# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/241 data_global #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Dr. Mike Ward School of Chemistry Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_fax '0117 9287655' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the four crystal structures in the paper 'New hybrid ditopic ligands...' by C. R. Rice, et al, submitted to New J. Chem. for publication. ; #======================================================== data_sad1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H29 Cl2 N7 O10 Ru' _chemical_formula_weight 891.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7139(4) _cell_length_b 12.6362(5) _cell_length_c 16.8896(7) _cell_angle_alpha 81.7780(10) _cell_angle_beta 80.3950(10) _cell_angle_gamma 78.8510(10) _cell_volume 1787.22(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.8268 _exptl_absorpt_correction_T_max 0.9370 _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 '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 18754 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8108 _reflns_number_gt 6910 _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^)+(0.0487P)^2^+1.3353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8108 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.61572(2) -0.323806(15) -0.259281(11) 0.02242(7) Uani 1 1 d . . . N11 N -0.5684(2) -0.28394(17) -0.15320(12) 0.0269(4) Uani 1 1 d . . . C12 C -0.5952(3) -0.1763(2) -0.14498(15) 0.0291(5) Uani 1 1 d . . . C13 C -0.5682(3) -0.1390(2) -0.07604(17) 0.0378(6) Uani 1 1 d . . . H13 H -0.5864 -0.0633 -0.0717 0.045 Uiso 1 1 calc R . . C14 C -0.5149(3) -0.2123(3) -0.01409(17) 0.0403(7) Uani 1 1 d . . . H14 H -0.4945 -0.1879 0.0331 0.048 Uiso 1 1 calc R . . C15 C -0.4914(4) -0.3222(3) -0.02136(17) 0.0393(6) Uani 1 1 d . . . H15 H -0.4576 -0.3743 0.0214 0.047 Uiso 1 1 calc R . . C16 C -0.5176(3) -0.3547(2) -0.09138(16) 0.0332(6) Uani 1 1 d . . . H16 H -0.4994 -0.4302 -0.0965 0.040 Uiso 1 1 calc R . . N21 N -0.6902(3) -0.15799(17) -0.27224(13) 0.0273(4) Uani 1 1 d . . . C22 C -0.6576(3) -0.1055(2) -0.21367(16) 0.0302(5) Uani 1 1 d . . . C23 C -0.6865(4) 0.0067(2) -0.2193(2) 0.0457(7) Uani 1 1 d . . . H23 H -0.6579 0.0423 -0.1795 0.055 Uiso 1 1 calc R . . C24 C -0.7565(5) 0.0669(3) -0.2825(2) 0.0544(9) Uani 1 1 d . . . H24 H -0.7782 0.1439 -0.2862 0.065 Uiso 1 1 calc R . . C25 C -0.7944(4) 0.0140(2) -0.3399(2) 0.0479(8) Uani 1 1 d . . . H25 H -0.8453 0.0538 -0.3833 0.057 Uiso 1 1 calc R . . C26 C -0.7576(4) -0.0982(2) -0.33383(17) 0.0369(6) Uani 1 1 d . . . H26 H -0.7810 -0.1344 -0.3748 0.044 Uiso 1 1 calc R . . N31 N -0.4076(2) -0.29251(17) -0.32894(12) 0.0268(4) Uani 1 1 d . . . C32 C -0.3962(3) -0.2991(2) -0.40926(15) 0.0285(5) Uani 1 1 d . . . C33 C -0.2686(3) -0.2709(2) -0.46352(17) 0.0366(6) Uani 1 1 d . . . H33 H -0.2621 -0.2774 -0.5194 0.044 Uiso 1 1 calc R . . C34 C -0.1512(3) -0.2333(3) -0.43573(18) 0.0403(7) Uani 1 1 d . . . H34 H -0.0632 -0.2133 -0.4721 0.048 Uiso 1 1 calc R . . C35 C -0.1637(3) -0.2252(2) -0.35450(18) 0.0382(6) Uani 1 1 d . . . H35 H -0.0847 -0.1988 -0.3342 0.046 Uiso 1 1 calc R . . C36 C -0.2917(3) -0.2557(2) -0.30264(17) 0.0338(6) Uani 1 1 d . . . H36 H -0.2985 -0.2507 -0.2465 0.041 Uiso 1 1 calc R . . N41 N -0.6497(2) -0.35125(16) -0.37246(12) 0.0249(4) Uani 1 1 d . . . C42 C -0.5303(3) -0.3353(2) -0.43358(15) 0.0283(5) Uani 1 1 d . . . C43 C -0.5388(4) -0.3508(2) -0.51250(16) 0.0360(6) Uani 1 1 d . . . H43 H -0.4548 -0.3386 -0.5546 0.043 Uiso 1 1 calc R . . C44 C -0.6710(4) -0.3842(2) -0.52887(17) 0.0386(6) Uani 1 1 d . . . H44 H -0.6796 -0.3941 -0.5826 0.046 Uiso 1 1 calc R . . C45 C -0.7905(3) -0.4030(2) -0.46663(17) 0.0359(6) Uani 1 1 d . . . H45 H -0.8814 -0.4272 -0.4767 0.043 Uiso 1 1 calc R . . C46 C -0.7757(3) -0.3861(2) -0.38961(16) 0.0307(5) Uani 1 1 d . . . H46 H -0.8579 -0.3996 -0.3469 0.037 Uiso 1 1 calc R . . N51 N -0.5514(2) -0.49062(16) -0.23469(12) 0.0238(4) Uani 1 1 d . . . C52 C -0.6719(3) -0.5401(2) -0.19263(14) 0.0239(5) Uani 1 1 d . . . C53 C -0.6565(3) -0.6527(2) -0.17144(14) 0.0266(5) Uani 1 1 d . . . C54 C -0.5099(3) -0.7167(2) -0.19635(16) 0.0310(5) Uani 1 1 d . . . H54 H -0.4948 -0.7935 -0.1849 0.037 Uiso 1 1 calc R . . C55 C -0.3891(3) -0.6663(2) -0.23744(16) 0.0332(6) Uani 1 1 d . . . H55 H -0.2889 -0.7084 -0.2537 0.040 Uiso 1 1 calc R . . C56 C -0.4129(3) -0.5533(2) -0.25546(15) 0.0295(5) Uani 1 1 d . . . H56 H -0.3273 -0.5201 -0.2835 0.035 Uiso 1 1 calc R . . N61 N -0.8243(2) -0.36245(16) -0.19454(12) 0.0245(4) Uani 1 1 d . . . C62 C -0.8177(3) -0.47079(19) -0.16909(14) 0.0240(5) Uani 1 1 d . . . C63 C -0.9453(3) -0.5141(2) -0.12266(14) 0.0270(5) Uani 1 1 d . . . C64 C -1.0848(3) -0.4411(2) -0.10087(16) 0.0324(6) Uani 1 1 d . . . H64 H -1.1743 -0.4666 -0.0696 0.039 Uiso 1 1 calc R . . C65 C -1.0895(3) -0.3325(2) -0.12549(16) 0.0342(6) Uani 1 1 d . . . H65 H -1.1826 -0.2823 -0.1107 0.041 Uiso 1 1 calc R . . C66 C -0.9582(3) -0.2951(2) -0.17226(16) 0.0305(5) Uani 1 1 d . . . H66 H -0.9644 -0.2195 -0.1887 0.037 Uiso 1 1 calc R . . C71 C -0.9277(3) -0.6292(2) -0.10119(16) 0.0309(5) Uani 1 1 d . . . C72 C -0.7888(3) -0.6958(2) -0.12499(15) 0.0279(5) Uani 1 1 d . . . O73 O -0.7671(2) -0.80613(15) -0.10728(12) 0.0371(4) Uani 1 1 d . . . C74 C -0.8932(5) -0.8440(3) -0.0515(3) 0.0637(11) Uani 1 1 d . . . H74A H -0.8746 -0.8408 0.0043 0.076 Uiso 1 1 calc R . . H74B H -0.8921 -0.9210 -0.0577 0.076 Uiso 1 1 calc R . . C75 C -1.0479(4) -0.7818(3) -0.0629(3) 0.0606(10) Uani 1 1 d . . . H75A H -1.0723 -0.7923 -0.1161 0.073 Uiso 1 1 calc R . . H75B H -1.1284 -0.8096 -0.0208 0.073 Uiso 1 1 calc R . . O76 O -1.0582(2) -0.66719(17) -0.05912(13) 0.0404(5) Uani 1 1 d . . . Cl1 Cl 0.02628(8) -0.63490(6) -0.33637(4) 0.03906(16) Uani 1 1 d . . . O11 O -0.0551(3) -0.5329(2) -0.3689(2) 0.0798(9) Uani 1 1 d . . . O12 O -0.0271(3) -0.6562(3) -0.25328(15) 0.0837(10) Uani 1 1 d . . . O13 O -0.0104(3) -0.7174(2) -0.37687(17) 0.0691(8) Uani 1 1 d . . . O14 O 0.1947(3) -0.6379(2) -0.34884(14) 0.0500(6) Uani 1 1 d . . . Cl2 Cl -1.19722(9) -1.00156(6) -0.15801(5) 0.04241(17) Uani 1 1 d . . . O21 O -1.1894(4) -0.9063(2) -0.2149(2) 0.0858(10) Uani 1 1 d . . . O22 O -1.3141(4) -0.9752(3) -0.0924(2) 0.0906(11) Uani 1 1 d . . . O23 O -1.2372(3) -1.08446(19) -0.19558(16) 0.0569(6) Uani 1 1 d . . . O24 O -1.0440(3) -1.0382(2) -0.13317(16) 0.0567(6) Uani 1 1 d . . . N200 N -0.0979(12) 0.0485(8) -0.4825(5) 0.094(3) Uani 0.50 1 d P A 1 C201 C -0.2128(16) 0.0562(9) -0.4381(6) 0.073(3) Uani 0.50 1 d P A 1 C202 C -0.3574(15) 0.0624(10) -0.3834(9) 0.077(3) Uani 0.50 1 d P A 1 H20A H -0.4137 0.0053 -0.3909 0.115 Uiso 0.50 1 calc PR A 1 H20B H -0.4234 0.1336 -0.3941 0.115 Uiso 0.50 1 calc PR A 1 H20C H -0.3344 0.0526 -0.3277 0.115 Uiso 0.50 1 calc PR A 1 N210 N -0.4479(12) 0.0390(9) -0.4785(6) 0.106(3) Uani 0.50 1 d P . 2 C211 C -0.3698(15) 0.0570(8) -0.4385(7) 0.078(3) Uani 0.50 1 d P B 2 C212 C -0.265(2) 0.0806(12) -0.3861(11) 0.108(5) Uani 0.50 1 d P B 2 H21A H -0.3018 0.1542 -0.3706 0.162 Uiso 0.50 1 calc PR B 2 H21B H -0.1570 0.0754 -0.4152 0.162 Uiso 0.50 1 calc PR B 2 H21C H -0.2657 0.0281 -0.3374 0.162 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02558(11) 0.01918(10) 0.02244(10) -0.00372(7) -0.00344(7) -0.00275(7) N11 0.0271(11) 0.0275(11) 0.0273(10) -0.0067(8) -0.0025(8) -0.0061(9) C12 0.0279(13) 0.0292(13) 0.0314(13) -0.0090(10) 0.0018(10) -0.0090(10) C13 0.0384(15) 0.0386(16) 0.0403(15) -0.0184(12) -0.0025(12) -0.0089(13) C14 0.0370(15) 0.0566(19) 0.0312(14) -0.0173(13) -0.0030(11) -0.0104(14) C15 0.0401(16) 0.0495(18) 0.0291(14) -0.0044(12) -0.0086(11) -0.0069(13) C16 0.0362(15) 0.0334(14) 0.0303(13) -0.0044(11) -0.0053(11) -0.0055(12) N21 0.0304(11) 0.0211(10) 0.0291(11) -0.0026(8) -0.0007(8) -0.0042(8) C22 0.0313(13) 0.0237(12) 0.0352(13) -0.0085(10) 0.0021(10) -0.0063(10) C23 0.061(2) 0.0252(14) 0.0511(18) -0.0108(13) -0.0014(15) -0.0092(14) C24 0.074(2) 0.0223(15) 0.063(2) -0.0051(14) -0.0036(18) -0.0029(15) C25 0.061(2) 0.0295(15) 0.0471(18) 0.0054(13) -0.0106(15) 0.0013(14) C26 0.0440(16) 0.0293(14) 0.0352(14) 0.0005(11) -0.0063(12) -0.0041(12) N31 0.0284(11) 0.0224(10) 0.0291(11) -0.0038(8) -0.0044(8) -0.0022(8) C32 0.0301(13) 0.0248(12) 0.0286(12) -0.0025(9) -0.0031(10) -0.0010(10) C33 0.0345(15) 0.0406(16) 0.0322(14) -0.0026(11) 0.0000(11) -0.0059(12) C34 0.0328(15) 0.0430(17) 0.0420(16) -0.0005(13) 0.0029(12) -0.0096(13) C35 0.0322(14) 0.0402(16) 0.0448(16) -0.0058(12) -0.0068(12) -0.0113(12) C36 0.0341(14) 0.0337(14) 0.0348(14) -0.0057(11) -0.0061(11) -0.0065(11) N41 0.0295(11) 0.0200(10) 0.0250(10) -0.0029(8) -0.0055(8) -0.0020(8) C42 0.0328(13) 0.0228(12) 0.0274(12) -0.0022(9) -0.0032(10) -0.0018(10) C43 0.0400(15) 0.0401(16) 