# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Luis M. Baraldo' _publ_contact_author_address ;DQIAyQF, INQUIMAE, FCEN, Universidad de Buenos Aires Pabellon 2, Ciudad Universitaria, C1428EHA, Buenos Aires, Argentina ; _publ_contact_author_email baraldo@qi.fcen.uba.ar _publ_contact_author_phone '+54-11-4576-3380 ' _publ_contact_author_fax +54-11-4576-3341 loop_ _publ_author_name _publ_author_address A.Cadranel 'DQIAyQF, INQUIMAE, FCEN, Universidad de Buenos Aires' P.Albores 'DQIAyQF, INQUIMAE, FCEN, Universidad de Buenos Aires' S.Yamazaki 'Department of Chemistry, University of Florida' V.D.Kleiman 'Department of Chemistry, University of Florida' L.M.Baraldo 'DQIAyQF, INQUIMAE, FCEN, Universidad de Buenos Aires' data_1a _database_code_depnum_ccdc_archive 'CCDC 843186' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 F6 N6 O P Ru' _chemical_formula_weight 679.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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_space_group_name_H-M P-1 _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8212(7) _cell_length_b 10.2954(8) _cell_length_c 16.2940(12) _cell_angle_alpha 77.855(6) _cell_angle_beta 77.051(7) _cell_angle_gamma 67.397(7) _cell_volume 1318.62(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 17522 _cell_measurement_theta_min 3.8523 _cell_measurement_theta_max 30.0926 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_T_min 0.67146 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET) (compiled Oct 27 2009,12:04:35) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48360 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 28.50 _reflns_number_total 6644 _reflns_number_gt 5866 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+1.4289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6644 _refine_ls_number_parameters 391 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.44441(3) 0.41935(2) 0.787234(13) 0.03274(9) Uani 1 1 d . . . P1 P 0.13943(13) 0.06458(11) 0.64007(7) 0.0563(2) Uani 1 1 d D . . F1 F -0.0219(4) 0.0500(3) 0.7010(2) 0.0855(8) Uani 1 1 d . A . N3 N 0.3614(3) 0.5912(2) 0.84277(14) 0.0331(5) Uani 1 1 d . . . N5 N 0.5386(3) 0.2504(3) 0.71665(16) 0.0368(5) Uani 1 1 d . . . C3 C 0.9263(4) 0.2839(4) 0.8720(2) 0.0555(9) Uani 1 1 d . . . H3 H 1.0273 0.2085 0.8678 0.067 Uiso 1 1 calc R . . N2 N 0.6516(3) 0.3946(3) 0.83833(15) 0.0374(5) Uani 1 1 d . . . N4 N 0.2072(3) 0.5121(3) 0.75711(15) 0.0349(5) Uani 1 1 d . . . N1 N 0.3279(4) 0.2350(4) 0.9499(2) 0.0571(8) Uani 