 1 d . . . H19D H 0.1644 0.2278 0.3441 0.055 Uiso 1 1 calc R . . H19E H 0.2224 0.1874 0.4324 0.055 Uiso 1 1 calc R . . H19F H 0.2358 0.1360 0.3529 0.055 Uiso 1 1 calc R . . C221 C 0.2621(9) -0.0331(8) 0.0688(7) 0.041(3) Uani 1 1 d . . . H22A H 0.3296 -0.0514 0.0765 0.062 Uiso 1 1 calc R . . H22B H 0.2338 -0.0826 0.0546 0.062 Uiso 1 1 calc R . . H22C H 0.2319 -0.0204 0.1244 0.062 Uiso 1 1 calc R . . C222 C 0.1450(9) 0.0867(10) -0.0254(9) 0.053(3) Uani 1 1 d . . . H22D H 0.1388 0.1414 -0.0752 0.080 Uiso 1 1 calc R . . H22E H 0.1134 0.1010 0.0290 0.080 Uiso 1 1 calc R . . H22F H 0.1158 0.0378 -0.0399 0.080 Uiso 1 1 calc R . . C291 C 0.5617(9) 0.2300(12) 0.1425(8) 0.060(4) Uani 1 1 d . . . H29A H 0.5228 0.2362 0.1963 0.090 Uiso 1 1 calc R . . H29B H 0.6221 0.2532 0.1434 0.090 Uiso 1 1 calc R . . H29C H 0.5730 0.1654 0.1411 0.090 Uiso 1 1 calc R . . C292 C 0.4801(9) 0.3901(11) 0.0569(10) 0.059(4) Uani 1 1 d . . . H29D H 0.4485 0.4216 0.0018 0.089 Uiso 1 1 calc R . . H29E H 0.5364 0.4190 0.0601 0.089 Uiso 1 1 calc R . . H29F H 0.4371 0.3941 0.1088 0.089 Uiso 1 1 calc R . . C521 C 0.2327(11) 0.9750(8) 0.5409(8) 0.054(3) Uani 1 1 d . . . H52A H 0.1941 0.9947 0.4885 0.080 Uiso 1 1 calc R . . H52B H 0.2988 0.9621 0.5214 0.080 Uiso 1 1 calc R . . H52C H 0.2267 1.0237 0.5729 0.080 Uiso 1 1 calc R . . C522 C 0.0919(9) 0.8987(9) 0.6264(8) 0.045(3) Uani 1 1 d . . . H52D H 0.0586 0.9200 0.5707 0.068 Uiso 1 1 calc R . . H52E H 0.0770 0.9435 0.6627 0.068 Uiso 1 1 calc R . . H52F H 0.0723 0.8398 0.6600 0.068 Uiso 1 1 calc R . . C621 C 0.4749(6) 0.6905(7) 0.4722(6) 0.028(2) Uani 1 1 d . . . H62A H 0.4745 0.6357 0.4499 0.042 Uiso 1 1 calc R . . H62B H 0.4396 0.6831 0.5302 0.042 Uiso 1 1 calc R . . H62C H 0.5401 0.6991 0.4794 0.042 Uiso 1 1 calc R . . C622 C 0.4274(8) 0.8622(8) 0.4384(7) 0.037(3) Uani 1 1 d . . . H62D H 0.3973 0.9147 0.3951 0.056 Uiso 1 1 calc R . . H62E H 0.4922 0.8723 0.4453 0.056 Uiso 1 1 calc R . . H62F H 0.3921 0.8549 0.4964 0.056 Uiso 1 1 calc R . . C691 C 0.0104(8) 0.6514(9) 0.3180(8) 0.046(3) Uani 1 1 d . . . H69A H 0.0409 0.5890 0.3401 0.069 Uiso 1 1 calc R . . H69B H -0.0370 0.6514 0.2759 0.069 Uiso 1 1 calc R . . H69C H -0.0201 0.6742 0.3685 0.069 Uiso 1 1 calc R . . C692 C 0.0405(7) 0.8140(8) 0.2341(7) 0.039(3) Uani 1 