0.0266(13) -0.0038(11) -0.0021(11) -0.0059(12) C44 0.0462(17) 0.0436(17) 0.0287(13) -0.0085(12) -0.0097(12) -0.0073(13) C45 0.0394(15) 0.0366(15) 0.0354(14) -0.0057(11) -0.0126(12) -0.0087(12) C46 0.0327(14) 0.0287(13) 0.0322(13) -0.0038(10) -0.0081(10) -0.0060(11) N51 0.0257(10) 0.0220(10) 0.0238(10) -0.0042(8) -0.0039(8) -0.0024(8) C52 0.0267(12) 0.0237(12) 0.0220(11) -0.0052(9) -0.0062(9) -0.0022(9) C53 0.0338(13) 0.0227(12) 0.0247(12) -0.0046(9) -0.0097(10) -0.0024(10) C54 0.0369(14) 0.0218(12) 0.0334(13) -0.0064(10) -0.0065(11) 0.0007(11) C55 0.0315(14) 0.0276(14) 0.0366(14) -0.0058(11) -0.0028(11) 0.0040(11) C56 0.0282(13) 0.0275(13) 0.0310(13) -0.0048(10) -0.0028(10) -0.0003(10) N61 0.0266(10) 0.0225(10) 0.0245(10) -0.0059(8) -0.0047(8) -0.0010(8) C62 0.0269(12) 0.0239(12) 0.0219(11) -0.0042(9) -0.0056(9) -0.0030(9) C63 0.0289(13) 0.0277(13) 0.0251(12) -0.0040(9) -0.0059(9) -0.0041(10) C64 0.0277(13) 0.0341(14) 0.0341(14) -0.0054(11) 0.0001(10) -0.0051(11) C65 0.0290(13) 0.0342(15) 0.0352(14) -0.0071(11) -0.0012(11) 0.0037(11) C66 0.0331(14) 0.0245(13) 0.0325(13) -0.0064(10) -0.0049(10) 0.0010(10) C71 0.0344(14) 0.0297(13) 0.0301(13) -0.0024(10) -0.0038(10) -0.0110(11) C72 0.0342(13) 0.0225(12) 0.0287(12) -0.0029(9) -0.0071(10) -0.0066(10) O73 0.0447(12) 0.0232(9) 0.0432(11) -0.0021(8) -0.0018(9) -0.0106(8) C74 0.065(2) 0.0354(18) 0.082(3) -0.0018(17) 0.018(2) -0.0164(17) C75 0.053(2) 0.0377(18) 0.089(3) 0.0018(18) 0.0038(19) -0.0214(16) O76 0.0375(11) 0.0343(11) 0.0477(12) -0.0011(9) 0.0033(9) -0.0124(9) Cl1 0.0359(4) 0.0429(4) 0.0378(4) -0.0014(3) -0.0053(3) -0.0078(3) O11 0.0471(15) 0.0545(17) 0.127(3) 0.0190(17) -0.0113(16) -0.0050(13) O12 0.0656(18) 0.157(3) 0.0368(13) -0.0080(16) -0.0052(12) -0.044(2) O13 0.0638(17) 0.081(2) 0.0724(18) -0.0248(15) -0.0193(14) -0.0174(15) O14 0.0369(12) 0.0539(14) 0.0592(14) -0.0074(11) -0.0064(10) -0.0076(10) Cl2 0.0410(4) 0.0272(3) 0.0583(4) -0.0131(3) -0.0034(3) -0.0013(3) O21 0.097(2) 0.0412(15) 0.115(3) 0.0180(16) -0.033(2) -0.0074(15) O22 0.072(2) 0.103(3) 0.099(2) -0.059(2) 0.0259(17) -0.0168(18) O23 0.0667(16) 0.0375(13) 0.0708(16) -0.0207(11) -0.0148(13) -0.0047(11) O24 0.0493(14) 0.0476(14) 0.0724(17) -0.0023(12) -0.0161(12) -0.0037(11) N200 0.115(7) 0.124(8) 0.066(5) -0.002(5) -0.010(5) -0.083(6) C201 0.107(9) 0.074(6) 0.051(5) 0.004(5) -0.020(6) -0.045(6) C202 0.083(8) 0.068(7) 0.072(8) 0.010(6) -0.010(7) -0.008(6) N210 0.088(7) 0.147(10) 0.073(6) -0.003(6) 0.001(5) -0.011(6) C211 0.102(9) 0.071(6) 0.047(6) 0.003(4) -0.004(5) 0.001(6) C212 0.159(17) 0.076(8) 0.102(12) 0.012(7) -0.057(14) -0.040(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 Ru1 N11 2.054(2) . ? Ru1 N21 2.061(2) . ? Ru1 N31 2.065(2) . ? Ru1 N61 2.065(2) . ? Ru1 N41 2.069(2) . ? Ru1 N51 2.074(2) . ? N11 C16 1.349(3) . ? N11 C12 1.358(3) . ? C12 C13 1.387(4) . ? C12 C22 1.473(4) . ? C13 C14 1.374(4) . ? C14 C15 1.384(4) . ? C15 C16 1.373(4) . ? N21 C26 1.344(3) . ? N21 C22 1.362(3) . ? C22 C23 1.383(4) . ? C23 C24 1.377(5) . ? C24 C25 1.368(5) . ? C25 C26 1.386(4) . ? N31 C36 1.350(3) . ? N31 C32 1.357(3) . ? C32 C33 1.386(4) . ? C32 C42 1.471(4) . ? C33 C34 1.380(4) . ? C34 C35 1.375(4) . ? C35 C36 1.379(4) . ? N41 C46 1.346(3) . ? N41 C42 1.361(3) . ? C42 C43 1.391(4) . ? C43 C44 1.382(4) . ? C44 C45 1.380(4) . ? C45 C46 1.379(4) . ? N51 C56 1.332(3) . ? N51 C52 1.370(3) . ? C52 C53 1.403(3) . ? C52 C62 1.428(3) . ? C53 C54 1.408(4) . ? C53 C72 1.435(4) . ? C54 C55 1.372(4) . ? C55 C56 1.400(4) . ? N61 C66 1.338(3) . ? N61 C62 1.368(3) . ? C62 C63 1.405(3) . ? C63 C64 1.407(4) . ? C63 C71 1.432(4) . ? C64 C65 1.370(4) . ? C65 C66 1.399(4) . ? C71 O76 1.369(3) . ? C71 C72 1.370(4) . ? C72 O73 1.366(3) . ? O73 C74 1.433(4) . ? C74 C75 1.451(6) . ? C75 O76 1.443(4) . ? Cl1 O12 1.407(3) . ? Cl1 O11 1.428(3) . ? Cl1 O13 1.437(3) . ? Cl1 O14 1.442(2) . ? Cl2 O22 1.405(3) . ? Cl2 O23 1.423(2) . ? Cl2 O21 1.434(3) . ? Cl2 O24 1.437(2) . ? N200 C201 1.144(14) . ? C201 C202 1.429(18) . ? N210 C211 1.108(14) . ? N210 N210 1.76(2) 2_454 ? C211 C212 1.471(19) . ? 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 Ru1 N21 78.95(8) . . ? N11 Ru1 N31 96.42(8) . . ? N21 Ru1 N31 86.09(8) . . ? N11 Ru1 N61 86.86(8) . . ? N21 Ru1 N61 96.30(8) . . ? N31 Ru1 N61 176.28(8) . . ? N11 Ru1 N41 173.83(8) . . ? N21 Ru1 N41 97.23(8) . . ? N31 Ru1 N41 78.39(8) . . ? N61 Ru1 N41 98.44(8) . . ? N11 Ru1 N51 96.93(8) . . ? N21 Ru1 N51 174.43(8) . . ? N31 Ru1 N51 98.17(8) . . ? N61 Ru1 N51 79.63(8) . . ? N41 Ru1 N51 87.19(8) . . ? C16 N11 C12 118.1(2) . . ? C16 N11 Ru1 125.89(18) . . ? C12 N11 Ru1 115.97(17) . . ? N11 C12 C13 121.5(3) . . ? N11 C12 C22 114.4(2) . . ? C13 C12 C22 124.1(2) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 119.2(3) . . ? C16 C15 C14 118.9(3) . . ? N11 C16 C15 122.7(3) . . ? C26 N21 C22 118.3(2) . . ? C26 N21 Ru1 126.73(19) . . ? C22 N21 Ru1 114.86(17) . . ? N21 C22 C23 120.9(3) . . ? N21 C22 C12 115.3(2) . . ? C23 C22 C12 123.8(3) . . ? C24 C23 C22 120.1(3) . . ? C25 C24 C23 119.0(3) . . ? C24 C25 C26 119.1(3) . . ? N21 C26 C25 122.5(3) . . ? C36 N31 C32 118.2(2) . . ? C36 N31 Ru1 125.43(18) . . ? C32 N31 Ru1 116.02(17) . . ? N31 C32 C33 121.7(2) . . ? N31 C32 C42 114.9(2) . . ? C33 C32 C42 123.4(2) . . ? C34 C33 C32 119.4(3) . . ? C35 C34 C33 118.9(3) . . ? C34 C35 C36 119.6(3) . . ? N31 C36 C35 122.2(3) . . ? C46 N41 C42 118.3(2) . . ? C46 N41 Ru1 125.82(17) . . ? C42 N41 Ru1 115.86(17) . . ? N41 C42 C43 121.5(2) . . ? N41 C42 C32 114.7(2) . . ? C43 C42 C32 123.8(2) . . ? C44 C43 C42 119.1(3) . . ? C45 C44 C43 119.5(3) . . ? C46 C45 C44 118.8(3) . . ? N41 C46 C45 122.8(3) . . ? C56 N51 C52 117.8(2) . . ? C56 N51 Ru1 128.80(18) . . ? C52 N51 Ru1 113.39(16) . . ? N51 C52 C53 123.2(2) . . ? N51 C52 C62 116.6(2) . . ? C53 C52 C62 120.1(2) . . ? C52 C53 C54 117.4(2) . . ? C52 C53 C72 118.7(2) . . ? C54 C53 C72 123.9(2) . . ? C55 C54 C53 119.0(2) . . ? C54 C55 C56 120.3(2) . . ? N51 C56 C55 122.3(2) . . ? C66 N61 C62 117.8(2) . . ? C66 N61 Ru1 128.18(18) . . ? C62 N61 Ru1 113.92(16) . . ? N61 C62 C63 123.2(2) . . ? N61 C62 C52 116.3(2) . . ? C63 C62 C52 120.5(2) . . ? C62 C63 C64 117.5(2) . . ? C62 C63 C71 118.8(2) . . ? C64 C63 C71 123.7(2) . . ? C65 C64 C63 118.9(2) . . ? C64 C65 C66 120.5(2) . . ? N61 C66 C65 122.0(2) . . ? O76 C71 C72 123.1(2) . . ? O76 C71 C63 116.1(2) . . ? C72 C71 C63 120.7(2) . . ? O73 C72 C71 122.9(2) . . ? O73 C72 C53 115.8(2) . . ? C71 C72 C53 121.2(2) . . ? C72 O73 C74 113.7(2) . . ? O73 C74 C75 113.3(3) . . ? O76 C75 C74 112.8(3) . . ? C71 O76 C75 111.9(2) . . ? O12 Cl1 O11 110.7(2) . . ? O12 Cl1 O13 107.98(19) . . ? O11 Cl1 O13 107.36(19) . . ? O12 Cl1 O14 109.60(16) . . ? O11 Cl1 O14 111.32(16) . . ? O13 Cl1 O14 109.78(16) . . ? O22 Cl2 O23 109.44(18) . . ? O22 Cl2 O21 108.7(2) . . ? O23 Cl2 O21 109.66(19) . . ? O22 Cl2 O24 111.8(2) . . ? O23 Cl2 O24 109.19(15) . . ? O21 Cl2 O24 108.04(18) . . ? N200 C201 C202 178.0(13) . . ? C211 N210 N210 157.8(14) . 2_454 ? N210 C211 C212 179.4(16) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.956 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.074 #=END data_espagnam _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Cl2 N10 O12 Ru' _chemical_formula_weight 1102.90 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 11.830(4) _cell_length_b 13.271(5) _cell_length_c 17.791(6) _cell_angle_alpha 97.664(6) _cell_angle_beta 92.213(6) _cell_angle_gamma 115.897(6) _cell_volume 2475.