1 1 d . . . C8 C 0.4084(5) 0.7395(4) 0.9200(2) 0.0494(8) Uani 1 1 d . . . H8 H 0.4784 0.7580 0.9473 0.059 Uiso 1 1 calc R . . C6 C 0.6280(4) 0.5027(3) 0.88166(18) 0.0383(6) Uani 1 1 d . . . N6 N 0.5422(3) 0.5084(3) 0.66921(15) 0.0361(5) Uani 1 1 d . . . C22 C 0.6225(4) 0.2729(3) 0.6371(2) 0.0403(6) Uani 1 1 d . . . C2 C 0.7988(4) 0.2873(4) 0.8343(2) 0.0462(7) Uani 1 1 d . . . H2 H 0.8157 0.2130 0.8052 0.055 Uiso 1 1 calc R . . C26 C 0.5208(4) 0.1237(3) 0.7417(2) 0.0481(7) Uani 1 1 d . . . H26 H 0.4627 0.1069 0.7955 0.058 Uiso 1 1 calc R . . C15 C -0.0208(5) 0.5375(4) 0.6922(3) 0.0546(8) Uani 1 1 d . . . H15 H -0.0671 0.5012 0.6606 0.066 Uiso 1 1 calc R . . C25 C 0.5852(5) 0.0173(4) 0.6908(3) 0.0602(10) Uani 1 1 d . . . H25 H 0.5693 -0.0689 0.7101 0.072 Uiso 1 1 calc R . . C21 C 0.6283(4) 0.4160(3) 0.61222(19) 0.0401(6) Uani 1 1 d . . . C17 C 0.5295(4) 0.6445(3) 0.6474(2) 0.0447(7) Uani 1 1 d . . . H17 H 0.4686 0.7077 0.6863 0.054 Uiso 1 1 calc R . . C7 C 0.4631(4) 0.6164(3) 0.88319(18) 0.0382(6) Uani 1 1 d . . . C24 C 0.6723(5) 0.0397(4) 0.6120(3) 0.0643(11) Uani 1 1 d . . . H24 H 0.7189 -0.0318 0.5775 0.077 Uiso 1 1 calc R . . C10 C 0.1456(4) 0.8078(3) 0.8731(2) 0.0473(7) Uani 1 1 d . . . H10 H 0.0380 0.8717 0.8698 0.057 Uiso 1 1 calc R . . C19 C 0.6984(6) 0.5995(5) 0.5147(2) 0.0678(11) Uani 1 1 d . . . H19 H 0.7551 0.6298 0.4636 0.081 Uiso 1 1 calc R . . C13 C -0.0388(4) 0.7186(4) 0.7677(3) 0.0515(8) Uani 1 1 d . . . H13 H -0.0976 0.8058 0.7871 0.062 Uiso 1 1 calc R . . C5 C 0.7522(4) 0.5032(4) 0.9210(2) 0.0503(8) Uani 1 1 d . . . H5 H 0.7342 0.5772 0.9505 0.060 Uiso 1 1 calc R . . C14 C -0.1081(5) 0.6665(4) 0.7200(3) 0.0603(10) Uani 1 1 d . . . H14 H -0.2140 0.7190 0.7067 0.072 Uiso 1 1 calc R . . C23 C 0.6902(5) 0.1684(4) 0.5846(3) 0.0553(9) Uani 1 1 d . . . H23 H 0.7478 0.1859 0.5307 0.066 Uiso 1 1 calc R . . C12 C 0.1192(4) 0.6393(3) 0.78603(19) 0.0366(6) Uani 1 1 d . . . C18 C 0.6020(5) 0.6948(4) 0.5706(2) 0.0568(9) Uani 1 1 d . . . H18 H 0.5868 0.7909 0.5563 0.068 Uiso 1 1 calc R . . C11 C 0.2061(4) 0.6845(3) 0.83615(18) 0.0363(6) Uani 1 1 d . . . C9 C 0.2491(5) 0.8341(4) 0.9154(2) 0.0538(8) Uani 1 1 d . . . H9 H 0.2104 0.9162 0.9409 0.065 Uiso 1 1 calc R . . C20 C 0.7104(5) 0.4608(5) 0.5345(2) 0.0606(10) Uani 1 1 d . . . H20 H 0.7729 0.3966 0.4965 0.073 Uiso 1 1 calc R . . C1 C 0.3663(4) 0.3068(3) 0.89192(19) 0.0388(6) Uani 1 1 d . . . C4 C 0.9031(5) 0.3916(5) 0.9154(3) 0.0586(9) Uani 1 1 d . . . H4 H 0.9881 0.3901 0.9410 0.070 Uiso 1 1 calc R . . C16 C 0.1366(4) 0.4623(3) 0.7118(2) 0.0426(6) Uani 1 1 d . . . H16 H 0.1957 0.3745 0.6931 0.051 Uiso 1 1 calc R . . O1W O 0.2761(6) 0.0162(5) 1.0789(3) 0.1052(14) Uani 1 1 d D . . F2A F 0.314(4) 0.067(13) 0.587(2) 0.127(5) Uani 0.50 1 d PD A 1 F2B F 0.295(4) 0.077(13) 0.572(2) 0.127(5) Uani 0.50 1 d PD A 2 F3A F 0.0732(15) 0.0392(13) 0.5673(6) 0.118(4) Uani 0.50 1 d PD A 1 F3B F 0.0631(15) 0.1340(13) 0.5568(6) 0.118(4) Uani 0.50 1 d PD A 2 F4A F 0.2428(11) -0.0871(7) 0.6651(6) 0.1084(19) Uani 0.50 1 d PD A 1 F4B F 0.1674(11) -0.0888(7) 0.6115(6) 0.1084(19) Uani 0.50 1 d PD A 2 F5A F 0.1823(8) 0.0962(9) 0.7257(4) 0.0937(14) Uani 0.50 1 d PD A 1 F5B F 0.2522(9) -0.0396(10) 0.7094(4) 0.0937(14) Uani 0.50 1 d PD A 2 F6A F 0.0234(10) 0.2331(6) 0.6324(6) 0.1122(18) Uani 0.50 1 d PD A 1 F6B F 0.1564(10) 0.1829(7) 0.6701(6) 0.1122(18) Uani 0.50 1 d PD A 2 H2W H 0.369(5) -0.040(7) 1.060(5) 0.135 Uiso 1 1 d D . . H1W H 0.299(10) 0.075(7) 1.038(3) 0.135 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03296(13) 0.03153(12) 0.03125(13) -0.00437(8) -0.00445(8) -0.00906(9) P1 0.0542(5) 0.0568(5) 0.0585(6) 0.0018(4) -0.0079(4) -0.0258(4) F1 0.0667(16) 0.097(2) 0.091(2) -0.0240(16) 0.0132(14) -0.0359(15) N3 0.0343(11) 0.0324(11) 0.0308(11) -0.0038(9) -0.0028(9) -0.0114(9) N5 0.0328(11) 0.0345(11) 0.0412(13) -0.0085(10) -0.0076(10) -0.0072(9) C3 0.0359(16) 0.064(2) 0.057(2) -0.0020(17) -0.0092(15) -0.0096(15) N2 0.0348(12) 0.0427(13) 0.0321(12) -0.0040(10) -0.0031(9) -0.0126(10) N4 0.0354(12) 0.0346(11) 0.0330(11) -0.0012(9) -0.0064(9) -0.0117(9) N1 0.067(2) 0.0589(18) 0.0456(16) 0.0063(14) -0.0080(14) -0.0298(16) C8 0.058(2) 0.0492(18) 0.0475(18) -0.0124(14) -0.0149(15) -0.0195(15) C6 0.0381(14) 0.0429(15) 0.0339(14) -0.0036(11) -0.0048(11) -0.0158(12) N6 0.0339(11) 0.0390(12) 0.0335(12) -0.0018(9) -0.0060(9) -0.0123(10) C22 0.0334(13) 0.0448(15) 0.0411(15) -0.0134(12) -0.0069(11) -0.0077(12) C2 0.0375(15) 0.0470(17) 0.0466(17) -0.0038(14) -0.0054(13) -0.0088(13) C26 0.0450(17) 0.0371(15) 0.060(2) -0.0102(14) -0.0072(15) -0.0107(13) C15 0.0518(19) 0.0541(19) 0.065(2) -0.0070(17) -0.0260(17) -0.0180(16) C25 0.055(2) 0.0399(17) 0.088(3) -0.0230(18) -0.012(2) -0.0113(15) C21 0.0392(15) 0.0485(16) 0.0320(14) -0.0074(12) -0.0055(11) -0.0140(13) C17 0.0486(17) 0.0438(16) 0.0418(16) -0.0019(13) -0.0077(13) -0.0184(14) C7 0.0414(15) 0.0414(15) 0.0325(13) -0.0046(11) -0.0050(11) -0.0161(12) C24 0.061(2) 0.057(2) 0.079(3) -0.039(2) -0.005(2) -0.0129(18) C10 0.0487(17) 0.0372(15) 