1 d . . . H69D H 0.0062 0.8362 0.2835 0.058 Uiso 1 1 calc R . . H69E H -0.0031 0.8164 0.1878 0.058 Uiso 1 1 calc R . . H69F H 0.0903 0.8527 0.2085 0.058 Uiso 1 1 calc R . . C821 C 0.1426(7) 0.5057(8) 0.5090(7) 0.036(2) Uani 1 1 d . . . H82A H 0.0889 0.5249 0.5462 0.054 Uiso 1 1 calc R . . H82B H 0.1468 0.4396 0.5154 0.054 Uiso 1 1 calc R . . H82C H 0.1339 0.5378 0.4461 0.054 Uiso 1 1 calc R . . C822 C 0.3224(7) 0.5011(7) 0.4851(7) 0.032(2) Uani 1 1 d . . . H82D H 0.3784 0.5173 0.5070 0.047 Uiso 1 1 calc R . . H82E H 0.3163 0.5328 0.4218 0.047 Uiso 1 1 calc R . . H82F H 0.3285 0.4349 0.4916 0.047 Uiso 1 1 calc R . . N11 N 0.2313(6) 0.3326(6) 0.0532(5) 0.0276(18) Uani 1 1 d . . . N20 N 0.3009(6) 0.2744(6) 0.2203(5) 0.0302(19) Uani 1 1 d . . . N21 N 0.2985(6) 0.1303(6) 0.0131(5) 0.0272(18) Uani 1 1 d . . . N30 N 0.4241(5) 0.2389(6) 0.0483(5) 0.0307(19) Uani 1 1 d . . . N31 N 0.3767(6) 0.0786(6) 0.1884(6) 0.0316(19) Uani 1 1 d . . . N41 N 0.1832(6) 0.1569(6) 0.1753(5) 0.0256(17) Uani 1 1 d . . . N51 N 0.2203(5) 0.8007(5) 0.5641(5) 0.0233(16) Uani 1 1 d . . . N60 N 0.2265(5) 0.6296(5) 0.5378(5) 0.0207(16) Uani 1 1 d . . . N61 N 0.3255(5) 0.7559(6) 0.3884(5) 0.0253(18) Uani 1 1 d . . . N70 N 0.1660(5) 0.7172(6) 0.3285(5) 0.0232(16) Uani 1 1 d . . . N71 N 0.1586(6) 0.8960(6) 0.3654(5) 0.0288(19) Uani 1 1 d . . . N611 N 0.0610(5) 0.7639(6) 0.4827(5) 0.0251(17) Uani 1 1 d . . . O24 O 0.3961(7) 0.0918(7) -0.1002(5) 0.056(2) Uani 1 1 d . . . O27 O 0.5279(6) 0.2086(6) -0.0637(5) 0.050(2) Uani 1 1 d . . . O32 O 0.3528(6) 0.0425(6) 0.2684(5) 0.045(2) Uani 1 1 d . . . O33 O 0.4464(6) 0.0435(6) 0.1477(6) 0.056(2) Uani 1 1 d . . . O54 O 0.2669(5) 0.7480(5) 0.7066(4) 0.0346(17) Uani 1 1 d . . . O57 O 0.2697(5) 0.5620(5) 0.6811(4) 0.0288(15) Uani 1 1 d . . . O64 O 0.4112(5) 0.7500(6) 0.2556(4) 0.0381(19) Uani 1 1 d . . . O67 O 0.2405(5) 0.7052(6) 0.1924(4) 0.0376(19) Uani 1 1 d . . . O71 O 0.9263(8) 0.1895(11) 0.1366(7) 0.100(5) Uani 1 1 d . . . O72 O 0.9186(6) 0.1676(7) -0.0117(6) 0.063(3) Uani 1 1 d . . . O73 O 0.8181(9) 0.2842(9) 0.0352(8) 0.092(4) Uani 1 1 d . . . O74 O 0.7910(9) 0.1331(10) 0.0990(8) 0.089(4) Uani 1 1 d . . . O81 O 0.5161(8) 0.4131(8) 0.2808(7) 0.073(3) Uani 1 1 d . . . O82 O 0.4014(6) 0.5436(7) 0.2406(6) 0.061(3) Uani 1 