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.94 _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 '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 25957 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.58 _reflns_number_total 11238 _reflns_number_gt 6370 _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^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11238 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.031 _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 0.90204(3) 0.82814(3) 0.743646(19) 0.02741(10) Uani 1 1 d . . . Cl1 Cl 0.34766(11) 0.74443(9) 0.05321(6) 0.0405(3) Uani 1 1 d . . . O100 O 0.4028(3) 0.8523(3) 0.0272(2) 0.0571(9) Uani 1 1 d . . . O101 O 0.2960(4) 0.7557(3) 0.1227(2) 0.0830(14) Uani 1 1 d . . . O102 O 0.4451(4) 0.7101(4) 0.0678(3) 0.0963(15) Uani 1 1 d . . . O103 O 0.2523(4) 0.6624(3) -0.0024(2) 0.0892(14) Uani 1 1 d . . . Cl2 Cl 0.30483(12) 0.64715(12) 0.40694(7) 0.0526(3) Uani 1 1 d . . . O201 O 0.2053(6) 0.5462(4) 0.4206(3) 0.130(2) Uani 1 1 d . . . O202 O 0.3966(4) 0.6207(4) 0.3708(2) 0.0821(13) Uani 1 1 d . . . O203 O 0.2522(4) 0.6942(4) 0.3586(2) 0.0885(14) Uani 1 1 d . . . O204 O 0.3574(5) 0.7204(6) 0.4754(3) 0.164(3) Uani 1 1 d . . . N11 N 0.9978(3) 0.7934(3) 0.65651(18) 0.0284(8) Uani 1 1 d . . . C12 C 0.9199(4) 0.7360(3) 0.5901(2) 0.0261(9) Uani 1 1 d . . . C13 C 0.7908(4) 0.7117(3) 0.5904(2) 0.0270(9) Uani 1 1 d . . . N14 N 0.7535(3) 0.7444(3) 0.65789(18) 0.0286(8) Uani 1 1 d . . . C15 C 0.6336(4) 0.7254(3) 0.6586(2) 0.0354(10) Uani 1 1 d . . . H15 H 0.6066 0.7466 0.7051 0.042 Uiso 1 1 calc R . . C16 C 0.5458(4) 0.6759(4) 0.5942(2) 0.0389(11) Uani 1 1 d . . . H16 H 0.4610 0.6643 0.5970 0.047 Uiso 1 1 calc R . . C17 C 0.5828(4) 0.6438(3) 0.5266(2) 0.0362(10) Uani 1 1 d . . . H17 H 0.5243 0.6117 0.4819 0.043 Uiso 1 1 calc R . . C18 C 0.7066(4) 0.6588(3) 0.5239(2) 0.0296(9) Uani 1 1 d . . . C19 C 0.7531(4) 0.6256(3) 0.4559(2) 0.0309(9) Uani 1 1 d . . . C20 C 0.8751(4) 0.6437(3) 0.4569(2) 0.0293(9) Uani 1 1 d . . . C21 C 0.9643(4) 0.7039(3) 0.5236(2) 0.0276(9) Uani 1 1 d . . . C22 C 1.0925(4) 0.7309(3) 0.5261(2) 0.0338(10) Uani 1 1 d . . . H22 H 1.1257 0.7097 0.4823 0.041 Uiso 1 1 calc R . . C23 C 1.1698(4) 0.7881(3) 0.5922(2) 0.0343(10) Uani 1 1 d . . . H23 H 1.2574 0.8074 0.5945 0.041 Uiso 1 1 calc R . . C24 C 1.1197(4) 0.8182(3) 0.6562(2) 0.0331(10) Uani 1 1 d . . . H24 H 1.1750 0.8582 0.7015 0.040 Uiso 1 1 calc R . . O31 O 0.9230(3) 0.6128(2) 0.39344(15) 0.0344(7) Uani 1 1 d . . . C32 C 0.8960(5) 0.4934(4) 0.3798(2) 0.0438(12) Uani 1 1 d . . . H32A H 0.8057 0.4447 0.3838 0.053 Uiso 1 1 calc R . . H32B H 0.9480 0.4784 0.4175 0.053 Uiso 1 1 calc R . . C33 C 0.9279(5) 0.4698(4) 0.3008(3) 0.0510(13) Uani 1 1 d . . . H33A H 1.0176 0.5218 0.2974 0.061 Uiso 1 1 calc R . . H33B H 0.9180 0.3910 0.2907 0.061 Uiso 1 1 calc R . . O34 O 0.8507(3) 0.4838(3) 0.24409(19) 0.0533(9) Uani 1 1 d . . . C35 C 0.7368(6) 0.3821(5) 0.2172(4) 0.0762(18) Uani 1 1 d . . . H35A H 0.7066 0.3386 0.2594 0.091 Uiso 1 1 calc R . . H35B H 0.7534 0.3338 0.1761 0.091 Uiso 1 1 calc R . . C36 C 0.6387(6) 0.4132(5) 0.1876(3) 0.0739(18) Uani 1 1 d . . . H36A H 0.6804 0.4836 0.1655 0.089 Uiso 1 1 calc R . . H36B H 0.5814 0.3520 0.1464 0.089 Uiso 1 1 calc R . . O37 O 0.5671(3) 0.4305(3) 0.24513(19) 0.0651(10) Uani 1 1 d . . . C38 C 0.5806(5) 0.5422(5) 0.2656(3) 0.0530(13) Uani 1 1 d . . . H38A H 0.5020 0.5381 0.2857 0.064 Uiso 1 1 calc R . . H38B H 0.5905 0.5776 0.2192 0.064 Uiso 1 1 calc R . . C39 C 0.6906(5) 0.6174(4) 0.3242(2) 0.0459(12) Uani 1 1 d . . . H39A H 0.7701 0.6201 0.3067 0.055 Uiso 1 1 calc R . . H39B H 0.6988 0.6957 0.3332 0.055 Uiso 1 1 calc R . . O40 O 0.6653(3) 0.5686(2) 0.39375(16) 0.0402(7) Uani 1 1 d . . . N41 N 0.8911(3) 0.6885(3) 0.78724(18) 0.0298(8) Uani 1 1 d . . . C42 C 0.9861(4) 0.7093(3) 0.8414(2) 0.0326(10) Uani 1 1 d . . . C43 C 0.9832(5) 0.6237(4) 0.8816(3) 0.0420(11) Uani 1 1 d . . . H43 H 1.0494 0.6391 0.9199 0.050 Uiso 1 1 calc R . . C44 C 0.8827(5) 0.5178(4) 0.8642(3) 0.0489(13) Uani 1 1 d . . . H44 H 0.8784 0.4593 0.8912 0.059 Uiso 1 1 calc R . . C45 C 0.7888(5) 0.4961(4) 0.8082(3) 0.0452(12) Uani 1 1 d . . . H45 H 0.7196 0.4226 0.7955 0.054 Uiso 1 1 calc R . . C46 C 0.7964(4) 0.5831(3) 0.7705(2) 0.0388(11) Uani 1 1 d . . . H46 H 0.7317 0.5675 0.7310 0.047 Uiso 1 1 calc R . . N51 N 1.0618(3) 0.8996(3) 0.81903(18) 0.0308(8) Uani 1 1 d . . . C52 C 1.0883(4) 0.8257(3) 0.8548(2) 0.0303(9) Uani 1 1 d . . . C53 C 1.2031(4) 0.8611(4) 0.8983(2) 0.0411(11) Uani 1 1 d . . . H53 H 1.2193 0.8084 0.9225 0.049 Uiso 1 1 calc R . . C54 C 1.2927(5) 0.9714(4) 0.9064(3) 0.0468(12) Uani 1 1 d . . . H54 H 1.3726 0.9953 0.9345 0.056 Uiso 1 1 calc R . . C55 C 1.2658(5) 1.0472(4) 0.8732(3) 0.0461(12) Uani 1 1 d . . . H55 H 1.3257 1.1249 0.8796 0.055 Uiso 1 1 calc R . . C56 C 1.1507(4) 1.0094(4) 0.8304(2) 0.0405(11) Uani 1 1 d . . . H56 H 1.1331 1.0627 0.8079 0.049 Uiso 1 1 calc R . . N61 N 0.7923(3) 0.8646(3) 0.81928(18) 0.0298(8) Uani 1 1 d . . . C62 C 0.7697(4) 0.9546(3) 0.8091(2) 0.0352(10) Uani 1 1 d . . . C63 C 0.6866(5) 0.9801(4) 0.8512(3) 0.0440(12) Uani 1 1 d . . . H63 H 0.6720 1.0431 0.8435 0.053 Uiso 1 1 calc R . . C64 C 0.6258(5) 0.9153(4) 0.9035(3) 0.0472(12) Uani 1 1 d . . . H64 H 0.5672 0.9317 0.9313 0.057 Uiso 1 1 calc R . . C65 C 0.6495(5) 0.8255(4) 0.9162(2) 0.0443(12) Uani 1 1 d . . . H65 H 0.6098 0.7807 0.9536 0.053 Uiso 1 1 calc R . . C66 C 0.7331(4) 0.8028(4) 0.8726(2) 0.0395(11) Uani 1 1 d . . . H66 H 0.7493 0.7408 0.8807 0.047 Uiso 1 1 calc R . . N71 N 0.9125(3) 0.9764(3) 0.71419(19) 0.0323(8) Uani 1 1 d . . . C72 C 0.8395(4) 1.0184(3) 0.7516(2) 0.0348(10) Uani 1 1 d . . . C73 C 0.8363(5) 1.1170(4) 0.7348(3) 0.0486(13) Uani 1 1 d . . . H73 H 0.7851 1.1458 0.7608 0.058 Uiso 1 1 calc R . . C74 C 0.9068(5) 1.1717(4) 0.6809(3) 0.0548(14) Uani 1 1 d . . . H74 H 0.9058 1.2394 0.6697 0.066 Uiso 1 1 calc R . . C75 C 0.9795(5) 1.1286(4) 0.6427(3) 0.0458(12) Uani 1 1 d . . . H75 H 1.0284 1.1654 0.6046 0.055 Uiso 1 1 calc R . . C76 C 0.9795(4) 1.0308(3) 0.6610(2) 0.0357(10) Uani 1 1 d . . . H76 H 1.0294 1.0009 0.6346 0.043 Uiso 1 1 calc R . . C400 C 0.6950(16) 0.6133(13) -0.0133(9) 0.110(5) Uiso 0.50 1 d P . . C401 C 0.5616(10) 0.5367(9) -0.0099(6) 0.152(4) Uiso 1 1 d . . . C402 C 1.0000 1.0000 0.0000 0.177(6) Uiso 1 2 d S . . C403 C 0.9983(10) 0.9065(8) 0.0244(5) 0.149(4) Uiso 1 1 d . . . N500 N 0.2148(6) 0.0796(5) 0.5534(4) 0.112(2) Uani 1 1 d . . . C501 C 0.2790(6) 0.0609(5) 0.5135(4) 0.0737(17) Uani 1 1 d . . . C502 C 0.3612(6) 0.0366(5) 0.4627(4) 0.085(2) Uani 1 1 d . . . N700 N 0.1893(10) 0.2663(9) 0.8364(6) 0.195(4) Uiso 1 1 d . . . C701 C 0.1305(14) 0.3070(11) 0.8768(7) 0.192(5) Uiso 1 1 d . . . C702 C 0.0561(9) 0.3604(7) 0.8996(5) 0.122(3) Uiso 1 1 d . . . N800 N 0.4604(13) -0.0513(12) 0.7026(8) 0.178(6) Uani 1 1 d . . . C801 C 0.4640(11) 0.0359(16) 0.7100(7) 0.150(7) Uani 1 1 d . . . C802 C 0.4677(11) 0.1491(11) 0.7210(6) 0.169(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 Ru1 0.0294(2) 0.02291(18) 0.02943(19) 0.00409(13) 0.00459(14) 0.01118(15) Cl1 0.0401(7) 0.0360(6) 0.0462(7) 0.0105(5) 0.0062(5) 0.0166(6) O100 0.052(2) 0.042(2) 0.073(2) 0.0261(17) 0.0149(18) 0.0117(17) O101 0.123(4) 0.053(2) 0.080(3) 0.022(2) 0.057(3) 0.040(3) O102 0.067(3) 0.082(3) 0.159(5) 0.026(3) -0.001(3) 0.050(3) O103 0.094(4) 0.051(2) 0.076(3) 0.006(2) -0.040(2) -0.004(2) Cl2 0.0483(8) 0.0739(9) 0.0497(8) 0.0022(7) 0.0031(6) 0.0424(8) O201 0.157(5) 0.103(4) 0.185(6) 0.086(4) 0.101(5) 0.084(4) O202 0.065(3) 0.147(4) 0.059(2) -0.014(2) -0.001(2) 0.079(3) O203 0.094(4) 0.114(4) 0.096(3) 0.041(3) 0.020(3) 0.074(3) O204 0.093(4) 0.280(8) 0.118(4) -0.120(5) -0.058(3) 0.131(5) N11 0.031(2) 0.0220(18) 0.033(2) 0.0063(14) 0.0039(16) 0.0123(16) C12 0.028(2) 0.019(2) 0.032(2) 0.0064(16) 0.0031(18) 0.0097(18) C13 0.028(2) 0.020(2) 0.032(2) 0.0040(17) 0.0061(18) 0.0094(18) N14 0.029(2) 0.0270(18) 0.0295(19) 0.0051(14) 0.0066(15) 0.0119(16) C15 0.032(3) 0.037(2) 0.037(3) 0.0021(19) 0.008(2) 0.016(2) C16 0.030(3) 0.046(3) 0.042(3) 0.007(2) 0.008(2) 0.018(2) C17 0.033(3) 0.037(2) 0.034(2) 0.0009(19) 0.0030(19) 0.013(2) C18 0.031(3) 0.023(2) 0.035(2) 0.0067(17) 0.0062(19) 0.0116(19) C19 0.034(3) 0.024(2) 0.031(2) 0.0028(17) 0.0048(19) 0.011(2) C20 0.037(3) 0.025(2) 0.029(2) 0.0065(17) 0.0077(19) 0.015(2) C21 0.033(3) 0.023(2) 0.033(2) 0.0104(17) 0.0105(19) 0.0154(19) C22 0.042(3) 0.032(2) 0.037(3) 0.0057(19) 0.011(2) 0.025(2) C23 0.028(3) 0.037(3) 0.042(3) 0.009(2) 0.006(2) 0.018(2) C24 0.028(3) 0.033(2) 0.038(2) 0.0089(18) 0.0030(19) 0.012(2) O31 0.046(2) 0.0274(15) 0.0335(16) 0.0046(12) 0.0128(14) 0.0188(14) C32 0.062(3) 0.029(2) 0.046(3) 0.007(2) 0.017(2) 0.024(2) C33 0.069(4) 0.048(3) 0.045(3) 0.000(2) 0.008(3) 0.037(3) O34 0.051(2) 0.049(2) 0.051(2) -0.0026(16) 0.0047(17) 0.0175(19) C35 0.059(4) 0.053(4) 0.092(5) -0.026(3) -0.001(3) 0.014(3) C36 0.052(4) 0.093(5) 0.052(4) -0.024(3) 0.007(3) 0.021(3) O37 0.057(3) 0.061(2) 0.055(2) -0.0136(18) 0.0077(18) 0.013(2) C38 0.044(3) 0.073(4) 0.039(3) -0.003(3) -0.004(2) 0.028(3) C39 0.054(3) 0.047(3) 0.033(3) 0.006(2) -0.002(2) 0.020(3) O40 0.040(2) 0.0432(18) 0.0292(17) -0.0014(13) 0.0005(14) 0.0129(16) N41 0.033(2) 0.0251(19) 0.032(2) 0.0064(15) 0.0083(16) 0.0131(17) C42 0.038(3) 0.032(2) 0.031(2) 0.0062(18) 0.009(2) 0.018(2) C43 0.048(3) 0.041(3) 0.043(3) 0.016(2) 0.007(2) 0.023(3) C44 0.061(4) 0.037(3) 0.059(3) 0.025(2) 0.017(3) 0.027(3) C45 0.045(3) 0.029(3) 0.055(3) 0.011(2) 0.006(2) 0.009(2) C46 0.045(3) 0.029(2) 0.042(3) 0.006(2) 0.009(2) 0.016(2) N51 0.034(2) 0.0275(19) 0.0295(19) 0.0021(15) 0.0051(15) 0.0126(17) C52 0.028(2) 0.032(2) 0.029(2) 0.0027(18) 0.0050(18) 0.012(2) C53 0.037(3) 0.041(3) 0.040(3) 0.002(2) -0.004(2) 0.015(2) C54 0.038(3) 0.054(3) 0.039(3) -0.007(2) -0.009(2) 0.017(3) C55 0.038(3) 0.035(3) 0.049(3) -0.002(2) 0.000(2) 0.005(2) C56 0.044(3) 0.025(2) 0.042(3) -0.0026(19) 0.000(2) 0.009(2) N61 0.032(2) 0.0242(18) 0.0294(19) 0.0030(14) 0.0008(15) 