# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Tai-Chu Lau' _publ_contact_author_email bhtclau@cityu.edu.hk _publ_section_title ; A novel triazidoruthenium(III) building block for the construction of polynuclear compounds ; _publ_author_name 'Tai-Chu Lau' # Attachment '- total.cif' data_101008a_xj _database_code_depnum_ccdc_archive 'CCDC 833814' #TrackingRef '- total.cif' _audit_creation_date 2011-07-05 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C6.5 H4 N5 O Ru0.5), C H2 Cl2, 2(C24 H20 P)' _chemical_formula_sum 'C62 H51 Cl2 N10 O2 P2 Ru' _chemical_formula_weight 1202.04 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 1 21/m 1' _space_group_name_Hall '-P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' 3 '-x, -y, -z' 4 'x, -y-1/2, z' _cell_length_a 9.80700(10) _cell_length_b 24.4502(3) _cell_length_c 12.8128(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.704(2) _cell_angle_gamma 90.00 _cell_volume 2971.67(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7340 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 71.4283 _cell_measurement_theta_min 6.2598 _exptl_absorpt_coefficient_mu 3.882 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.59564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.2 (release 28-02-2008 CrysAlis171 .NET) (compiled Feb 28 2008,18:34:21) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1234 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_unetI/netI 0.0214 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9020 _diffrn_reflns_theta_full 67.00 _diffrn_reflns_theta_max 67.00 _diffrn_reflns_theta_min 6.26 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4840 _reflns_number_total 5246 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.304 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.100 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 544 _refine_ls_number_reflns 5246 _refine_ls_number_restraints 239 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0564 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+5.0127P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1711 _refine_ls_wR_factor_ref 0.1741 _refine_special_details ; Since NEGATIVE PART instruction was used to fix the disorder of the aromatic ring (C1 to C6), no PART instruction and hydrogens were added to the disordered imine carbon (C7) and (C7A). 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.55739(4) 0.2500 0.17504(3) 0.03287(18) Uani 1 2 d SD . . Cl1 Cl 0.7082(4) 0.57179(19) 0.4708(4) 0.1014(12) Uani 0.50 1 d PD . . Cl2 Cl 0.5988(5) 0.67856(15) 0.3898(3) 0.0942(11) Uani 0.50 1 d PD . . P1 P 0.11348(10) 0.55628(4) 0.22565(8) 0.0332(3) Uani 1 1 d . . . O1 O 0.5935(5) 0.2500 0.3348(4) 0.0529(11) Uani 1 2 d S . . O2 O 0.5251(5) 0.2500 0.0133(4) 0.0436(10) Uani 1 2 d S . . N1 N 0.7718(14) 0.2500 0.2374(8) 0.033(3) Uani 0.32 2 d SPD . . N1A N 0.7560(8) 0.2500 0.1612(5) 0.0283(13) Uani 0.68 2 d SPD . . N2 N 0.5620(4) 0.33477(16) 0.1737(3) 0.0468(9) Uani 1 1 d . . . N3 N 0.4806(4) 0.35950(14) 0.2118(3) 0.0446(9) Uani 1 1 d . . . N4 N 0.4070(5) 0.38541(19) 0.2501(4) 0.0650(13) Uani 1 1 d . . . N5 N 0.3388(5) 0.2500 0.1604(4) 0.0436(12) Uani 1 2 d S . . N6 N 0.2836(8) 0.257(2) 0.2290(6) 0.049(8) Uani 0.50 1 d P A -2 N7 N 0.2264(13) 0.2659(5) 0.2947(11) 0.099(5) Uani 0.50 1 d P A -2 C1 C 0.7257(9) 0.2587(7) 0.3943(6) 0.038(4) Uani 0.50 1 d PD . -1 C2 C 0.7473(10) 0.2640(3) 0.5075(7) 0.049(3) Uani 0.50 1 d PD . -1 H2 H 0.6676 0.2658 0.5366 0.059 Uiso 0.50 1 calc PR . -1 C3 C 0.8760(12) 0.2664(5) 0.5745(8) 0.073(5) Uani 0.50 1 d PD . -1 H3 H 0.8866 0.2703 0.6499 0.087 Uiso 0.50 1 calc PR . -1 C4 C 0.9946(11) 0.2631(7) 0.5337(9) 0.074(7) Uani 0.50 1 d PD . -1 H4 H 1.0863 0.2637 0.5814 0.089 Uiso 0.50 1 calc PR . -1 C5 C 0.9791(10) 0.2592(8) 0.4262(9) 0.055(5) Uani 0.50 1 d PD . -1 H5 H 1.0608 0.2602 0.3992 0.066 Uiso 0.50 1 calc PR . -1 C6 C 0.8425(9) 0.254(2) 0.3508(6) 0.047(5) Uani 0.50 1 d PD . -1 C7 C 0.847(2) 0.2500 0.1667(12) 0.030(3) Uani 0.32 2 d SPD . . C7A C 0.8621(10) 0.2500 0.2448(7) 0.0335(17) Uani 0.68 2 d SPD . . C8 C 0.7770(7) 0.2500 0.0532(4) 0.0396(13) Uani 1 2 d SD . . C9 C 0.8953(7) 0.2500 0.0127(6) 0.0524(17) Uani 1 2 d S . . H9 H 0.9860 0.2500 0.0617 0.063 Uiso 1 2 calc SR . . C10 C 0.8855(8) 0.2500 -0.0965(7) 0.0584(18) Uani 1 2 d S . . H10 H 0.9683 0.2500 -0.1221 0.070 Uiso 1 2 calc SR . . C11 C 0.7543(9) 0.2500 -0.1684(6) 0.0596(19) Uani 1 2 d S . . H11 H 0.7468 0.2500 -0.2438 0.072 Uiso 1 2 calc SR . . C12 C 0.6313(7) 0.2500 -0.1307(5) 0.0496(15) Uani 1 2 d S . . H12 H 0.5412 0.2500 -0.1805 0.060 Uiso 1 2 calc SR . . C13 C 0.6424(7) 0.2500 -0.0203(5) 0.0380(12) Uani 1 2 d S . . C14 C 0.0275(4) 0.49045(16) 0.2066(3) 0.0340(8) Uani 1 1 d . B . C15 C 0.1011(5) 0.44347(19) 0.2452(5) 0.0556(12) Uani 1 1 d . . . H15 H 0.1986 0.4454 0.2809 0.067 Uiso 1 1 calc R B . C16 C 0.0329(6) 0.3936(2) 0.2319(5) 0.0658(15) Uani 1 1 d . B . H16 H 0.0848 0.3613 0.2565 0.079 Uiso 1 1 calc R . . C17 C -0.1070(5) 0.39008(19) 0.1845(4) 0.0500(11) Uani 1 1 d . . . H17 H -0.1531 0.3556 0.1779 0.060 Uiso 1 1 calc R B . C18 C -0.1799(6) 0.4353(2) 0.1469(5) 0.0632(14) Uani 1 1 d . B . H18 H -0.2781 0.4328 0.1141 0.076 Uiso 1 1 calc R . . C19 C -0.1130(5) 0.4858(2) 0.1555(5) 0.0584(13) Uani 1 1 d . . . H19 H -0.1649 0.5174 0.1258 0.070 Uiso 1 1 calc R B . C20 C -0.0145(4) 0.60617(16) 0.1631(4) 0.0367(9) Uani 1 1 d . B . C21 C -0.0581(5) 0.60831(19) 0.0510(4) 0.0473(10) Uani 1 1 d . . . H21 H -0.0133 0.5861 0.0087 0.057 Uiso 1 1 calc R B . C22 C -0.1678(5) 0.6431(2) 0.0010(5) 0.0571(13) Uani 1 1 d . B . H22 H -0.1963 0.6451 -0.0755 0.069 Uiso 1 1 calc R . . C23 C -0.2349(5) 0.6745(2) 0.0612(5) 0.0540(12) Uani 1 1 d . . . H23 H -0.3112 0.6973 0.0264 0.065 Uiso 1 1 calc R B . C24 C -0.1921(5) 0.6729(2) 0.1718(5) 0.0576(13) Uani 1 1 d . B . H24 H -0.2381 0.6952 0.2131 0.069 Uiso 1 1 calc R . . C25 C -0.0812(5) 0.63867(19) 0.2242(4) 0.0481(11) Uani 1 1 d . . . H25 H -0.0518 0.6377 0.3008 0.058 Uiso 1 1 calc R B . C26 C 0.1777(19) 0.5632(9) 0.3677(16) 0.033(4) Uani 0.50 1 d PDU B 1 C27 C 0.089(2) 0.5544(10) 0.4324(19) 0.062(6) Uani 0.50 1 d PDU B 1 H27 H -0.0023 0.5401 0.4024 0.074 Uiso 0.50 1 calc PR B 1 C28 C 0.131(2) 0.5659(11) 0.5406(18) 0.062(5) Uani 0.50 1 d PDU B 1 H28 H 0.0691 0.5595 0.5853 0.074 Uiso 0.50 1 calc PR B 1 C29 C 