data_k1251 _publ_author_name ; Randolph P. Thummel ; _publ_contact_author_address ; Department of Chemistry University of Houston Houston, TX 77204-5003 ; _publ_requested_journal ; Inorganic Chemistry ; _publ_title_name ; A Ru(II) Bis-terpyridine-like Complex that catalyzes water oxidation: the influence of steric strain ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H17 N5 O4 Ru, 2(C H4 O), H2 O' _chemical_formula_sum 'C31 H27 N5 O7 Ru' _chemical_formula_weight 682.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2890(5) _cell_length_b 16.0184(7) _cell_length_c 17.6378(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.315(1) _cell_angle_gamma 90.00 _cell_volume 2828.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8156 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.04 _exptl_crystal_description block _exptl_crystal_colour 'Dark carmine' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details 'SAINT v7.12a' _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (1271 frames at 6 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.30\% in omega and an exposure time of 35 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 8156 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was shown unambiguously to be P2(1)/n. The asymmetric unit consists of one organometallic complex, two methanols, and one solvent water molecule. One of the methanol molecules (O6) was found to be disordered over two slightly different orientations, and the minor component was modeled as an ideal rigid body. This moiety was not stable during the refinement, so finally the atomic positions were fixed in the most chemically reasonable location. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme for key atoms. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Fig. 2 -- Isotropic view of the molecule. Fig. 3 -- Intermolecular hydrogen bonding. Fig. 4 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(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 'Bruker APEX II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 14285 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0109 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5175 _reflns_number_gt 4330 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v6.12 (G.M. Sheldrick, 2001)' _computing_structure_refinement 'SHELXL v6.12 (G.M. Sheldrick, 2001)' _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^ > 4sigma(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^)+(0.0465P)^2^+2.6099P] 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_number_reflns 4975 _refine_ls_number_parameters 399 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _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 Ru Ru 0.660494(17) 0.297610(11) 0.570618(10) 0.02832(8) Uani 1 1 d . . . O1 O 0.56332(17) 0.35589(11) 0.65027(10) 0.0391(4) Uani 1 1 d . . . O2 O 0.4457(3) 0.32648(16) 0.73915(15) 0.0712(7) Uani 1 1 d . . . O3 O 0.75122(19) 0.31499(12) 0.38432(11) 0.0454(4) Uani 1 1 d . . . O4 O 0.9642(2) 0.29352(13) 0.44408(14) 0.0604(6) Uani 1 1 d . . . N1 N 0.5869(2) 0.20215(12) 0.61733(13) 0.0379(5) Uani 1 1 d . . . C2 C 0.5213(3) 0.21429(18) 0.67333(17) 0.0449(6) Uani 1 1 d . . . C3 C 0.4746(3) 0.1457(2) 0.70904(19) 0.0553(8) Uani 1 1 d . . . H3 H 0.4279 0.1541 0.7484 0.066 Uiso 1 1 calc R . . C4 C 0.4979(3) 0.0665(2) 0.6860(2) 0.0627(9) Uani 1 1 d . . . H4 H 0.4656 0.0206 0.7093 0.075 Uiso 1 1 calc R . . C5 C 0.5688(3) 0.05306(19) 0.6284(2) 0.0583(8) Uani 1 1 d . . . C6 C 0.6038(4) -0.0259(2) 0.6000(3) 0.0765(11) Uani 1 1 d . . . H6 H 0.5768 -0.0755 0.6202 0.092 Uiso 1 1 calc R . . C7 C 0.6746(4) -0.0298(2) 0.5450(3) 0.0793(11) Uani 1 1 d . . . H7 H 0.6946 -0.0827 0.5275 0.095 Uiso 1 1 calc R . . C8 C 0.7219(3) 0.04353(18) 0.5111(2) 0.0590(8) Uani 1 1 d . . . C9 C 0.8014(3) 0.04377(19) 0.4559(2) 0.0642(9) Uani 1 1 d . . . H9 H 0.8267 -0.0068 0.4365 0.077 Uiso 1 1 calc R . . C10 C 0.8414(3) 0.11824(19) 0.43087(18) 0.0522(7) Uani 1 1 d . . . H10 H 0.8953 0.1185 0.3945 0.063 Uiso 1 1 calc R . . C11 C 0.8027(3) 0.19469(15) 0.45904(16) 0.0381(6) Uani 1 1 d . . . N12 N 0.7275(2) 0.19773(12) 0.51169(13) 0.0349(5) Uani 1 1 d . . . C13 C 0.6889(3) 0.12185(15) 0.53782(17) 0.0443(6) Uani 1 1 d . . . C14 C 0.6128(3) 0.12449(16) 0.59493(17) 0.0442(6) Uani 1 1 d . . . C15 C 0.5075(3) 0.30514(18) 0.69019(17) 0.0466(7) Uani 1 1 d . . . C16 C 0.8438(2) 0.27559(18) 0.42674(14) 0.0375(6) Uani 1 1 d . . . N17 N 0.50623(18) 0.32978(12) 0.47743(11) 0.0303(4) Uani 1 1 d . . . C18 C 0.3906(2) 0.28838(16) 0.45013(15) 0.0364(5) Uani 1 1 d . . . H18 H 0.3753 0.2385 0.4748 0.044 Uiso 1 1 calc R . . C19 C 0.2941(3) 0.31648(18) 0.38743(16) 0.0430(6) Uani 1 1 d . . . H19 H 0.2146 0.2862 0.3698 0.052 Uiso 1 1 calc R . . C20 C 0.3160(3) 0.38946(18) 0.35123(14) 0.0420(6) Uani 1 1 d . . . H20 H 0.2517 0.4093 0.3082 0.050 Uiso 1 1 calc R . . C21 C 0.4328(2) 0.43329(16) 0.37846(14) 0.0365(5) Uani 1 1 d . . . H21 H 0.4484 0.4836 0.3546 0.044 Uiso 1 1 calc R . . C22 C 0.5273(2) 0.40227(14) 0.44155(13) 0.0297(5) Uani 1 1 d . . . N23 N 0.73154(18) 0.40091(11) 0.53431(10) 0.0275(4) Uani 1 1 d . . . C24 C 0.6544(2) 0.44475(14) 0.47543(13) 0.0288(5) Uani 1 1 d . . . C25 C 0.6970(2) 0.52181(14) 0.45422(14) 0.0343(5) Uani 1 1 d . . . H25 H 0.6443 0.5523 0.4128 0.041 Uiso 1 1 calc R . . C26 C 0.8189(3) 0.55281(15) 0.49540(15) 0.0386(6) Uani 1 1 d . . . H26 H 0.8492 0.6047 0.4816 0.046 Uiso 1 1 calc R . . C27 C 0.8962(2) 0.50799(15) 0.55677(14) 0.0348(5) Uani 1 1 d . . . H27 H 0.9779 0.5295 0.5853 0.042 Uiso 1 1 calc R . . C28 C 0.8507(2) 0.43079(14) 0.57518(13) 0.0305(5) Uani 1 1 d . . . N29 N 0.8417(2) 0.30644(12) 0.64933(12) 0.0330(4) Uani 1 1 d . . . C30 C 0.9159(2) 0.37428(15) 0.63853(13) 0.0324(5) Uani 1 1 d . . . C31 C 1.0436(2) 0.38682(17) 0.68437(15) 0.0414(6) Uani 1 1 d . . . H31 H 1.0943 0.4333 0.6760 0.050 Uiso 1 1 calc R . . C32 C 1.0953(3) 0.3297(2) 0.74257(16) 0.0520(7) Uani 1 1 d . . . H32 H 1.1822 0.3367 0.7734 0.062 Uiso 1 1 calc R . . C33 C 1.0193(3) 0.2634(2) 0.75492(16) 0.0513(7) Uani 1 1 d . . . H33 H 1.0523 0.2253 0.7953 0.062 Uiso 1 1 calc R . . C34 C 0.8939(3) 0.25307(17) 0.70741(15) 0.0420(6) Uani 1 1 d . . . H34 H 0.8427 0.2069 0.7158 0.050 Uiso 1 1 calc R . . O5 O 1.1594(2) 0.18647(16) 0.51485(16) 0.0674(6) Uani 1 1 d D . . H5X H 1.094(3) 0.221(2) 0.4835(18) 0.081 Uiso 1 1 d D . . C35 C 1.1515(4) 0.1958(3) 0.5911(2) 0.0805(12) Uani 1 1 d . . . H35A H 1.1957 0.2471 0.6118 0.113 Uiso 1 1 calc R . . H35B H 1.1949 0.1488 0.6215 0.113 Uiso 1 1 calc R . . H35C H 1.0585 0.1979 0.5938 0.113 Uiso 1 1 calc R . . O6 O 0.4366(5) 0.4840(3) 0.7721(3) 0.1088(14) Uiso 0.70 1 d PD A 1 H6X H 0.427(7) 0.4255(12) 0.759(4) 0.131 Uiso 0.70 1 d PD B 1 C36 C 0.5592(8) 0.4939(5) 0.8203(4) 0.115(2) Uiso 0.70 1 d P A 1 H36A H 0.6226 0.4574 0.8037 0.160 Uiso 0.70 1 calc PR A 1 H36B H 0.5549 0.4799 0.8731 0.160 Uiso 0.70 1 calc PR A 1 H36C H 0.5875 0.5515 0.8184 0.160 Uiso 0.70 1 calc PR A 1 O6' O 0.4147 0.4789 0.7852 0.080 Uiso 0.30 1 d P C 2 H6Y H 0.4377 0.4229 0.7742 0.096 Uiso 0.30 1 d P D 2 C36' C 0.5279 0.5220 0.8221 0.071(4) Uiso 0.30 1 d P C 2 H36D H 0.5753 0.5409 0.7836 0.100 Uiso 0.30 1 d P E 2 H36E H 0.5853 0.4855 0.8592 0.100 Uiso 0.30 1 d P F 2 H36F H 0.5025 0.5698 0.8492 0.100 Uiso 0.30 1 d P G 2 O7 O 0.2045(3) 0.55325(15) 0.69941(16) 0.0730(7) Uani 1 1 d G . . H7B H 0.2861 0.5385 0.7344 0.088 Uiso 1 1 d G . . H7A H 0.2131 0.5991 0.6668 0.088 Uiso 1 1 d G . . 