0.0488(18) -0.0110(13) -0.0089(14) -0.0041(13) C19 0.082(3) 0.081(3) 0.0397(19) 0.0018(18) 0.0052(18) -0.042(2) C13 0.0445(17) 0.0379(15) 0.069(2) -0.0072(15) -0.0165(16) -0.0074(13) C5 0.0453(17) 0.065(2) 0.0455(18) -0.0072(15) -0.0089(14) -0.0244(16) C14 0.0454(18) 0.0497(19) 0.086(3) -0.0062(18) -0.0313(19) -0.0070(15) C23 0.0499(19) 0.061(2) 0.055(2) -0.0284(17) -0.0004(15) -0.0133(16) C12 0.0376(14) 0.0317(13) 0.0382(14) -0.0009(11) -0.0068(11) -0.0114(11) C18 0.070(2) 0.057(2) 0.0453(19) 0.0070(16) -0.0076(17) -0.0329(18) C11 0.0399(14) 0.0321(13) 0.0342(14) -0.0036(10) -0.0045(11) -0.0111(11) C9 0.066(2) 0.0410(16) 0.055(2) -0.0183(15) -0.0132(17) -0.0118(15) C20 0.068(2) 0.072(2) 0.0395(18) -0.0143(17) 0.0073(16) -0.026(2) C1 0.0375(14) 0.0375(14) 0.0390(15) -0.0006(11) -0.0097(12) -0.0112(11) C4 0.0437(18) 0.077(3) 0.057(2) -0.0018(19) -0.0166(16) -0.0223(18) C16 0.0463(16) 0.0414(15) 0.0428(16) -0.0058(12) -0.0127(13) -0.0153(13) O1W 0.093(3) 0.081(3) 0.101(3) 0.026(2) 0.016(2) -0.024(2) F2A 0.086(6) 0.233(13) 0.073(11) 0.057(15) -0.028(6) -0.098(12) F2B 0.086(6) 0.233(13) 0.073(11) 0.057(15) -0.028(6) -0.098(12) F3A 0.084(3) 0.208(13) 0.077(3) -0.025(6) -0.010(2) -0.065(8) F3B 0.084(3) 0.208(13) 0.077(3) -0.025(6) -0.010(2) -0.065(8) F4A 0.117(5) 0.071(3) 0.120(6) -0.029(3) 0.008(4) -0.022(3) F4B 0.117(5) 0.071(3) 0.120(6) -0.029(3) 0.008(4) -0.022(3) F5A 0.084(3) 0.128(4) 0.072(3) 0.003(3) -0.020(2) -0.045(3) F5B 0.084(3) 0.128(4) 0.072(3) 0.003(3) -0.020(2) -0.045(3) F6A 0.118(4) 0.055(3) 0.159(5) -0.018(3) -0.008(4) -0.032(3) F6B 0.118(4) 0.055(3) 0.159(5) -0.018(3) -0.008(4) -0.032(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 Ru1 N3 1.966(2) . ? Ru1 C1 1.995(3) . ? Ru1 N4 2.064(2) . ? Ru1 N2 2.081(3) . ? Ru1 N5 2.083(2) . ? Ru1 N6 2.099(2) . ? P1 F6B 1.473(7) . ? P1 F4A 1.497(7) . ? P1 F3A 1.541(9) . ? P1 F3B 1.561(9) . ? P1 F1 1.582(3) . ? P1 F2A 1.591(11) . ? P1 F2B 1.591(11) . ? P1 F5B 1.609(6) . ? P1 F6A 1.635(6) . ? P1 F5A 1.649(6) . ? P1 F4B 1.652(7) . ? N3 C7 1.349(4) . ? N3 C11 1.350(4) . ? N5 C26 1.341(4) . ? N5 C22 1.362(4) . ? C3 C4 1.365(6) . ? C3 C2 1.383(5) . ? N2 C2 1.342(4) . ? N2 C6 1.367(4) . ? N4 C16 1.345(4) . ? N4 C12 1.362(4) . ? N1 C1 1.145(4) . ? C8 C9 1.376(5) . ? C8 C7 1.385(5) . ? C6 C5 1.389(4) . ? C6 C7 1.475(4) . ? N6 C17 1.338(4) . ? N6 C21 1.358(4) . ? C22 C23 1.382(4) . ? C22 C21 1.462(4) . ? C26 C25 1.379(5) . ? C15 C14 1.368(6) . ? C15 C16 1.378(5) . ? C25 C24 1.364(6) . ? C21 C20 1.392(5) . ? C17 C18 1.367(5) . ? C24 C23 1.365(6) . ? C10 C11 1.385(4) . ? C10 C9 1.390(5) . ? C19 C20 1.363(6) . ? C19 C18 1.379(6) . ? C13 C14 1.381(5) . ? C13 C12 1.381(4) . ? C5 C4 1.384(5) . ? C12 C11 1.478(4) . ? 