0.2618(17) 0.5863(7) 0.5833(11) 0.067(4) Uani 0.50 1 d PDU B 1 H29 H 0.2919 0.5943 0.6581 0.081 Uiso 0.50 1 calc PR B 1 C30 C 0.3480(14) 0.5950(7) 0.5192(9) 0.077(4) Uani 0.50 1 d PDU B 1 H30 H 0.4402 0.6086 0.5500 0.092 Uiso 0.50 1 calc PR B 1 C31 C 0.3075(12) 0.5848(6) 0.4099(8) 0.058(3) Uani 0.50 1 d PDU B 1 H31 H 0.3688 0.5928 0.3652 0.069 Uiso 0.50 1 calc PR B 1 C26A C 0.167(2) 0.5757(9) 0.3676(15) 0.035(4) Uani 0.50 1 d PDU B 2 C27A C 0.084(2) 0.5610(10) 0.4330(17) 0.055(4) Uani 0.50 1 d PDU B 2 H27A H 0.0029 0.5387 0.4064 0.066 Uiso 0.50 1 calc PR B 2 C28A C 0.118(2) 0.5789(11) 0.5377(19) 0.070(6) Uani 0.50 1 d PDU B 2 H28A H 0.0572 0.5704 0.5826 0.084 Uiso 0.50 1 calc PR B 2 C29A C 0.236(2) 0.6085(7) 0.5789(14) 0.078(5) Uani 0.50 1 d PDU B 2 H29A H 0.2642 0.6165 0.6538 0.094 Uiso 0.50 1 calc PR B 2 C30A C 0.3116(15) 0.6262(6) 0.5135(11) 0.070(3) Uani 0.50 1 d PDU B 2 H30A H 0.3910 0.6491 0.5404 0.085 Uiso 0.50 1 calc PR B 2 C31A C 0.2748(16) 0.6113(5) 0.4067(11) 0.065(3) Uani 0.50 1 d PDU B 2 H31A H 0.3254 0.6262 0.3592 0.078 Uiso 0.50 1 calc PR B 2 C32 C 0.2589(10) 0.5580(4) 0.1603(9) 0.029(2) Uani 0.65 1 d PDU B 1 C33 C 0.3341(7) 0.5110(3) 0.1517(6) 0.0455(15) Uani 0.65 1 d PDU B 1 H33 H 0.3025 0.4763 0.1694 0.055 Uiso 0.65 1 calc PR B 1 C34 C 0.4575(8) 0.5156(3) 0.1163(7) 0.058(2) Uani 0.65 1 d PDU B 1 H34 H 0.5115 0.4839 0.1111 0.070 Uiso 0.65 1 calc PR B 1 C35 C 0.5008(12) 0.5660(5) 0.0891(11) 0.058(4) Uani 0.65 1 d PDU B 1 H35 H 0.5811 0.5683 0.0606 0.069 Uiso 0.65 1 calc PR B 1 C36 C 0.4303(13) 0.6130(5) 0.1023(11) 0.044(3) Uani 0.65 1 d PDU B 1 H36 H 0.4656 0.6478 0.0889 0.053 Uiso 0.65 1 calc PR B 1 C37 C 0.3058(13) 0.6088(5) 0.1357(10) 0.036(2) Uani 0.65 1 d PDU B 1 H37 H 0.2531 0.6407 0.1416 0.043 Uiso 0.65 1 calc PR B 1 C32A C 0.272(2) 0.5624(9) 0.1878(18) 0.040(5) Uani 0.35 1 d PDU B 2 C33A C 0.3846(14) 0.5284(6) 0.2346(13) 0.065(4) Uani 0.35 1 d PDU B 2 H33A H 0.3768 0.5031 0.2889 0.078 Uiso 0.35 1 calc PR B 2 C34A C 0.5103(16) 0.5318(7) 0.2008(15) 0.070(4) Uani 0.35 1 d PDU B 2 H34A H 0.5873 0.5083 0.2314 0.084 Uiso 0.35 1 calc PR B 2 C35A C 0.520(3) 0.5693(9) 0.1231(19) 0.054(5) Uani 0.35 1 d PDU B 2 H35A H 0.6052 0.5716 0.1004 0.065 Uiso 0.35 1 calc PR B 2 C36A C 0.410(3) 0.6036(9) 0.078(2) 0.050(6) Uani 0.35 1 d PDU B 2 H36A H 0.4195 0.6296 0.0250 0.060 Uiso 0.35 1 calc PR B 2 C37A C 0.286(3) 0.6000(9) 0.110(2) 0.049(7) Uani 0.35 1 d PDU B 2 H37A H 0.2088 0.6233 0.0784 0.059 Uiso 0.35 1 calc PR B 2 C38 C 0.7102(14) 0.6403(5) 0.4987(9) 0.099(6) Uani 0.50 1 d PD . . H38A H 0.8080 0.6541 0.5123 0.119 Uiso 0.50 1 calc PR . . H38B H 0.6779 0.6460 0.5651 0.119 Uiso 0.50 1 calc PR . . 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 0.0289(3) 0.0257(3) 0.0460(3) 0.000 0.01313(18) 0.000 Cl1 0.074(2) 0.110(3) 0.111(3) -0.010(2) 0.0074(19) 0.023(2) Cl2 0.128(3) 0.077(2) 0.102(2) 0.0204(18) 0.074(2) -0.004(2) P1 0.0329(5) 0.0256(5) 0.0406(5) 0.0011(4) 0.0084(4) 0.0019(4) O1 0.044(3) 0.066(3) 0.045(2) 0.000 0.0045(19) 0.000 O2 0.046(2) 0.036(2) 0.057(3) 0.000 0.029(2) 0.000 N1 0.035(9) 0.024(7) 0.045(10) 0.000 0.017(8) 0.000 N1A 0.027(4) 0.020(3) 0.041(4) 0.000 0.013(3) 0.000 N2 0.044(2) 0.031(2) 0.069(3) -0.0045(16) 0.0218(19) -0.0015(15) N3 0.0406(19) 0.0297(17) 0.057(2) -0.0089(16) -0.0001(17) 0.0051(16) N4 0.059(3) 0.054(3) 0.075(3) -0.020(2) 0.005(2) 0.020(2) N5 0.029(2) 0.049(3) 0.052(3) 0.000 0.010(2) 0.000 N6 0.045(3) 0.04(3) 0.069(4) 0.004(6) 0.029(3) 0.006(6) N7 0.084(7) 0.103(14) 0.138(10) -0.001(7) 0.083(7) 0.009(6) C1 0.048(4) 0.025(13) 0.040(3) 0.000(3) 0.010(3) 0.000(4) C2 0.049(4) 0.059(10) 0.045(4) -0.003(4) 0.022(4) -0.010(4) C3 0.076(7) 0.105(14) 0.034(4) -0.002(5) 0.008(4) -0.036(7) C4 0.044(5) 0.10(2) 0.066(6) 0.011(7) -0.004(4) -0.018(6) C5 0.049(4) 0.040(17) 0.083(6) 0.006(5) 0.030(4) 0.000(4) C6 0.063(4) 0.042(13) 0.040(3) -0.012(12) 0.017(3) -0.012(13) C7 0.036(11) 0.018(8) 0.036(11) 0.000 0.009(8) 0.000 C7A 0.033(5) 0.028(4) 0.043(5) 0.000 0.017(4) 0.000 C8 0.054(4) 0.024(3) 0.040(3) 0.000 0.010(3) 0.000 C9 0.044(4) 0.036(3) 0.071(5) 0.000 0.004(3) 0.000 C10 0.048(4) 0.053(4) 0.084(5) 0.000 0.035(4) 0.000 C11 0.073(5) 0.069(5) 0.046(4) 0.000 0.032(4) 0.000 C12 0.047(4) 0.059(4) 0.042(3) 0.000 0.009(3) 0.000 C13 0.048(3) 0.029(3) 0.042(3) 0.000 0.021(3) 0.000 C14 0.039(2) 0.0271(19) 0.0363(19) 0.0002(15) 0.0110(16) 0.0006(16) C15 0.046(3) 0.035(2) 0.084(4) 0.005(2) 0.012(2) 0.004(2) C16 0.069(4) 0.028(2) 0.103(5) 0.003(3) 0.029(3) 0.006(2) C17 0.062(3) 0.033(2) 0.059(3) -0.006(2) 0.024(2) -0.011(2) C18 0.046(3) 0.047(3) 0.096(4) -0.001(3) 0.016(3) -0.009(2) C19 0.042(3) 0.036(2) 0.094(4) 0.005(2) 0.011(2) -0.0005(19) C20 0.033(2) 0.0244(18) 0.052(2) 0.0018(16) 0.0102(17) 0.0024(15) C21 0.047(2) 0.041(2) 0.049(2) -0.0023(19) 0.0031(19) 0.0073(19) C22 0.051(3) 0.045(3) 0.066(3) 0.004(2) -0.004(2) 0.006(2) C23 0.039(2) 0.038(2) 0.080(3) 0.014(2) 0.006(2) 0.0044(19) C24 0.051(3) 0.037(2) 0.091(4) 0.007(2) 0.031(3) 0.013(2) C25 0.051(3) 0.036(2) 0.060(3) 0.004(2) 0.020(2) 0.0087(19) C26 0.036(5) 0.017(8) 0.044(5) -0.007(5) 0.009(4) 0.004(5) C27 0.067(9) 0.065(11) 0.060(7) -0.025(8) 0.028(6) -0.039(9) C28 0.077(8) 0.063(10) 0.054(6) -0.009(6) 0.032(6) -0.023(8) C29 0.066(7) 0.097(12) 0.037(5) -0.017(7) 0.011(4) -0.010(8) C30 0.062(7) 0.117(11) 0.047(4) -0.012(7) 0.007(4) -0.032(8) C31 0.039(5) 0.094(10) 0.039(4) -0.001(6) 0.008(4) -0.014(6) C26A 0.038(5) 0.027(10) 0.038(5) -0.002(5) 0.003(4) 0.008(5) C27A 0.071(8) 0.052(8) 0.044(6) 0.003(6) 0.019(5) 0.002(6) C28A 0.080(8) 0.082(14) 0.051(6) -0.011(7) 0.024(6) -0.004(7) C29A 0.069(8) 0.091(12) 0.070(7) -0.024(7) 0.007(6) 0.004(7) C30A 0.062(7) 0.065(8) 0.076(6) -0.029(6) 0.002(5) -0.008(5) C31A 0.065(8) 0.052(7) 0.069(5) -0.014(6) 0.001(5) -0.014(5) C32 0.028(3) 0.030(3) 0.028(6) -0.001(4) 0.007(3) 0.002(2) C33 0.050(4) 0.034(3) 0.061(4) 0.010(3) 0.030(3) 0.011(3) C34 0.052(4) 0.050(3) 0.084(6) 0.013(4) 0.039(4) 0.023(3) C35 0.042(5) 0.064(5) 0.078(9) 0.013(6) 0.035(6) 0.011(4) C36 0.039(4) 0.043(4) 0.052(7) 0.001(5) 0.014(5) -0.007(4) C37 0.036(4) 0.029(3) 0.044(6) -0.001(4) 0.011(4) 0.001(3) C32A 0.049(7) 0.038(8) 0.028(10) -0.008(6) 0.000(6) 0.002(5) C33A 0.050(7) 0.057(8) 0.089(11) 0.025(7) 0.020(7) 0.010(6) C34A 0.054(7) 0.062(9) 0.098(11) 0.019(7) 0.026(8) 0.010(7) C35A 0.046(7) 0.054(9) 