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 Ru 0.02670(12) 0.02372(12) 0.03316(12) 0.00416(7) 0.00403(8) -0.00034(7) O1 0.0398(9) 0.0379(9) 0.0419(9) 0.0077(8) 0.0143(8) 0.0030(7) O2 0.0837(17) 0.0682(15) 0.0786(16) 0.0136(13) 0.0535(14) 0.0045(13) O3 0.0416(10) 0.0440(10) 0.0472(11) -0.0007(8) 0.0029(9) 0.0021(8) O4 0.0343(11) 0.0621(14) 0.0797(16) 0.0068(11) 0.0025(10) -0.0088(9) N1 0.0315(11) 0.0336(12) 0.0449(12) 0.0105(9) 0.0014(9) -0.0026(8) C2 0.0359(14) 0.0493(16) 0.0483(16) 0.0186(12) 0.0073(12) 0.0000(11) C3 0.0441(15) 0.0568(19) 0.0637(18) 0.0283(15) 0.0097(14) -0.0052(14) C4 0.0543(18) 0.0526(19) 0.077(2) 0.0318(17) 0.0073(16) -0.0111(15) C5 0.0540(18) 0.0377(16) 0.077(2) 0.0189(15) 0.0031(16) -0.0064(13) C6 0.087(3) 0.0320(16) 0.109(3) 0.0184(18) 0.020(2) -0.0050(16) C7 0.095(3) 0.0238(15) 0.116(3) 0.0007(18) 0.017(3) 0.0008(16) C8 0.0615(19) 0.0304(15) 0.081(2) -0.0033(14) 0.0074(17) 0.0024(13) C9 0.068(2) 0.0332(16) 0.087(2) -0.0183(15) 0.0087(18) 0.0089(14) C10 0.0484(17) 0.0430(17) 0.0625(19) -0.0160(13) 0.0073(14) 0.0051(12) C11 0.0309(13) 0.0346(14) 0.0432(14) -0.0088(10) -0.0030(11) 0.0018(10) N12 0.0305(10) 0.0266(11) 0.0429(12) -0.0005(8) -0.0010(9) -0.0005(8) C13 0.0425(14) 0.0249(13) 0.0590(17) 0.0019(11) -0.0019(12) 0.0001(10) C14 0.0419(14) 0.0287(13) 0.0561(16) 0.0105(11) -0.0009(12) -0.0039(11) C15 0.0418(15) 0.0523(17) 0.0485(16) 0.0142(13) 0.0160(13) 0.0021(12) C16 0.0353(14) 0.0393(14) 0.0369(13) -0.0121(11) 0.0065(11) -0.0010(10) N17 0.0274(9) 0.0290(10) 0.0345(10) 0.0005(8) 0.0070(8) 0.0012(8) C18 0.0303(13) 0.0376(13) 0.0404(13) -0.0019(10) 0.0060(10) -0.0021(10) C19 0.0322(13) 0.0505(15) 0.0441(15) -0.0083(12) 0.0046(11) -0.0012(11) C20 0.0372(13) 0.0528(16) 0.0328(13) -0.0022(11) 0.0014(10) 0.0105(12) C21 0.0401(13) 0.0378(13) 0.0321(12) 0.0029(10) 0.0093(10) 0.0088(11) C22 0.0312(12) 0.0287(11) 0.0299(11) 0.0003(9) 0.0086(9) 0.0045(9) N23 0.0293(9) 0.0243(9) 0.0300(9) -0.0017(8) 0.0092(8) 0.0007(7) C24 0.0331(12) 0.0257(11) 0.0295(11) -0.0006(9) 0.0111(9) 0.0036(9) C25 0.0428(13) 0.0286(12) 0.0348(12) 0.0040(10) 0.0161(10) 0.0053(10) C26 0.0470(15) 0.0272(12) 0.0488(14) -0.0025(11) 0.0259(12) -0.0052(10) C27 0.0340(12) 0.0313(12) 0.0423(13) -0.0081(10) 0.0153(10) -0.0057(10) C28 0.0307(12) 0.0293(12) 0.0331(12) -0.0062(9) 0.0108(10) -0.0004(9) N29 0.0322(10) 0.0322(11) 0.0337(10) 0.0005(8) 0.0054(8) 0.0028(8) C30 0.0301(11) 0.0340(12) 0.0328(12) -0.0050(10) 0.0067(9) 0.0004(9) C31 0.0331(13) 0.0475(15) 0.0417(14) -0.0104(12) 0.0046(11) -0.0035(11) C32 0.0384(15) 0.069(2) 0.0417(15) -0.0056(14) -0.0052(12) 0.0031(14) C33 0.0450(16) 0.0608(19) 0.0425(15) 0.0106(14) -0.0016(12) 0.0081(14) C34 0.0411(14) 0.0432(15) 0.0389(13) 0.0084(11) 0.0039(11) 0.0051(11) O5 0.0479(13) 0.0738(16) 0.0828(17) -0.0009(13) 0.0196(12) 0.0129(11) C35 0.078(3) 0.081(3) 0.077(3) -0.003(2) 0.005(2) 0.026(2) O7 0.0897(17) 0.0563(14) 0.0866(18) -0.0004(12) 0.0485(15) -0.0161(13) _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 Ru N1 1.969(2) . ? Ru N23 1.9744(18) . ? Ru N29 2.057(2) . ? Ru N17 2.0699(19) . ? Ru N12 2.109(2) . ? Ru O1 2.1194(17) . ? O1 C15 1.293(3) . ? O2 C15 1.233(4) . ? O3 C16 1.240(3) . ? O4 C16 1.239(3) . ? N1 C2 1.333(4) . ? N1 C14 1.350(3) . ? C2 C3 1.404(4) . ? C2 C15 1.499(4) . ? C3 C4 1.370(5) . ? C4 C5 1.398(5) . ? C5 C14 1.409(4) . ? C5 C6 1.436(5) . ? C6 C7 1.342(6) . ? C7 C8 1.452(5) . ? C8 C9 1.408(5) . ? C8 C13 1.409(4) . ? C9 C10 1.368(5) . ? C10 C11 1.413(4) . ? C11 N12 1.339(4) . ? C11 C16 1.515(4) . ? N12 C13 1.390(3) . ? C13 C14 1.412(4) . ? N17 C18 1.350(3) . ? N17 C22 1.364(3) . ? C18 C19 1.381(4) . ? C19 C20 1.375(4) . ? C20 C21 1.379(4) . ? C21 C22 1.390(3) . ? C22 C24 1.473(3) . ? N23 C24 1.350(3) . ? N23 C28 1.358(3) . ? C24 C25 1.389(3) . ? C25 C26 1.388(4) . ? C26 C27 1.387(4) . ? C27 C28 1.387(3) . ? C28 C30 1.474(3) . ? N29 C34 1.347(3) . ? N29 C30 1.366(3) . ? C30 C31 1.390(3) . ? C31 C32 1.386(4) . ? C32 C33 1.366(4) . ? C33 C34 1.377(4) . ? O5 C35 1.374(5) . ? O6 C36 1.358(8) . ? O6' C36' 1.3805 . ? 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 Ru N23 173.35(8) . . ? N1 Ru N29 98.46(8) . . ? N23 Ru N29 79.38(8) . . ? N1 Ru N17 103.12(8) . . ? N23 Ru N17 78.89(7) . . ? N29 Ru N17 158.26(8) . . ? N1 Ru N12 79.52(9) . . ? N23 Ru N12 106.77(8) . . ? N29 Ru N12 92.08(8) . . ? N17 Ru N12 94.33(8) . . ? N1 Ru O1 77.24(8) . . ? N23 Ru O1 96.45(7) . . ? N29 Ru O1 90.85(7) . . ? N17 Ru O1 91.38(7) . . ? N12 Ru O1 156.75(8) . . ? C15 O1 Ru 114.86(17) . . ? C2 N1 C14 121.3(2) . . ? C2 N1 Ru 120.40(18) . . ? C14 N1 Ru 118.18(19) . . ? N1 C2 C3 120.1(3) . . ? N1 C2 C15 112.1(2) . . ? C3 C2 C15 127.8(3) . . ? C4 C3 C2 119.4(3) . . ? C3 C4 C5 120.9(3) . . ? C4 C5 C14 116.8(3) . . ? C4 C5 C6 127.2(3) . . ? C14 C5 C6 115.9(3) . . ? C7 C6 C5 121.1(3) . . ? C6 C7 C8 123.2(3) . . ? C9 C8 C13 116.8(3) . . ? C9 C8 C7 126.1(3) . . ? C13 C8 C7 117.0(3) . . ? C10 C9 C8 119.5(3) . . ? C9 C10 C11 120.8(3) . . ? N12 C11 C10 122.0(3) . . ? N12 C11 C16 119.1(2) . . ? C10 C11 C16 118.9(3) . . ? C11 N12 C13 116.9(2) . . ? C11 N12 Ru 132.53(16) . . ? C13 N12 Ru 110.43(18) . . ? N12 C13 C8 124.0(3) . . ? N12 C13 C14 117.3(2) . . ? C8 C13 C14 118.8(3) . . ? N1 C14 C5 121.4(3) . . ? N1 C14 C13 114.6(2) . . ? C5 C14 C13 124.0(3) . . ? O2 C15 O1 124.9(3) . . ? O2 C15 C2 119.7(3) . . ? O1 C15 C2 115.4(2) . . ? O4 C16 O3 128.1(3) . . ? O4 C16 C11 117.1(2) . . ? O3 C16 C11 114.8(2) . . ? C18 N17 C22 118.3(2) . . ? C18 N17 Ru 127.77(17) . . ? C22 N17 Ru 113.93(15) . . ? N17 C18 C19 122.5(2) . . ? C20 C19 C18 119.0(2) . . ? C19 C20 C21 119.6(2) . . ? C20 C21 C22 119.3(2) . . ? N17 C22 C21 121.3(2) . . ? N17 C22 C24 115.24(19) . . ? C21 C22 C24 123.5(2) . . ? C24 N23 C28 121.59(19) . . ? C24 N23 Ru 119.33(15) . . ? C28 N23 Ru 118.65(15) . . ? N23 C24 C25 120.2(2) . . ? N23 C24 C22 112.42(19) . . ? C25 C24 C22 127.3(2) . . ? C26 C25 C24 118.7(2) . . ? C25 C26 C27 120.7(2) . . ? C26 C27 C28 118.7(2) . . ? N23 C28 C27 120.2(2) . . ? N23 C28 C30 112.6(2) . . ? C27 C28 C30 127.3(2) . . ? C34 N29 C30 118.2(2) . . ? C34 N29 Ru 127.62(17) . . ? C30 N29 Ru 114.15(15) . . ? N29 C30 C31 121.2(2) . . ? N29 C30 C28 115.0(2) . . ? C31 C30 C28 123.8(2) . . ? C32 C31 C30 119.0(3) . . ? C33 C32 C31 119.7(3) . . ? C32 C33 C34 119.1(3) . . ? N29 C34 C33 122.