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 N3 Ru1 C1 92.18(11) . . ? N3 Ru1 N4 79.47(10) . . ? C1 Ru1 N4 91.19(11) . . ? N3 Ru1 N2 79.10(10) . . ? C1 Ru1 N2 90.19(11) . . ? N4 Ru1 N2 158.56(10) . . ? N3 Ru1 N5 173.96(9) . . ? C1 Ru1 N5 93.84(11) . . ? N4 Ru1 N5 99.86(10) . . ? N2 Ru1 N5 101.39(10) . . ? N3 Ru1 N6 96.57(9) . . ? C1 Ru1 N6 171.22(11) . . ? N4 Ru1 N6 91.07(9) . . ? N2 Ru1 N6 90.81(9) . . ? N5 Ru1 N6 77.42(10) . . ? F6B P1 F4A 122.1(5) . . ? F6B P1 F3A 138.8(6) . . ? F4A P1 F3A 96.9(6) . . ? F6B P1 F3B 104.1(6) . . ? F4A P1 F3B 128.7(6) . . ? F3A P1 F3B 34.8(5) . . ? F6B P1 F1 101.6(3) . . ? F4A P1 F1 93.0(3) . . ? F3A P1 F1 87.6(5) . . ? F3B P1 F1 98.7(4) . . ? F6B P1 F2A 78(4) . . ? F4A P1 F2A 82(4) . . ? F3A P1 F2A 97(3) . . ? F3B P1 F2A 87.8(14) . . ? F1 P1 F2A 173.3(18) . . ? F6B P1 F2B 82(4) . . ? F4A P1 F2B 88(4) . . ? F3A P1 F2B 87(3) . . ? F3B P1 F2B 76.9(14) . . ? F1 P1 F2B 175(3) . . ? F2A P1 F2B 11(3) . . ? F6B P1 F5B 87.0(5) . . ? F4A P1 F5B 36.8(4) . . ? F3A P1 F5B 133.5(6) . . ? F3B P1 F5B 164.0(6) . . ? F1 P1 F5B 90.1(3) . . ? F2A P1 F5B 83.2(18) . . ? F2B P1 F5B 93.6(18) . . ? F6B P1 F6A 49.9(4) . . ? F4A P1 F6A 168.7(5) . . ? F3A P1 F6A 93.0(6) . . ? F3B P1 F6A 62.4(6) . . ? F1 P1 F6A 82.0(3) . . ? F2A P1 F6A 103(4) . . ? F2B P1 F6A 98(4) . . ? F5B P1 F6A 132.6(5) . . ? F6B P1 F5A 41.8(4) . . ? F4A P1 F5A 85.8(5) . . ? F3A P1 F5A 171.6(5) . . ? F3B P1 F5A 144.8(5) . . ? F1 P1 F5A 84.2(3) . . ? F2A P1 F5A 91(3) . . ? F2B P1 F5A 101(3) . . ? F5B P1 F5A 49.0(4) . . ? F6A P1 F5A 83.6(4) . . ? F6B P1 F4B 165.9(5) . . ? F4A P1 F4B 45.1(4) . . ? F3A P1 F4B 52.1(6) . . ? F3B P1 F4B 85.8(5) . . ? F1 P1 F4B 86.5(3) . . ? F2A P1 F4B 93(5) . . ? F2B P1 F4B 90(5) . . ? F5B P1 F4B 81.4(5) . . ? F6A P1 F4B 143.7(5) . . ? F5A P1 F4B 129.4(5) . . ? C7 N3 C11 121.5(2) . . ? C7 N3 Ru1 119.4(2) . . ? C11 N3 Ru1 118.96(19) . . ? C26 N5 C22 117.5(3) . . ? C26 N5 Ru1 126.0(2) . . ? C22 N5 Ru1 116.6(2) . . ? C4 C3 C2 119.7(3) . . ? C2 N2 C6 118.4(3) . . ? C2 N2 Ru1 128.1(2) . . ? C6 N2 Ru1 113.49(19) . . ? C16 N4 C12 119.0(3) . . ? C16 N4 Ru1 127.2(2) . . ? C12 N4 Ru1 113.72(19) . . ? C9 C8 C7 119.0(3) . . ? N2 C6 C5 121.5(3) . . ? N2 C6 C7 115.1(3) . . ? C5 C6 C7 123.3(3) . . ? C17 N6 C21 118.9(3) . . ? C17 N6 Ru1 125.7(2) . . ? C21 