0.062(12) -0.008(7) 0.015(7) -0.008(6) C36A 0.056(9) 0.047(10) 0.043(10) -0.007(7) 0.007(7) -0.011(7) C37A 0.054(9) 0.048(11) 0.043(11) 0.002(9) 0.009(8) 0.006(8) C38 0.091(10) 0.160(16) 0.048(6) -0.007(8) 0.018(6) -0.074(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 O1 1.987(5) . ? Ru1 O2 2.015(4) . ? Ru1 N1 2.051(13) . ? Ru1 N1A 2.000(7) . ? Ru1 N2 2.073(4) . ? Ru1 N2 2.073(4) 4_565 ? Ru1 N5 2.103(5) . ? Cl1 C38 1.712(14) . ? Cl2 C38 1.801(12) . ? P1 C14 1.804(4) . ? P1 C20 1.787(4) . ? P1 C26 1.777(18) . ? P1 C26A 1.823(18) . ? P1 C32 1.828(10) . ? P1 C32A 1.75(2) . ? O1 C1 1.344(10) 4_565 ? O1 C1 1.344(10) . ? O2 C13 1.327(7) . ? N1 C6 1.444(8) . ? N1 C6 1.444(8) 4_565 ? N1 C7 1.305(16) . ? N1A C7A 1.291(10) . ? N1A C8 1.449(7) . ? N2 N3 1.199(5) . ? N3 N4 1.159(6) . ? N5 N6 1.155(13) . ? N5 N6 1.155(13) 4_565 ? N6 N7 1.146(17) . ? C1 C2 1.416(11) . ? C1 C6 1.401(13) . ? C2 H2 0.9500 . ? C2 C3 1.335(14) . ? C3 H3 0.9500 . ? C3 C4 1.394(16) . ? C4 H4 0.9500 . ? C4 C5 1.350(15) . ? C5 H5 0.9500 . ? C5 C6 1.446(14) . ? C6 C7A 1.422(11) . ? C7 C8 1.441(15) . ? C7A C6 1.422(11) 4_565 ? C8 C9 1.386(10) . ? C8 C13 1.413(9) . ? C9 H9 0.9500 . ? C9 C10 1.377(11) . ? C10 H10 0.9500 . ? C10 C11 1.379(12) . ? C11 H11 0.9500 . ? C11 C12 1.408(10) . ? C12 H12 0.9500 . ? C12 C13 1.391(9) . ? C14 C15 1.380(6) . ? C14 C19 1.372(7) . ? C15 H15 0.9500 . ? C15 C16 1.380(7) . ? C16 H16 0.9500 . ? C16 C17 1.355(8) . ? C17 H17 0.9500 . ? C17 C18 1.338(8) . ? C18 H18 0.9500 . ? C18 C19 1.390(7) . ? C19 H19 0.9500 . ? C20 C21 1.392(6) . ? C20 C25 1.390(6) . ? C21 H21 0.9500 . ? C21 C22 1.393(7) . ? C22 H22 0.9500 . ? C22 C23 1.368(8) . ? C23 H23 0.9500 . ? C23 C24 1.372(8) . ? C24 H24 0.9500 . ? C24 C25 1.401(7) . ? C25 H25 0.9500 . ? C26 C27 1.359(12) . ? C26 C31 1.358(13) . ? C27 H27 0.9500 . ? C27 C28 1.371(13) . ? C28 H28 0.9500 . ? C28 C29 1.353(14) . ? C29 H29 0.9500 . ? C29 C30 1.337(14) . ? C30 H30 0.9500 . ? C30 C31 1.377(13) . ? C31 H31 0.9500 . ? C26A C27A 1.362(13) . ? C26A C31A 1.362(13) . ? C27A H27A 0.9500 . ? C27A C28A 1.371(13) . ? C28A H28A 0.9500 . ? C28A C29A 1.353(15) . ? C29A H29A 0.9500 . ? C29A C30A 1.325(16) . ? C30A H30A 0.9500 . ? C30A C31A 1.372(14) . ? C31A H31A 0.9500 . ? C32 C33 1.385(10) . ? C32 C37 1.388(11) . ? C33 H33 0.9500 . ? C33 C34 1.401(9) . ? C34 H34 0.9500 . ? C34 C35 1.375(12) . ? C35 H35 0.9500 . ? C35 C36 1.375(12) . ? C36 H36 0.9500 . ? C36 C37 1.396(10) . ? C37 H37 0.9500 . ? C32A C33A 1.389(16) . ? C32A C37A 1.385(16) . ? C33A H33A 0.9500 . ? C33A C34A 1.408(16) . ? C34A H34A 0.9500 . ? C34A C35A 1.376(17) . ? C35A H35A 0.9500 . ? C35A C36A 1.374(17) . ? C36A H36A 0.9500 . ? C36A C37A 1.390(16) . ? C37A H37A 0.9500 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 O1 Ru1 O2 178.82(17) . . ? O1 Ru1 N1 72.6(4) . . ? O1 Ru1 N1A 99.7(2) . . ? O1 Ru1 N2 90.57(11) . 4_565 ? O1 Ru1 N2 90.57(11) . . ? O1 Ru1 N5 90.2(2) . . ? O2 Ru1 N1 106.2(4) . . ? O2 Ru1 N2 89.41(11) . . ? O2 Ru1 N2 89.41(11) . 4_565 ? O2 Ru1 N5 91.0(2) . . ? N1 Ru1 N2 88.90(10) . 4_565 ? N1 Ru1 N2 88.90(10) . . ? N1 Ru1 N5 162.8(4) . . ? N1A Ru1 O2 79.1(2) . . ? N1A Ru1 N1 27.1(4) . . ? N1A Ru1 N2 88.60(10) . . ? N1A Ru1 N2 88.60(10) . 4_565 ? N1A Ru1 N5 170.1(2) . . ? N2 Ru1 N2 177.1(2) 4_565 . ? N2 Ru1 N5 91.32(10) . . ? N2 Ru1 N5 91.32(10) 4_565 . ? C14 P1 C26A 112.0(6) . . ? C14 P1 C32 110.5(4) . . ? C20 P1 C14 107.30(19) . . ? C20 P1 C26A 105.2(8) . . ? C20 P1 C32 108.6(3) . . ? C26 P1 C14 104.8(6) . . ? C26 P1 C20 114.9(8) . . ? C26 P1 C26A 10.2(14) . . ? C26 P1 C32 110.6(7) . . ? C26A P1 C32 112.9(7) . . ? C32A P1 C14 117.2(7) . . ? C32A P1 C20 112.9(6) . . ? C32A P1 C26 99.6(9) . . ? C32A P1 C26A 101.6(10) . . ? C32A P1 C32 11.3(10) . . ? C1 O1 Ru1 118.6(5) 4_565 . ? C1 O1 Ru1 118.6(5) . . ? C1 O1 C1 18.3(14) . 4_565 ? C13 O2 Ru1 114.3(4) . . ? C6 N1 Ru1 125.1(9) . . ? C6 N1 Ru1 125.1(9) 4_565 . ? C6 N1 C6 7(5) 4_565 . ? C7 N1 Ru1 115.6(9) . . ? C7 N1 C6 119.1(11) . 4_565 ? C7 N1 C6 119.1(11) . . ? C7A N1A Ru1 121.6(6) . . ? C7A N1A C8 120.8(7) . . ? C8 N1A Ru1 117.6(5) . . ? N3 N2 Ru1 118.8(3) . . ? N4 N3 N2 176.6(5) . . ? N6 N5 Ru1 126.6(6) . . ? N6 N5 Ru1 126.6(6) 4_565 . ? N6 N5 N6 16(6) 4_565 . ? N7 N6 N5 176(5) . . ? O1 C1 C2 117.9(7) . . ? O1 C1 C6 121.9(9) . . ? C6 C1 C2 119.3(7) . . ? C1 C2 H2 118.9 . . ? C3 C2 C1 122.3(8) . . ? C3 C2 H2 118.9 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 119.9(9) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.9(9) . . ? C5 C4 H4 120.1 . . ? C4 C5 H5 118.9 . . ? C4 C5 C6 122.3(8) . . ? C6 C5 H5 118.9 . . ? N1 C6 C5 143.6(10) . . ? C1 C6 N1 100.0(9) . . ? C1 C6 C5 116.0(10) . . ? C1 C6 C7A 135.1(8) . . ? C7A C6 N1 35.2(6) . . ? C7A C6 C5 108.5(8) . . ? N1 C7 C8 119.6(14) . . ? N1A C7A C6 121.1(8) . 4_565 ? N1A C7A C6 121.1(8) . . ? C6 C7A C6 7(5) 4_565 . ? C7 C8 N1A 35.3(7) . . ? C9 C8 N1A 133.9(6) . . ? C9 C8 C7 98.6(9) . . ? C9 C8 C13 118.6(5) . . ? C13 C8 N1A 107.5(5) . . ? C13 C8 C7 142.8(9) . . ? C8 C9 H9 119.0 . . ? C10 C9 C8 122.1(6) . . ? C10 C9 H9 119.0 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.4(6) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 119.8 . . ? C10 C11 C12 120.4(7) . . ? C12 C11 H11 119.8 . . ? C11 C12 H12 120.1 . . ? C13 C12 C11 119.7(6) . . ? C13 C12 H12 120.1 . . ? O2 C13 C8 121.6(5) . . ? O2 C13 C12 118.7(6) . . ? C12 C13 C8 119.8(6) . . ? C15 C14 P1 120.7(3) . . ? C19 C14 P1 121.1(3) . . ? C19 C14 C15 118.2(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.1 . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 121.1(5) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 120.1 . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.1 . . ? C17 C18 H18 119.8 . . ? C17 C18 C19 120.5(5) . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 120.5(5) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 P1 119.0(3) . . ? C25 C20 P1 121.0(3) . . ? C25 C20 C21 119.6(4) . . ? C20 C21 H21 120.1 . . ? C20 C21 C22 119.8(5) . . ? C22 C21 H21 120.1 . . ? C21 C22 H22 119.7 . . ? C23 C22 C21 120.6(5) . . ? C23 C22 H22 119.7 . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 120.1(4) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.5(5) . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 119.4(5) . . ? C20 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C27 C26 P1 119.7(12) . . ? C31 C26 P1 119.8(13) . . ? C31 C26 C27 119.8(13) . . ? C26 C27 H27 119.7 . . ? C26 C27 C28 120.7(12) . . ? C28 C27 H27 119.7 . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.6(13) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 120.3 . . ? C30 C29 C28 119.4(12) . . ? C30 C29 H29 120.3 . . ? C29 C30 H30 118.9 . . ? C29 C30 C31 122.1(11) . . ? C31 C30 H30 118.9 . . ? C26 C31 C30 118.3(11) . . ? C26 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C27A C26A P1 118.6(12) . . ? C27A C26A C31A 118.3(13) . . ? C31A C26A P1 122.4(14) . . ? C26A C27A H27A 120.6 . . ? C26A C27A C28A 118.8(14) . . ? C28A C27A H27A 120.6 . . ? C27A C28A H28A 119.1 . . ? C29A C28A C27A 121.7(15) . . ? C29A C28A H28A 119.1 . . ? C28A C29A H29A 120.4 . . ? C30A C29A C28A 119.3(14) . . ? C30A C29A H29A 120.4 . . ? C29A C30A H30A 120.1 . . ? C29A C30A C31A 119.8(13) . . ? C31A C30A H30A 120.1 . . ? C26A C31A C30A 121.3(13) . . ? C26A C31A H31A 119.3 . . ? C30A C31A H31A 119.3 . . ? C33 C32 P1 120.7(7) . . ? C33 C32 C37 120.6(8) . . ? C37 C32 P1 117.9(7) . . ? C32 C33 H33 120.6 . . ? C32 C33 C34 118.7(7) . . ? C34 C33 H33 120.6 . . ? C33 C34 H34 120.0 . . ? C35 C34 C33 120.1(7) . . ? C35 C34 H34 120.0 . . ? C34 C35 H35 119.3 . . ? C36 C35 C34 121.4(8) . . ? C36 C35 H35 119.3 . . ? C35 C36 H36 120.6 . . ? C35 C36 C37 118.8(10) . . ? C37 C36 H36 120.6 . . ? C32 C37 C36 120.2(9) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C33A C32A P1 119.5(15) . . ? C37A C32A P1 120.6(14) . . ? C37A C32A C33A 119.9(17) . . ? C32A C33A H33A 120.2 . . ? C32A C33A C34A 119.5(15) . . ? C34A C33A H33A 120.2 . . ? C33A C34A H34A 120.3 . . ? C35A C34A C33A 119.4(15) . . ? C35A C34A H34A 120.3 . . ? C34A C35A H35A 119.4 . . ? C36A C35A C34A 121.3(17) . . ? C36A C35A H35A 119.4 . . ? C35A C36A H36A 120.2 . . ? C35A C36A C37A 119.5(17) . . ? C37A C36A H36A 120.2 . . ? C32A C37A C36A 120.4(17) . . ? C32A C37A H37A 119.8 . . ? C36A C37A H37A 119.8 . . ? Cl1 C38 Cl2 112.0(6) . . ? Cl1 C38 H38A 109.2 . . ? Cl1 C38 H38B 109.2 . . ? Cl2 C38 H38A 109.2 . . ? Cl2 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? data_ic14085 _database_code_depnum_ccdc_archive 'CCDC 833815' #TrackingRef '- total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H48 Co N6 O12 Ru2' _chemical_formula_weight 993.85 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' Co Co 0.3494 0.9721 '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 11.4815(3) _cell_length_b 11.8715(3) _cell_length_c 17.2232(4) _cell_angle_alpha 108.3420(13) _cell_angle_beta 91.5545(15) _cell_angle_gamma 111.7158(11) _cell_volume 2042.54(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7414 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details ? _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_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21555 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7183 _reflns_number_gt 4739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7183 _refine_ls_number_parameters 503 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.009 _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 0.80180(4) 0.85749(5) 0.87249(3) 0.03085(15) Uani 1 1 d U . . Ru2 Ru 0.85667(5) 0.77336(5) 0.66918(3) 0.03171(16) Uani 1 1 d U . . Co1 Co 1.07943(7) 0.91747(8) 0.95604(5) 0.0304(2) Uani 1 1 d . . . O1 O 0.7062(4) 0.9611(4) 0.8531(2) 0.0408(11) Uani 1 1 d . . . O2 O 0.8930(4) 0.7617(4) 0.9094(2) 0.0363(10) Uani 1 1 d . . . O3 O 0.9213(4) 0.9545(4) 0.6656(3) 0.0438(11) Uani 1 1 d . . . O4 O 0.7904(4) 0.5829(4) 0.6494(3) 0.0421(11) Uani 1 1 d . . . O5 O 0.9718(3) 1.0142(4) 0.9272(2) 0.0294(9) Uani 1 1 d . . . O6 O 0.7714(4) 0.9142(4) 0.9933(2) 0.0401(11) Uani 1 1 d . . . O7 O 0.8822(4) 0.7121(4) 0.5407(2) 0.0440(11) Uani 1 1 d . . . H7 H 0.8687 0.6278 0.5164 0.066 Uiso 1 1 d R . . O8 O 1.1830(4) 0.8306(4) 1.0056(2) 0.0412(11) Uani 1 1 d . . . H8 H 1.2245 0.8898 1.0548 0.062 Uiso 1 1 d R . . N1 N 0.8331(4) 0.8170(5) 0.7712(3) 0.0289(11) Uani 1 1 d . . . N2 N 1.0424(5) 0.7883(6) 0.6997(3) 0.0451(15) Uani 1 1 d . . . N3 N 1.0843(5) 0.8259(5) 0.7720(3) 0.0388(13) Uani 1 1 d . . . N4 N 1.1307(5) 0.8598(6) 0.8392(3) 0.0492(15) Uani 1 1 d . . . N5 N 0.6297(5) 0.7152(6) 0.8362(3) 0.0486(14) Uani 1 1 d U . . N6 N 0.6904(6) 0.7694(7) 0.6257(4) 0.0533(15) Uani 1 1 d U . . C1 C 0.5842(6) 0.8862(6) 0.8176(3) 0.0345(15) Uani 1 1 d . . . C2 C 0.5087(6) 0.9398(7) 0.7908(4) 0.0418(16) Uani 1 1 d . . . H2 H 0.5430 1.0290 0.7974 0.050 Uiso 1 1 calc R . . C3 C 0.3846(7) 0.8631(8) 0.7548(4) 0.0510(19) Uani 1 1 d . . . H3 H 0.3337 0.8997 0.7360 0.061 Uiso 1 1 calc R . . C4 C 0.3321(6) 0.7330(8) 0.7455(4) 0.054(2) Uani 1 1 d . . . H4 H 0.2456 0.6813 0.7214 0.064 Uiso 1 1 calc R . . C5 C 0.4061(7) 0.6794(7) 0.7712(4) 0.0503(19) Uani 1 1 d . . . H5 H 0.3708 0.5902 0.7646 0.060 Uiso 1 1 calc R . . C6 C 0.5306(6) 0.7537(7) 0.8065(4) 0.0427(16) Uani 1 1 d U . . C7 C 0.6095(8) 0.6069(8) 0.8346(4) 0.057(2) Uani 1 1 d U . . H7A H 0.5257 0.5432 0.8126 0.068 Uiso 1 1 calc R . . C8 C 0.6999(7) 0.5656(6) 0.8627(4) 0.0433(16) Uani 1 1 d U . . C9 C 0.6449(8) 0.4328(7) 0.8540(4) 0.062(2) Uani 1 1 d . . . H9A H 0.5576 0.3833 0.8313 0.074 Uiso 1 1 calc R . . C10 C 0.7160(10) 0.3749(8) 0.8778(5) 0.079(3) Uani 1 1 d . . . H10 H 0.6784 0.2849 0.8687 0.095 Uiso 1 1 calc R . . C11 C 0.8403(9) 0.4451(7) 0.9144(4) 0.064(2) Uani 1 1 d . . . H11 H 0.8875 0.4045 0.9326 0.076 Uiso 1 1 calc R . . C12 C 0.8964(7) 0.5730(7) 0.9250(4) 0.0463(17) Uani 1 1 d . . . H12 H 0.9828 0.6209 0.9505 0.056 Uiso 1 1 calc R . . C13 C 0.8290(6) 0.6358(6) 0.8987(3) 0.0333(14) Uani 1 1 d . . . C14 C 0.8285(7) 0.9857(7) 0.6416(4) 0.0438(17) Uani 1 1 d . . . C15 C 0.8590(7) 1.1097(7) 0.6396(4) 0.0488(18) Uani 1 1 d . . . H15 H 0.9441 1.1721 0.6574 0.059 Uiso 1 1 calc R . . C16 C 0.7673(8) 1.1422(8) 0.6121(5) 0.062(2) Uani 1 1 d . . . H16 H 0.7894 1.2264 0.6098 0.075 Uiso 1 1 calc R . . C17 C 0.6412(8) 1.0520(9) 0.5873(5) 0.070(2) Uani 1 1 d . . . H17 H 0.5776 1.0746 0.5681 0.084 Uiso 1 1 calc R . . C18 C 0.6098(8) 0.9312(8) 0.5909(5) 0.061(2) Uani 1 1 d . . . H18 H 0.5241 0.8701 0.5749 0.074 Uiso 1 1 calc R . . C19 C 0.7026(8) 0.8980(8) 0.6177(4) 0.0545(19) Uani 1 1 d U . . C20 C 0.5929(10) 0.6805(8) 0.6093(5) 0.067(2) Uani 1 1 d U . . H20 H 0.5204 0.6912 0.5906 0.080 Uiso 1 1 calc R . . C21 