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru O1 C15 1.11(18) . . . . ? N23 Ru O1 C15 -176.78(19) . . . . ? N29 Ru O1 C15 -97.37(19) . . . . ? N17 Ru O1 C15 104.25(19) . . . . ? N12 Ru O1 C15 -0.1(3) . . . . ? N29 Ru N1 C2 86.7(2) . . . . ? N17 Ru N1 C2 -90.7(2) . . . . ? N12 Ru N1 C2 177.2(2) . . . . ? O1 Ru N1 C2 -2.30(19) . . . . ? N29 Ru N1 C14 -88.83(19) . . . . ? N17 Ru N1 C14 93.78(19) . . . . ? N12 Ru N1 C14 1.73(18) . . . . ? O1 Ru N1 C14 -177.8(2) . . . . ? C14 N1 C2 C3 -1.6(4) . . . . ? Ru N1 C2 C3 -176.9(2) . . . . ? C14 N1 C2 C15 178.3(2) . . . . ? Ru N1 C2 C15 2.9(3) . . . . ? N1 C2 C3 C4 0.3(4) . . . . ? C15 C2 C3 C4 -179.5(3) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C14 -1.0(5) . . . . ? C3 C4 C5 C6 178.2(3) . . . . ? C4 C5 C6 C7 -178.9(4) . . . . ? C14 C5 C6 C7 0.2(5) . . . . ? C5 C6 C7 C8 0.7(7) . . . . ? C6 C7 C8 C9 177.0(4) . . . . ? C6 C7 C8 C13 -0.8(6) . . . . ? C13 C8 C9 C10 -0.4(5) . . . . ? C7 C8 C9 C10 -178.2(3) . . . . ? C8 C9 C10 C11 -0.7(5) . . . . ? C9 C10 C11 N12 0.9(4) . . . . ? C9 C10 C11 C16 -177.1(3) . . . . ? C10 C11 N12 C13 0.1(4) . . . . ? C16 C11 N12 C13 178.1(2) . . . . ? C10 C11 N12 Ru 176.12(18) . . . . ? C16 C11 N12 Ru -5.9(3) . . . . ? N1 Ru N12 C11 -177.9(2) . . . . ? N23 Ru N12 C11 -0.1(2) . . . . ? N29 Ru N12 C11 -79.6(2) . . . . ? N17 Ru N12 C11 79.6(2) . . . . ? O1 Ru N12 C11 -176.67(19) . . . . ? N1 Ru N12 C13 -1.63(16) . . . . ? N23 Ru N12 C13 176.12(16) . . . . ? N29 Ru N12 C13 96.59(17) . . . . ? N17 Ru N12 C13 -104.20(17) . . . . ? O1 Ru N12 C13 -0.4(3) . . . . ? C11 N12 C13 C8 -1.3(4) . . . . ? Ru N12 C13 C8 -178.2(2) . . . . ? C11 N12 C13 C14 178.3(2) . . . . ? Ru N12 C13 C14 1.4(3) . . . . ? C9 C8 C13 N12 1.5(4) . . . . ? C7 C8 C13 N12 179.5(3) . . . . ? C9 C8 C13 C14 -178.1(3) . . . . ? C7 C8 C13 C14 -0.2(4) . . . . ? C2 N1 C14 C5 1.5(4) . . . . ? Ru N1 C14 C5 177.0(2) . . . . ? C2 N1 C14 C13 -176.9(2) . . . . ? Ru N1 C14 C13 -1.5(3) . . . . ? C4 C5 C14 N1 -0.2(4) . . . . ? C6 C5 C14 N1 -179.5(3) . . . . ? C4 C5 C14 C13 178.0(3) . . . . ? C6 C5 C14 C13 -1.2(5) . . . . ? N12 C13 C14 N1 -0.1(4) . . . . ? C8 C13 C14 N1 179.6(2) . . . . ? N12 C13 C14 C5 -178.5(2) . . . . ? C8 C13 C14 C5 1.2(4) . . . . ? Ru O1 C15 O2 -179.7(3) . . . . ? Ru O1 C15 C2 0.1(3) . . . . ? N1 C2 C15 O2 177.9(3) . . . . ? C3 C2 C15 O2 -2.2(5) . . . . ? N1 C2 C15 O1 -1.8(4) . . . . ? C3 C2 C15 O1 178.0(3) . . . . ? N12 C11 C16 O4 112.9(3) . . . . ? C10 C11 C16 O4 -69.0(3) . . . . ? N12 C11 C16 O3 -68.5(3) . . . . ? C10 C11 C16 O3 109.5(3) . . . . ? N1 Ru N17 C18 -7.5(2) . . . . ? N23 Ru N17 C18 179.0(2) . . . . ? N29 Ru N17 C18 179.5(2) . . . . ? N12 Ru N17 C18 72.8(2) . . . . ? O1 Ru N17 C18 -84.7(2) . . . . ? N1 Ru N17 C22 171.77(15) . . . . ? N23 Ru N17 C22 -1.74(15) . . . . ? N29 Ru N17 C22 -1.2(3) . . . . ? N12 Ru N17 C22 -108.00(16) . . . . ? O1 Ru N17 C22 94.56(15) . . . . ? C22 N17 C18 C19 0.3(4) . . . . ? Ru N17 C18 C19 179.49(19) . . . . ? N17 C18 C19 C20 0.0(4) . . . . ? C18 C19 C20 C21 -0.5(4) . . . . ? C19 C20 C21 C22 0.8(4) . . . . ? C18 N17 C22 C21 0.0(3) . . . . ? Ru N17 C22 C21 -179.27(17) . . . . ? C18 N17 C22 C24 178.9(2) . . . . ? Ru N17 C22 C24 -0.4(2) . . . . ? C20 C21 C22 N17 -0.6(3) . . . . ? C20 C21 C22 C24 -179.4(2) . . . . ? N29 Ru N23 C24 -175.85(17) . . . . ? N17 Ru N23 C24 3.96(16) . . . . ? N12 Ru N23 C24 95.18(16) . . . . ? O1 Ru N23 C24 -86.19(16) . . . . ? N29 Ru N23 C28 -3.28(16) . . . . ? N17 Ru N23 C28 176.53(17) . . . . ? N12 Ru N23 C28 -92.25(16) . . . . ? O1 Ru N23 C28 86.38(16) . . . . ? C28 N23 C24 C25 1.1(3) . . . . ? Ru N23 C24 C25 173.48(16) . . . . ? C28 N23 C24 C22 -177.54(18) . . . . ? Ru N23 C24 C22 -5.2(2) . . . . ? N17 C22 C24 N23 3.5(3) . . . . ? C21 C22 C24 N23 -177.7(2) . . . . ? N17 C22 C24 C25 -175.1(2) . . . . ? C21 C22 C24 C25 3.7(4) . . . . ? N23 C24 C25 C26 -0.8(3) . . . . ? C22 C24 C25 C26 177.6(2) . . . . ? C24 C25 C26 C27 -0.4(3) . . . . ? C25 C26 C27 C28 1.3(3) . . . . ? C24 N23 C28 C27 -0.2(3) . . . . ? Ru N23 C28 C27 -172.59(16) . . . . ? C24 N23 C28 C30 177.94(19) . . . . ? Ru N23 C28 C30 5.5(2) . . . . ? C26 C27 C28 N23 -1.0(3) . . . . ? C26 C27 C28 C30 -178.8(2) . . . . ? N1 Ru N29 C34 7.9(2) . . . . ? N23 Ru N29 C34 -178.5(2) . . . . ? N17 Ru N29 C34 -179.0(2) . . . . ? N12 Ru N29 C34 -71.8(2) . . . . ? O1 Ru N29 C34 85.1(2) . . . . ? N1 Ru N29 C30 -173.52(16) . . . . ? N23 Ru N29 C30 0.11(15) . . . . ? N17 Ru N29 C30 -0.4(3) . . . . ? N12 Ru N29 C30 106.78(16) . . . . ? O1 Ru N29 C30 -96.29(16) . . . . ? C34 N29 C30 C31 2.1(3) . . . . ? Ru N29 C30 C31 -176.64(18) . . . . ? C34 N29 C30 C28 -178.6(2) . . . . ? Ru N29 C30 C28 2.7(2) . . . . ? N23 C28 C30 N29 -5.3(3) . . . . ? C27 C28 C30 N29 172.7(2) . . . . ? N23 C28 C30 C31 174.1(2) . . . . ? C27 C28 C30 C31 -8.0(4) . . . . ? N29 C30 C31 C32 -0.8(4) . . . . ? C28 C30 C31 C32 179.9(2) . . . . ? C30 C31 C32 C33 -1.3(4) . . . . ? C31 C32 C33 C34 2.1(5) . . . . ? C30 N29 C34 C33 -1.3(4) . . . . ? Ru N29 C34 C33 177.2(2) . . . . ? C32 C33 C34 N29 -0.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5X O4 0.944(10) 1.787(13) 2.716(3) 168(4) . O6 H6X O2 0.963(10) 1.646(19) 2.595(6) 168(7) . O6' H6Y O2 0.96 1.672(3) 2.616(3) 166.95(9) . O7 H7B O6 0.95 1.77 2.677(6) 158.9 . O7 H7B O6' 0.95 1.71 2.622(3) 160.3 . O7 H7A O3 0.95 1.73 2.674(3) 172.5 3_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.620 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.057 #===END data_k1338cu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 N6 Ru 2+, 2 (F6 P -), C7 H8, C3 H6 O' _chemical_formula_sum 'C46 H38 F12 N6 O P2 Ru' _chemical_formula_weight 1081.83 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' 'F' 'F' 0.0727 0.0534 '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' 'Ru' 'Ru' 0.0552 3.2960 '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 8.8235(2) _cell_length_b 13.1861(3) _cell_length_c 18.6756(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.768(1) _cell_angle_gamma 90.00 _cell_volume 2168.16(8) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8093 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 66.58 _exptl_crystal_description plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 4.496 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SAINT v7.12A' _publ_section_experimental ; All measurements were made with a Bruker DUO platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (2713 frames at 4 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.50\% in omega and an exposure time of 15 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 8093 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was shown to be P2(1) or P2(1)/m. The refinement showed heavy disorder in almost every molecule in the asymmetric unit. One of the PF6 anions, the acetone solvent, and the toluene solvent were found to occupy two slightly different postions, and these were treated by use of rigid body models. The main ligand of the cation was also found to be disordered such that the opposite ends exchange places. Since there was no appropriate rigid model to use due the the twisting of this moiety, distance constraints had to be used which forced homologous bonds to have essentially the same length. The two separate orientations refined to occupancies of approximately 75%:25%. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme. Thermal ellipsoids are 60% equiprobability envelopes, with hydrogens omitted. Only one orientation of the main cation ligand is shown. Fig. 2 -- Isotropic view of the molecule. Fig. 3 -- View of the disorder in the main ligand. Fig. 4 -- View down the N12-Ru bond showing the twist of the main ligand. Fig. 5 -- Packing of the molecules in the unit cell. Only one orientation of each disordered group is shown at any site. ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II DUO CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 14218 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 66.58 _reflns_number_total 6066 _reflns_number_gt 5881 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v6.12 (G.M. Sheldrick, 2001)' _computing_structure_refinement 'SHELXL v6.12 (G.M. Sheldrick, 2001)' _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^ > 4sigma(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^)+(0.0413P)^2^+4.3042P] 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 noref _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.037(9) _refine_ls_number_reflns 6066 _refine_ls_number_parameters 583 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 Ru Ru 0.43873(3) 0.50212(7) 0.278306(13) 0.01372(9) Uani 1 1 d D . . N1 N 0.5450(7) 0.4986(7) 0.3801(2) 0.0129(12) Uani 0.75 1 d PD A 1 C2 C 0.5864(17) 0.5750(7) 0.4226(9) 0.020(3) Uani 0.75 1 d PD A 1 H2 H 0.5548 0.6416 0.4091 0.024 Uiso 0.75 1 calc PR A 1 C3 C 0.675(3) 0.5619(9) 0.4870(10) 0.024(2) Uani 0.75 1 d PD A 1 H3 H 0.7072 0.6189 0.5151 0.029 Uiso 0.75 1 calc PR A 1 C4 C 0.7156(14) 0.4655(7) 0.5088(6) 0.0232(19) Uani 0.75 1 d PD A 1 H4 H 0.7747 0.4555 0.5526 0.028 Uiso 0.75 1 calc PR A 1 C5 C 0.6692(17) 0.3817(7) 0.4662(6) 0.0214(14) Uani 0.75 1 d PD A 1 C6 C 0.6995(8) 0.2792(5) 0.4849(4) 0.0263(15) Uani 0.75 1 d PD A 1 H6 H 0.7618 0.2641 0.5270 0.032 Uiso 0.75 1 calc PR A 1 C7 C 0.6414(8) 0.2029(5) 0.4440(4) 0.0237(14) Uani 0.75 1 d PD A 1 H7 H 0.6617 0.1349 0.4585 0.028 Uiso 0.75 1 calc PR A 1 C8 C 0.5501(7) 0.2211(5) 0.3794(3) 0.0232(13) Uani 0.75 1 d PD A 1 C9 C 0.4869(8) 0.1450(5) 0.3333(4) 0.0291(15) Uani 0.75 1 d PD A 1 H9 H 0.5054 0.0755 0.3441 0.035 Uiso 0.75 1 calc PR A 1 C10 C 0.3993(9) 0.1712(5) 0.2732(4) 0.0234(15) Uani 0.75 1 d PD A 1 H10 H 0.3579 0.1193 0.2425 0.028 Uiso 0.75 1 calc PR A 1 C11 C 0.3684(7) 0.2749(5) 0.2553(3) 0.0204(12) Uani 0.75 1 d PD A 1 N12 N 0.4348(6) 0.3476(5) 0.2960(3) 0.0186(12) Uani 0.75 1 d PD A 1 C13 C 0.5206(7) 0.3210(5) 0.3584(3) 0.0179(12) Uani 0.75 1 d PD A 1 C14 C 0.582(2) 0.4017(6) 0.4030(7) 0.0185(17) Uani 0.75 1 d PD A 1 C15 C 0.2643(7) 0.2992(5) 0.1918(3) 0.0236(13) Uani 0.75 1 d PD A 1 C16 C 0.1646(8) 0.2228(6) 0.1671(4) 0.0237(15) Uani 0.75 1 d PD A 1 H16 H 0.1610 0.1624 0.1947 0.028 Uiso 0.75 1 calc PR A 1 C17 C 0.0710(8) 0.2294(6) 0.1053(4) 0.0318(15) Uani 0.75 1 d PD A 1 H17 H 0.0001 0.1769 0.0931 0.038 Uiso 0.75 1 calc PR A 1 C18 C 0.0808(8) 0.3120(5) 0.0616(4) 0.0279(15) Uani 0.75 1 d PD A 1 H18 H 0.0247 0.3138 0.0164 0.033 Uiso 0.75 1 calc PR A 1 C19 C 0.1754(11) 0.3957(7) 0.0839(5) 0.024(2) Uani 0.75 1 d PD A 1 C20 C 0.1795(16) 0.4819(8) 0.0400(5) 0.025(3) Uani 0.75 1 d PD A 1 H20 H 0.1219 0.4836 -0.0047 0.030 Uiso 0.75 1 calc PR A 1 C21 C 0.265(4) 0.5620(15) 0.0613(8) 0.0289(17) Uani 0.75 1 d PD A 1 H21 H 0.2726 0.6193 0.0309 0.035 Uiso 0.75 1 calc PR A 1 C22 C 0.3420(14) 0.5597(6) 0.1288(5) 0.022(2) Uani 0.75 1 d PD A 1 H22 H 0.4000 0.6176 0.1438 0.027 Uiso 0.75 1 calc PR A 1 N23 N 0.3392(15) 0.4795(4) 0.1745(4) 0.0196(14) Uani 0.75 1 d PD A 1 C24 C 0.2652(15) 0.3926(6) 0.1513(5) 0.0213(14) Uani 0.75 1 d PD A 1 N1' N 0.345(5) 0.5040(13) 0.1745(11) 0.0225(13) Uiso 0.25 1 d PD A 2 C2' C 0.328(6) 0.5797(15) 0.1284(14) 0.0225(13) Uiso 0.25 1 d PD A 2 H2' H 0.3608 0.6456 0.1430 0.027 Uiso 0.25 1 calc PR A 2 C3' C 0.264(12) 0.566(3) 0.058(2) 0.0225(13) Uiso 0.25 1 d PD A 2 H3' H 0.2645 0.6195 0.0244 0.027 Uiso 0.25 1 calc PR A 2 C4' C 0.199(7) 0.474(2) 0.0397(14) 0.0225(13) Uiso 0.25 1 d PD A 2 H4' H 0.1532 0.4640 -0.0072 0.027 Uiso 0.25 1 calc PR A 2 C5' C 0.202(5) 0.3945(18) 0.0900(13) 0.0225(13) Uiso 0.25 1 d PD A 2 C6' C 0.128(2) 0.2997(12) 0.0789(8) 0.0225(13) Uiso 0.25 1 d PD A 2 H6' H 0.0674 0.2882 0.0358 0.027 Uiso 0.25 1 calc PR A 2 C7' C 0.144(2) 0.2260(10) 0.1287(8) 0.0225(13) Uiso 0.25 1 d PD A 2 H7' H 0.0897 0.1642 0.1206 0.027 Uiso 0.25 1 calc PR A 2 C8' C 0.238(2) 0.2374(9) 0.1930(7) 0.0225(13) Uiso 0.25 1 d PD A 2 C9' C 0.2682(17) 0.1623(9) 0.2461(7) 0.0225(13) Uiso 0.25 1 d PD A 2 H9' H 0.2201 0.0980 0.2409 0.027 Uiso 0.25 1 calc PR A 2 C10' C 0.365(3) 0.1808(10) 0.3047(9) 0.0225(13) Uiso 0.25 1 d PD A 2 H10' H 0.3900 0.1275 0.3377 0.027 Uiso 0.25 1 calc PR A 2 C11' C 0.4297(17) 0.2791(8) 0.3171(7) 0.0225(13) Uiso 0.25 1 d PD A 2 N12' N 0.398(2) 0.3512(6) 0.2685(6) 0.0225(13) Uiso 0.25 1 d PD A 2 C13' C 0.303(2) 0.3323(9) 0.2079(7) 0.0225(13) Uiso 0.25 1 d PD A 2 C14' C 0.278(5) 0.4125(14) 0.1566(14) 0.0225(13) Uiso 0.25 1 d PD A 2 C15' C 0.547(2) 0.2957(9) 0.3769(9) 0.0225(13) Uiso 0.25 1 d PD A 2 C16' C 0.621(2) 0.2100(9) 0.4056(9) 0.0225(13) Uiso 0.25 1 d PD A 2 H16' H 0.6035 0.1471 0.3817 0.027 Uiso 0.25 1 calc PR A 2 C17' C 0.718(2) 0.2112(11) 0.4665(8) 0.0225(13) Uiso 0.25 1 d PD A 2 H17' H 0.7596 0.1495 0.4854 0.027 Uiso 0.25 1 calc PR A 2 C18' C 0.755(2) 0.3012(12) 0.4997(9) 0.0225(13) Uiso 0.25 1 d PD A 2 H18' H 0.8286 0.3030 0.5390 0.027 Uiso 0.25 1 calc PR A 2 C19' C 0.681(5) 0.3926(14) 0.4750(19) 0.0225(13) Uiso 0.25 1 d PD A 2 C20' C 0.726(4) 0.4851(14) 0.5072(17) 0.0225(13) Uiso 0.25 1 d PD A 2 H20' H 0.8040 0.4866 0.5445 0.027 Uiso 0.25 1 calc PR A 2 C21' C 0.657(8) 0.571(2) 0.485(3) 0.0225(13) Uiso 0.25 1 d PD A 2 H21' H 0.6703 0.6321 0.5119 0.027 Uiso 0.25 1 calc PR A 2 C22' C 0.565(7) 0.5698(14) 0.421(3) 0.0225(13) Uiso 0.25 1 d PD A 2 H22' H 0.5279 0.6326 0.4023 0.027 Uiso 0.25 1 calc PR A 2 N23' N 0.526(3) 0.4837(9) 0.3846(7) 0.0225(13) Uiso 0.25 1 d PD A 2 C24' C 0.585(7) 0.3928(11) 0.409(3) 0.0225(13) Uiso 0.25 1 d PD A 2 N25 N 0.2329(4) 0.5448(3) 0.31642(19) 0.0190(8) Uani 1 1 d . A . C26 C 0.1227(5) 0.4849(5) 0.3383(2) 0.0253(13) Uani 1 1 d . . . H26 H 0.1352 0.4135 0.3354 0.030 Uiso 1 1 calc R A . C27 C -0.0083(5) 0.5225(5) 0.3648(3) 0.0334(17) Uani 1 1 d . A . H27 H -0.0838 0.4776 0.3802 0.040 Uiso 1 1 calc R . . C28 C -0.0286(6) 0.6271(5) 0.3686(3) 0.0328(13) Uani 1 1 d . . . H28 H -0.1178 0.6547 0.3869 0.039 Uiso 1 1 calc R A . C29 C 0.0837(6) 0.6902(4) 0.3452(3) 0.0285(11) Uani 1 1 d . A . H29 H 0.0715 0.7618 0.3462 0.034 Uiso 1 1 calc R . . C30 C 0.2151(5) 0.6475(4) 0.3202(2) 0.0228(10) Uani 1 1 d . . . N31 N 0.4575(5) 0.6514(4) 0.2739(2) 0.0191(10) Uani 1 1 d . A . C32 C 0.3429(5) 0.7078(4) 0.2970(2) 0.0203(10) Uani 1 1 d . A . C33 C 0.3583(7) 0.8126(4) 0.2981(3) 0.0273(12) Uani 1 1 d . . . H33 H 0.2793 0.8538 0.3144 0.033 Uiso 1 1 calc R A . C34 C 0.4898(7) 0.8572(4) 0.2753(3) 0.0343(12) Uani 1 1 d . A . H34 H 0.5006 0.9289 