1 d . . . O83 O 0.5271(7) 0.5466(10) 0.3311(8) 0.091(4) Uani 1 1 d . . . O84 O 0.5600(7) 0.5488(8) 0.1784(7) 0.077(3) Uani 1 1 d . . . O91 O 1.0658(6) 0.6709(7) 0.6838(6) 0.062(3) Uani 1 1 d . . . O92 O 1.0392(8) 0.5279(7) 0.7856(6) 0.067(3) Uani 1 1 d . . . O93 O 0.9276(5) 0.6610(6) 0.7841(5) 0.0404(19) Uani 1 1 d . . . O94 O 0.9439(6) 0.5870(7) 0.6604(5) 0.051(2) Uani 1 1 d . . . O101 O 0.7466(17) 0.7204(10) 0.4330(9) 0.163(9) Uani 1 1 d . . . O102 O 0.8270(8) 0.8350(9) 0.3594(10) 0.096(4) Uani 1 1 d . . . O103 O 0.6669(7) 0.8587(11) 0.3632(11) 0.110(5) Uani 1 1 d . . . O104 O 0.7419(10) 0.7577(8) 0.2795(7) 0.087(4) Uani 1 1 d . . . Ru1 Ru 0.18453(5) 0.76133(5) 0.44736(4) 0.01847(18) Uani 1 1 d . . . Ru2 Ru 0.29290(5) 0.19760(6) 0.12151(5) 0.0236(2) Uani 1 1 d . . . Cl7 Cl 0.8643(2) 0.1941(2) 0.06633(18) 0.0429(7) Uani 1 1 d . . . Cl8 Cl 0.5008(2) 0.5117(2) 0.25800(18) 0.0423(7) Uani 1 1 d . . . Cl9 Cl 0.99517(17) 0.6100(2) 0.72960(16) 0.0352(6) Uani 1 1 d . . . Cl10 Cl 0.74626(18) 0.79382(19) 0.35615(17) 0.0331(6) 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 C12 0.029(5) 0.031(5) 0.017(4) -0.002(4) -0.007(3) 0.004(4) C13 0.053(7) 0.039(6) 0.023(5) 0.000(5) -0.011(5) 0.007(5) O62 0.024(4) 0.073(6) 0.031(4) -0.008(4) -0.004(3) 0.004(4) O14 0.050(4) 0.025(4) 0.028(4) -0.005(3) -0.007(3) 0.007(3) C15 0.031(5) 0.034(6) 0.019(4) 0.001(4) -0.008(4) -0.004(4) C16 0.026(5) 0.037(6) 0.021(4) 0.000(4) 0.002(4) -0.011(4) O17 0.045(4) 0.028(4) 0.027(3) -0.014(3) -0.003(3) -0.002(3) C18 0.036(6) 0.057(8) 0.025(5) -0.020(5) -0.003(4) -0.003(5) C19 0.042(6) 0.043(6) 0.013(4) -0.005(4) 0.000(4) -0.011(5) C22 0.058(7) 0.037(6) 0.016(4) -0.008(4) -0.006(4) -0.004(5) C23 0.092(11) 0.052(8) 0.031(6) -0.005(6) 0.001(6) -0.015(8) C25 0.043(6) 0.047(7) 0.024(5) -0.014(5) -0.003(4) 0.013(5) C26 0.039(6) 0.040(6) 0.023(5) -0.004(5) 0.012(4) 0.002(5) C28 0.047(7) 0.059(8) 0.034(6) -0.012(6) 0.015(5) -0.014(6) C29 0.040(6) 0.038(6) 0.028(5) -0.005(5) 0.006(4) -0.005(5) O42 0.033(4) 0.047(5) 0.041(4) -0.011(4) 0.003(3) -0.014(3) C52 0.049(6) 0.031(6) 0.019(4) -0.011(4) -0.008(4) 0.001(5) C53 0.051(7) 0.046(7) 0.026(5) -0.022(5) -0.007(5) -0.004(5) C55 0.023(4) 0.043(6) 0.009(4) -0.007(4) -0.003(3) 0.007(4) C56 0.021(4) 0.035(5) 0.012(4) -0.002(4) 