C 0.5725(7) 0.5551(7) 0.6150(4) 0.0477(17) Uani 1 1 d U . . C22 C 0.4435(7) 0.4711(8) 0.5980(4) 0.056(2) Uani 1 1 d . . . H22 H 0.3813 0.4992 0.5835 0.067 Uiso 1 1 calc R . . C23 C 0.4059(8) 0.3504(8) 0.6018(5) 0.059(2) Uani 1 1 d . . . H23 H 0.3183 0.2946 0.5905 0.071 Uiso 1 1 calc R . . C24 C 0.4964(7) 0.3106(7) 0.6223(4) 0.055(2) Uani 1 1 d . . . H24 H 0.4701 0.2262 0.6250 0.066 Uiso 1 1 calc R . . C25 C 0.6228(7) 0.3877(7) 0.6389(4) 0.0473(18) Uani 1 1 d . . . H25 H 0.6827 0.3568 0.6534 0.057 Uiso 1 1 calc R . . C26 C 0.6650(6) 0.5119(6) 0.6349(4) 0.0388(16) Uani 1 1 d . . . C27 C 1.0244(6) 1.1037(6) 0.8841(4) 0.0363(15) Uani 1 1 d . . . H27A H 0.9616 1.1363 0.8723 0.054 Uiso 1 1 calc R . . H27B H 1.0462 1.0592 0.8320 0.054 Uiso 1 1 calc R . . H27C H 1.1010 1.1762 0.9189 0.054 Uiso 1 1 calc R . . C28 C 0.6534(7) 0.8728(8) 1.0217(4) 0.062(2) Uani 1 1 d . . . H28A H 0.5897 0.8830 0.9886 0.093 Uiso 1 1 calc R . . H28B H 0.6630 0.9253 1.0801 0.093 Uiso 1 1 calc R . . H28C H 0.6259 0.7816 1.0160 0.093 Uiso 1 1 calc R . . C29 C 0.9555(8) 0.7894(8) 0.4971(5) 0.067(2) Uani 1 1 d . . . H29A H 1.0449 0.8300 0.5233 0.100 Uiso 1 1 calc R . . H29B H 0.9247 0.8566 0.4985 0.100 Uiso 1 1 calc R . . H29C H 0.9476 0.7349 0.4395 0.100 Uiso 1 1 calc R . . C30 C 1.2714(7) 0.7852(8) 0.9602(4) 0.057(2) Uani 1 1 d . . . H30A H 1.3274 0.8524 0.9408 0.085 Uiso 1 1 calc R . . H30B H 1.2239 0.7066 0.9125 0.085 Uiso 1 1 calc R . . H30C H 1.3226 0.7662 0.9967 0.085 Uiso 1 1 calc R . . O9 O 0.9703(5) 0.4788(5) 0.6523(3) 0.0554(13) Uani 1 1 d . . . H9 H 0.9213 0.5166 0.6524 0.083 Uiso 1 1 calc R . . C31 C 0.9996(8) 0.4818(8) 0.7328(4) 0.062(2) Uani 1 1 d . . . H31A H 1.0642 0.4466 0.7340 0.093 Uiso 1 1 calc R . . H31B H 0.9228 0.4296 0.7492 0.093 Uiso 1 1 calc R . . H31C H 1.0322 0.5714 0.7715 0.093 Uiso 1 1 calc R . . O10 O 0.8350(6) 0.8653(6) 0.3038(4) 0.0859(19) Uani 1 1 d . . . H10A H 0.9108 0.9154 0.3247 0.129 Uiso 1 1 calc R . . C32 C 0.7612(15) 0.9304(16) 0.3224(10) 0.179(7) Uiso 1 1 d . . . H32A H 0.7344 0.9296 0.3758 0.268 Uiso 1 1 calc R . . H32B H 0.6861 0.8898 0.2792 0.268 Uiso 1 1 calc R . . H32C H 0.8085 1.0200 0.3259 0.268 Uiso 1 1 calc R . . O11 O 0.7050(7) 0.6128(7) 0.2021(4) 0.115(3) Uani 1 1 d . . . H11A H 0.7638 0.6803 0.2343 0.173 Uiso 1 1 calc R . . C33 C 0.7346(12) 0.5852(11) 0.1234(7) 0.131(5) Uani 1 1 d . . . H33A H 0.7309 0.6501 0.1008 0.196 Uiso 1 1 calc R . . H33B H 0.6736 0.4992 0.0879 0.196 Uiso 1 1 calc R . . H33C H 0.8205 0.5865 0.1254 0.196 Uiso 1 1 calc R . . O12 O 0.8500(5) 0.4808(5) 0.4461(3) 0.0609(14) Uani 1 1 d . . . H12A H 0.9038 0.4825 0.4139 0.091 Uiso 1 1 calc R . . C34 C 0.8071(7) 0.3607(7) 0.4603(4) 0.058(2) Uani 1 1 d . . . H34A H 0.7845 0.2892 0.4072 0.087 Uiso 1 1 calc R . . H34B H 0.7325 0.3509 0.4881 0.087 Uiso 1 1 calc R . . H34C H 0.8750 0.3596 0.4954 0.087 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 0.0236(3) 0.0336(3) 0.0265(3) 0.0061(2) 0.0019(2) 0.0057(2) Ru2 0.0306(3) 0.0339(3) 0.0283(3) 0.0079(2) 0.0036(2) 0.0129(2) Co1 0.0259(4) 0.0329(5) 0.0276(4) 0.0056(4) 0.0012(3) 0.0109(4) O1 0.024(2) 0.052(3) 0.036(2) 0.006(2) -0.0055(18) 0.014(2) O2 0.037(2) 0.027(2) 0.036(2) 0.0086(19) 0.0011(19) 0.005(2) O3 0.057(3) 0.042(3) 0.043(3) 0.020(2) 0.013(2) 0.026(2) O4 0.037(3) 0.037(3) 0.042(3) 0.006(2) 0.010(2) 0.010(2) O5 0.025(2) 0.031(2) 0.031(2) 0.0109(18) 0.0052(17) 0.0095(19) O6 0.029(2) 0.046(3) 0.032(2) 0.007(2) 0.0029(18) 0.007(2) O7 0.049(3) 0.045(3) 0.039(3) 0.013(2) 0.010(2) 0.020(2) O8 0.040(3) 0.045(3) 0.034(2) 0.003(2) 0.0010(19) 0.022(2) N1 0.025(2) 0.031(3) 0.028(3) 0.005(2) 0.001(2) 0.012(2) N2 0.035(3) 0.068(4) 0.027(3) 0.007(3) 0.002(2) 0.023(3) N3 0.035(3) 0.040(3) 0.046(4) 0.017(3) 0.009(3) 0.018(3) N4 0.039(3) 0.074(4) 0.031(3) 0.004(3) 0.002(3) 0.030(3) N5 0.033(2) 0.042(4) 0.050(3) 0.007(3) 0.001(2) 0.0005(14) N6 0.040(3) 0.071(4) 0.052(4) 0.020(3) 0.004(3) 0.027(4) C1 0.032(4) 0.047(4) 0.023(3) 0.007(3) 0.004(3) 0.019(3) C2 0.040(4) 0.045(4) 0.039(4) 0.011(3) 0.005(3) 0.019(3) C3 0.039(4) 0.081(6) 0.046(4) 0.024(4) 0.005(3) 0.037(4) C4 0.023(4) 0.075(6) 0.042(4) 0.006(4) 0.004(3) 0.009(4) C5 0.049(5) 0.048(5) 0.041(4) 0.008(3) 0.018(3) 0.012(4) C6 0.043(4) 0.056(5) 0.023(3) 0.008(3) 0.013(3) 0.016(3) C7 0.074(6) 0.065(6) 0.045(4) 0.023(4) 0.019(4) 0.038(4) C8 0.048(4) 0.036(4) 0.036(4) 0.012(3) 0.004(3) 0.006(3) C9 0.063(5) 0.042(5) 0.049(4) 0.016(4) -0.008(4) -0.013(4) C10 0.129(9) 0.029(4) 0.061(5) 0.022(4) -0.008(5) 0.009(5) C11 0.099(7) 0.042(5) 0.051(5) 0.016(4) -0.008(4) 0.031(5) C12 0.045(4) 0.050(5) 0.040(4) 0.013(3) -0.001(3) 0.017(4) C13 0.038(4) 0.033(4) 0.023(3) 0.006(3) 0.002(3) 0.012(3) C14 0.061(5) 0.039(4) 0.035(4) 0.015(3) 0.011(3) 0.021(4) C15 0.055(5) 0.038(4) 0.059(5) 0.021(4) 0.010(4) 0.021(4) C16 0.081(6) 0.046(5) 0.071(5) 0.025(4) 0.010(5) 0.034(5) C17 0.061(6) 0.085(7) 0.074(6) 0.025(5) 0.001(4) 0.044(5) C18 0.061(5) 0.054(5) 0.061(5) 0.014(4) 0.002(4) 0.019(4) C19 0.067(5) 0.065(4) 0.033(4) 0.014(4) 0.018(4) 0.029(5) C20 0.095(7) 0.051(4) 0.044(4) 0.013(4) 0.023(5) 0.019(5) C21 0.058(5) 0.055(4) 0.029(3) 0.009(3) 0.013(3) 0.024(4) C22 0.055(5) 0.078(6) 0.037(4) 0.010(4) 0.007(3) 0.038(5) C23 0.049(5) 0.055(5) 0.057(5) 0.009(4) 0.004(4) 0.012(4) C24 0.054(5) 0.039(4) 0.063(5) 0.014(4) 0.019(4) 0.010(4) C25 0.047(4) 0.040(4) 0.055(4) 0.016(3) 0.012(3) 0.017(4) C26 0.044(4) 0.032(4) 0.033(3) 0.007(3) 0.006(3) 0.009(3) C27 0.035(4) 0.032(4) 0.036(3) 0.013(3) 0.001(3) 0.007(3) C28 0.040(4) 0.083(6) 0.039(4) 0.010(4) 0.013(3) 0.007(4) C29 0.093(7) 0.063(6) 0.055(5) 0.027(4) 0.033(5) 0.037(5) C30 0.060(5) 0.074(6) 0.049(4) 0.020(4) 0.009(4) 0.043(5) O9 0.069(4) 0.054(3) 0.055(3) 0.022(3) 0.018(3) 0.036(3) C31 0.074(6) 0.052(5) 0.049(5) 0.016(4) 0.003(4) 0.015(4) O10 0.064(4) 0.065(4) 0.117(5) 0.035(4) 0.011(4) 0.010(3) O11 0.110(6) 0.073(5) 0.102(5) 0.019(4) 0.040(5) -0.021(4) C33 0.160(12) 0.094(9) 0.116(10) 0.037(8) 0.080(9) 0.023(9) O12 0.066(4) 0.050(3) 0.052(3) 0.005(3) 0.020(3) 0.019(3) C34 0.058(5) 0.061(5) 0.045(4) 0.010(4) 0.004(4) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.742(4) . ? Ru1 N5 1.987(5) . ? Ru1 O1 2.017(4) . ? Ru1 O2 2.023(4) . ? Ru1 O6 2.059(4) . ? Ru1 O5 2.066(4) . ? Ru2 N1 1.728(4) . ? Ru2 O4 2.009(4) . ? Ru2 N6 2.011(6) . ? Ru2 O3 2.021(4) . ? Ru2 N2 2.111(5) . ? Ru2 O7 