0.0102(16) C62 0.038(3) 0.032(2) 0.036(2) -0.0001(19) 0.004(2) 0.018(2) C63 0.047(3) 0.047(3) 0.044(3) 0.003(2) 0.009(2) 0.027(3) C64 0.047(3) 0.051(3) 0.046(3) 0.002(2) 0.015(2) 0.026(3) C65 0.049(3) 0.048(3) 0.034(3) 0.009(2) 0.014(2) 0.018(3) C66 0.046(3) 0.040(3) 0.033(2) 0.005(2) 0.007(2) 0.019(2) N71 0.033(2) 0.0266(19) 0.034(2) 0.0045(15) 0.0021(16) 0.0112(17) C72 0.034(3) 0.032(2) 0.040(3) 0.0065(19) 0.004(2) 0.016(2) C73 0.052(3) 0.044(3) 0.065(3) 0.019(2) 0.016(3) 0.032(3) C74 0.059(4) 0.045(3) 0.079(4) 0.029(3) 0.018(3) 0.035(3) C75 0.046(3) 0.042(3) 0.057(3) 0.026(2) 0.016(2) 0.020(2) C76 0.036(3) 0.032(2) 0.038(3) 0.0124(19) 0.008(2) 0.013(2) N500 0.102(5) 0.083(4) 0.155(6) 0.034(4) 0.073(5) 0.036(4) C501 0.072(5) 0.063(4) 0.083(5) 0.020(3) 0.016(4) 0.025(4) C502 0.067(5) 0.082(5) 0.106(5) 0.009(4) 0.034(4) 0.034(4) N800 0.088(7) 0.248(15) 0.137(8) -0.038(10) -0.039(5) 0.043(10) C801 0.044(5) 0.26(2) 0.072(6) -0.005(12) -0.008(4) 0.009(12) C802 0.134(10) 0.178(11) 0.100(8) 0.048(8) 0.010(6) -0.022(9) _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 2.042(4) . ? Ru1 N71 2.056(3) . ? Ru1 N41 2.057(3) . ? Ru1 N61 2.059(3) . ? Ru1 N14 2.070(3) . ? Ru1 N11 2.074(3) . ? Cl1 O103 1.410(4) . ? Cl1 O101 1.419(4) . ? Cl1 O102 1.439(4) . ? Cl1 O100 1.441(3) . ? Cl2 O204 1.382(4) . ? Cl2 O203 1.400(4) . ? Cl2 O201 1.404(5) . ? Cl2 O202 1.429(3) . ? N11 C24 1.333(5) . ? N11 C12 1.374(5) . ? C12 C21 1.402(5) . ? C12 C13 1.418(5) . ? C13 N14 1.377(5) . ? C13 C18 1.399(5) . ? N14 C15 1.329(5) . ? C15 C16 1.390(6) . ? C16 C17 1.373(5) . ? C17 C18 1.394(6) . ? C18 C19 1.443(5) . ? C19 C20 1.354(6) . ? C19 O40 1.369(5) . ? C20 O31 1.376(4) . ? C20 C21 1.441(6) . ? C21 C22 1.395(6) . ? C22 C23 1.366(6) . ? C23 C24 1.395(5) . ? O31 C32 1.456(4) . ? C32 C33 1.497(6) . ? C33 O34 1.419(6) . ? O34 C35 1.433(6) . ? C35 C36 1.491(8) . ? C36 O37 1.411(6) . ? O37 C38 1.416(6) . ? C38 C39 1.503(6) . ? C39 O40 1.453(5) . ? N41 C46 1.340(5) . ? N41 C42 1.358(5) . ? C42 C43 1.409(5) . ? C42 C52 1.467(6) . ? C43 C44 1.372(7) . ? C44 C45 1.366(7) . ? C45 C46 1.384(6) . ? N51 C56 1.355(5) . ? N51 C52 1.374(5) . ? C52 C53 1.388(6) . ? C53 C54 1.365(6) . ? C54 C55 1.374(6) . ? C55 C56 1.380(6) . ? N61 C66 1.349(5) . ? N61 C62 1.366(5) . ? C62 C63 1.387(5) . ? C62 C72 1.459(6) . ? C63 C64 1.359(6) . ? C64 C65 1.381(6) . ? C65 C66 1.388(6) . ? N71 C76 1.337(5) . ? N71 C72 1.367(5) . ? C72 C73 1.396(5) . ? C73 C74 1.365(6) . ? C74 C75 1.379(6) . ? C75 C76 1.380(5) . ? C400 C401 1.465(17) . ? C401 C401 1.446(19) 2_665 ? C402 C403 1.362(10) . ? C402 C403 1.362(10) 2_775 ? N500 C501 1.141(7) . ? C501 C502 1.459(8) . ? N700 C701 1.248(14) . ? C701 C702 1.392(14) . ? N800 C801 1.13(2) . ? C801 C802 1.469(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 N71 97.25(13) . . ? N51 Ru1 N41 78.98(14) . . ? N71 Ru1 N41 172.66(13) . . ? N51 Ru1 N61 94.61(13) . . ? N71 Ru1 N61 78.80(13) . . ? N41 Ru1 N61 95.14(12) . . ? N51 Ru1 N14 171.64(12) . . ? N71 Ru1 N14 86.51(13) . . ? N41 Ru1 N14 98.08(13) . . ? N61 Ru1 N14 93.43(13) . . ? N51 Ru1 N11 91.79(13) . . ? N71 Ru1 N11 96.71(12) . . ? N41 Ru1 N11 89.75(12) . . ? N61 Ru1 N11 172.59(13) . . ? N14 Ru1 N11 80.33(13) . . ? O103 Cl1 O101 109.9(3) . . ? O103 Cl1 O102 110.3(3) . . ? O101 Cl1 O102 107.9(3) . . ? O103 Cl1 O100 110.0(2) . . ? O101 Cl1 O100 109.6(2) . . ? O102 Cl1 O100 109.0(2) . . ? O204 Cl2 O203 110.4(3) . . ? O204 Cl2 O201 109.2(4) . . ? O203 Cl2 O201 106.7(3) . . ? O204 Cl2 O202 111.0(3) . . ? O203 Cl2 O202 110.5(3) . . ? O201 Cl2 O202 108.9(3) . . ? C24 N11 C12 117.4(3) . . ? C24 N11 Ru1 129.9(3) . . ? C12 N11 Ru1 112.7(3) . . ? N11 C12 C21 122.6(4) . . ? N11 C12 C13 117.2(3) . . ? C21 C12 C13 120.3(4) . . ? N14 C13 C18 122.2(4) . . ? N14 C13 C12 117.1(4) . . ? C18 C13 C12 120.7(3) . . ? C15 N14 C13 117.9(4) . . ? C15 N14 Ru1 129.3(3) . . ? C13 N14 Ru1 112.7(3) . . ? N14 C15 C16 122.9(4) . . ? C17 C16 C15 119.3(4) . . ? C16 C17 C18 119.7(4) . . ? C17 C18 C13 117.9(4) . . ? C17 C18 C19 123.5(4) . . ? C13 C18 C19 118.6(4) . . ? C20 C19 O40 123.2(4) . . ? C20 C19 C18 120.5(4) . . ? O40 C19 C18 116.1(4) . . ? C19 C20 O31 122.4(4) . . ? C19 C20 C21 121.4(4) . . ? O31 C20 C21 116.1(4) . . ? C22 C21 C12 118.0(4) . . ? C22 C21 C20 123.7(4) . . ? C12 C21 C20 118.3(4) . . ? C23 C22 C21 119.4(4) . . ? C22 C23 C24 119.7(4) . . ? N11 C24 C23 122.9(4) . . ? C20 O31 C32 114.1(3) . . ? O31 C32 C33 106.4(3) . . ? O34 C33 C32 112.6(4) . . ? C33 O34 C35 113.0(4) . . ? O34 C35 C36 109.1(5) . . ? O37 C36 C35 112.2(5) . . ? C38 O37 C36 116.8(4) . . ? O37 C38 C39 114.3(4) . . ? O40 C39 C38 106.7(4) . . ? C19 O40 C39 116.6(3) . . ? C46 N41 C42 118.4(4) . . ? C46 N41 Ru1 126.1(3) . . ? C42 N41 Ru1 115.4(3) . . ? N41 C42 C43 121.1(4) . . ? N41 C42 C52 115.2(3) . . ? C43 C42 C52 123.7(4) . . ? C44 C43 C42 118.6(5) . . ? C45 C44 C43 120.2(4) . . ? C44 C45 C46 118.8(4) . . ? N41 C46 C45 122.8(4) . . ? C56 N51 C52 117.0(4) . . ? C56 N51 Ru1 126.6(3) . . ? C52 N51 Ru1 116.0(3) . . ? N51 C52 C53 121.4(4) . . ? N51 C52 C42 113.7(4) . . ? C53 C52 C42 124.9(4) . . ? C54 C53 C52 120.2(4) . . ? C53 C54 C55 119.0(5) . . ? C54 C55 C56 119.3(4) . . ? N51 C56 C55 123.0(4) . . ? C66 N61 C62 117.8(3) . . ? C66 N61 Ru1 126.3(3) . . ? C62 N61 Ru1 115.7(3) . . ? N61 C62 C63 121.0(4) . . ? N61 C62 C72 114.4(3) . . ? C63 C62 C72 124.7(4) . . ? C64 C63 C62 120.2(4) . . ? C63 C64 C65 119.9(4) . . ? C64 C65 C66 117.9(4) . . ? N61 C66 C65 123.1(4) . . ? C76 N71 C72 118.7(3) . . ? C76 N71 Ru1 126.0(3) . . ? C72 N71 Ru1 115.2(3) . . ? N71 C72 C73 120.3(4) . . ? N71 C72 C62 115.5(3) . . ? C73 C72 C62 124.2(4) . . ? C74 C73 C72 119.8(4) . . ? C73 C74 C75 119.8(4) . . ? C76 C75 C74 118.4(4) . . ? N71 C76 C75 122.9(4) . . ? C401 C401 C400 168.1(15) 2_665 . ? C403 C402 C403 180.0(7) . 2_775 ? N500 C501 C502 179.8(8) . . ? N700 C701 C702 161.6(13) . . ? N800 C801 C802 178.9(17) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.984 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.093 #=END data_spoons _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H45 Cl2 F0 N7 Na0 O14 P0 Ru' _chemical_formula_weight 1067.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.748(4) _cell_length_b 13.181(4) _cell_length_c 13.847(4) _cell_angle_alpha 90.00(3) _cell_angle_beta 107.04(3) _cell_angle_gamma 90.00(2) _cell_volume 2224.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(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 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.90 _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 '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 14570 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9568 _reflns_number_gt 7471 _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^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.71(4) _refine_ls_number_reflns 9568 _refine_ls_number_parameters 615 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.009 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 1.64130(3) -2.12734(4) 1.23276(3) 0.02850(11) Uani 1 1 d . . . O72 O 1.1819(3) -1.9419(3) 0.9407(3) 0.0428(10) Uani 1 1 d . . . O75 O 1.0065(4) -1.7997(4) 0.8638(4) 0.0524(12) Uani 1 1 d . . . O78 O 0.7882(4) -1.8077(5) 0.7221(5) 0.0703(19) Uani 1 1 d . . . O81 O 0.7500(4) -1.9899(4) 0.6196(4) 0.0555(13) Uani 1 1 d . . . O84 O 0.9486(4) -2.1055(4) 0.7435(4) 0.0598(15) Uani 1 1 d . . . O87 O 1.1495(3) -2.1546(3) 0.9065(3) 0.0399(11) Uani 1 1 d . . . N11 N 1.7153(4) -2.0972(3) 1.1235(3) 0.0297(11) Uani 1 1 d . . . N21 N 1.7677(4) -2.0350(4) 1.3094(4) 0.0311(11) Uani 1 1 d . . . N31 N 1.5873(4) -2.1622(4) 1.3557(4) 0.0355(12) Uani 1 1 d . . . N41 N 1.7357(4) -2.2527(4) 1.2910(4) 0.0325(12) Uani 1 1 d . . . N51 N 1.5342(4) -2.0101(4) 1.1763(4) 0.0336(12) Uani 1 1 d . . . N61 N 1.5114(4) -2.2082(4) 1.1392(4) 0.0328(11) Uani 1 1 d . . . C12 C 1.8115(5) -2.0439(4) 1.1542(4) 0.0314(12) Uani 1 1 d . . . C13 C 1.8745(5) -2.0270(5) 1.0899(5) 0.0406(14) Uani 1 1 d . . . H13A H 1.9418 -1.9909 1.1130 0.049 Uiso 1 1 calc R . . C14 C 1.8395(6) -2.0626(6) 0.9925(5) 0.0480(16) Uani 1 1 d . . . H14B H 1.8836 -2.0533 0.9485 0.058 Uiso 1 1 calc R . . C15 C 1.7404(5) -2.1119(6) 0.9592(4) 0.0415(17) Uani 1 1 d . . . H15A H 1.7137 -2.1343 0.8912 0.050 Uiso 1 1 calc R . . C16 C 1.6802(4) -2.1285(7) 1.0261(4) 0.0357(10) Uani 1 1 d . . . H16A H 1.6119 -2.1630 1.0030 0.043 Uiso 1 1 calc R . . C22 C 1.8405(5) -2.0072(5) 1.2597(5) 0.0347(14) Uani 1 1 d . . . C23 C 1.9276(5) -1.9443(5) 1.3023(5) 0.0424(15) Uani 1 1 d . . . H23A H 1.9767 -1.9257 1.2653 0.051 Uiso 1 1 calc R . . C24 C 1.9435(5) -1.9082(5) 1.3991(5) 0.0441(15) Uani 1 1 d . . . H24A H 2.0032 -1.8641 1.4289 0.053 Uiso 1 1 calc R . . C25 C 1.8728(5) -1.9362(5) 1.4519(5) 