0.004(3) -0.006(4) C58 0.047(6) 0.026(5) 0.024(5) 0.000(4) -0.002(4) -0.007(5) C59 0.027(4) 0.022(5) 0.020(4) 0.000(4) -0.001(3) -0.004(4) C62 0.019(4) 0.035(5) 0.016(4) -0.001(4) -0.002(3) -0.007(4) C63 0.027(5) 0.072(9) 0.025(5) -0.006(5) 0.002(4) -0.015(5) C65 0.023(5) 0.053(7) 0.012(4) -0.007(4) -0.002(3) 0.009(4) C66 0.027(4) 0.047(6) 0.007(3) -0.010(4) -0.006(3) 0.007(4) C68 0.043(6) 0.053(7) 0.025(5) -0.026(5) -0.013(4) 0.001(5) C69 0.024(5) 0.042(6) 0.025(5) -0.007(4) -0.009(4) -0.013(4) O721 0.050(5) 0.045(5) 0.026(4) 0.005(3) -0.003(3) -0.009(4) O731 0.060(5) 0.040(5) 0.035(4) 0.004(4) -0.005(4) 0.010(4) C121 0.047(6) 0.051(7) 0.022(5) -0.006(5) -0.002(4) 0.003(5) C122 0.042(6) 0.048(7) 0.025(5) -0.002(5) -0.011(4) 0.007(5) C191 0.051(7) 0.048(7) 0.028(5) 0.000(5) -0.011(5) -0.002(6) C192 0.048(6) 0.044(7) 0.020(4) -0.011(5) 0.005(4) -0.013(5) C221 0.077(8) 0.028(6) 0.023(5) -0.004(4) -0.004(5) -0.025(6) C222 0.062(8) 0.056(8) 0.054(8) -0.029(7) -0.028(6) -0.003(7) C291 0.035(6) 0.099(12) 0.039(7) 0.000(7) 0.005(5) -0.023(7) C292 0.043(7) 0.076(10) 0.057(8) -0.012(8) 0.002(6) -0.011(7) C521 0.098(11) 0.027(6) 0.037(6) -0.016(5) -0.004(7) 0.000(7) C522 0.055(7) 0.046(7) 0.035(6) -0.018(5) -0.012(5) 0.018(6) C621 0.020(4) 0.035(6) 0.028(5) -0.004(4) -0.007(4) 0.000(4) C622 0.036(6) 0.036(6) 0.035(6) -0.003(5) -0.009(4) 0.004(5) C691 0.043(6) 0.058(8) 0.036(6) -0.001(6) -0.013(5) -0.018(6) C692 0.032(5) 0.056(7) 0.028(5) -0.006(5) -0.011(4) -0.010(5) C821 0.033(5) 0.045(7) 0.029(5) -0.011(5) -0.003(4) -0.002(5) C822 0.039(6) 0.026(5) 0.030(5) -0.010(4) 0.003(4) -0.002(4) N11 0.030(4) 0.029(5) 0.021(4) -0.002(3) -0.001(3) 0.003(3) N20 0.034(4) 0.041(5) 0.017(4) -0.010(4) -0.004(3) -0.002(4) N21 0.041(5) 0.023(4) 0.017(4) -0.007(3) -0.004(3) 0.003(3) N30 0.021(4) 0.043(5) 0.023(4) -0.008(4) 0.003(3) 0.011(3) N31 0.033(4) 0.033(5) 0.025(4) 0.000(4) -0.007(3) 0.001(4) N41 0.032(4) 0.024(4) 0.023(4) -0.013(3) -0.005(3) 0.002(3) N51 0.030(4) 0.023(4) 0.017(3) -0.006(3) -0.003(3) -0.001(3) N60 0.023(4) 0.026(4) 0.013(3) -0.003(3) -0.005(3) -0.003(3) N61 0.015(3) 0.041(5) 0.015(3) 0.001(3) -0.003(3) 0.001(3) N70 0.028(4) 0.034(5) 0.012(3) -0.012(3) -0.004(3) -0.005(3) N71 0.041(5) 0.030(5) 0.013(3) 0.005(3) -0.008(3) -0.012(4) N611 