2.166(4) . ? Co1 O6 1.994(4) 2_777 ? Co1 N4 2.088(5) . ? Co1 O5 2.108(4) 2_777 ? Co1 O5 2.114(4) . ? Co1 O8 2.147(4) . ? Co1 O2 2.165(4) . ? O1 C1 1.348(7) . ? O2 C13 1.347(7) . ? O3 C14 1.344(8) . ? O4 C26 1.340(8) . ? O5 C27 1.445(7) . ? O5 Co1 2.108(4) 2_777 ? O6 C28 1.418(8) . ? O6 Co1 1.994(4) 2_777 ? O7 C29 1.418(8) . ? O8 C30 1.455(8) . ? N2 N3 1.201(7) . ? N3 N4 1.140(7) . ? N5 C7 1.211(9) . ? N5 C6 1.505(9) . ? N6 C20 1.169(10) . ? N6 C19 1.531(10) . ? C1 C2 1.393(9) . ? C1 C6 1.406(9) . ? C2 C3 1.371(9) . ? C3 C4 1.387(11) . ? C4 C5 1.372(10) . ? C5 C6 1.368(9) . ? C7 C8 1.432(10) . ? C8 C13 1.410(9) . ? C8 C9 1.419(9) . ? C9 C10 1.372(12) . ? C10 C11 1.366(12) . ? C11 C12 1.361(10) . ? C12 C13 1.405(9) . ? C14 C19 1.389(10) . ? C14 C15 1.393(9) . ? C15 C16 1.367(10) . ? C16 C17 1.400(11) . ? C17 C18 1.365(11) . ? C18 C19 1.379(11) . ? C20 C21 1.454(10) . ? C21 C22 1.405(10) . ? C21 C26 1.415(10) . ? C22 C23 1.359(11) . ? C23 C24 1.369(11) . ? C24 C25 1.363(10) . ? C25 C26 1.397(9) . ? O9 C31 1.404(8) . ? O10 C32 1.328(15) . ? O11 C33 1.374(10) . ? O12 C34 1.429(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N5 90.7(2) . . ? N1 Ru1 O1 93.04(19) . . ? N5 Ru1 O1 82.2(2) . . ? N1 Ru1 O2 95.39(19) . . ? N5 Ru1 O2 98.0(2) . . ? O1 Ru1 O2 171.56(16) . . ? N1 Ru1 O6 177.2(2) . . ? N5 Ru1 O6 91.8(2) . . ? O1 Ru1 O6 86.25(17) . . ? O2 Ru1 O6 85.31(17) . . ? N1 Ru1 O5 97.81(19) . . ? N5 Ru1 O5 171.36(19) . . ? O1 Ru1 O5 95.85(16) . . ? O2 Ru1 O5 82.68(16) . . ? O6 Ru1 O5 79.63(15) . . ? N1 Ru2 O4 95.0(2) . . ? N1 Ru2 N6 93.8(2) . . ? O4 Ru2 N6 95.2(2) . . ? N1 Ru2 O3 95.6(2) . . ? O4 Ru2 O3 169.18(17) . . ? N6 Ru2 O3 81.8(2) . . ? N1 Ru2 N2 93.7(2) . . ? O4 Ru2 N2 89.3(2) . . ? N6 Ru2 N2 170.9(2) . . ? O3 Ru2 N2 92.3(2) . . ? N1 Ru2 O7 178.1(2) . . ? O4 Ru2 O7 83.12(17) . . ? N6 Ru2 O7 85.9(2) . . ? O3 Ru2 O7 86.29(17) . . ? N2 Ru2 O7 86.77(18) . . ? O6 Co1 N4 98.1(2) 2_777 . ? O6 Co1 O5 80.11(16) 2_777 2_777 ? N4 Co1 O5 176.6(2) . 2_777 ? O6 Co1 O5 90.27(17) 2_777 . ? N4 Co1 O5 96.73(19) . . ? O5 Co1 O5 80.45(15) 2_777 . ? O6 Co1 O8 87.68(17) 2_777 . ? N4 Co1 O8 92.58(19) . . ? O5 Co1 O8 90.22(15) 2_777 . ? O5 Co1 O8 170.66(15) . . ? O6 Co1 O2 166.96(17) 2_777 . ? N4 Co1 O2 89.5(2) . . ? O5 Co1 O2 91.74(15) 2_777 . ? O5 Co1 O2 78.28(15) . . ? O8 Co1 O2 102.61(17) . . ? C1 O1 Ru1 112.4(4) . . ? C13 O2 Ru1 119.3(4) . . ? C13 O2 Co1 141.6(4) . . ? Ru1 O2 Co1 99.07(17) . . ? C14 O3 Ru2 113.3(4) . . ? C26 O4 Ru2 120.3(4) . . ? C27 O5 Ru1 118.3(3) . . ? C27 O5 Co1 118.7(3) . 2_777 ? Ru1 O5 Co1 97.45(15) . 2_777 ? C27 O5 Co1 119.2(3) . . ? Ru1 O5 Co1 99.42(17) . . ? Co1 O5 Co1 99.55(15) 2_777 . ? C28 O6 Co1 127.6(4) . 2_777 ? C28 O6 Ru1 126.4(4) . . ? Co1 O6 Ru1 101.41(18) 2_777 . ? C29 O7 Ru2 128.0(4) . . ? C30 O8 Co1 121.1(4) . . ? Ru2 N1 Ru1 177.4(3) . . ? N3 N2 Ru2 117.1(4) . . ? N4 N3 N2 175.5(7) . . ? N3 N4 Co1 136.5(5) . . ? C7 N5 C6 124.0(6) . . ? C7 N5 Ru1 122.4(6) . . ? C6 N5 Ru1 113.5(5) . . ? C20 N6 C19 122.3(7) . . ? C20 N6 Ru2 124.8(7) . . ? C19 N6 Ru2 112.9(5) . . ? O1 C1 C2 119.9(6) . . ? O1 C1 C6 121.3(6) . . ? C2 C1 C6 118.8(6) . . ? C3 C2 C1 119.6(7) . . ? C2 C3 C4 121.1(7) . . ? C5 C4 C3 119.5(7) . . ? C6 C5 C4 120.4(7) . . ? C5 C6 C1 120.6(7) . . ? C5 C6 N5 129.5(7) . . ? C1 C6 N5 109.9(6) . . ? N5 C7 C8 126.2(8) . . ? C13 C8 C9 117.3(7) . . ? C13 C8 C7 130.5(7) . . ? C9 C8 C7 112.1(7) . . ? C10 C9 C8 121.0(7) . . ? C11 C10 C9 120.8(7) . . ? C12 C11 C10 120.1(8) . . ? C11 C12 C13 121.3(7) . . ? O2 C13 C12 117.4(6) . . ? O2 C13 C8 123.3(6) . . ? C12 C13 C8 119.4(6) . . ? O3 C14 C19 122.2(7) . . ? O3 C14 C15 119.3(7) . . ? C19 C14 C15 118.4(7) . . ? C16 C15 C14 120.4(7) . . ? C15 C16 C17 120.3(8) . . ? C18 C17 C16 119.7(8) . . ? C17 C18 C19 120.0(8) . . ? C18 C19 C14 121.1(8) . . ? C18 C19 N6 129.2(7) . . ? C14 C19 N6 109.7(7) . . ? N6 C20 C21 126.0(10) . . ? C22 C21 C26 119.2(7) . . ? C22 C21 C20 113.0(7) . . ? C26 C21 C20 127.9(7) . . ? C23 C22 C21 121.3(7) . . ? C22 C23 C24 118.8(8) . . ? C25 C24 C23 122.4(8) . . ? C24 C25 C26 120.3(7) . . ? O4 C26 C25 118.3(6) . . ? O4 C26 C21 123.8(6) . . ? C25 C26 C21 117.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.308 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.154 data_ic14269 _database_code_depnum_ccdc_archive 'CCDC 833816' #TrackingRef '- total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H96 N12 Ni2 O24 Ru4' _chemical_formula_weight 1987.27 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' Ni Ni 0.3393 1.1124 '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 11.4249(6) _cell_length_b 11.8191(5) _cell_length_c 17.1649(7) _cell_angle_alpha 108.293(3) _cell_angle_beta 91.440(3) _cell_angle_gamma 111.629(3) _cell_volume 2019.52(16) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17976 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details ? _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_measurement_device_type 'NONIUS Kappaccd' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17976 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7088 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0928P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7088 _refine_ls_number_parameters 497 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.062 _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 0.80084(5) 0.85869(6) 0.87323(3) 0.03955(19) Uani 1 1 d . . . Ru2 Ru 0.85700(5) 0.77393(6) 0.66988(4) 0.0427(2) Uani 1 1 d U . . Ni1 Ni 1.07785(8) 0.91839(9) 0.95677(5) 0.0400(3) Uani 1 1 d . . . O1 O 0.7040(4) 0.9626(5) 0.8539(3) 0.0519(14) Uani 1 1 d . . . O2 O 0.8925(4) 0.7627(4) 0.9094(3) 0.0452(12) Uani 1 1 d . . . O3 O 0.9190(6) 0.9545(5) 0.6656(3) 0.0601(15) Uani 1 1 d . . . O4 O 0.7929(5) 0.5833(5) 0.6511(3) 0.0558(14) Uani 1 1 d . . . O5 O 0.9721(4) 1.0161(4) 0.9294(3) 0.0401(11) Uani 1 1 d . . . O6 O 0.7713(4) 0.9131(5) 0.9942(3) 0.0474(13) Uani 1 1 d . . . O7 O 0.8855(5) 0.7123(6) 0.5428(3) 0.0580(14) Uani 1 1 d . . . H7 H 0.8719 0.6280 0.5185 0.087 Uiso 1 1 d R . . O8 O 1.1789(4) 0.8309(5) 1.0049(3) 0.0490(13) Uani 1 1 d . . . H8 H 1.2204 0.8901 1.0541 0.073 Uiso 1 1 d R . . N1 N 0.8322(5) 0.8176(5) 0.7713(3) 0.0408(14) Uani 1 1 d . . . N2 N 1.0453(6) 0.7943(8) 0.7039(4) 0.064(2) Uani 1 1 d . . . N3 N 1.0854(6) 0.8294(6) 0.7753(4) 0.0476(15) Uani 1 1 d . . . N4 N 