N6 Ru1 115.4(2) . . ? N5 C22 C23 121.6(3) . . ? N5 C22 C21 114.5(3) . . ? C23 C22 C21 123.9(3) . . ? N2 C2 C3 122.0(3) . . ? N5 C26 C25 122.7(4) . . ? C14 C15 C16 119.0(3) . . ? C24 C25 C26 119.4(4) . . ? N6 C21 C20 120.3(3) . . ? N6 C21 C22 115.7(3) . . ? C20 C21 C22 124.0(3) . . ? N6 C17 C18 122.9(3) . . ? N3 C7 C8 120.1(3) . . ? N3 C7 C6 112.8(3) . . ? C8 C7 C6 127.1(3) . . ? C25 C24 C23 119.0(3) . . ? C11 C10 C9 118.6(3) . . ? C20 C19 C18 119.9(3) . . ? C14 C13 C12 119.1(3) . . ? C4 C5 C6 118.8(4) . . ? C15 C14 C13 119.9(3) . . ? C24 C23 C22 119.8(4) . . ? N4 C12 C13 121.0(3) . . ? N4 C12 C11 115.1(2) . . ? C13 C12 C11 123.9(3) . . ? C17 C18 C19 118.3(4) . . ? N3 C11 C10 120.2(3) . . ? N3 C11 C12 112.7(2) . . ? C10 C11 C12 127.1(3) . . ? C8 C9 C10 120.5(3) . . ? C19 C20 C21 119.5(4) . . ? N1 C1 Ru1 175.8(3) . . ? C3 C4 C5 119.5(3) . . ? N4 C16 C15 122.0(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.154 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.089 #END data_1b _database_code_depnum_ccdc_archive 'CCDC 843187' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 F12 N18 O5 P2 Ru2' _chemical_formula_weight 1364.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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_space_group_name_H-M C2/c _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2142(8) _cell_length_b 20.1734(9) _cell_length_c 17.2470(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.311(5) _cell_angle_gamma 90.00 _cell_volume 5255.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 20286 _cell_measurement_theta_min 3.6873 _cell_measurement_theta_max 27.4245 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET) (compiled Oct 27 2009,12:04:35) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ? _diffrn_ambient_temperature 298(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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37688 _diffrn_reflns_av_R_equivalents 0.1366 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5734 _reflns_number_gt 4671 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+21.5232P] 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 5734 _refine_ls_number_parameters 382 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1899 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.27524(2) 0.459249(19) 0.06481(2) 0.04400(17) Uani 1 1 d . . . N9 N 0.4072(3) 0.4803(2) 0.0914(2) 0.0474(9) Uani 1 1 d . . . N4 N 0.3070(3) 0.4015(2) 0.1744(2) 0.0471(9) Uani 1 1 d . . . N8 N 0.3123(3) 