0.2758 0.041 Uiso 1 1 calc R . . C35 C 0.6064(6) 0.7956(4) 0.2516(3) 0.0252(10) Uani 1 1 d . . . H35 H 0.6973 0.8246 0.2362 0.030 Uiso 1 1 calc R A . C36 C 0.5857(5) 0.6916(4) 0.2512(2) 0.0216(9) Uani 1 1 d . A . N37 N 0.6498(4) 0.5161(4) 0.23683(18) 0.0192(9) Uani 1 1 d . A . C38 C 0.6925(5) 0.6151(4) 0.2281(2) 0.0204(9) Uani 1 1 d . . . C39 C 0.8288(5) 0.6379(4) 0.1977(3) 0.0289(11) Uani 1 1 d . A . H39 H 0.8578 0.7065 0.1913 0.035 Uiso 1 1 calc R . . C40 C 0.9218(6) 0.5600(5) 0.1768(3) 0.0330(14) Uani 1 1 d . . . H40 H 1.0143 0.5745 0.1556 0.040 Uiso 1 1 calc R A . C41 C 0.8784(6) 0.4619(5) 0.1873(3) 0.0300(13) Uani 1 1 d . A . H41 H 0.9416 0.4074 0.1745 0.036 Uiso 1 1 calc R . . C42 C 0.7401(5) 0.4425(4) 0.2171(3) 0.0247(10) Uani 1 1 d . . . H42 H 0.7100 0.3741 0.2234 0.030 Uiso 1 1 calc R A . P1 P 0.07344(17) 0.89615(14) 0.14636(8) 0.0408(4) Uani 1 1 d . . . F1 F -0.0706(5) 0.8381(4) 0.1111(2) 0.0679(13) Uani 1 1 d . . . F2 F 0.2129(4) 0.9581(3) 0.1835(2) 0.0626(11) Uani 1 1 d . . . F3 F 0.1317(4) 0.9184(4) 0.0697(2) 0.0686(14) Uani 1 1 d . . . F4 F 0.0138(5) 0.8761(4) 0.22422(19) 0.0581(10) Uani 1 1 d . . . F5 F -0.0218(4) 0.9990(5) 0.1391(2) 0.0684(10) Uani 1 1 d . . . F6 F 0.1683(7) 0.7958(4) 0.1525(3) 0.0736(15) Uani 1 1 d . . . P2 P 0.78674(18) 0.88734(15) 0.45554(9) 0.0268(3) Uiso 0.72 1 d PG B 1 F7 F 0.6990(3) 0.78614(19) 0.43342(18) 0.0556(6) Uiso 0.72 1 d PG B 1 F8 F 0.8745(3) 0.98856(19) 0.47765(17) 0.0556(6) Uiso 0.72 1 d PG B 1 F9 F 0.6442(3) 0.9519(2) 0.42660(17) 0.0556(6) Uiso 0.72 1 d PG B 1 F10 F 0.9293(3) 0.8228(2) 0.48448(17) 0.0556(6) Uiso 0.72 1 d PG B 1 F11 F 0.8525(3) 0.8922(3) 0.37863(11) 0.0556(6) Uiso 0.72 1 d PG B 1 F12 F 0.7210(3) 0.8825(3) 0.53242(11) 0.0556(6) Uiso 0.72 1 d PG B 1 P2' P 0.7633(5) 0.8855(4) 0.4567(2) 0.0268(3) Uiso 0.28 1 d PG C 2 F7' F 0.6186(7) 0.8143(6) 0.4487(5) 0.0576(15) Uiso 0.28 1 d PG C 2 F8' F 0.9080(7) 0.9567(6) 0.4646(5) 0.0576(15) Uiso 0.28 1 d PG C 2 F9' F 0.6824(10) 0.9639(6) 0.4023(4) 0.0576(15) Uiso 0.28 1 d PG C 2 F10' F 0.8442(10) 0.8071(6) 0.5109(4) 0.0576(15) Uiso 0.28 1 d PG C 2 F11' F 0.8329(9) 0.8287(6) 0.3916(4) 0.0576(15) Uiso 0.28 1 d PG C 2 F12' F 0.6936(9) 0.9423(7) 0.5217(4) 0.0576(15) Uiso 0.28 1 d PG C 2 O1 O 0.9090(7) 0.2779(4) 0.3045(4) 0.0614(12) Uiso 0.72 1 d PG D 1 C43 C 0.9342(6) 0.1886(4) 0.3216(3) 0.0614(12) Uiso 0.72 1 d PG D 1 C44 C 0.8515(11) 0.1062(5) 0.2826(5) 0.0614(12) Uiso 0.72 1 d PG D 1 H44A H 0.7831 0.1344 0.2460 0.092 Uiso 0.72 1 d PG D 1 H44B H 0.9223 0.0627 0.2611 0.092 Uiso 0.72 1 d PG D 1 H44C H 0.7954 0.0680 0.3154 0.092 Uiso 0.72 1 d PG D 1 C45 C 1.0470(10) 0.1645(6) 0.3809(4) 0.0614(12) Uiso 0.72 1 d PG D 1 H45A H 1.0900 0.2260 0.4004 0.092 Uiso 0.72 1 d PG D 1 H45B H 0.9986 0.1286 0.4177 0.092 Uiso 0.72 1 d PG D 1 H45C H 1.1255 0.1233 0.3634 0.092 Uiso 0.72 1 d PG D 1 O1' O 0.881(2) 0.2418(12) 0.2733(10) 0.067(3) Uiso 0.28 1 d PG E 2 C43' C 0.8827(15) 0.1517(12) 0.2916(7) 0.067(3) Uiso 0.28 1 d PG E 2 C44' C 0.758(2) 0.0837(16) 0.2659(14) 0.067(3) Uiso 0.28 1 d PG E 2 H44D H 0.6859 0.1210 0.2358 0.100 Uiso 0.28 1 d PG E 2 H44E H 0.7982 0.0293 0.2391 0.100 Uiso 0.28 1 d PG E 2 H44F H 0.7094 0.0569 0.3060 0.100 Uiso 0.28 1 d PG E 2 C45' C 1.009(2) 0.1122(17) 0.3392(13) 0.067(3) Uiso 0.28 1 d PG E 2 H45D H 1.0797 0.1655 0.3510 0.100 Uiso 0.28 1 d PG E 2 H45E H 0.9702 0.0865 0.3823 0.100 Uiso 0.28 1 d PG E 2 H45F H 1.0590 0.0588 0.3153 0.100 Uiso 0.28 1 d PG E 2 C46 C 0.5007(6) 0.7697(4) -0.0004(3) 0.045(2) Uiso 0.65 1 d PG F 1 C47 C 0.3758(6) 0.7812(5) -0.0490(3) 0.046(2) Uiso 0.65 1 d PG F 1 H47 H 0.3116 0.8383 -0.0459 0.055 Uiso 0.65 1 d PG F 1 C48 C 0.3451(7) 0.7091(5) -0.1022(3) 0.047(2) Uiso 0.65 1 d PG F 1 H48 H 0.2600 0.7170 -0.1353 0.056 Uiso 0.65 1 d PG F 1 C49 C 0.4392(8) 0.6254(5) -0.1067(3) 0.053(3) Uiso 0.65 1 d PG F 1 H49 H 0.4183 0.5762 -0.1429 0.064 Uiso 0.65 1 d PG F 1 C50 C 0.5641(8) 0.6139(5) -0.0581(4) 0.066(3) Uiso 0.65 1 d PG F 1 H50 H 0.6283 0.5568 -0.0612 0.079 Uiso 0.65 1 d PG F 1 C51 C 0.5948(6) 0.6860(5) -0.0050(3) 0.052(4) Uiso 0.65 1 d PG F 1 H51 H 0.6799 0.6781 0.0281 0.063 Uiso 0.65 1 d PG F 1 C52 C 0.5337(9) 0.8474(6) 0.0567(4) 0.063 Uiso 0.65 1 d PG F 1 H52A H 0.6380 0.8388 0.0772 0.079 Uiso 0.65 1 calc PR F 1 H52B H 0.4627 0.8390 0.0945 0.079 Uiso 0.65 1 calc PR F 1 H52C H 0.5219 0.9154 0.0359 0.079 Uiso 0.65 1 calc PR F 1 C46' C 0.5806(11) 0.6708(9) -0.0120(6) 0.050(7) Uiso 0.35 1 d PG G 2 C47' C 0.5597(14) 0.7504(10) 0.0350(6) 0.052(5) Uiso 0.35 1 d PG G 2 H47' H 0.6222 0.7561 0.0780 0.063 Uiso 0.35 1 d PG G 2 C48' C 0.4470(16) 0.8217(9) 0.0188(7) 0.060(6) Uiso 0.35 1 d PG G 2 H48' H 0.4327 0.8761 0.0508 0.072 Uiso 0.35 1 d PG G 2 C49' C 0.3552(14) 0.8135(9) -0.0443(7) 0.062(6) Uiso 0.35 1 d PG G 2 H49' H 0.2784 0.8622 -0.0553 0.074 Uiso 0.35 1 d PG G 2 C50' C 0.3761(13) 0.7339(10) -0.0912(6) 0.040(4) Uiso 0.35 1 d PG G 2 H50' H 0.3135 0.7282 -0.1342 0.048 Uiso 0.35 1 d PG G 2 C51' C 0.4888(13) 0.6625(9) -0.0751(6) 0.056(5) Uiso 0.35 1 d PG G 2 H51' H 0.5031 0.6082 -0.1071 0.067 Uiso 0.35 1 d PG G 2 C52' C 0.7019(17) 0.5939(13) 0.0054(9) 0.079(7) Uiso 0.35 1 d PG G 2 H52D H 0.7140 0.5509 -0.0367 0.118 Uiso 0.35 1 calc PR G 2 H52E H 0.6733 0.5518 0.0456 0.118 Uiso 0.35 1 calc PR G 2 H52F H 0.7979 0.6286 0.0186 0.118 Uiso 0.35 1 calc PR G 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 Ru 0.01439(14) 0.01371(15) 0.01308(14) 0.00033(15) 0.00107(9) 0.00074(16) N1 0.010(3) 0.014(2) 0.0158(19) -0.001(3) 0.0039(16) -0.008(3) C2 0.019(7) 0.018(3) 0.022(3) 0.003(3) 0.002(3) 0.002(3) C3 0.030(9) 0.024(5) 0.016(4) -0.001(4) -0.005(3) -0.006(4) C4 0.025(4) 0.029(4) 0.015(3) 0.011(3) -0.001(3) -0.006(4) C5 0.029(4) 0.019(4) 0.018(4) 0.002(3) 0.009(3) 0.005(3) C6 0.033(4) 0.026(4) 0.019(3) 0.008(3) -0.004(3) 0.003(3) C7 0.030(3) 0.009(3) 0.033(4) 0.008(3) 0.004(3) 0.005(2) C8 0.025(3) 0.016(3) 0.029(3) -0.003(3) 0.008(3) 0.006(2) C9 0.041(4) 0.011(3) 0.035(4) 0.004(3) 0.004(3) 0.002(3) C10 0.031(4) 0.017(4) 0.023(4) -0.003(3) 0.011(3) -0.004(3) C11 0.022(3) 0.015(3) 0.025(3) 0.002(2) 0.003(3) -0.002(2) N12 0.018(3) 0.022(3) 0.016(3) -0.010(3) 0.007(2) -0.001(2) C13 0.018(3) 0.013(3) 0.023(3) 0.001(2) 0.008(2) 0.001(2) C14 0.016(3) 0.021(4) 0.019(4) 0.004(3) 0.010(3) 0.003(3) C15 0.021(3) 0.030(4) 0.020(3) -0.008(3) 0.004(2) 0.007(3) C16 0.021(3) 0.025(4) 0.024(4) -0.004(3) -0.003(3) 0.004(3) C17 0.028(3) 0.030(4) 0.037(4) -0.009(3) -0.005(3) 0.000(3) C18 0.024(4) 0.030(4) 0.029(4) -0.002(3) 0.000(3) 0.006(3) C19 0.017(6) 0.035(4) 0.019(3) -0.006(3) 0.003(3) 0.008(3) C20 0.018(5) 0.039(6) 0.018(3) -0.010(3) 0.001(2) 0.002(4) C21 0.028(4) 0.045(5) 0.013(3) 0.005(3) -0.001(3) -0.009(4) C22 0.015(4) 0.032(4) 0.020(3) 0.001(3) 0.003(2) -0.001(4) N23 0.013(2) 0.028(4) 0.018(2) 0.002(2) 0.0036(17) 0.008(4) C24 0.015(4) 0.030(4) 0.019(3) -0.002(3) 0.007(2) 0.009(4) N25 0.0186(18) 0.0244(19) 0.0140(17) -0.0002(14) -0.0002(14) 0.0016(15) C26 0.023(2) 0.037(4) 0.0159(18) 0.002(2) 0.0004(16) -0.001(2) C27 0.022(2) 0.055(5) 0.024(2) -0.006(2) 