1.1290(6) 0.8633(7) 0.8419(4) 0.062(2) Uani 1 1 d . . . N5 N 0.6292(7) 0.7168(8) 0.8366(4) 0.0623(18) Uani 1 1 d U . . N6 N 0.6896(7) 0.7623(9) 0.6248(4) 0.077(2) Uani 1 1 d U . . C1 C 0.5826(6) 0.8881(8) 0.8187(4) 0.0451(18) Uani 1 1 d . . . C2 C 0.5065(7) 0.9417(8) 0.7903(4) 0.052(2) Uani 1 1 d . . . H2 H 0.5415 1.0308 0.7957 0.063 Uiso 1 1 calc R . . C3 C 0.3811(7) 0.8652(9) 0.7545(5) 0.060(2) Uani 1 1 d . . . H3 H 0.3293 0.9021 0.7365 0.072 Uiso 1 1 calc R . . C4 C 0.3301(7) 0.7341(10) 0.7448(5) 0.067(3) Uani 1 1 d . . . H4 H 0.2437 0.6816 0.7200 0.080 Uiso 1 1 calc R . . C5 C 0.4053(8) 0.6799(9) 0.7712(5) 0.064(2) Uani 1 1 d . . . H5 H 0.3706 0.5905 0.7649 0.077 Uiso 1 1 calc R . . C6 C 0.5294(7) 0.7561(9) 0.8064(5) 0.058(2) Uani 1 1 d U . . C7 C 0.6111(10) 0.6089(11) 0.8368(5) 0.071(3) Uani 1 1 d . . . H7A H 0.5267 0.5454 0.8156 0.085 Uiso 1 1 calc R . . C8 C 0.6984(8) 0.5650(8) 0.8643(5) 0.055(2) Uani 1 1 d . . . C9 C 0.6462(9) 0.4320(9) 0.8543(6) 0.076(3) Uani 1 1 d . . . H9A H 0.5592 0.3814 0.8303 0.091 Uiso 1 1 calc R . . C10 C 0.7159(11) 0.3749(9) 0.8779(6) 0.087(3) Uani 1 1 d . . . H10 H 0.6782 0.2845 0.8687 0.104 Uiso 1 1 calc R . . C11 C 0.8417(11) 0.4458(10) 0.9153(6) 0.081(3) Uani 1 1 d . . . H11 H 0.8890 0.4057 0.9344 0.097 Uiso 1 1 calc R . . C12 C 0.8969(8) 0.5732(8) 0.9245(5) 0.057(2) Uani 1 1 d . . . H12 H 0.9839 0.6208 0.9493 0.068 Uiso 1 1 calc R . . C13 C 0.8305(7) 0.6376(7) 0.8989(4) 0.0459(18) Uani 1 1 d . . . C14 C 0.8279(9) 0.9881(8) 0.6426(5) 0.057(2) Uani 1 1 d . . . C15 C 0.8606(9) 1.1114(8) 0.6403(6) 0.066(2) Uani 1 1 d . . . H15 H 0.9462 1.1734 0.6583 0.080 Uiso 1 1 calc R . . C16 C 0.7682(10) 1.1439(10) 0.6117(6) 0.081(3) Uani 1 1 d . . . H16 H 0.7913 1.2280 0.6085 0.097 Uiso 1 1 calc R . . C17 C 0.6413(10) 1.0555(11) 0.5873(6) 0.083(3) Uani 1 1 d . . . H17 H 0.5779 1.0794 0.5687 0.100 Uiso 1 1 calc R . . C18 C 0.6096(9) 0.9340(10) 0.5906(6) 0.078(3) Uani 1 1 d . . . H18 H 0.5235 0.8730 0.5743 0.093 Uiso 1 1 calc R . . C19 C 0.7006(9) 0.8995(11) 0.6172(5) 0.077(2) Uani 1 1 d U . . C20 C 0.5896(12) 0.6832(11) 0.6071(7) 0.092(3) Uiso 1 1 d U . . H20 H 0.5188 0.6966 0.5879 0.110 Uiso 1 1 calc R . . C21 C 0.5753(8) 0.5585(8) 0.6156(5) 0.057(2) Uani 1 1 d U . . C22 C 0.4454(9) 0.4732(10) 0.5994(5) 0.069(3) Uani 1 1 d . . . H22 H 0.3834 0.5025 0.5853 0.083 Uiso 1 1 calc R . . C23 C 0.4049(9) 0.3535(10) 0.6028(6) 0.076(3) Uani 1 1 d . . . H23 H 0.3167 0.2987 0.5907 0.092 Uiso 1 1 calc R . . C24 C 0.4955(9) 0.3119(9) 0.6244(6) 0.072(3) Uani 1 1 d . . . H24 H 0.4687 0.2278 0.6281 0.086 Uiso 1 1 calc R . . C25 C 0.6221(8) 0.3894(8) 0.6404(5) 0.063(2) Uani 1 1 d . . . H25 H 0.6821 0.3580 0.6546 0.075 Uiso 1 1 calc R . . C26 C 0.6653(7) 0.5127(7) 0.6364(5) 0.0498(19) Uani 1 1 d . . . C27 C 1.0259(7) 1.1053(7) 0.8872(4) 0.0455(18) Uani 1 1 d . . . H27A H 0.9608 1.1322 0.8701 0.068 Uiso 1 1 calc R . . H27B H 1.0563 1.0633 0.8379 0.068 Uiso 1 1 calc R . . H27C H 1.0975 1.1817 0.9244 0.068 Uiso 1 1 calc R . . C28 C 0.6520(7) 0.8762(9) 1.0217(5) 0.065(2) Uani 1 1 d . . . H28A H 0.5910 0.8892 0.9879 0.097 Uiso 1 1 calc R . . H28B H 0.6616 0.9293 1.0801 0.097 Uiso 1 1 calc R . . H28C H 0.6207 0.7844 1.0161 0.097 Uiso 1 1 calc R . . C29 C 0.9532(11) 0.7882(11) 0.4976(6) 0.091(3) Uani 1 1 d . . . H29A H 1.0373 0.8486 0.5300 0.137 Uiso 1 1 calc R . . H29B H 0.9061 0.8373 0.4863 0.137 Uiso 1 1 calc R . . H29C H 0.9636 0.7318 0.4450 0.137 Uiso 1 1 calc R . . C30 C 1.2673(8) 0.7828(9) 0.9582(5) 0.068(3) Uani 1 1 d . . . H30A H 1.3181 0.8457 0.9336 0.103 Uiso 1 1 calc R . . H30B H 1.2186 0.6994 0.9141 0.103 Uiso 1 1 calc R . . H30C H 1.3241 0.7710 0.9960 0.103 Uiso 1 1 calc R . . O9 O 0.9725(7) 0.4789(7) 0.6530(4) 0.0767(18) Uani 1 1 d . . . H9 H 0.9307 0.5245 0.6535 0.115 Uiso 1 1 calc R . . C31 C 1.0016(10) 0.4834(10) 0.7340(6) 0.082(3) Uani 1 1 d . . . H31A H 1.0561 0.4358 0.7340 0.123 Uiso 1 1 calc R . . H31B H 0.9226 0.4434 0.7541 0.123 Uiso 1 1 calc R . . H31C H 1.0466 0.5739 0.7706 0.123 Uiso 1 1 calc R . . O10 O 0.8345(8) 0.8657(8) 0.3024(6) 0.111(3) Uani 1 1 d D . . H10A H 0.9117 0.9168 0.3143 0.167 Uiso 1 1 calc R . . C32 C 0.759(2) 0.936(2) 0.3321(13) 0.219(10) Uiso 1 1 d D . . H32A H 0.7036 0.8971 0.3678 0.329 Uiso 1 1 calc R . . H32B H 0.7055 0.9324 0.2850 0.329 Uiso 1 1 calc R . . H32C H 0.8136 1.0262 0.3641 0.329 Uiso 1 1 calc R . . O11 O 0.7051(9) 0.6156(9) 0.2021(6) 0.137(4) Uani 1 1 d D . . H11A H 0.7712 0.6697 0.2360 0.205 Uiso 1 1 calc R . . C33 C 0.7348(16) 0.5846(14) 0.1228(9) 0.157(7) Uani 1 1 d D . . H33A H 0.7032 0.6273 0.0918 0.236 Uiso 1 1 calc R . . H33B H 0.6948 0.4903 0.0943 0.236 Uiso 1 1 calc R . . H33C H 0.8276 0.6141 0.1258 0.236 Uiso 1 1 calc R . . O12 O 0.8502(6) 0.4810(6) 0.4467(4) 0.0776(19) Uani 1 1 d . . . H12A H 0.9012 0.4814 0.4123 0.116 Uiso 1 1 calc R . . C34 C 0.8066(9) 0.3588(9) 0.4602(6) 0.075(3) Uani 1 1 d . . . H34A H 0.8009 0.2897 0.4086 0.112 Uiso 1 1 calc R . . H34B H 0.7224 0.3403 0.4773 0.112 Uiso 1 1 calc R . . H34C H 0.8669 0.3634 0.5039 0.112 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 0.0241(3) 0.0443(4) 0.0379(3) 0.0057(3) 0.0032(2) 0.0076(2) Ru2 0.0344(3) 0.0473(4) 0.0405(3) 0.0088(3) 0.0046(2) 0.0154(3) Ni1 0.0273(4) 0.0449(5) 0.0397(5) 0.0052(4) 0.0021(4) 0.0138(4) O1 0.031(3) 0.058(3) 0.051(3) 0.000(3) 0.000(2) 0.017(2) O2 0.039(3) 0.040(3) 0.048(3) 0.010(2) 0.005(2) 0.011(2) O3 0.074(4) 0.061(4) 0.059(3) 0.029(3) 0.019(3) 0.034(3) O4 0.049(3) 0.050(3) 0.059(3) 0.010(3) 0.013(3) 0.016(3) O5 0.030(2) 0.043(3) 0.043(3) 0.011(2) 0.006(2) 0.013(2) O6 0.030(2) 0.057(3) 0.038(2) 0.002(2) 0.008(2) 0.011(2) O7 0.062(4) 0.063(4) 0.046(3) 0.013(3) 0.015(3) 0.026(3) O8 0.041(3) 0.060(3) 0.040(3) 0.002(2) -0.002(2) 0.028(2) N1 0.028(3) 0.040(3) 0.049(3) 0.015(3) -0.002(2) 0.009(2) N2 0.034(4) 0.105(6) 0.045(4) 0.015(4) 0.005(3) 0.028(4) N3 0.033(3) 0.055(4) 0.055(4) 0.017(3) 0.008(3) 0.018(3) N4 0.036(4) 0.095(6) 0.042(4) -0.001(4) 0.003(3) 0.035(4) N5 0.053(4) 0.073(5) 0.046(4) 0.009(4) 0.008(3) 0.018(4) N6 0.046(4) 0.122(6) 0.058(4) 0.017(4) 0.000(3) 0.038(5) C1 0.027(4) 0.062(5) 0.034(4) 0.006(4) 0.005(3) 0.013(3) C2 0.048(5) 0.066(5) 0.047(4) 0.015(4) 0.007(4) 0.031(4) C3 0.041(5) 0.084(7) 0.061(5) 0.022(5) 0.005(4) 0.035(5) C4 0.032(4) 0.094(7) 0.050(5) 0.002(5) 0.002(4) 0.017(5) C5 0.053(5) 0.072(6) 0.046(5) 