0.0440(15) Uani 1 1 d . . . H25A H 1.8823 -1.9121 1.5186 0.053 Uiso 1 1 calc R . . C26 C 1.7857(5) -2.0013(5) 1.4050(5) 0.0371(13) Uani 1 1 d . . . H26A H 1.7374 -2.0226 1.4420 0.045 Uiso 1 1 calc R . . C32 C 1.6346(5) -2.2422(5) 1.4106(4) 0.0372(13) Uani 1 1 d . . . C33 C 1.6060(5) -2.2712(6) 1.4969(5) 0.0510(17) Uani 1 1 d . . . H33A H 1.6400 -2.3283 1.5354 0.061 Uiso 1 1 calc R . . C34 C 1.5300(6) -2.2173(7) 1.5247(6) 0.057(2) Uani 1 1 d . . . H34A H 1.5108 -2.2361 1.5836 0.068 Uiso 1 1 calc R . . C35 C 1.4796(5) -2.1351(9) 1.4686(5) 0.0532(16) Uani 1 1 d . . . H35A H 1.4255 -2.0973 1.4878 0.064 Uiso 1 1 calc R . . C36 C 1.5089(5) -2.1090(5) 1.3849(5) 0.0427(17) Uani 1 1 d . . . H36A H 1.4743 -2.0526 1.3456 0.051 Uiso 1 1 calc R . . C42 C 1.7183(5) -2.2935(5) 1.3744(4) 0.0358(13) Uani 1 1 d . . . C43 C 1.7765(6) -2.3773(5) 1.4199(5) 0.0453(15) Uani 1 1 d . . . H43A H 1.7624 -2.4061 1.4778 0.054 Uiso 1 1 calc R . . C44 C 1.8545(5) -2.4195(5) 1.3821(5) 0.0459(15) Uani 1 1 d . . . H44A H 1.8940 -2.4779 1.4132 0.055 Uiso 1 1 calc R . . C45 C 1.8754(5) -2.3768(5) 1.2985(5) 0.0433(15) Uani 1 1 d . . . H45A H 1.9306 -2.4034 1.2721 0.052 Uiso 1 1 calc R . . C46 C 1.8128(5) -2.2936(5) 1.2546(5) 0.0362(14) Uani 1 1 d . . . H46A H 1.8251 -2.2643 1.1961 0.043 Uiso 1 1 calc R . . C52 C 1.4397(5) -2.0410(5) 1.1067(4) 0.0332(12) Uani 1 1 d . . . C53 C 1.3557(5) -1.9741(5) 1.0566(5) 0.0360(13) Uani 1 1 d . . . C54 C 1.3725(6) -1.8701(5) 1.0803(6) 0.0482(17) Uani 1 1 d . . . H54A H 1.3178 -1.8219 1.0485 0.058 Uiso 1 1 calc R . . C55 C 1.4668(6) -1.8392(5) 1.1485(6) 0.0525(18) Uani 1 1 d . . . H55A H 1.4787 -1.7693 1.1647 0.063 Uiso 1 1 calc R . . C56 C 1.5466(5) -1.9113(5) 1.1948(5) 0.0450(15) Uani 1 1 d . . . H56A H 1.6127 -1.8883 1.2417 0.054 Uiso 1 1 calc R . . C62 C 1.4267(4) -2.1465(4) 1.0874(4) 0.0291(13) Uani 1 1 d . . . C63 C 1.3308(5) -2.1839(5) 1.0184(4) 0.0343(12) Uani 1 1 d . . . C64 C 1.3239(5) -2.2898(5) 1.0016(5) 0.0403(15) Uani 1 1 d . . . H64A H 1.2611 -2.3189 0.9550 0.048 Uiso 1 1 calc R . . C65 C 1.4096(5) -2.3497(5) 1.0538(5) 0.0418(15) Uani 1 1 d . . . H65A H 1.4057 -2.4209 1.0428 0.050 Uiso 1 1 calc R . . C66 C 1.5025(5) -2.3083(4) 1.1227(5) 0.0384(14) Uani 1 1 d . . . H66A H 1.5603 -2.3519 1.1584 0.046 Uiso 1 1 calc R . . C71 C 1.2584(5) -2.0126(5) 0.9882(5) 0.0340(12) Uani 1 1 d . . . C73 C 1.0732(5) -1.9530(5) 0.9511(5) 0.0403(14) Uani 1 1 d . . . H73A H 1.0766 -1.9919 1.0130 0.048 Uiso 1 1 calc R . . H73B H 1.0261 -1.9906 0.8924 0.048 Uiso 1 1 calc R . . C74 C 1.0248(6) -1.8486(5) 0.9569(5) 0.0482(16) Uani 1 1 d . . . H74A H 0.9548 -1.8553 0.9737 0.058 Uiso 1 1 calc R . . H74B H 1.0761 -1.8081 1.0106 0.058 Uiso 1 1 calc R . . C76 C 0.9277(6) -1.7192(6) 0.8438(8) 0.068(2) Uani 1 1 d . . . H76A H 0.9403 -1.6754 0.7901 0.081 Uiso 1 1 calc R . . H76B H 0.9405 -1.6773 0.9055 0.081 Uiso 1 1 calc R . . C77 C 0.8118(7) -1.7523(7) 0.8122(7) 0.070(2) Uani 1 1 d . . . H77A H 0.7974 -1.7948 0.8658 0.084 Uiso 1 1 calc R . . H77B H 0.7633 -1.6921 0.8025 0.084 Uiso 1 1 calc R . . C79 C 0.6820(6) -1.8499(7) 0.7024(6) 0.060(2) Uani 1 1 d . . . H79A H 0.6258 -1.7957 0.6893 0.072 Uiso 1 1 calc R . . H79B H 0.6764 -1.8910 0.7605 0.072 Uiso 1 1 calc R . . C80 C 0.6667(7) -1.9154(7) 0.6104(6) 0.061(2) Uani 1 1 d . . . H80A H 0.5949 -1.9502 0.5960 0.073 Uiso 1 1 calc R . . H80B H 0.6644 -1.8713 0.5520 0.073 Uiso 1 1 calc R . . C82 C 0.7572(7) -2.0617(7) 0.6956(6) 0.064(2) Uani 1 1 d . . . H82A H 0.6849 -2.0944 0.6855 0.077 Uiso 1 1 calc R . . H82B H 0.7779 -2.0277 0.7623 0.077 Uiso 1 1 calc R . . C83 C 0.8396(6) -2.1390(9) 0.6935(6) 0.072(2) Uani 1 1 d . . . H83A H 0.8243 -2.2015 0.7267 0.087 Uiso 1 1 calc R . . H83B H 0.8338 -2.1558 0.6225 0.087 Uiso 1 1 calc R . . C85 C 1.0286(6) -2.1800(6) 0.7409(6) 0.058(2) Uani 1 1 d . . . H85A H 1.0274 -2.1925 0.6701 0.069 Uiso 1 1 calc R . . H85B H 1.0111 -2.2445 0.7693 0.069 Uiso 1 1 calc R . . C86 C 1.1396(5) -2.1451(6) 0.8002(5) 0.0491(18) Uani 1 1 d . . . H86A H 1.1964 -2.1867 0.7833 0.059 Uiso 1 1 calc R . . H86B H 1.1503 -2.0734 0.7837 0.059 Uiso 1 1 calc R . . C88 C 1.2451(4) -2.1142(6) 0.9691(4) 0.0345(14) Uani 1 1 d . . . N101 N 1.9862(7) -1.1773(6) 1.4628(6) 0.075(2) Uani 1 1 d . . . C100 C 2.1867(8) -1.1516(9) 1.4654(9) 0.100(4) Uani 1 1 d . . . H10A H 2.2158 -1.2149 1.4464 0.150 Uiso 1 1 calc R . . H10B H 2.2305 -1.1316 1.5335 0.150 Uiso 1 1 calc R . . H10C H 2.1902 -1.0981 1.4173 0.150 Uiso 1 1 calc R . . C101 C 2.0726(8) -1.1669(6) 1.4641(6) 0.059(2) Uani 1 1 d . . . Cl1 Cl 1.57309(19) -1.57258(19) 1.25641(18) 0.0702(6) Uani 1 1 d . . . O11 O 1.4799(10) -1.5908(8) 1.1969(12) 0.262(10) Uani 1 1 d . . . O12 O 1.5664(8) -1.5025(7) 1.3260(8) 0.140(4) Uani 1 1 d . . . O13 O 1.6183(16) -1.5339(12) 1.1884(12) 0.266(11) Uani 1 1 d . . . O14 O 1.6309(6) -1.6601(5) 1.2990(5) 0.086(2) Uani 1 1 d . . . Cl2 Cl 0.7805(4) -2.4368(4) 0.7349(3) 0.1308(15) Uani 1 1 d D . . O21 O 0.7273(15) -2.5182(12) 0.7468(16) 0.362(17) Uani 1 1 d DU . . O22 O 0.6908(15) -2.375(2) 0.716(2) 0.51(3) Uani 1 1 d DU . . O23 O 0.8632(6) -2.4355(11) 0.8124(5) 0.169(6) Uani 1 1 d DU . . O24 O 0.8125(6) -2.4189(8) 0.6557(5) 0.116(3) Uani 1 1 d DU . . 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 0.02386(17) 0.02798(18) 0.03195(19) 0.0006(3) 0.00552(13) -0.0030(2) O72 0.032(2) 0.044(3) 0.052(3) 0.016(2) 0.0111(19) 0.0047(18) O75 0.040(3) 0.059(3) 0.057(3) 0.010(2) 0.011(2) 0.018(2) O78 0.033(3) 0.088(5) 0.073(4) -0.025(3) -0.011(3) 0.021(3) O81 0.055(3) 0.071(3) 0.038(3) 0.006(2) 0.010(2) 0.018(3) O84 0.054(3) 0.048(4) 0.057(3) -0.009(2) -0.016(2) 0.008(2) O87 0.0275(19) 0.048(3) 0.036(2) 0.0003(17) -0.0041(15) -0.0070(16) N11 0.030(2) 0.026(3) 0.030(2) 0.0054(16) 0.0035(18) 0.0001(16) N21 0.029(3) 0.028(3) 0.033(3) 0.000(2) 0.006(2) -0.003(2) N31 0.028(2) 0.039(3) 0.039(3) -0.006(2) 0.009(2) -0.0106(19) N41 0.034(3) 0.027(3) 0.034(3) -0.001(2) 0.006(2) -0.009(2) N51 0.030(3) 0.030(3) 0.039(3) 0.004(2) 0.006(2) -0.004(2) N61 0.033(3) 0.030(3) 0.035(3) 0.001(2) 0.008(2) -0.005(2) C12 0.031(3) 0.023(3) 0.037(3) 0.004(2) 0.004(2) -0.004(2) C13 0.035(3) 0.047(4) 0.040(3) 0.005(3) 0.010(3) -0.013(3) C14 0.045(4) 0.059(4) 0.042(4) 0.000(3) 0.016(3) -0.016(3) C15 0.050(3) 0.043(5) 0.031(3) 0.003(3) 0.010(2) -0.010(3) C16 0.038(2) 0.031(2) 0.034(2) 0.001(4) 0.0035(19) -0.003(4) C22 0.026(3) 0.036(3) 0.037(3) 0.009(3) 0.003(2) -0.005(2) C23 0.037(3) 0.050(4) 0.035(3) -0.002(3) 0.003(3) -0.016(3) C24 0.042(3) 0.040(4) 0.043(4) -0.002(3) 0.001(3) -0.014(3) C25 0.045(4) 0.045(4) 0.037(3) -0.010(3) 0.005(3) -0.005(3) C26 0.030(3) 0.037(3) 0.044(3) -0.008(3) 0.010(3) -0.001(3) C32 0.029(3) 0.047(4) 0.031(3) 0.005(3) 0.002(2) -0.011(3) C33 0.038(3) 0.079(5) 0.034(3) 0.002(3) 0.008(3) -0.011(3) C34 0.054(4) 0.080(6) 0.045(4) -0.005(4) 0.026(3) -0.025(4) C35 0.039(3) 0.069(5) 0.056(4) -0.007(5) 0.021(3) -0.007(5) C36 0.035(3) 0.037(5) 0.058(4) 0.000(3) 0.016(3) -0.008(3) C42 0.040(3) 0.036(3) 0.028(3) 0.004(2) 0.005(2) -0.009(3) C43 0.049(4) 0.045(4) 0.037(3) 0.012(3) 0.006(3) 0.005(3) C44 0.045(4) 0.042(4) 0.042(4) 0.006(3) -0.001(3) 0.008(3) C45 0.040(3) 0.037(3) 0.049(4) -0.002(3) 0.007(3) 0.006(3) C46 0.033(3) 0.040(4) 0.031(3) -0.001(3) 0.002(2) 0.003(3) C52 0.026(3) 0.035(3) 0.037(3) 0.001(3) 0.006(2) -0.003(2) C53 0.025(3) 0.032(3) 0.049(4) 0.004(3) 0.008(3) 0.002(2) C54 0.037(4) 0.033(4) 0.069(5) 0.010(3) 0.006(3) 0.009(3) C55 0.056(4) 0.022(3) 0.076(5) -0.001(3) 0.013(4) 0.003(3) C56 0.030(3) 0.038(3) 0.059(4) -0.007(3) 0.001(3) -0.003(3) C62 0.030(2) 0.026(4) 0.030(2) 0.002(2) 0.0070(19) -0.002(2) C63 0.031(3) 0.036(3) 0.034(3) -0.007(2) 0.007(2) -0.007(2) C64 0.034(3) 0.037(3) 0.046(4) -0.003(3) 0.006(3) -0.013(3) C65 0.041(4) 0.025(3) 0.055(4) -0.002(3) 0.008(3) -0.009(3) C66 0.043(3) 0.028(3) 0.044(4) 0.002(3) 0.011(3) -0.003(3) C71 0.027(3) 0.034(3) 0.040(3) 0.007(3) 0.008(2) -0.001(2) C73 0.033(3) 0.047(4) 0.042(3) 0.002(3) 0.012(3) 0.001(3) C74 0.046(4) 0.052(4) 0.050(4) -0.002(3) 0.021(3) 0.000(3) C76 0.040(4) 0.053(5) 0.102(7) -0.012(4) 0.006(4) 0.002(3) C77 0.047(5) 0.075(6) 0.078(6) -0.015(5) 0.005(4) 0.020(4) C79 0.033(4) 0.101(7) 0.041(4) -0.012(4) 0.003(3) 0.008(4) C80 0.054(4) 0.076(6) 0.051(4) 0.015(4) 0.011(4) 0.017(4) C82 0.060(5) 0.072(5) 0.053(5) 0.015(4) 0.004(4) -0.006(4) C83 0.059(4) 0.075(7) 0.063(4) 0.002(5) -0.014(3) -0.006(5) C85 0.068(5) 0.046(4) 0.045(4) -0.009(3) -0.006(3) 0.009(4) C86 0.050(3) 0.050(5) 0.042(3) -0.002(3) 0.006(3) 0.004(3) C88 0.030(2) 0.037(4) 0.034(3) 0.003(3) 0.0054(19) -0.004(3) N101 0.076(5) 0.061(4) 0.085(6) -0.002(4) 0.016(4) 0.003(4) C100 0.078(6) 0.114(11) 0.114(8) -0.034(7) 0.039(6) -0.021(6) C101 0.070(5) 0.045(4) 0.054(5) -0.002(3) 0.005(4) -0.002(4) Cl1 0.0642(13) 