0.0060(18) -0.003(2) C28 0.023(2) 0.051(4) 0.025(2) -0.006(2) 0.006(2) 0.011(2) C29 0.029(2) 0.031(3) 0.025(2) -0.005(2) -0.002(2) 0.013(2) C30 0.023(2) 0.031(3) 0.013(2) -0.0018(18) -0.0058(17) 0.006(2) N31 0.021(2) 0.023(2) 0.013(2) 0.0054(16) -0.0015(16) 0.0014(18) C32 0.027(2) 0.018(2) 0.015(2) -0.0026(17) -0.0049(19) 0.008(2) C33 0.033(3) 0.019(3) 0.029(3) -0.004(2) -0.006(2) 0.005(2) C34 0.044(3) 0.016(3) 0.041(3) -0.001(2) -0.008(2) -0.001(2) C35 0.029(2) 0.016(2) 0.030(2) 0.0026(19) -0.006(2) -0.0061(19) C36 0.027(2) 0.021(2) 0.016(2) 0.0019(18) -0.0052(18) -0.0033(19) N37 0.0199(16) 0.019(3) 0.0181(15) -0.0013(16) -0.0001(13) -0.0027(17) C38 0.021(2) 0.026(3) 0.014(2) 0.0027(18) -0.0012(17) -0.005(2) C39 0.025(2) 0.031(3) 0.030(2) 0.004(2) 0.001(2) -0.009(2) C40 0.024(3) 0.045(4) 0.031(3) 0.001(2) 0.010(2) -0.011(3) C41 0.020(2) 0.037(3) 0.033(3) -0.004(2) 0.010(2) 0.003(2) C42 0.020(2) 0.026(3) 0.028(2) -0.003(2) 0.004(2) 0.001(2) P1 0.0400(8) 0.0410(9) 0.0398(8) 0.0218(7) -0.0095(6) -0.0100(7) F1 0.066(2) 0.077(3) 0.057(2) 0.034(2) -0.027(2) -0.040(2) F2 0.057(2) 0.057(2) 0.069(3) 0.022(2) -0.027(2) -0.0183(19) F3 0.049(2) 0.111(4) 0.045(2) 0.031(2) -0.0018(17) -0.014(2) F4 0.065(2) 0.062(3) 0.047(2) 0.0238(19) -0.0014(17) -0.009(2) F5 0.065(2) 0.056(2) 0.083(3) 0.034(3) -0.0063(19) 0.009(3) F6 0.097(4) 0.058(3) 0.062(3) -0.003(2) -0.019(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N31 1.978(5) . ? Ru N12' 2.029(8) . ? Ru N1' 2.057(8) . ? Ru N12 2.065(6) . ? Ru N1 2.065(4) . ? Ru N37 2.072(3) . ? Ru N25 2.072(4) . ? Ru N23' 2.095(9) . ? Ru N23 2.097(6) . ? N1 C2 1.320(11) . ? N1 C14 1.379(11) . ? C2 C3 1.401(12) . ? C3 C4 1.375(13) . ? C4 C5 1.407(11) . ? C5 C14 1.392(10) . ? C5 C6 1.418(11) . ? C6 C7 1.344(10) . ? C7 C8 1.426(10) . ? C8 C13 1.393(9) . ? C8 C9 1.414(9) . ? C9 C10 1.364(10) . ? C10 C11 1.429(9) . ? C11 N12 1.335(8) . ? C11 C15 1.487(9) . ? N12 C13 1.393(9) . ? C13 C14 1.434(10) . ? C15 C16 1.396(11) . ? C15 C24 1.445(11) . ? C16 C17 1.378(10) . ? C17 C18 1.368(10) . ? C18 C19 1.430(11) . ? C19 C20 1.403(11) . ? C19 C24 1.443(10) . ? C20 C21 1.342(13) . ? C21 C22 1.393(12) . ? C22 N23 1.360(10) . ? N23 C24 1.375(10) . ? N1' C2' 1.321(12) . ? N1' C14' 1.377(12) . ? C2' C3' 1.402(13) . ? C3' C4' 1.376(14) . ? C4' C5' 1.406(12) . ? C5' C14' 1.392(11) . ? C5' C6' 1.417(12) . ? C6' C7' 1.346(11) . ? C7' C8' 1.425(11) . ? C8' C13' 1.396(10) . ? C8' C9' 1.414(10) . ? C9' C10' 1.366(11) . ? C10' C11' 1.429(10) . ? C11' N12' 1.331(9) . ? C11' C15' 1.486(10) . ? N12' C13' 1.386(10) . ? C13' C14' 1.433(11) . ? C15' C16' 1.395(11) . ? C15' C24' 1.447(12) . ? C16' C17' 1.378(11) . ? C17' C18' 1.367(11) . ? C18' C19' 1.432(12) . ? C19' C20' 1.405(12) . ? C19' C24' 1.444(11) . ? C20' C21' 1.343(14) . ? C21' C22' 1.394(13) . ? C22' N23' 1.359(12) . ? N23' C24' 1.375(11) . ? N25 C26 1.337(6) . ? N25 C30 1.365(7) . ? C26 C27 1.380(7) . ? C27 C28 1.393(9) . ? C28 C29 1.387(8) . ? C29 C30 1.397(7) . ? C30 C32 1.468(7) . ? N31 C36 1.342(7) . ? N31 C32 1.349(7) . ? C32 C33 1.389(7) . ? C33 C34 1.392(9) . ? C34 C35 1.406(8) . ? C35 C36 1.382(7) . ? C36 C38 1.465(7) . ? N37 C42 1.323(6) . ? N37 C38 1.372(7) . ? C38 C39 1.396(7) . ? C39 C40 1.387(8) . ? C40 C41 1.366(8) . ? C41 C42 1.397(7) . ? P1 F6 1.566(5) . ? P1 F3 1.580(4) . ? P1 F1 1.589(4) . ? P1 F5 1.597(6) . ? P1 F2 1.597(4) . ? P1 F4 1.600(4) . ? P2 F9 1.5838 . ? P2 F7 1.5839 . ? P2 F10 1.5839 . ? P2 F8 1.5840 . ? P2 F12 1.5848 . ? P2 F11 1.5851 . ? P2' F8' 1.5836 . ? P2' F7' 1.5836 . ? P2' F12' 1.5845 . ? P2' F10' 1.5847 . ? P2' F9' 1.5847 . ? P2' F11' 1.5848 . ? O1 C43 1.2354 . ? C43 C44 1.4747 . ? C43 C45 1.4751 . ? O1' C43' 1.2354 . ? C43' C44' 1.4746 . ? C43' C45' 1.4746 . ? C46 C51 1.3872 . ? C46 C47 1.3891 . ? C46 C52 1.4950 . ? C47 C48 1.3880 . ? C48 C49 1.3870 . ? C49 C50 1.3888 . ? C50 C51 1.3879 . ? C46' C47' 1.3875 . ? C46' C51' 1.3895 . ? C46' C52' 1.4944 . ? C47' C48' 1.3876 . ? C48' C49' 1.3893 . ? C49' C50' 1.3876 . ? C50' C51' 1.3877 . ? 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 Ru N12' 170.9(3) . . ? N31 Ru N1' 88.7(4) . . ? N12' Ru N1' 82.5(4) . . ? N31 Ru N12 172.43(18) . . ? N12' Ru N12 16.6(3) . . ? N1' Ru N12 98.8(4) . . ? N31 Ru N1 91.5(3) . . ? N12' Ru N1 97.4(3) . . ? N1' Ru N1 176.6(15) . . ? N12 Ru N1 80.9(3) . . ? N31 Ru N37 79.39(18) . . ? N12' Ru N37 102.3(6) . . ? N1' Ru N37 87.8(14) . . ? N12 Ru N37 99.9(2) . . ? N1 Ru N37 88.95(19) . . ? N31 Ru N25 79.73(17) . . ? N12' Ru N25 98.2(6) . . ? N1' Ru N25 90.8(15) . . ? N12 Ru N25 100.88(19) . . ? N1 Ru N25 92.6(2) . . ? N37 Ru N25 159.09(16) . . ? N31 Ru N23' 97.4(4) . . ? N12' Ru N23' 91.4(4) . . ? N1' Ru N23' 173.7(6) . . ? N12 Ru N23' 75.1(4) . . ? N1 Ru N23' 7.5(8) . . ? N37 Ru N23' 94.7(9) . . ? N25 Ru N23' 89.0(9) . . ? N31 Ru N23 97.68(18) . . ? N12' Ru N23 73.5(3) . . ? N1' Ru N23 9.0(4) . . ? N12 Ru N23 89.9(2) . . ? N1 Ru N23 170.3(3) . . ? N37 Ru N23 89.9(4) . . ? N25 Ru N23 91.9(4) . . ? N23' Ru N23 164.8(5) . . ? C2 N1 C14 118.1(6) . . ? C2 N1 Ru 128.9(7) . . ? C14 N1 Ru 112.9(5) . . ? N1 C2 C3 122.6(8) . . ? C4 C3 C2 119.2(7) . . ? C3 C4 C5 119.9(7) . . ? C14 C5 C4 117.1(7) . . ? C14 C5 C6 118.3(7) . . ? C4 C5 C6 124.5(7) . . ? C7 C6 C5 120.9(6) . . ? C6 C7 C8 121.9(6) . . ? C13 C8 C9 116.1(6) . . ? C13 C8 C7 118.8(6) . . ? C9 C8 C7 125.1(6) . . ? C10 C9 C8 120.1(6) . . ? C9 C10 C11 121.6(6) . . ? N12 C11 C10 119.0(6) . . ? N12 C11 C15 121.6(6) . . ? C10 C11 C15 119.4(6) . . ? C11 N12 C13 119.3(6) . . ? C11 N12 Ru 129.0(4) . . ? C13 N12 Ru 111.7(4) . . ? N12 C13 C8 123.7(6) . . ? N12 C13 C14 117.5(6) . . ? C8 C13 C14 118.8(6) . . ? N1 C14 C5 122.9(7) . . ? N1 C14 C13 115.8(6) . . ? C5 C14 C13 121.2(7) . . ? C16 C15 C24 117.9(6) . . ? C16 C15 C11 116.8(6) . . ? C24 C15 C11 125.2(7) . . ? C17 C16 C15 124.1(7) . . ? C18 C17 C16 119.5(7) . . ? C17 C18 C19 120.0(7) . . ? C20 C19 C18 119.5(6) . . ? C20 C19 C24 119.9(7) . . ? C18 C19 C24 120.6(7) . . ? C21 C20 C19 120.0(7) . . ? C20 C21 C22 118.8(8) . . ? N23 C22 C21 123.8(8) . . ? C22 N23 C24 118.6(6) . . ? C22 N23 Ru 116.5(5) . . ? C24 N23 Ru 124.8(5) . . ? N23 C24 C15 124.4(6) . . ? N23 C24 C19 118.2(7) . . ? C15 C24 C19 117.3(7) . . ? C2' N1' C14' 118.4(9) . . ? C2' N1' Ru 130.2(10) . . ? C14' N1' Ru 111.0(8) . . ? N1' C2' C3' 122.1(11) . . ? C4' C3' C2' 119.1(11) . . ? C3' C4' C5' 119.9(10) . . ? C14' C5' C4' 117.1(9) . . ? C14' C5' C6' 118.0(9) . . ? C4' C5' C6' 124.8(9) . . ? C7' C6' C5' 120.7(9) . . ? C6' C7' C8' 122.2(8) . . ? C13' C8' C9' 115.7(8) . . ? C13' C8' C7' 118.1(7) . . ? C9' C8' C7' 126.1(8) . . ? C10' C9' C8' 121.0(8) . . ? C9' C10' C11' 120.9(8) . . ? N12' C11' C10' 118.2(8) . . ? N12' C11' C15' 120.9(8) . . ? C10' C11' C15' 120.3(8) . . ? C11' N12' C13' 121.2(7) . . ? C11' N12' Ru 127.6(7) . . ? C13' N12' Ru 110.1(6) . . ? N12' C13' C8' 122.7(7) . . ? N12' C13' C14' 118.2(8) . . ? C8' C13' C14' 119.0(8) . . ? N1' C14' C5' 122.7(9) . . ? N1' C14' C13' 116.0(8) . . ? C5' C14' C13' 121.0(9) . . ? C16' C15' C24' 117.7(8) . . ? C16' C15' C11' 