0.007(4) 0.016(4) 0.012(4) C6 0.040(4) 0.077(6) 0.037(4) 0.002(4) 0.010(3) 0.016(4) C7 0.080(7) 0.080(7) 0.055(5) 0.019(5) 0.015(5) 0.038(6) C8 0.056(5) 0.050(5) 0.049(4) 0.011(4) 0.000(4) 0.015(4) C9 0.068(6) 0.062(6) 0.067(6) 0.020(5) -0.015(5) -0.004(5) C10 0.119(9) 0.039(5) 0.074(7) 0.018(5) -0.013(6) 0.006(5) C11 0.110(9) 0.066(6) 0.069(6) 0.023(5) -0.006(6) 0.040(6) C12 0.058(5) 0.061(5) 0.052(5) 0.018(4) 0.001(4) 0.024(4) C13 0.045(4) 0.047(4) 0.036(4) 0.007(3) 0.001(3) 0.014(3) C14 0.070(6) 0.053(5) 0.059(5) 0.025(4) 0.020(4) 0.029(4) C15 0.075(6) 0.055(5) 0.075(6) 0.029(5) 0.011(5) 0.027(5) C16 0.094(8) 0.061(6) 0.097(8) 0.027(6) 0.010(6) 0.041(6) C17 0.072(7) 0.096(8) 0.081(7) 0.020(6) 0.002(5) 0.043(6) C18 0.060(6) 0.072(7) 0.076(6) 0.009(5) 0.013(5) 0.012(5) C19 0.062(6) 0.115(7) 0.048(5) 0.012(5) 0.020(4) 0.041(6) C21 0.068(6) 0.057(5) 0.051(5) 0.021(4) 0.018(4) 0.029(4) C22 0.055(6) 0.089(7) 0.060(5) 0.017(5) 0.012(4) 0.032(5) C23 0.057(6) 0.070(7) 0.063(6) -0.001(5) 0.000(5) 0.003(5) C24 0.068(6) 0.057(6) 0.074(6) 0.010(5) 0.016(5) 0.018(5) C25 0.061(5) 0.049(5) 0.070(6) 0.012(4) 0.015(4) 0.021(4) C26 0.049(5) 0.044(4) 0.045(4) 0.007(4) 0.007(3) 0.013(4) C27 0.041(4) 0.044(4) 0.041(4) 0.011(3) 0.001(3) 0.009(3) C28 0.034(4) 0.078(6) 0.060(5) 0.013(5) 0.017(4) 0.007(4) C29 0.108(9) 0.098(8) 0.069(6) 0.029(6) 0.033(6) 0.040(7) C30 0.057(5) 0.081(6) 0.066(5) 0.007(5) 0.006(4) 0.042(5) O9 0.090(5) 0.073(4) 0.077(4) 0.023(4) 0.022(4) 0.045(4) C31 0.091(8) 0.076(7) 0.071(6) 0.021(5) 0.010(6) 0.027(6) O10 0.082(5) 0.097(6) 0.138(7) 0.049(5) 0.021(5) 0.010(4) O11 0.117(7) 0.095(7) 0.129(7) 0.015(6) 0.043(6) -0.014(5) C33 0.198(18) 0.102(11) 0.143(13) 0.039(10) 0.101(13) 0.028(11) O12 0.075(5) 0.077(4) 0.067(4) 0.005(3) 0.023(3) 0.030(4) C34 0.074(6) 0.072(6) 0.063(6) 0.008(5) 0.012(5) 0.025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.747(6) . ? Ru1 N5 1.976(7) . ? Ru1 O2 2.013(5) . ? Ru1 O1 2.020(5) . ? Ru1 O6 2.048(5) . ? Ru1 O5 2.077(4) . ? Ru2 N1 1.716(6) . ? Ru2 N6 1.985(7) . ? Ru2 O4 2.008(5) . ? Ru2 O3 2.012(6) . ? Ru2 N2 2.120(6) . ? Ru2 O7 2.147(5) . ? Ni1 O6 1.998(5) 2_777 ? Ni1 O5 2.043(5) 2_777 ? Ni1 N4 2.047(6) . ? Ni1 O5 2.087(5) . ? Ni1 O8 2.110(5) . ? Ni1 O2 2.152(5) . ? O1 C1 1.337(8) . ? O2 C13 1.333(9) . ? O3 C14 1.334(10) . ? O4 C26 1.356(9) . ? O5 C27 1.429(8) . ? O5 Ni1 2.043(5) 2_777 ? O6 C28 1.412(8) . ? O6 Ni1 1.998(5) 2_777 ? O7 C29 1.400(12) . ? O8 C30 1.470(8) . ? N2 N3 1.182(9) . ? N3 N4 1.119(8) . ? N5 C7 1.215(11) . ? N5 C6 1.515(11) . ? N6 C20 1.135(13) . ? N6 C19 1.626(14) . ? C1 C6 1.392(12) . ? C1 C2 1.406(10) . ? C2 C3 1.378(11) . ? C3 C4 1.392(13) . ? C4 C5 1.386(12) . ? C5 C6 1.365(11) . ? C7 C8 1.414(12) . ? C8 C9 1.411(12) . ? C8 C13 1.430(11) . ? C9 C10 1.344(14) . ? C10 C11 1.381(14) . ? C11 C12 1.354(13) . ? C12 C13 1.402(11) . ? C14 C15 1.378(12) . ? C14 C19 1.400(13) . ? C15 C16 1.376(12) . ? C16 C17 1.396(14) . ? C17 C18 1.366(14) . ? C18 C19 1.364(14) . ? C20 C21 1.476(14) . ? C21 C26 1.411(11) . ? C21 C22 1.413(12) . ? C22 C23 1.337(14) . ? C23 C24 1.385(13) . ? C24 C25 1.361(12) . ? C25 C26 1.380(11) . ? O9 C31 1.402(11) . ? O10 C32 1.408(14) . ? O11 C33 1.381(12) . ? O12 C34 1.439(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N5 90.2(3) . . ? N1 Ru1 O2 95.1(2) . . ? N5 Ru1 O2 98.1(3) . . ? N1 Ru1 O1 93.2(2) . . ? N5 Ru1 O1 82.0(3) . . ? O2 Ru1 O1 171.78(19) . . ? N1 Ru1 O6 177.7(2) . . ? N5 Ru1 O6 92.1(2) . . ? O2 Ru1 O6 84.7(2) . . ? O1 Ru1 O6 87.1(2) . . ? N1 Ru1 O5 98.6(2) . . ? N5 Ru1 O5 171.1(2) . . ? O2 Ru1 O5 82.27(19) . . ? O1 Ru1 O5 96.33(19) . . ? O6 Ru1 O5 79.10(18) . . ? N1 Ru2 N6 94.2(3) . . ? N1 Ru2 O4 95.0(2) . . ? N6 Ru2 O4 93.7(3) . . ? N1 Ru2 O3 95.4(2) . . ? N6 Ru2 O3 83.2(3) . . ? O4 Ru2 O3 169.4(2) . . ? N1 Ru2 N2 92.7(2) . . ? N6 Ru2 N2 172.0(3) . . ? O4 Ru2 N2 89.9(3) . . ? O3 Ru2 N2 92.0(3) . . ? N1 Ru2 O7 178.0(2) . . ? N6 Ru2 O7 86.0(3) . . ? O4 Ru2 O7 83.0(2) . . ? O3 Ru2 O7 86.7(2) . . ? N2 Ru2 O7 87.3(2) . . ? O6 Ni1 O5 81.09(18) 2_777 2_777 ? O6 Ni1 N4 96.8(3) 2_777 . ? O5 Ni1 N4 176.5(3) 2_777 . ? O6 Ni1 O5 89.9(2) 2_777 . ? O5 Ni1 O5 80.4(2) 2_777 . ? N4 Ni1 O5 96.8(2) . . ? O6 Ni1 O8 88.2(2) 2_777 . ? O5 Ni1 O8 90.07(18) 2_777 . ? N4 Ni1 O8 92.7(2) . . ? O5 Ni1 O8 170.43(18) . . ? O6 Ni1 O2 167.70(19) 2_777 . ? O5 Ni1 O2 92.20(18) 2_777 . ? N4 Ni1 O2 89.3(2) . . ? O5 Ni1 O2 78.81(18) . . ? O8 Ni1 O2 102.2(2) . . ? C1 O1 Ru1 112.6(5) . . ? C13 O2 Ru1 119.9(4) . . ? C13 O2 Ni1 140.9(5) . . ? Ru1 O2 Ni1 99.1(2) . . ? C14 O3 Ru2 115.0(5) . . ? C26 O4 Ru2 118.9(5) . . ? C27 O5 Ni1 119.0(4) . 2_777 ? C27 O5 Ru1 118.3(4) . . ? Ni1 O5 Ru1 97.90(19) 2_777 . ? C27 O5 Ni1 118.6(4) . . ? Ni1 O5 Ni1 99.6(2) 2_777 . ? Ru1 O5 Ni1 99.2(2) . . ? C28 O6 Ni1 127.4(5) . 2_777 ? C28 O6 Ru1 125.8(4) . . ? Ni1 O6 Ru1 100.4(2) 2_777 . ? C29 O7 Ru2 128.6(6) . . ? C30 O8 Ni1 121.3(5) . . ? Ru2 N1 Ru1 177.9(3) . . ? N3 N2 Ru2 118.3(5) . . ? N4 N3 N2 176.6(8) . . ? N3 N4 Ni1 138.0(6) . . ? C7 N5 C6 125.5(8) . . ? C7 N5 Ru1 121.1(7) . . ? C6 N5 Ru1 113.4(6) . . ? C20 N6 C19 115.1(9) . . ? C20 N6 Ru2 133.6(10) . . ? C19 N6 Ru2 111.3(6) . . ? O1 C1 C6 121.7(7) . . ? O1 C1 C2 120.0(7) . . ? C6 C1 C2 118.2(7) . . ? C3 C2 C1 120.0(8) . . ? C2 C3 C4 120.2(8) . . ? C5 C4 C3 120.1(8) . . ? C6 C5 C4 119.4(9) . . ? C5 C6 C1 121.9(9) . . ? C5 C6 N5 128.4(9) . . ? C1 C6 N5 109.7(7) . . ? N5 C7 C8 128.8(10) . . ? C9 C8 C7 114.3(9) . . ? C9 C8 C13 117.5(8) . . ? C7 C8 C13 128.2(8) . . ? C10 C9 C8 122.0(9) . . ? C9 C10 C11 120.8(9) . . ? C12 C11 C10 119.4(9) . . ? C11 C12 C13 122.5(8) . . ? O2 C13 C12 118.7(7) . . ? O2 C13 C8 123.6(7) . . ? C12 C13 C8 117.7(7) . . ? O3 C14 C15 119.2(8) . . ? O3 C14 C19 121.6(8) . . ? C15 C14 C19 119.1(9) . . ? C16 C15 C14 119.4(9) . . ? C15 C16 C17 121.2(10) . . ? C18 C17 C16 118.9(9) . . ? C19 C18 C17 120.6(10) . . ? C18 C19 C14 120.8(11) . . ? C18 C19 N6 130.4(9) . . ? C14 C19 N6 108.8(8) . . ? N6 C20 C21 116.6(12) . . ? C26 C21 C22 117.1(8) . . ? C26 C21 C20 132.1(9) . . ? C22 C21 C20 110.8(8) . . ? C23 C22 C21 123.5(9) . . ? C22 C23 C24 118.1(9) . . ? C25 C24 C23 121.2(10) . . ? C24 C25 C26 121.4(9) . . ? O4 C26 C25 118.2(7) . . ? O4 C26 C21 123.0(7) . . ? C25 C26 C21 118.8(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.298 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.254