0.026(4) 0.032(4) 0.016(3) -0.001(3) -0.013(3) 0.003(3) O24 0.073(6) 0.062(6) 0.031(4) -0.019(4) 0.015(4) -0.006(5) O27 0.046(5) 0.062(6) 0.035(4) -0.004(4) 0.018(4) -0.005(4) O32 0.060(5) 0.044(5) 0.023(4) 0.000(3) -0.007(3) 0.005(4) O33 0.049(5) 0.046(5) 0.057(5) 0.003(4) 0.001(4) 0.016(4) O54 0.045(4) 0.049(5) 0.012(3) -0.014(3) -0.010(3) 0.003(3) O57 0.033(4) 0.032(4) 0.017(3) 0.005(3) -0.009(3) -0.003(3) O64 0.022(3) 0.069(6) 0.020(3) -0.010(4) 0.004(3) 0.000(3) O67 0.035(4) 0.067(6) 0.014(3) -0.018(3) -0.008(3) 0.004(4) O71 0.063(7) 0.204(15) 0.042(5) -0.033(8) -0.019(5) -0.032(8) O72 0.052(5) 0.088(7) 0.037(5) -0.006(5) 0.018(4) 0.007(5) O73 0.120(10) 0.082(9) 0.062(7) -0.019(6) 0.018(7) 0.018(7) O74 0.097(8) 0.125(11) 0.067(7) -0.053(7) 0.032(6) -0.059(8) O81 0.079(7) 0.071(7) 0.065(7) -0.002(6) -0.001(5) -0.026(6) O82 0.036(4) 0.084(7) 0.062(6) -0.009(5) -0.014(4) -0.018(5) O83 0.060(6) 0.143(11) 0.102(9) -0.096(9) -0.038(6) 0.024(7) O84 0.062(6) 0.102(9) 0.051(6) 0.011(6) 0.011(5) -0.016(6) O91 0.037(5) 0.085(7) 0.058(6) -0.006(5) 0.011(4) -0.018(5) O92 0.092(7) 0.059(6) 0.036(5) 0.011(4) -0.023(5) 0.010(5) O93 0.034(4) 0.057(5) 0.037(4) -0.025(4) -0.002(3) -0.004(4) O94 0.044(5) 0.078(7) 0.038(4) -0.032(5) -0.005(4) 0.009(4) O101 0.35(3) 0.069(9) 0.049(7) 0.004(7) 0.006(11) -0.008(13) O102 0.057(6) 0.099(10) 0.163(13) -0.087(9) 0.028(7) -0.027(6) O103 0.040(6) 0.152(13) 0.180(14) -0.125(12) -0.027(7) 0.017(7) O104 0.149(11) 0.075(8) 0.045(6) -0.038(6) -0.029(6) 0.011(7) Ru1 0.0204(3) 0.0238(4) 0.0103(3) -0.0039(3) -0.0017(2) 0.0004(3) Ru2 0.0274(4) 0.0279(4) 0.0142(3) -0.0042(3) -0.0022(3) 0.0008(3) Cl7 0.0455(15) 0.059(2) 0.0258(12) -0.0114(13) 0.0018(11) -0.0123(14) Cl8 0.0372(14) 0.062(2) 0.0304(13) -0.0108(13) -0.0035(10) -0.0135(13) Cl9 0.0295(12) 0.0494(16) 0.0225(11) -0.0064(11) 0.0006(9) 0.0049(11) Cl10 0.0319(12) 0.0400(15) 0.0273(11) -0.0077(11) -0.0018(9) -0.0050(10) _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 C12 C121 1.503(14) . ? C12 C13 1.529(15) . ? C12 N11 1.531(11) . ? C12 C122 1.538(14) . ? C13 O14 1.491(12) . ? O62 N611 1.135(10) . ? O14 C15 1.327(12) . ? C15 N11 1.263(13) . ? C15 C16 1.511(13) . ? C16 N20 1.271(13) . ? C16 O17 1.296(12) . ? O17 C18 1.492(12) . ? C18 C19 