0.0703(14) 0.0719(14) 0.0008(11) 0.0132(11) -0.0057(11) O11 0.161(9) 0.129(10) 0.342(18) -0.126(11) -0.166(11) 0.058(8) O12 0.153(8) 0.120(7) 0.158(8) -0.085(7) 0.065(7) -0.034(6) O13 0.41(2) 0.249(15) 0.252(14) 0.187(13) 0.279(16) 0.235(16) O14 0.075(4) 0.070(5) 0.097(5) 0.024(3) -0.001(4) 0.000(3) Cl2 0.145(4) 0.145(4) 0.110(3) 0.028(3) 0.050(3) 0.017(3) O21 0.37(3) 0.35(3) 0.50(3) -0.23(2) 0.35(3) -0.30(2) O22 0.114(13) 0.91(7) 0.50(4) 0.33(4) 0.089(17) 0.17(3) O23 0.074(5) 0.373(19) 0.042(4) 0.034(7) -0.013(4) 0.024(8) O24 0.095(5) 0.213(10) 0.052(4) 0.045(5) 0.038(4) 0.044(6) _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 N11 2.043(5) . ? Ru1 N21 2.050(5) . ? Ru1 N51 2.059(5) . ? Ru1 N41 2.064(6) . ? Ru1 N31 2.065(5) . ? Ru1 N61 2.073(5) . ? O72 C71 1.370(7) . ? O72 C73 1.441(7) . ? O75 C74 1.399(8) . ? O75 C76 1.432(9) . ? O78 C77 1.400(10) . ? O78 C79 1.414(10) . ? O81 C82 1.398(9) . ? O81 C80 1.425(9) . ? O84 C85 1.423(9) . ? O84 C83 1.429(9) . ? O87 C88 1.379(7) . ? O87 C86 1.446(7) . ? N11 C16 1.355(7) . ? N11 C12 1.368(7) . ? N21 C26 1.350(8) . ? N21 C22 1.357(8) . ? N31 C32 1.336(8) . ? N31 C36 1.375(8) . ? N41 C46 1.343(8) . ? N41 C42 1.349(8) . ? N51 C56 1.328(8) . ? N51 C52 1.366(8) . ? N61 C66 1.338(8) . ? N61 C62 1.375(8) . ? C12 C13 1.380(8) . ? C12 C22 1.480(9) . ? C13 C14 1.373(9) . ? C14 C15 1.374(9) . ? C15 C16 1.383(7) . ? C22 C23 1.374(8) . ? C23 C24 1.381(9) . ? C24 C25 1.368(9) . ? C25 C26 1.403(8) . ? C32 C33 1.401(8) . ? C32 C42 1.470(9) . ? C33 C34 1.347(11) . ? C34 C35 1.378(13) . ? C35 C36 1.362(9) . ? C42 C43 1.377(9) . ? C43 C44 1.370(10) . ? C44 C45 1.382(9) . ? C45 C46 1.387(9) . ? C52 C53 1.404(9) . ? C52 C62 1.416(8) . ? C53 C54 1.411(9) . ? C53 C71 1.416(9) . ? C54 C55 1.356(10) . ? C55 C56 1.402(9) . ? C62 C63 1.402(8) . ? C63 C64 1.414(9) . ? C63 C88 1.437(9) . ? C64 C65 1.369(9) . ? C65 C66 1.396(9) . ? C71 C88 1.365(10) . ? C73 C74 1.520(10) . ? C76 C77 1.478(11) . ? C79 C80 1.503(11) . ? C82 C83 1.470(13) . ? C85 C86 1.486(10) . ? N101 C101 1.104(11) . ? C100 C101 1.464(13) . ? Cl1 O11 1.255(9) . ? Cl1 O13 1.341(10) . ? Cl1 O12 1.355(8) . ? Cl1 O14 1.403(6) . ? Cl2 O23 1.264(7) . ? Cl2 O24 1.299(6) . ? Cl2 O21 1.305(10) . ? Cl2 O22 1.365(12) . ? 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 Ru1 N21 78.7(2) . . ? N11 Ru1 N51 88.38(19) . . ? N21 Ru1 N51 94.8(2) . . ? N11 Ru1 N41 95.86(19) . . ? N21 Ru1 N41 89.6(2) . . ? N51 Ru1 N41 174.4(2) . . ? N11 Ru1 N31 172.29(19) . . ? N21 Ru1 N31 96.1(2) . . ? N51 Ru1 N31 97.8(2) . . ? N41 Ru1 N31 78.3(2) . . ? N11 Ru1 N61 95.46(19) . . ? N21 Ru1 N61 172.5(2) . . ? N51 Ru1 N61 80.2(2) . . ? N41 Ru1 N61 95.7(2) . . ? N31 Ru1 N61 90.15(19) . . ? C71 O72 C73 116.9(4) . . ? C74 O75 C76 115.9(6) . . ? C77 O78 C79 108.7(7) . . ? C82 O81 C80 114.6(6) . . ? C85 O84 C83 112.2(6) . . ? C88 O87 C86 113.8(4) . . ? C16 N11 C12 118.0(5) . . ? C16 N11 Ru1 126.0(4) . . ? C12 N11 Ru1 115.9(4) . . ? C26 N21 C22 117.6(5) . . ? C26 N21 Ru1 125.8(4) . . ? C22 N21 Ru1 116.6(4) . . ? C32 N31 C36 118.7(5) . . ? C32 N31 Ru1 116.2(4) . . ? C36 N31 Ru1 125.1(4) . . ? C46 N41 C42 118.9(6) . . ? C46 N41 Ru1 125.6(4) . . ? C42 N41 Ru1 115.5(4) . . ? C56 N51 C52 117.3(5) . . ? C56 N51 Ru1 129.4(4) . . ? C52 N51 Ru1 113.2(4) . . ? C66 N61 C62 118.7(5) . . ? C66 N61 Ru1 128.7(5) . . ? C62 N61 Ru1 112.5(4) . . ? N11 C12 C13 121.4(5) . . ? N11 C12 C22 114.6(5) . . ? C13 C12 C22 124.1(5) . . ? C14 C13 C12 119.7(6) . . ? C13 C14 C15 119.6(6) . . ? C14 C15 C16 119.1(6) . . ? N11 C16 C15 122.1(6) . . ? N21 C22 C23 122.2(6) . . ? N21 C22 C12 113.8(5) . . ? C23 C22 C12 123.9(5) . . ? C22 C23 C24 119.6(6) . . ? C25 C24 C23 119.7(6) . . ? C24 C25 C26 118.2(6) . . ? N21 C26 C25 122.6(6) . . ? N31 C32 C33 121.0(6) . . ? N31 C32 C42 114.8(5) . . ? C33 C32 C42 124.2(6) . . ? C34 C33 C32 119.3(7) . . ? C33 C34 C35 120.6(6) . . ? C36 C35 C34 118.7(7) . . ? C35 C36 N31 121.8(7) . . ? N41 C42 C43 120.7(6) . . ? N41 C42 C32 115.2(5) . . ? C43 C42 C32 124.1(5) . . ? C44 C43 C42 120.3(6) . . ? C43 C44 C45 119.6(6) . . ? C44 C45 C46 117.6(6) . . ? N41 C46 C45 122.9(6) . . ? N51 C52 C53 123.2(6) . . ? N51 C52 C62 117.2(5) . . ? C53 C52 C62 119.6(5) . . ? C52 C53 C54 117.0(6) . . ? C52 C53 C71 119.8(6) . . ? C54 C53 C71 123.2(6) . . ? C55 C54 C53 119.8(6) . . ? C54 C55 C56 119.4(6) . . ? N51 C56 C55 123.1(6) . . ? N61 C62 C63 122.8(5) . . ? N61 C62 C52 116.9(5) . . ? C63 C62 C52 120.3(5) . . ? C62 C63 C64 117.3(6) . . ? C62 C63 C88 119.2(6) . . ? C64 C63 C88 123.5(6) . . ? C65 C64 C63 118.8(6) . . ? C64 C65 C66 121.5(6) . . ? N61 C66 C65 120.9(6) . . ? C88 C71 O72 123.0(5) . . ? C88 C71 C53 121.0(5) . . ? O72 C71 C53 115.9(5) . . ? O72 C73 C74 109.3(5) . . ? O75 C74 C73 109.2(5) . . ? O75 C76 C77 115.0(7) . . ? O78 C77 C76 110.7(7) . . ? O78 C79 C80 105.6(6) . . ? O81 C80 C79 114.3(6) . . ? O81 C82 C83 110.1(7) . . ? O84 C83 C82 112.0(9) . . ? O84 C85 C86 110.2(6) . . ? O87 C86 C85 108.7(6) . . ? C71 C88 O87 122.4(6) . . ? C71 C88 C63 120.1(5) . . ? O87 C88 C63 117.4(6) . . ? N101 C101 C100 179.2(11) . . ? O11 Cl1 O13 97.5(12) . . ? O11 Cl1 O12 110.7(8) . . ? O13 Cl1 O12 111.7(9) . . ? O11 Cl1 O14 113.4(6) . . ? O13 Cl1 O14 109.1(6) . . ? O12 Cl1 O14 113.3(6) . . ? O23 Cl2 O24 108.9(6) . . ? O23 Cl2 O21 103.9(10) . . ? O24 Cl2 O21 124.0(10) . . ? O23 Cl2 O22 126.9(16) . . ? O24 Cl2 O22 100.2(9) . . ? O21 Cl2 O22 94.6(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.511 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.098 #=END data_sad2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Cl3 Li N10 O17 Ru' _chemical_formula_weight 1253.34 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' 'Li' 'Li' -0.0003 0.0001 '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' 'F' 'F' 0.0171 0.0103 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.485(2) _cell_length_b 13.085(4) _cell_length_c 17.988(4) _cell_angle_alpha 71.249(14) _cell_angle_beta 76.915(16) _cell_angle_gamma 82.05(2) _cell_volume 2703.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(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 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.88 _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 '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 28774 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0659 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12322 _reflns_number_gt 8089 _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^)+(0.1245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12322 _refine_ls_number_parameters 749 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.015 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 0.28112(3) 2.38502(3) -0.744385(19) 0.03521(13) Uani 1 1 d . . . Li1 Li 0.1571(7) 2.0543(8) -0.2494(5) 0.054(2) Uani 1 1 d . . . O72 O 0.3144(3) 2.0963(3) -0.37519(18) 0.0474(8) Uani 1 1 d . . . O75 O 0.2837(3) 1.9426(3) -0.23119(18) 0.0517(9) Uani 1 1 d . . . O78 O 0.1200(3) 1.9814(3) -0.1172(2) 0.0566(9) Uani 1 1 d . . . O81 O 0.0155(3) 1.9876(3) -0.23026(17) 0.0477(8) Uani 1 1 d . . . O84 O 0.0953(3) 2.1002(3) -0.37297(16) 0.0426(8) Uani 1 1 d . . . N11 N 0.2300(3) 2.5269(3) -0.7157(2) 0.0425(9) Uani 1 1 d . . . N21 N 0.1833(3) 2.4635(3) -0.8276(2) 0.0419(9) Uani 1 1 d . . . N31 N 0.3328(3) 2.2565(3) -0.78898(19) 0.0367(8) Uani 1 1 d . . . N41 N 0.4175(3) 2.4446(3) -0.8299(2) 0.0398(9) Uani 1 1 d . . . N51 N 0.1573(3) 2.3106(3) -0.65354(19) 0.0346(8) Uani 1 1 d . . . N61 N 0.3688(3) 2.3130(3) -0.6542(2) 0.0379(8) Uani 1 1 d . . . C12 C 0.1645(4) 2.6002(4) -0.7642(3) 0.0523(13) Uani 1 1 d . . . C13 C 0.1243(5) 2.6971(5) -0.7506(4) 0.0676(16) Uani 1 1 d . . . H13A H 0.0792 2.7453 -0.7827 0.081 Uiso 1 1 calc R . . C14 C 0.1517(6) 2.7220(5) -0.6885(5) 0.080(2) Uani 1 1 d . . . H14A H 0.1256 2.7876 -0.6789 0.096 Uiso 1 1 calc R . . C15 C 0.2181(5) 2.6490(5) -0.6405(4) 0.0693(17) Uani 1 1 d . . . H15A H 0.2375 2.6650 -0.5988 0.083 Uiso 1 1 calc R . . C16 C 0.2543(4) 2.5536(4) -0.6557(3) 0.0533(13) Uani 1 1 d . . . H16A H 0.2981 2.5045 -0.6230 0.064 Uiso 1 1 calc R . . C22 C 0.1444(4) 2.5652(4) -0.8285(3) 0.0467(12) Uani 1 1 d . . . C23 C 0.0893(5) 2.6316(5) -0.8896(4) 0.0689(17) Uani 1 1 d . . . H23A H 0.0638 2.7019 -0.8900 0.083 Uiso 1 1 calc R . . C24 C 0.0738(5) 2.5938(6) -0.9467(4) 0.0719(19) Uani 1 1 d . . . H24A H 0.0390 2.6379 -0.9876 0.086 Uiso 1 1 calc R . . C25 C 0.1097(4) 2.4888(6) -0.9444(3) 0.0641(17) Uani 1 1 d . . . H25A H 0.0979 2.4608 -0.9830 0.077 Uiso 1 1 calc R . . C26 C 0.1634(4) 2.4254(5) -0.8844(3) 0.0500(12) Uani 1 1 d . . . H26A H 0.1867 2.3543 -0.8830 0.060 Uiso 1 1 calc R . . C32 C 0.4181(3) 2.2757(4) -0.8542(2) 0.0405(10) Uani 1 1 d . . . C33 C 0.4513(4) 2.2014(4) -0.8968(3) 