117.1(8) . . ? C24' C15' C11' 125.2(9) . . ? C17' C16' C15' 124.0(9) . . ? C18' C17' C16' 119.9(9) . . ? C17' C18' C19' 119.7(9) . . ? C20' C19' C18' 119.0(10) . . ? C20' C19' C24' 119.6(11) . . ? C18' C19' C24' 120.2(10) . . ? C21' C20' C19' 119.7(11) . . ? C20' C21' C22' 118.5(12) . . ? N23' C22' C21' 123.8(12) . . ? C22' N23' C24' 118.8(9) . . ? C22' N23' Ru 116.5(16) . . ? C24' N23' Ru 121.7(15) . . ? N23' C24' C15' 123.9(9) . . ? N23' C24' C19' 118.3(9) . . ? C15' C24' C19' 117.5(9) . . ? C26 N25 C30 118.9(4) . . ? C26 N25 Ru 128.0(4) . . ? C30 N25 Ru 113.2(3) . . ? N25 C26 C27 122.7(6) . . ? C26 C27 C28 119.2(5) . . ? C29 C28 C27 118.7(4) . . ? C28 C29 C30 119.3(5) . . ? N25 C30 C29 121.2(5) . . ? N25 C30 C32 115.4(4) . . ? C29 C30 C32 123.4(5) . . ? C36 N31 C32 123.2(5) . . ? C36 N31 Ru 118.8(4) . . ? C32 N31 Ru 117.9(4) . . ? N31 C32 C33 118.6(5) . . ? N31 C32 C30 113.7(4) . . ? C33 C32 C30 127.7(5) . . ? C32 C33 C34 120.0(5) . . ? C33 C34 C35 119.6(5) . . ? C36 C35 C34 118.4(5) . . ? N31 C36 C35 120.3(5) . . ? N31 C36 C38 113.1(4) . . ? C35 C36 C38 126.6(5) . . ? C42 N37 C38 119.3(4) . . ? C42 N37 Ru 127.7(4) . . ? C38 N37 Ru 113.0(3) . . ? N37 C38 C39 120.3(5) . . ? N37 C38 C36 115.7(4) . . ? C39 C38 C36 124.1(5) . . ? C40 C39 C38 119.7(5) . . ? C41 C40 C39 119.0(4) . . ? C40 C41 C42 119.4(5) . . ? N37 C42 C41 122.3(5) . . ? F6 P1 F3 91.1(3) . . ? F6 P1 F1 91.9(3) . . ? F3 P1 F1 90.7(2) . . ? F6 P1 F5 179.1(3) . . ? F3 P1 F5 88.0(2) . . ? F1 P1 F5 88.4(3) . . ? F6 P1 F2 90.4(3) . . ? F3 P1 F2 90.6(2) . . ? F1 P1 F2 177.3(3) . . ? F5 P1 F2 89.3(3) . . ? F6 P1 F4 90.0(3) . . ? F3 P1 F4 178.8(3) . . ? F1 P1 F4 89.7(2) . . ? F5 P1 F4 90.9(2) . . ? F2 P1 F4 88.8(2) . . ? F9 P2 F7 90.0 . . ? F9 P2 F10 180.0 . . ? F7 P2 F10 90.0 . . ? F9 P2 F8 90.0 . . ? F7 P2 F8 179.99(9) . . ? F10 P2 F8 90.0 . . ? F9 P2 F12 90.1 . . ? F7 P2 F12 90.0 . . ? F10 P2 F12 89.9 . . ? F8 P2 F12 90.0 . . ? F9 P2 F11 89.9 . . ? F7 P2 F11 89.9 . . ? F10 P2 F11 90.1 . . ? F8 P2 F11 90.0 . . ? F12 P2 F11 180.0 . . ? F8' P2' F7' 180.0 . . ? F8' P2' F12' 90.0 . . ? F7' P2' F12' 90.0 . . ? F8' P2' F10' 90.0 . . ? F7' P2' F10' 90.0 . . ? F12' P2' F10' 89.9 . . ? F8' P2' F9' 90.0 . . ? F7' P2' F9' 90.0 . . ? F12' P2' F9' 90.1 . . ? F10' P2' F9' 180.0 . . ? F8' P2' F11' 90.0 . . ? F7' P2' F11' 89.9 . . ? F12' P2' F11' 180.0 . . ? F10' P2' F11' 90.1 . . ? F9' P2' F11' 89.9 . . ? O1 C43 C44 120.0 . . ? O1 C43 C45 120.0 . . ? C44 C43 C45 120.0 . . ? O1' C43' C44' 120.0 . . ? O1' C43' C45' 120.0 . . ? C44' C43' C45' 120.0 . . ? C51 C46 C47 120.0 . . ? C51 C46 C52 120.0 . . ? C47 C46 C52 120.0 . . ? C48 C47 C46 120.1 . . ? C49 C48 C47 119.9 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.1 . . ? C46 C51 C50 119.9 . . ? C47' C46' C51' 120.1 . . ? C47' C46' C52' 120.0 . . ? C51' C46' C52' 120.0 . . ? C46' C47' C48' 119.9 . . ? C47' C48' C49' 120.1 . . ? C50' C49' C48' 120.0 . . ? C49' C50' C51' 119.9 . . ? C50' C51' C46' 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 Ru N1 C2 6.8(12) . . . . ? N12' Ru N1 C2 -171.6(13) . . . . ? N12 Ru N1 C2 -173.6(13) . . . . ? N37 Ru N1 C2 86.2(12) . . . . ? N25 Ru N1 C2 -73.0(12) . . . . ? N23' Ru N1 C2 -134(7) . . . . ? N31 Ru N1 C14 -169.7(10) . . . . ? N12' Ru N1 C14 11.9(12) . . . . ? N12 Ru N1 C14 9.9(10) . . . . ? N37 Ru N1 C14 -90.4(10) . . . . ? N25 Ru N1 C14 110.5(10) . . . . ? N23' Ru N1 C14 49(6) . . . . ? C14 N1 C2 C3 5(3) . . . . ? Ru N1 C2 C3 -171.6(16) . . . . ? N1 C2 C3 C4 -3(3) . . . . ? C2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C14 -1(2) . . . . ? C3 C4 C5 C6 -177.5(17) . . . . ? C14 C5 C6 C7 -2.1(18) . . . . ? C4 C5 C6 C7 174.8(12) . . . . ? C5 C6 C7 C8 1.4(13) . . . . ? C6 C7 C8 C13 0.0(10) . . . . ? C6 C7 C8 C9 179.1(7) . . . . ? C13 C8 C9 C10 -1.7(10) . . . . ? C7 C8 C9 C10 179.1(7) . . . . ? C8 C9 C10 C11 -0.3(11) . . . . ? C9 C10 C11 N12 4.3(11) . . . . ? C9 C10 C11 C15 -176.1(6) . . . . ? C10 C11 N12 C13 -6.0(9) . . . . ? C15 C11 N12 C13 174.4(6) . . . . ? C10 C11 N12 Ru 170.9(5) . . . . ? C15 C11 N12 Ru -8.7(9) . . . . ? N12' Ru N12 C11 1(2) . . . . ? N1' Ru N12 C11 -9.2(16) . . . . ? N1 Ru N12 C11 174.2(6) . . . . ? N37 Ru N12 C11 -98.5(6) . . . . ? N25 Ru N12 C11 83.3(6) . . . . ? N23' Ru N12 C11 169.2(11) . . . . ? N23 Ru N12 C11 -8.6(7) . . . . ? N12' Ru N12 C13 178(2) . . . . ? N1' Ru N12 C13 167.9(16) . . . . ? N1 Ru N12 C13 -8.7(4) . . . . ? N37 Ru N12 C13 78.6(4) . . . . ? N25 Ru N12 C13 -99.6(4) . . . . ? N23' Ru N12 C13 -13.6(10) . . . . ? N23 Ru N12 C13 168.5(6) . . . . ? C11 N12 C13 C8 4.1(9) . . . . ? Ru N12 C13 C8 -173.3(5) . . . . ? C11 N12 C13 C14 -176.1(11) . . . . ? Ru N12 C13 C14 6.5(11) . . . . ? C9 C8 C13 N12 -0.1(9) . . . . ? C7 C8 C13 N12 179.1(6) . . . . ? C9 C8 C13 C14 -179.9(11) . . . . ? C7 C8 C13 C14 -0.7(13) . . . . ? C2 N1 C14 C5 -5(2) . . . . ? Ru N1 C14 C5 172.4(14) . . . . ? C2 N1 C14 C13 173.7(14) . . . . ? Ru N1 C14 C13 -9.3(18) . . . . ? C4 C5 C14 N1 2(2) . . . . ? C6 C5 C14 N1 179.5(16) . . . . ? C4 C5 C14 C13 -175.8(16) . . . . ? C6 C5 C14 C13 1(2) . . . . ? N12 C13 C14 N1 2(2) . . . . ? C8 C13 C14 N1 -178.3(11) . . . . ? N12 C13 C14 C5 -179.8(13) . . . . ? C8 C13 C14 C5 0(2) . . . . ? N12 C11 C15 C16 -159.8(6) . . . . ? C10 C11 C15 C16 20.6(9) . . . . ? N12 C11 C15 C24 24.3(11) . . . . ? C10 C11 C15 C24 -155.3(9) . . . . ? C24 C15 C16 C17 2.4(11) . . . . ? C11 C15 C16 C17 -173.7(6) . . . . ? C15 C16 C17 C18 4.6(11) . . . . ? C16 C17 C18 C19 -6.8(11) . . . . ? C17 C18 C19 C20 -177.2(10) . . . . ? C17 C18 C19 C24 2.1(15) . . . . ? C18 C19 C20 C21 178(2) . . . . ? C24 C19 C20 C21 -1(3) . . . . ? C19 C20 C21 C22 -3(4) . . . . ? C20 C21 C22 N23 2(4) . . . . ? C21 C22 N23 C24 5(3) . . . . ? C21 C22 N23 Ru -172(2) . . . . ? N31 Ru N23 C22 12.8(11) . . . . ? N12' Ru N23 C22 -169.3(13) . . . . ? N1' Ru N23 C22 10(11) . . . . ? N12 Ru N23 C22 -166.4(10) . . . . ? N37 Ru N23 C22 -66.5(10) . . . . ? N25 Ru N23 C22 92.7(10) . . . . ? N23' Ru N23 C22 -174(3) . . . . ? N31 Ru N23 C24 -163.4(11) . . . . ? N12' Ru N23 C24 14.5(12) . . . . ? N1' Ru N23 C24 -166(13) . . . . ? N12 Ru N23 C24 17.4(12) . . . . ? N37 Ru N23 C24 117.3(12) . . . . ? N25 Ru N23 C24 -83.5(12) . . . . ? N23' Ru N23 C24 10(4) . . . . ? C22 N23 C24 C15 174.5(12) . . . . ? Ru N23 C24 C15 -9.4(19) . . . . ? C22 N23 C24 C19 -9.0(18) . . . . ? Ru N23 C24 C19 167.1(9) . . . . ? C16 C15 C24 N23 169.6(11) . . . . ? C11 C15 C24 N23 -14.6(18) . . . . ? C16 C15 C24 C19 -6.8(14) . . . . ? C11 C15 C24 C19 169.0(9) . . . . ? C20 C19 C24 N23 7.4(18) . . . . ? C18 C19 C24 N23 -172.0(12) . . . . ? C20 C19 C24 C15 -175.9(12) . . . . ? C18 C19 C24 C15 4.7(17) . . . . ? N31 Ru N1' C2' 6(5) . . . . ? N12' Ru N1' C2' -176(6) . . . . ? N12 Ru N1' C2' -173(5) . . . . ? N37 Ru N1' C2' -73(5) . . . . ? N25 Ru N1' C2' 86(5) . . . . ? N23 Ru N1' C2' -177(16) . . . . ? N31 Ru N1' C14' -166(4) . . . . ? N12' Ru N1' C14' 12(4) . . . . ? N12 Ru N1' C14' 15(4) . . . . ? N37 Ru N1' C14' 114(4) . . . . ? N25 Ru N1' C14' -86(4) . . . . ? N23 Ru N1' C14' 