1.537(16) . ? C19 N20 1.510(11) . ? C19 C191 1.515(15) . ? C19 C192 1.548(14) . ? C22 C222 1.473(16) . ? C22 N21 1.524(14) . ? C22 C221 1.545(14) . ? C22 C23 1.546(16) . ? C23 O24 1.502(16) . ? C25 N21 1.302(13) . ? C25 O24 1.321(13) . ? C25 C26 1.430(17) . ? C26 N30 1.305(13) . ? C26 O27 1.325(12) . ? C28 O27 1.480(15) . ? C28 C29 1.546(14) . ? C29 N30 1.503(14) . ? C29 C291 1.538(16) . ? C29 C292 1.543(18) . ? O42 N41 1.118(10) . ? C52 C522 1.508(16) . ? C52 C521 1.519(15) . ? C52 C53 1.536(14) . ? C52 N51 1.545(13) . ? C53 O54 1.494(14) . ? C55 N51 1.265(11) . ? C55 O54 1.320(10) . ? C55 C56 1.439(14) . ? C56 N60 1.294(11) . ? C56 O57 1.333(10) . ? C58 O57 1.474(13) . ? C58 C59 1.573(13) . ? C59 N60 1.474(12) . ? C59 C822 1.493(13) . ? C59 C821 1.530(13) . ? C62 C622 1.511(15) . ? C62 C621 1.515(12) . ? C62 C63 1.562(13) . ? C62 N61 1.564(11) . ? C63 O64 1.470(13) . ? C65 N61 1.296(12) . ? C65 O64 1.318(11) . ? C65 C66 1.463(14) . ? C66 N70 1.305(11) . ? C66 O67 1.320(10) . ? C68 O67 1.489(13) . ? C68 C69 1.544(14) . ? C69 C691 1.512(14) . ? C69 N70 1.512(11) . ? C69 C692 1.521(15) . ? O721 N71 1.250(10) . ? O731 N71 1.232(12) . ? N11 Ru2 2.121(8) . ? N20 Ru2 2.119(8) . ? N21 Ru2 2.121(8) . ? N30 Ru2 2.151(8) . ? N31 O32 1.232(10) . ? N31 O33 1.240(11) . ? N31 Ru2 2.072(8) . ? N41 Ru2 1.787(8) . ? N51 Ru1 2.114(8) . ? N60 Ru1 2.131(7) . ? N61 Ru1 2.104(7) . ? N70 Ru1 2.112(7) . ? N71 Ru1 2.079(8) . ? N611 Ru1 1.771(8) . ? O71 Cl7 1.413(9) . ? O72 Cl7 1.462(9) . ? O73 Cl7 1.395(12) . ? O74 Cl7 1.438(11) . ? O81 Cl8 1.412(11) . ? O82 Cl8 1.438(9) . ? O83 Cl8 1.429(10) . ? O84 Cl8 1.438(9) . ? O91 Cl9 1.447(9) . ? O92 Cl9 1.400(9) . ? O93 Cl9 1.468(8) . ? O94 Cl9 1.451(8) . ? O101 Cl10 1.381(12) . ? O102 Cl10 1.370(10) . ? O103 Cl10 1.391(11) . ? O104 Cl10 1.406(10) . ? 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 C121 C12 C13 112.6(9) . . ? C121 C12 N11 111.5(8) . . ? C13 C12 N11 100.2(8) . . ? C121 C12 C122 111.8(9) . . ? C13 C12 C122 113.4(9) . . ? N11 C12 C122 106.7(7) . . ? O14 C13 C12 105.7(8) . . ? C15 O14 C13 102.2(8) . . ? N11 C15 O14 122.1(8) . . ? N11 C15 C16 117.5(9) . . ? O14 C15 C16 120.3(9) . . ? N20 C16 O17 121.7(9) . . ? N20 C16 C15 117.3(10) . . ? O17 C16 C15 120.7(9) . . ? C16 O17 C18 104.1(8) . . ? O17 