0.0479(12) Uani 1 1 d . . . H33A H 0.5043 2.2183 -0.9437 0.057 Uiso 1 1 calc R . . C34 C 0.4061(4) 2.1029(5) -0.8701(3) 0.0503(12) Uani 1 1 d . . . H34A H 0.4287 2.0522 -0.8978 0.060 Uiso 1 1 calc R . . C35 C 0.3263(4) 2.0814(4) -0.8013(3) 0.0502(12) Uani 1 1 d . . . H35A H 0.2953 2.0149 -0.7810 0.060 Uiso 1 1 calc R . . C36 C 0.2929(4) 2.1594(4) -0.7628(3) 0.0442(11) Uani 1 1 d . . . H36A H 0.2397 2.1432 -0.7161 0.053 Uiso 1 1 calc R . . C42 C 0.4680(3) 2.3793(4) -0.8742(2) 0.0403(11) Uani 1 1 d . . . C43 C 0.5656(4) 2.4072(4) -0.9300(3) 0.0484(12) Uani 1 1 d . . . H43A H 0.6007 2.3617 -0.9599 0.058 Uiso 1 1 calc R . . C44 C 0.6087(4) 2.5026(5) -0.9397(3) 0.0559(14) Uani 1 1 d . . . H44A H 0.6739 2.5218 -0.9762 0.067 Uiso 1 1 calc R . . C45 C 0.5559(4) 2.5699(5) -0.8957(3) 0.0572(14) Uani 1 1 d . . . H45A H 0.5846 2.6347 -0.9019 0.069 Uiso 1 1 calc R . . C46 C 0.4581(4) 2.5387(4) -0.8416(3) 0.0484(12) Uani 1 1 d . . . H46A H 0.4203 2.5848 -0.8129 0.058 Uiso 1 1 calc R . . C52 C 0.1909(3) 2.2574(3) -0.5828(2) 0.0331(9) Uani 1 1 d . . . C53 C 0.1204(4) 2.2047(4) -0.5128(2) 0.0361(9) Uani 1 1 d . . . C54 C 0.0078(3) 2.2095(4) -0.5168(2) 0.0390(10) Uani 1 1 d . . . H54A H -0.0433 2.1779 -0.4715 0.047 Uiso 1 1 calc R . . C55 C -0.0251(4) 2.2610(4) -0.5879(2) 0.0400(10) Uani 1 1 d . . . H55A H -0.0986 2.2627 -0.5914 0.048 Uiso 1 1 calc R . . C56 C 0.0513(3) 2.3111(4) -0.6551(3) 0.0388(10) Uani 1 1 d . . . H56A H 0.0272 2.3462 -0.7028 0.047 Uiso 1 1 calc R . . C62 C 0.3065(3) 2.2575(4) -0.5840(2) 0.0347(9) Uani 1 1 d . . . C63 C 0.3488(4) 2.2017(4) -0.5146(3) 0.0402(10) Uani 1 1 d . . . C64 C 0.4629(4) 2.2059(4) -0.5198(3) 0.0514(13) Uani 1 1 d . . . H64A H 0.4951 2.1712 -0.4755 0.062 Uiso 1 1 calc R . . C65 C 0.5251(4) 2.2613(5) -0.5901(3) 0.0577(14) Uani 1 1 d . . . H65A H 0.6003 2.2638 -0.5940 0.069 Uiso 1 1 calc R . . C66 C 0.4765(4) 2.3146(4) -0.6569(3) 0.0478(12) Uani 1 1 d . . . H66A H 0.5205 2.3521 -0.7043 0.057 Uiso 1 1 calc R . . C71 C 0.2753(4) 2.1468(4) -0.4436(3) 0.0418(10) Uani 1 1 d . . . C73 C 0.3661(4) 1.9882(4) -0.3684(3) 0.0487(12) Uani 1 1 d . . . H73A H 0.4347 1.9911 -0.4070 0.058 Uiso 1 1 calc R . . H73B H 0.3177 1.9439 -0.3781 0.058 Uiso 1 1 calc R . . C74 C 0.3874(4) 1.9421(5) -0.2848(3) 0.0535(13) Uani 1 1 d . . . H74A H 0.4208 1.8689 -0.2765 0.064 Uiso 1 1 calc R . . H74B H 0.4372 1.9856 -0.2757 0.064 Uiso 1 1 calc R . . C76 C 0.2929(4) 1.8911(5) -0.1485(3) 0.0576(14) Uani 1 1 d . . . H76A H 0.3307 1.9357 -0.1302 0.069 Uiso 1 1 calc R . . H76B H 0.3339 1.8212 -0.1424 0.069 Uiso 1 1 calc R . . C77 C 0.1766(4) 1.8777(5) -0.1011(3) 0.0612(15) Uani 1 1 d . . . H77A H 0.1406 1.8291 -0.1171 0.073 Uiso 1 1 calc R . . H77B H 0.1771 1.8476 -0.0444 0.073 Uiso 1 1 calc R . . C79 C 0.0016(4) 1.9778(5) -0.0960(3) 0.0579(14) Uani 1 1 d . . . H79A H -0.0320 2.0499 -0.0983 0.070 Uiso 1 1 calc R . . H79B H -0.0187 1.9314 -0.0416 0.070 Uiso 1 1 calc R . . C80 C -0.0421(4) 1.9359(5) -0.1515(3) 0.0530(13) Uani 1 1 d . . . H80A H -0.0284 1.8579 -0.1385 0.064 Uiso 1 1 calc R . . H80B H -0.1208 1.9538 -0.1474 0.064 Uiso 1 1 calc R . . C82 C -0.0234(4) 1.9664(4) -0.2923(3) 0.0444(11) Uani 1 1 d . . . H82A H -0.0909 2.0105 -0.3020 0.053 Uiso 1 1 calc R . . H82B H -0.0385 1.8909 -0.2769 0.053 Uiso 1 1 calc R . . C83 C 0.0641(4) 1.9929(4) -0.3656(3) 0.0414(10) Uani 1 1 d . . . H83A H 0.1267 1.9401 -0.3601 0.050 Uiso 1 1 calc R . . H83B H 0.0362 1.9945 -0.4121 0.050 Uiso 1 1 calc R . . C85 C 0.1653(4) 2.1485(4) -0.4429(2) 0.0375(10) Uani 1 1 d . . . Cl1 Cl 0.33996(11) 1.83579(11) 0.08818(8) 0.0555(3) Uani 1 1 d . . . O11 O 0.3247(3) 1.7500(3) 0.0596(2) 0.0668(11) Uani 1 1 d . . . O12 O 0.3760(6) 1.7911(5) 0.1622(3) 0.1105(19) Uani 1 1 d . . . O13 O 0.2396(4) 1.8967(5) 0.0991(4) 0.116(2) Uani 1 1 d . . . O14 O 0.4212(4) 1.9008(4) 0.0329(3) 0.0870(15) Uani 1 1 d . . . Cl2 Cl -0.73153(10) 2.92921(10) -0.56749(7) 0.0450(3) Uani 1 1 d . . . O21 O -0.7432(5) 2.8693(5) -0.6162(4) 0.1123(19) Uani 1 1 d . . . O22 O -0.6353(3) 2.9845(4) -0.5930(3) 0.0874(15) Uani 1 1 d . . . O23 O -0.8261(3) 3.0074(4) -0.5724(3) 0.0719(12) Uani 1 1 d . . . O24 O -0.7386(3) 2.8621(4) -0.4869(3) 0.0918(17) Uani 1 1 d . . . Cl3 Cl -0.18714(12) 1.34626(14) 0.21873(9) 0.0672(4) Uani 1 1 d . . . O31 O -0.1013(6) 1.2611(6) 0.2239(6) 0.164(3) Uani 1 1 d . . . O32 O -0.2875(4) 1.3069(6) 0.2183(4) 0.128(2) Uani 1 1 d . . . O33 O -0.2046(7) 1.3731(7) 0.2922(4) 0.161(3) Uani 1 1 d . . . O34 O -0.1615(6) 1.4303(6) 0.1499(4) 0.159(3) Uani 1 1 d . . . N101 N 0.1860(6) 2.2631(6) -0.9983(5) 0.112(2) Uani 1 1 d . . . C102 C 0.2394(6) 2.2050(6) -1.0307(5) 0.080(2) Uani 1 1 d . . . C103 C 0.3111(7) 2.1322(7) -1.0676(5) 0.101(3) Uani 1 1 d . . . H10A H 0.3864 2.1445 -1.0713 0.151 Uiso 1 1 calc R . . H10B H 0.2974 2.1443 -1.1203 0.151 Uiso 1 1 calc R . . H10C H 0.2975 2.0589 -1.0360 0.151 Uiso 1 1 calc R . . N201 N -0.4640(15) 2.5919(12) -0.6790(14) 0.357(15) Uani 1 1 d . . . C202 C -0.4800(9) 2.6765(13) -0.6967(6) 0.125(4) Uani 1 1 d . . . C203 C -0.4902(9) 2.7909(12) -0.7023(8) 0.159(5) Uani 1 1 d . . . H20A H -0.5004 2.8335 -0.7550 0.238 Uiso 1 1 calc R . . H20B H -0.4244 2.8097 -0.6921 0.238 Uiso 1 1 calc R . . H20C H -0.5524 2.8049 -0.6636 0.238 Uiso 1 1 calc R . . N301 N 0.0000 2.5000 -0.5000 0.73(8) Uani 0.80(2) 2 d SPD . 1 C302 C -0.071(2) 2.510(3) -0.5230(15) 0.31(5) Uani 0.400(10) 1 d PD . 1 C303 C -0.145(3) 2.552(3) -0.5721(13) 0.30(4) Uani 0.400(10) 1 d PD . 1 N311 N -0.351(2) 2.430(2) -0.5418(10) 0.206(10) Uani 0.600(10) 1 d PD . 2 C312 C -0.314(3) 2.5220(15) -0.5469(14) 0.218(19) Uani 0.600(10) 1 d P . 2 C313 C -0.282(3) 2.597(2) -0.570(3) 0.34(3) Uani 0.600(10) 1 d PD . 2 N91 N 0.1613(4) 2.2039(4) -0.2480(3) 0.0646(13) Uani 1 1 d . . . C92 C 0.1675(7) 2.2824(9) -0.2449(7) 0.121(3) Uani 1 1 d . . . C93 C 0.1795(11) 2.3895(11) -0.2294(13) 0.289(12) Uani 1 1 d . . . H93A H 0.1100 2.4136 -0.2023 0.433 Uiso 1 1 calc R . . H93B H 0.2022 2.4435 -0.2795 0.433 Uiso 1 1 calc R . . H93C H 0.2339 2.3780 -0.1968 0.433 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02400(19) 0.0435(2) 0.02791(18) 0.00054(13) -0.00081(12) -0.00318(14) Li1 0.035(4) 0.061(5) 0.059(5) -0.005(4) -0.014(4) -0.003(4) O72 0.049(2) 0.053(2) 0.0328(16) 0.0020(14) -0.0139(14) -0.0050(16) O75 0.0319(17) 0.071(2) 0.0364(17) 0.0063(15) -0.0108(13) -0.0005(16) O78 0.043(2) 0.076(3) 0.0458(19) -0.0099(17) -0.0129(16) -0.0031(18) O81 0.0356(18) 0.070(2) 0.0304(15) -0.0019(15) -0.0036(13) -0.0154(16) O84 0.0433(18) 0.0506(19) 0.0264(14) -0.0023(13) 0.0012(12) -0.0146(15) N11 0.031(2) 0.046(2) 0.042(2) -0.0042(17) -0.0004(16) -0.0048(17) N21 0.0252(19) 0.053(2) 0.0338(18) 0.0033(16) -0.0006(14) -0.0055(17) N31 0.0275(18) 0.046(2) 0.0274(16) -0.0016(15) -0.0020(13) -0.0026(16) N41 0.0299(19) 0.047(2) 0.0308(18) 0.0037(16) -0.0025(14) -0.0073(16) N51 0.0273(18) 0.041(2) 0.0294(17) -0.0042(14) -0.0023(13) -0.0022(15) N61 0.0248(18) 0.046(2) 0.0352(18) -0.0028(15) -0.0034(14) -0.0034(16) C12 0.029(2) 0.045(3) 0.067(3) 0.001(2) 0.000(2) -0.006(2) C13 0.050(3) 0.058(4) 0.083(4) -0.006(3) -0.014(3) 0.002(3) C14 0.072(5) 0.056(4) 0.103(5) -0.024(4) 0.000(4) 0.002(3) C15 0.071(4) 0.074(4) 0.056(3) -0.017(3) 0.001(3) -0.008(3) C16 0.051(3) 0.050(3) 0.048(3) -0.006(2) -0.001(2) -0.001(2) C22 0.030(2) 0.047(3) 0.051(3) 0.005(2) -0.009(2) -0.007(2) C23 0.048(3) 0.054(3) 0.094(5) 0.006(3) -0.033(3) -0.003(3) C24 0.051(4) 0.079(5) 0.075(4) 0.012(3) -0.039(3) -0.009(3) C25 0.033(3) 0.101(5) 0.049(3) 0.000(3) -0.012(2) -0.019(3) C26 0.028(2) 0.072(4) 0.040(2) -0.005(2) -0.0028(19) -0.006(2) C32 0.025(2) 0.055(3) 0.031(2) -0.0005(19) -0.0038(16) 0.0004(19) C33 0.031(2) 0.069(3) 0.039(2) -0.013(2) -0.0051(19) 0.004(2) C34 0.039(3) 0.064(3) 0.048(3) -0.018(2) -0.009(2) 0.000(2) C35 0.033(3) 0.057(3) 0.055(3) -0.011(2) -0.004(2) -0.007(2) C36 0.036(3) 0.052(3) 0.039(2) -0.008(2) -0.0019(19) -0.007(2) C42 0.026(2) 0.058(3) 0.0255(19) 0.0005(18) -0.0058(16) 0.003(2) C43 0.033(2) 0.067(3) 0.029(2) 0.004(2) -0.0009(18) -0.002(2) C44 0.032(3) 0.075(4) 0.038(3) 0.009(2) 0.0002(19) -0.002(3) C45 0.041(3) 0.059(3) 0.054(3) 0.007(2) -0.005(2) -0.015(2) C46 0.032(2) 0.052(3) 0.048(3) -0.001(2) -0.002(2) -0.006(2) C52 0.023(2) 0.040(2) 0.031(2) -0.0057(17) -0.0006(15) -0.0023(17) C53 0.031(2) 0.041(2) 0.033(2) -0.0057(18) -0.0050(17) -0.0042(18) C54 0.027(2) 0.049(3) 0.032(2) -0.0030(18) 0.0034(16) -0.0107(19) C55 0.024(2) 0.055(3) 0.037(2) -0.007(2) -0.0028(17) -0.0062(19) C56 0.024(2) 0.051(3) 0.034(2) -0.0054(19) -0.0057(16) 0.0003(19) C62 0.026(2) 0.042(2) 0.030(2) -0.0020(17) -0.0055(16) -0.0048(18) C63 0.027(2) 0.049(3) 0.037(2) -0.0023(19) -0.0053(17) -0.0023(19) C64 0.029(2) 0.069(3) 0.043(3) 0.006(2) -0.0132(19) -0.005(2) C65 0.025(2) 