11(9) . . . . ? C14' N1' C2' C3' -9(9) . . . . ? Ru N1' C2' C3' 179(6) . . . . ? N1' C2' C3' C4' 8(12) . . . . ? C2' C3' C4' C5' -1(13) . . . . ? C3' C4' C5' C14' -3(10) . . . . ? C3' C4' C5' C6' 174(7) . . . . ? C14' C5' C6' C7' -6(6) . . . . ? C4' C5' C6' C7' 176(5) . . . . ? C5' C6' C7' C8' -3(4) . . . . ? C6' C7' C8' C13' 7(3) . . . . ? C6' C7' C8' C9' -176(2) . . . . ? C13' C8' C9' C10' -5(3) . . . . ? C7' C8' C9' C10' 178(2) . . . . ? C8' C9' C10' C11' 5(3) . . . . ? C9' C10' C11' N12' -3(3) . . . . ? C9' C10' C11' C15' -174(2) . . . . ? C10' C11' N12' C13' 1(3) . . . . ? C15' C11' N12' C13' 172.1(19) . . . . ? C10' C11' N12' Ru 168.0(17) . . . . ? C15' C11' N12' Ru -21(3) . . . . ? N1' Ru N12' C11' 179(2) . . . . ? N12 Ru N12' C11' 8.9(13) . . . . ? N1 Ru N12' C11' 2.0(19) . . . . ? N37 Ru N12' C11' 92.5(18) . . . . ? N25 Ru N12' C11' -91.7(18) . . . . ? N23' Ru N12' C11' -3(2) . . . . ? N23 Ru N12' C11' 179(2) . . . . ? N1' Ru N12' C13' -13(2) . . . . ? N12 Ru N12' C13' 177(3) . . . . ? N1 Ru N12' C13' 170.2(14) . . . . ? N37 Ru N12' C13' -99.2(14) . . . . ? N25 Ru N12' C13' 76.5(14) . . . . ? N23' Ru N12' C13' 165.7(17) . . . . ? N23 Ru N12' C13' -13.0(14) . . . . ? C11' N12' C13' C8' -2(3) . . . . ? Ru N12' C13' C8' -170.7(18) . . . . ? C11' N12' C13' C14' -178(3) . . . . ? Ru N12' C13' C14' 13(3) . . . . ? C9' C8' C13' N12' 4(3) . . . . ? C7' C8' C13' N12' -179(2) . . . . ? C9' C8' C13' C14' -180(3) . . . . ? C7' C8' C13' C14' -3(4) . . . . ? C2' N1' C14' C5' 5(8) . . . . ? Ru N1' C14' C5' 178(4) . . . . ? C2' N1' C14' C13' 178(5) . . . . ? Ru N1' C14' C13' -8(6) . . . . ? C4' C5' C14' N1' 1(8) . . . . ? C6' C5' C14' N1' -176(5) . . . . ? C4' C5' C14' C13' -172(5) . . . . ? C6' C5' C14' C13' 11(7) . . . . ? N12' C13' C14' N1' -3(6) . . . . ? C8' C13' C14' N1' -180(4) . . . . ? N12' C13' C14' C5' 171(4) . . . . ? C8' C13' C14' C5' -6(6) . . . . ? N12' C11' C15' C16' -153(2) . . . . ? C10' C11' C15' C16' 18(3) . . . . ? N12' C11' C15' C24' 30(4) . . . . ? C10' C11' C15' C24' -159(4) . . . . ? C24' C15' C16' C17' 6(5) . . . . ? C11' C15' C16' C17' -171.8(19) . . . . ? C15' C16' C17' C18' -5(3) . . . . ? C16' C17' C18' C19' 6(4) . . . . ? C17' C18' C19' C20' -177(4) . . . . ? C17' C18' C19' C24' -9(6) . . . . ? C18' C19' C20' C21' -180(6) . . . . ? C24' C19' C20' C21' 13(8) . . . . ? C19' C20' C21' C22' -13(10) . . . . ? C20' C21' C22' N23' 8(11) . . . . ? C21' C22' N23' C24' -3(10) . . . . ? C21' C22' N23' Ru -164(6) . . . . ? N31 Ru N23' C22' 2(4) . . . . ? N12' Ru N23' C22' -176(4) . . . . ? N12 Ru N23' C22' -179(4) . . . . ? N1 Ru N23' C22' 41(6) . . . . ? N37 Ru N23' C22' 82(4) . . . . ? N25 Ru N23' C22' -78(4) . . . . ? N23 Ru N23' C22' -171(4) . . . . ? N31 Ru N23' C24' -158(4) . . . . ? N12' Ru N23' C24' 24(4) . . . . ? N12 Ru N23' C24' 21(4) . . . . ? N1 Ru N23' C24' -119(9) . . . . ? N37 Ru N23' C24' -78(4) . . . . ? N25 Ru N23' C24' 122(4) . . . . ? N23 Ru N23' C24' 29(6) . . . . ? C22' N23' C24' C15' 177(6) . . . . ? Ru N23' C24' C15' -23(9) . . . . ? C22' N23' C24' C19' 3(9) . . . . ? Ru N23' C24' C19' 163(4) . . . . ? C16' C15' C24' N23' 177(5) . . . . ? C11' C15' C24' N23' -5(9) . . . . ? C16' C15' C24' C19' -9(7) . . . . ? C11' C15' C24' C19' 169(4) . . . . ? C20' C19' C24' N23' -8(8) . . . . ? C18' C19' C24' N23' -175(6) . . . . ? C20' C19' C24' C15' 178(5) . . . . ? C18' C19' C24' C15' 10(8) . . . . ? N31 Ru N25 C26 -179.2(4) . . . . ? N12' Ru N25 C26 9.8(4) . . . . ? N1' Ru N25 C26 92.3(5) . . . . ? N12 Ru N25 C26 -6.8(4) . . . . ? N1 Ru N25 C26 -88.0(4) . . . . ? N37 Ru N25 C26 178.2(3) . . . . ? N23' Ru N25 C26 -81.4(5) . . . . ? N23 Ru N25 C26 83.4(4) . . . . ? N31 Ru N25 C30 -0.9(3) . . . . ? N12' Ru N25 C30 -171.9(4) . . . . ? N1' Ru N25 C30 -89.4(5) . . . . ? N12 Ru N25 C30 171.5(3) . . . . ? N1 Ru N25 C30 90.3(4) . . . . ? N37 Ru N25 C30 -3.5(6) . . . . ? N23' Ru N25 C30 96.9(5) . . . . ? N23 Ru N25 C30 -98.3(3) . . . . ? C30 N25 C26 C27 -0.2(6) . . . . ? Ru N25 C26 C27 178.0(3) . . . . ? N25 C26 C27 C28 0.6(7) . . . . ? C26 C27 C28 C29 0.3(7) . . . . ? C27 C28 C29 C30 -1.5(7) . . . . ? C26 N25 C30 C29 -1.0(6) . . . . ? Ru N25 C30 C29 -179.5(3) . . . . ? C26 N25 C30 C32 178.4(4) . . . . ? Ru N25 C30 C32 0.0(5) . . . . ? C28 C29 C30 N25 1.9(7) . . . . ? C28 C29 C30 C32 -177.5(4) . . . . ? N1' Ru N31 C36 -90.3(15) . . . . ? N1 Ru N31 C36 86.4(4) . . . . ? N37 Ru N31 C36 -2.2(3) . . . . ? N25 Ru N31 C36 178.7(3) . . . . ? N23' Ru N31 C36 91.2(10) . . . . ? N23 Ru N31 C36 -90.7(5) . . . . ? N1' Ru N31 C32 92.8(15) . . . . ? N1 Ru N31 C32 -90.6(4) . . . . ? N37 Ru N31 C32 -179.2(3) . . . . ? N25 Ru N31 C32 1.7(3) . . . . ? N23' Ru N31 C32 -85.8(10) . . . . ? N23 Ru N31 C32 92.3(5) . . . . ? C36 N31 C32 C33 -0.5(7) . . . . ? Ru N31 C32 C33 176.3(3) . . . . ? C36 N31 C32 C30 -179.1(4) . . . . ? Ru N31 C32 C30 -2.2(5) . . . . ? N25 C30 C32 N31 1.4(6) . . . . ? C29 C30 C32 N31 -179.1(4) . . . . ? N25 C30 C32 C33 -177.0(5) . . . . ? C29 C30 C32 C33 2.4(7) . . . . ? N31 C32 C33 C34 0.3(7) . . . . ? C30 C32 C33 C34 178.6(5) . . . . ? C32 C33 C34 C35 -0.3(8) . . . . ? C33 C34 C35 C36 0.5(7) . . . . ? C32 N31 C36 C35 0.8(7) . . . . ? Ru N31 C36 C35 -176.0(3) . . . . ? C32 N31 C36 C38 -179.4(4) . . . . ? Ru N31 C36 C38 3.8(5) . . . . ? C34 C35 C36 N31 -0.8(7) . . . . ? C34 C35 C36 C38 179.5(4) . . . . ? N31 Ru N37 C42 -177.8(4) . . . . ? N12' Ru N37 C42 -6.9(4) . . . . ? N1' Ru N37 C42 -88.7(7) . . . . ? N12 Ru N37 C42 9.9(4) . . . . ? N1 Ru N37 C42 90.4(4) . . . . ? N25 Ru N37 C42 -175.1(4) . . . . ? N23' Ru N37 C42 85.5(5) . . . . ? N23 Ru N37 C42 -80.0(4) . . . . ? N31 Ru N37 C38 0.1(3) . . . . ? N12' Ru N37 C38 171.0(4) . . . . ? N1' Ru N37 C38 89.2(6) . . . . ? N12 Ru N37 C38 -172.2(3) . . . . ? N1 Ru N37 C38 -91.7(4) . . . . ? N25 Ru N37 C38 2.8(5) . . . . ? N23' Ru N37 C38 -96.6(4) . . . . ? N23 Ru N37 C38 97.9(3) . . . . ? C42 N37 C38 C39 0.9(6) . . . . ? Ru N37 C38 C39 -177.2(3) . . . . ? C42 N37 C38 C36 179.9(4) . . . . ? Ru N37 C38 C36 1.8(4) . . . . ? N31 C36 C38 N37 -3.6(5) . . . . ? C35 C36 C38 N37 176.2(4) . . . . ? N31 C36 C38 C39 175.3(4) . . . . ? C35 C36 C38 C39 -4.9(7) . . . . ? N37 C38 C39 C40 -0.5(7) . . . . ? C36 C38 C39 C40 -179.4(5) . . . . ? C38 C39 C40 C41 -0.7(9) . . . . ? C39 C40 C41 C42 1.5(9) . . . . ? C38 N37 C42 C41 -0.1(7) . . . . ? Ru N37 C42 C41 177.6(4) . . . . ? C40 C41 C42 N37 -1.1(9) . . . . ? C51 C46 C47 C48 0.0 . . . . ? C52 C46 C47 C48 180.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C47 C46 C51 C50 0.0 . . . . ? C52 C46 C51 C50 180.0 . . . . ? C49 C50 C51 C46 0.0 . . . . ? C51' C46' C47' C48' 0.0 . . . . ? C52' C46' C47' C48' 180.0 . . . . ? C46' C47' C48' C49' 0.0 . . . . ? C47' C48' C49' C50' 0.0 . . . . ? C48' C49' C50' C51' 0.0 . . . . ? C49' C50' C51' C46' 0.0 . . . . ? C47' C46' C51' C50' 0.0 . . . . ? C52' C46' C51' C50' 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 66.58 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.762 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.081 #===END