C18 C19 104.9(8) . . ? N20 C19 C191 114.5(9) . . ? N20 C19 C18 101.4(8) . . ? C191 C19 C18 110.6(9) . . ? N20 C19 C192 107.6(8) . . ? C191 C19 C192 110.6(9) . . ? C18 C19 C192 111.9(9) . . ? C222 C22 N21 112.3(10) . . ? C222 C22 C221 111.8(10) . . ? N21 C22 C221 107.5(8) . . ? C222 C22 C23 114.0(10) . . ? N21 C22 C23 99.4(9) . . ? C221 C22 C23 111.1(10) . . ? O24 C23 C22 106.4(10) . . ? N21 C25 O24 117.8(11) . . ? N21 C25 C26 118.7(10) . . ? O24 C25 C26 123.2(10) . . ? N30 C26 O27 116.5(11) . . ? N30 C26 C25 120.4(9) . . ? O27 C26 C25 123.1(10) . . ? O27 C28 C29 103.8(9) . . ? N30 C29 C291 108.4(9) . . ? N30 C29 C292 111.6(9) . . ? C291 C29 C292 113.5(11) . . ? N30 C29 C28 102.3(9) . . ? C291 C29 C28 108.7(10) . . ? C292 C29 C28 111.7(10) . . ? C522 C52 C521 112.1(10) . . ? C522 C52 C53 113.2(9) . . ? C521 C52 C53 112.0(10) . . ? C522 C52 N51 106.6(9) . . ? C521 C52 N51 113.3(8) . . ? C53 C52 N51 98.9(8) . . ? O54 C53 C52 104.2(8) . . ? N51 C55 O54 118.6(10) . . ? N51 C55 C56 118.5(8) . . ? O54 C55 C56 122.8(8) . . ? N60 C56 O57 117.5(9) . . ? N60 C56 C55 118.9(8) . . ? O57 C56 C55 123.4(8) . . ? O57 C58 C59 104.6(7) . . ? N60 C59 C822 111.7(8) . . ? N60 C59 C821 110.1(8) . . ? C822 C59 C821 112.7(9) . . ? N60 C59 C58 100.4(7) . . ? C822 C59 C58 110.8(8) . . ? C821 C59 C58 110.5(8) . . ? C622 C62 C621 110.7(8) . . ? C622 C62 C63 112.1(9) . . ? C621 C62 C63 112.3(9) . . ? C622 C62 N61 112.4(8) . . ? C621 C62 N61 108.5(7) . . ? C63 C62 N61 100.5(7) . . ? O64 C63 C62 105.5(7) . . ? N61 C65 O64 120.6(9) . . ? N61 C65 C66 117.1(8) . . ? O64 C65 C66 122.2(8) . . ? N70 C66 O67 119.5(8) . . ? N70 C66 C65 118.1(8) . . ? O67 C66 C65 122.3(8) . . ? O67 C68 C69 104.4(7) . . ? C691 C69 N70 114.6(8) . . ? C691 C69 C692 111.6(9) . . ? N70 C69 C692 106.8(8) . . ? C691 C69 C68 111.5(9) . . ? N70 C69 C68 99.4(7) . . ? C692 C69 C68 112.3(8) . . ? C15 N11 C12 105.3(8) . . ? C15 N11 Ru2 113.2(6) . . ? C12 N11 Ru2 141.3(7) . . ? C16 N20 C19 106.2(8) . . ? C16 N20 Ru2 113.2(7) . . ? C19 N20 Ru2 137.5(7) . . ? C25 N21 C22 109.4(9) . . ? C25 N21 Ru2 111.8(7) . . ? C22 N21 Ru2 137.0(6) . . ? C26 N30 C29 108.2(8) . . ? C26 N30 Ru2 109.6(7) . . ? C29 N30 Ru2 140.8(6) . . ? O32 N31 O33 121.6(8) . . ? O32 N31 Ru2 117.7(7) . . ? O33 N31 Ru2 