0.082(4) 0.052(3) 0.001(3) -0.010(2) -0.001(2) C66 0.024(2) 0.065(3) 0.040(2) 0.003(2) -0.0024(18) -0.010(2) C71 0.041(3) 0.046(3) 0.032(2) -0.0032(19) -0.0072(18) -0.005(2) C73 0.033(3) 0.059(3) 0.042(3) -0.004(2) -0.0040(19) 0.001(2) C74 0.027(2) 0.069(3) 0.049(3) 0.004(2) -0.010(2) -0.001(2) C76 0.043(3) 0.074(4) 0.042(3) 0.006(2) -0.014(2) -0.005(3) C77 0.046(3) 0.084(4) 0.035(2) 0.009(2) -0.012(2) -0.001(3) C79 0.041(3) 0.085(4) 0.038(3) -0.006(2) -0.005(2) -0.006(3) C80 0.034(3) 0.076(4) 0.032(2) 0.003(2) 0.0019(18) -0.006(2) C82 0.031(2) 0.057(3) 0.038(2) -0.003(2) -0.0037(18) -0.012(2) C83 0.033(2) 0.051(3) 0.033(2) -0.0021(19) -0.0045(17) -0.010(2) C85 0.036(2) 0.044(3) 0.027(2) -0.0036(17) -0.0005(16) -0.0100(19) Cl1 0.0466(7) 0.0602(8) 0.0506(7) -0.0124(6) 0.0020(5) -0.0030(6) O11 0.056(2) 0.077(3) 0.064(2) -0.015(2) -0.0090(19) -0.014(2) O12 0.156(6) 0.116(4) 0.074(3) -0.029(3) -0.049(3) -0.008(4) O13 0.064(3) 0.089(4) 0.153(5) -0.013(3) 0.017(3) 0.017(3) O14 0.072(3) 0.093(3) 0.088(3) -0.034(3) 0.024(2) -0.028(3) Cl2 0.0377(6) 0.0537(7) 0.0406(6) -0.0056(5) -0.0097(5) -0.0112(5) O21 0.109(5) 0.120(5) 0.134(5) -0.080(4) -0.020(4) 0.001(4) O22 0.038(2) 0.092(3) 0.111(4) 0.011(3) -0.022(2) -0.024(2) O23 0.044(2) 0.079(3) 0.084(3) -0.010(2) -0.020(2) 0.005(2) O24 0.050(3) 0.126(4) 0.065(3) 0.030(3) -0.019(2) -0.019(3) Cl3 0.0508(8) 0.0863(11) 0.0619(8) -0.0138(7) -0.0184(6) -0.0038(7) O31 0.127(6) 0.162(6) 0.272(9) -0.133(7) -0.131(6) 0.075(5) O32 0.055(3) 0.158(6) 0.160(6) -0.027(5) -0.022(3) -0.024(4) O33 0.176(7) 0.217(8) 0.124(5) -0.087(5) -0.089(5) 0.060(6) O34 0.134(6) 0.164(7) 0.120(5) 0.028(5) 0.016(4) -0.053(5) N101 0.090(5) 0.107(6) 0.112(6) -0.008(4) -0.006(4) -0.003(4) C102 0.067(5) 0.073(5) 0.082(5) -0.006(4) 0.004(4) -0.016(4) C103 0.112(7) 0.094(6) 0.102(6) -0.037(5) -0.021(5) -0.008(5) N201 0.225(16) 0.140(12) 0.52(3) 0.028(15) 0.048(18) 0.085(12) C202 0.091(7) 0.183(12) 0.095(6) -0.041(7) -0.033(5) 0.031(8) C203 0.112(9) 0.220(15) 0.179(12) -0.123(11) -0.002(8) -0.017(9) N301 0.65(8) 0.31(5) 1.08(13) -0.49(7) 0.79(10) -0.41(5) C302 0.74(14) 0.12(3) 0.054(17) -0.052(19) 0.00(3) -0.03(5) C303 0.57(10) 0.14(3) 0.039(12) 0.014(14) 0.07(3) 0.15(5) N311 0.26(3) 0.26(3) 0.099(12) -0.024(14) -0.065(14) -0.05(2) C312 0.51(6) 0.055(10) 0.159(19) -0.043(12) -0.22(3) 0.037(19) C313 0.33(5) 0.108(19) 0.69(9) -0.18(4) -0.25(5) 0.05(3) N91 0.062(3) 0.050(3) 0.081(3) -0.019(3) -0.013(3) -0.008(2) C92 0.063(5) 0.113(8) 0.176(10) -0.049(7) -0.001(6) 0.000(5) C93 0.166(13) 0.140(11) 0.56(3) -0.210(17) 0.118(17) -0.086(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 Ru1 N31 2.055(4) . ? Ru1 N61 2.063(4) . ? Ru1 N51 2.063(3) . ? Ru1 N11 2.064(4) . ? Ru1 N21 2.068(4) . ? Ru1 N41 2.070(3) . ? Li1 N91 1.974(11) . ? Li1 O81 1.990(9) . ? Li1 O75 2.007(9) . ? Li1 O78 2.225(9) . ? Li1 O84 2.384(9) . ? Li1 O72 2.601(9) . ? O72 C71 1.360(5) . ? O72 C73 1.449(6) . ? O75 C74 1.430(6) . ? O75 C76 1.447(5) . ? O78 C77 1.414(7) . ? O78 C79 1.444(6) . ? O81 C82 1.428(5) . ? O81 C80 1.427(5) . ? O84 C85 1.375(5) . ? O84 C83 1.466(6) . ? N11 C16 1.340(7) . ? N11 C12 1.386(6) . ? N21 C22 1.349(6) . ? N21 C26 1.354(6) . ? N31 C36 1.330(6) . ? N31 C32 1.375(5) . ? N41 C46 1.333(6) . ? N41 C42 1.350(6) . ? N51 C56 1.330(5) . ? N51 C52 1.368(5) . ? N61 C66 1.337(6) . ? N61 C62 1.360(5) . ? C12 C13 1.374(8) . ? C12 C22 1.454(8) . ? C13 C14 1.380(10) . ? C14 C15 1.386(9) . ? C15 C16 1.358(8) . ? C22 C23 1.414(7) . ? C23 C24 1.334(9) . ? C24 C25 1.375(9) . ? C25 C26 1.378(7) . ? C32 C33 1.390(7) . ? C32 C42 1.474(7) . ? C33 C34 1.374(7) . ? C34 C35 1.378(7) . ? C35 C36 1.378(7) . ? C42 C43 1.399(6) . ? C43 C44 1.372(8) . ? C44 C45 1.374(8) . ? C45 C46 1.396(6) . ? C52 C53 1.394(5) . ? C52 C62 1.439(6) . ? C53 C54 1.415(6) . ? C53 C85 1.430(6) . ? C54 C55 1.365(6) . ? C55 C56 1.394(6) . ? C62 C63 1.406(6) . ? C63 C64 1.414(6) . ? C63 C71 1.431(6) . ? C64 C65 1.360(7) . ? C65 C66 1.404(7) . ? C71 C85 1.368(6) . ? C73 C74 1.499(7) . ? C76 C77 1.510(7) . ? C79 C80 1.509(8) . ? C82 C83 1.488(6) . ? Cl1 O13 1.398(5) . ? Cl1 O14 1.407(4) . ? Cl1 O12 1.419(5) . ? Cl1 O11 1.427(4) . ? Cl2 O21 1.391(5) . ? Cl2 O22 1.398(4) . ? Cl2 O24 1.423(4) . ? Cl2 O23 1.451(4) . ? Cl3 O34 1.374(6) . ? Cl3 O32 1.422(6) . ? Cl3 O31 1.431(6) . ? Cl3 O33 1.437(7) . ? N101 C102 1.153(10) . ? C102 C103 1.433(11) . ? N201 C202 1.053(16) . ? C202 C203 1.457(16) . ? N301 C302 1.041(19) . ? C302 C303 1.361(19) . ? N311 C312 1.32(3) . ? C312 C313 1.03(4) . ? N91 C92 1.061(10) . ? C92 C93 1.547(15) . ? 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 N31 Ru1 N61 89.24(15) . . ? N31 Ru1 N51 96.93(14) . . ? N61 Ru1 N51 79.65(14) . . ? N31 Ru1 N11 172.16(14) . . ? N61 Ru1 N11 97.29(15) . . ? N51 Ru1 N11 88.53(14) . . ? N31 Ru1 N21 95.29(15) . . ? N61 Ru1 N21 174.78(15) . . ? N51 Ru1 N21 97.19(14) . . ? N11 Ru1 N21 78.39(16) . . ? N31 Ru1 N41 79.24(15) . . ? N61 Ru1 N41 94.75(14) . . ? N51 Ru1 N41 173.31(14) . . ? N11 Ru1 N41 95.84(15) . . ? N21 Ru1 N41 88.66(14) . . ? N91 Li1 O81 121.8(5) . . ? N91 Li1 O75 122.8(5) . . ? O81 Li1 O75 112.1(5) . . ? N91 Li1 O78 95.8(4) . . ? O81 Li1 O78 77.0(3) . . ? O75 Li1 O78 78.0(3) . . ? N91 Li1 O84 96.7(4) . . ? O81 Li1 O84 71.1(3) . . ? O75 Li1 O84 118.5(5) . . ? O78 Li1 O84 147.7(4) . . ? N91 Li1 O72 87.5(4) . . ? O81 Li1 O72 130.3(5) . . ? O75 Li1 O72 70.5(3) . . ? O78 Li1 O72 144.3(4) . . ? O84 Li1 O72 66.0(2) . . ? C71 O72 C73 115.7(4) . . ? C71 O72 Li1 112.2(3) . . ? C73 O72 Li1 100.0(3) . . ? C74 O75 C76 112.3(4) . . ? C74 O75 Li1 125.8(4) . . ? C76 O75 Li1 115.6(4) . . ? C77 O78 C79 113.2(4) . . ? C77 O78 Li1 106.1(4) . . ? C79 O78 Li1 105.2(3) . . ? C82 O81 C80 113.9(4) . . ? C82 O81 Li1 122.6(4) . . ? C80 O81 Li1 122.0(4) . . ? C85 O84 C83 115.5(3) . . ? C85 O84 Li1 119.1(3) . . ? C83 O84 Li1 97.9(3) . . ? C16 N11 C12 118.3(4) . . ? C16 N11 Ru1 126.4(3) . . ? C12 N11 Ru1 115.4(3) . . ? C22 N21 C26 118.0(4) . . ? C22 N21 Ru1 115.8(3) . . ? C26 N21 Ru1 125.9(3) . . ? C36 N31 C32 117.5(4) . . ? C36 N31 Ru1 127.8(3) . . ? C32 N31 Ru1 114.8(3) . . ? C46 N41 C42 119.9(4) . . ? C46 N41 Ru1 124.7(3) . . ? C42 N41 Ru1 115.4(3) . . ? C56 N51 C52 117.5(3) . . ? C56 N51 Ru1 128.4(3) . . ? C52 N51 Ru1 114.0(3) . . ? C66 N61 C62 117.8(4) . . ? C66 N61 Ru1 128.3(3) . . ? C62 N61 Ru1 113.9(3) . . ? C13 C12 N11 120.8(5) . . ? C13 C12 C22 124.9(5) . . ? N11 C12 C22 114.3(4) . . ? C12 C13 C14 119.3(6) . . ? C13 C14 C15 119.8(6) . . ? C16 C15 C14 118.7(6) . . ? N11 C16 C15 123.2(5) . . ? N21 C22 C23 120.7(5) . . ? N21 C22 C12 115.6(4) . . ? C23 C22 C12 123.7(5) . . ? C24 C23 C22 120.3(6) . . ? C23 C24 C25 119.3(5) . . ? C24 C25 C26 119.6(6) . . ? N21 C26 C25 122.1(6) . . ? N31 C32 C33 120.7(4) . . ? N31 C32 C42 115.0(4) . . ? C33 C32 C42 124.3(4) . . ? C34 C33 C32 120.3(4) . . ? C33 C34 C35 118.2(5) . . ? C36 C35 C34 119.3(5) . . ? N31 C36 C35 123.5(4) . . ? N41 C42 C43 120.6(5) . . ? N41 C42 C32 115.1(4) . . ? C43 C42 C32 124.0(4) . . ? C44 C43 C42 119.0(5) . . ? C43 C44 C45 120.2(5) . . ? C44 C45 C46 118.4(5) . . ? N41 C46 C45 121.8(5) . . ? N51 C52 C53 123.8(4) . . ? N51 C52 C62 115.8(3) . . ? C53 C52 C62 120.4(4) . . ? C52 C53 C54 116.6(4) . . ? C52 C53 C85 118.9(4) . . ? C54 C53 C85 124.4(4) . . ? C55 C54 C53 119.5(4) . . ? C54 C55 C56 120.0(4) . . ? N51 C56 C55 122.5(4) . . ? N61 C62 C63 123.8(4) . . ? N61 C62 C52 116.6(4) . . ? C63 C62 C52 119.6(4) . . ? C62 C63 C64 116.6(4) . . ? C62 C63 C71 119.2(4) . . ? C64 C63 C71 124.2(4) . . ? C65 C64 C63 119.5(4) . . ? C64 C65 C66 120.3(5) . . ? N61 C66 C65 122.0(4) . . ? O72 C71 C85 119.5(4) . . ? O72 C71 C63 119.7(4) . . ? C85 C71 C63 120.7(4) . . ? O72 C73 C74 106.7(4) . . ? O75 C74 C73 107.4(4) . . ? O75 C76 C77 106.3(4) . . ? O78 C77 C76 107.2(5) . . ? O78 C79 C80 111.6(4) . . ? O81 C80 C79 105.9(4) . . ? O81 C82 C83 107.6(4) . . ? O84 C83 C82 104.8(4) . . ? C71 C85 O84 119.7(4) . . ? C71 C85 C53 121.2(4) . . ? O84 C85 C53 119.0(4) . . ? O13 Cl1 O14 110.8(3) . . ? O13 Cl1 O12 109.8(4) . . ? O14 Cl1 O12 108.7(4) . . ? O13 Cl1 O11 109.0(4) . . ? O14 Cl1 O11 109.5(3) . . ? O12 Cl1 O11 109.1(3) . . ? O21 Cl2 O22 114.2(4) . . ? O21 Cl2 O24 110.4(4) . . ? O22 Cl2 O24 110.3(3) . . ? O21 Cl2 O23 103.6(3) . . ? O22 Cl2 O23 108.9(3) . . ? O24 Cl2 O23 109.1(3) . . ? O34 Cl3 O32 108.5(5) . . ? O34 Cl3 O31 110.9(5) . . ? O32 Cl3 O31 109.9(4) . . ? O34 Cl3 O33 115.6(5) . . ? O32 Cl3 O33 105.9(5) . . ? O31 Cl3 O33 105.9(4) . . ? N101 C102 C103 176.2(10) . . ? N201 C202 C203 164.7(19) . . ? N301 C302 C303 160(4) . . ? C313 C312 N311 162(4) . . ? C92 N91 Li1 176.3(8) . . ? N91 C92 C93 172.6(15) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.168 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.103 #=END