120.6(6) . . ? O42 N41 Ru2 176.5(8) . . ? C55 N51 C52 107.4(8) . . ? C55 N51 Ru1 113.4(7) . . ? C52 N51 Ru1 137.0(6) . . ? C56 N60 C59 109.5(7) . . ? C56 N60 Ru1 111.5(6) . . ? C59 N60 Ru1 139.0(6) . . ? C65 N61 C62 105.5(7) . . ? C65 N61 Ru1 113.0(6) . . ? C62 N61 Ru1 140.9(6) . . ? C66 N70 C69 105.8(7) . . ? C66 N70 Ru1 112.1(6) . . ? C69 N70 Ru1 138.2(6) . . ? O731 N71 O721 121.1(8) . . ? O731 N71 Ru1 119.6(6) . . ? O721 N71 Ru1 119.2(7) . . ? O62 N611 Ru1 175.2(8) . . ? C25 O24 C23 105.1(9) . . ? C26 O27 C28 107.9(9) . . ? C55 O54 C53 105.0(7) . . ? C56 O57 C58 105.5(7) . . ? C65 O64 C63 105.7(8) . . ? C66 O67 C68 103.1(7) . . ? N611 Ru1 N71 89.9(3) . . ? N611 Ru1 N61 172.2(3) . . ? N71 Ru1 N61 88.1(3) . . ? N611 Ru1 N70 93.7(3) . . ? N71 Ru1 N70 85.5(3) . . ? N61 Ru1 N70 78.6(3) . . ? N611 Ru1 N51 92.7(3) . . ? N71 Ru1 N51 96.3(3) . . ? N61 Ru1 N51 95.1(3) . . ? N70 Ru1 N51 173.3(3) . . ? N611 Ru1 N60 95.1(3) . . ? N71 Ru1 N60 172.4(3) . . ? N61 Ru1 N60 87.7(3) . . ? N70 Ru1 N60 99.8(3) . . ? N51 Ru1 N60 77.8(3) . . ? N41 Ru2 N31 93.4(3) . . ? N41 Ru2 N20 91.1(3) . . ? N31 Ru2 N20 95.9(3) . . ? N41 Ru2 N21 95.9(3) . . ? N31 Ru2 N21 85.3(3) . . ? N20 Ru2 N21 172.8(3) . . ? N41 Ru2 N11 96.4(3) . . ? N31 Ru2 N11 168.8(3) . . ? N20 Ru2 N11 78.4(3) . . ? N21 Ru2 N11 99.1(3) . . ? N41 Ru2 N30 174.8(4) . . ? N31 Ru2 N30 85.9(3) . . ? N20 Ru2 N30 94.1(3) . . ? N21 Ru2 N30 79.0(3) . . ? N11 Ru2 N30 84.9(3) . . ? O73 Cl7 O71 111.3(9) . . ? O73 Cl7 O74 107.4(8) . . ? O71 Cl7 O74 110.6(7) . . ? O73 Cl7 O72 107.7(6) . . ? O71 Cl7 O72 110.4(7) . . ? O74 Cl7 O72 109.3(6) . . ? O81 Cl8 O83 110.2(7) . . ? O81 Cl8 O84 110.1(7) . . ? O83 Cl8 O84 107.4(8) . . ? O81 Cl8 O82 110.5(6) . . ? O83 Cl8 O82 109.1(6) . . ? O84 Cl8 O82 109.6(6) . . ? O92 Cl9 O91 111.0(6) . . ? O92 Cl9 O94 109.5(6) . . ? O91 Cl9 O94 108.2(5) . . ? O92 Cl9 O93 110.5(5) . . ? O91 Cl9 O93 108.1(6) . . ? O94 Cl9 O93 109.4(5) . . ? O102 Cl10 O101 105.2(11) . . ? O102 Cl10 O103 107.6(7) . . ? O101 Cl10 O103 109.2(11) . . ? O102 Cl10 O104 115.9(8) . . ? O101 Cl10 O104 107.8(8) . . ? O103 Cl10 O104 110.8(7) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 4.715 _refine_diff_density_min -1.337 _refine_diff_density_rms 0.202 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END