0.3823(2) 0.0051(2) 0.0469(9) Uani 1 1 d . . . N6 N 0.2471(3) 0.5348(2) 0.1338(3) 0.0512(10) Uani 1 1 d . . . C11 C 0.1785(4) 0.4502(3) 0.1902(4) 0.0583(13) Uani 1 1 d . . . H11 H 0.1475 0.4480 0.2294 0.070 Uiso 1 1 calc R . . N2 N 0.1442(3) 0.4324(2) 0.0429(3) 0.0523(9) Uani 1 1 d . . . C13 C 0.5410(4) 0.5416(4) 0.1521(4) 0.0694(17) Uani 1 1 d . . . H13 H 0.5696 0.5786 0.1820 0.083 Uiso 1 1 calc R . . C1 C 0.2344(3) 0.5121(3) -0.0404(4) 0.0546(12) Uani 1 1 d . . . C12 C 0.4520(4) 0.5320(3) 0.1350(4) 0.0591(13) Uani 1 1 d . . . H12 H 0.4218 0.5628 0.1547 0.071 Uiso 1 1 calc R . . N5 N 0.2514(3) 0.4049(2) 0.2173(3) 0.0542(10) Uani 1 1 d . . . N1 N 0.2052(4) 0.5402(3) -0.1022(4) 0.0797(17) Uani 1 1 d . . . C15 C 0.5431(4) 0.4422(4) 0.0799(4) 0.0643(15) Uani 1 1 d . . . H15 H 0.5730 0.4112 0.0601 0.077 Uiso 1 1 calc R . . C2 C 0.3623(4) 0.3533(3) 0.2103(3) 0.0554(12) Uani 1 1 d . . . H2 H 0.4083 0.3397 0.1938 0.067 Uiso 1 1 calc R . . C14 C 0.5872(3) 0.4957(4) 0.1244(4) 0.0667(16) Uani 1 1 d . . . H14 H 0.6474 0.5011 0.1358 0.080 Uiso 1 1 calc R . . N7 N 0.2090(3) 0.5168(3) 0.1894(3) 0.0547(10) Uani 1 1 d . . . C17 C 0.3997(4) 0.3800(3) 0.0163(3) 0.0517(11) Uani 1 1 d . . . C16 C 0.4530(3) 0.4341(3) 0.0643(3) 0.0495(11) Uani 1 1 d . . . N3 N 0.1171(3) 0.4317(3) 0.1087(3) 0.0590(11) Uani 1 1 d . . . C19 C 0.2893(5) 0.2848(3) -0.0765(4) 0.0732(17) Uani 1 1 d . . . H19 H 0.2501 0.2533 -0.1091 0.088 Uiso 1 1 calc R . . C18 C 0.2592(4) 0.3349(3) -0.0401(3) 0.0595(13) Uani 1 1 d . . . H18 H 0.1995 0.3358 -0.0471 0.071 Uiso 1 1 calc R . . C10 C 0.0303(4) 0.4145(4) 0.0842(5) 0.0717(16) Uani 1 1 d . . . H10 H -0.0025 0.4101 0.1183 0.086 Uiso 1 1 calc R . . C8 C 0.0735(4) 0.4168(3) -0.0224(4) 0.0649(14) Uani 1 1 d . . . H8 H 0.0722 0.4140 -0.0766 0.078 Uiso 1 1 calc R . . C4 C 0.2725(4) 0.3583(3) 0.2780(3) 0.0615(13) Uani 1 1 d . . . H4 H 0.2431 0.3506 0.3144 0.074 Uiso 1 1 calc R . . C3 C 0.3438(4) 0.3250(3) 0.2759(4) 0.0647(14) Uani 1 1 d . . . H3 H 0.3740 0.2907 0.3107 0.078 Uiso 1 1 calc R . . C6 C 0.2309(5) 0.6228(4) 0.2052(5) 0.0773(18) Uani 1 1 d . . . H6 H 0.2337 0.6663 0.2239 0.093 Uiso 1 1 calc R . . C5 C 0.2598(4) 0.5988(3) 0.1435(4) 0.0618(13) Uani 1 1 d . . . H5 H 0.2848 0.6248 0.1133 0.074 Uiso 1 1 calc R . . C7 C 0.1982(4) 0.5702(4) 0.2320(4) 0.0680(16) Uani 1 1 d . . . H7 H 0.1727 0.5704 0.2724 0.082 Uiso 1 1 calc R . . C9 C 0.0009(4) 0.4050(4) 0.0010(5) 0.082(2) Uani 1 1 d . . . H9 H -0.0561 0.3931 -0.0336 0.099 Uiso 1 1 calc R . . C20 C 0.3771(6) 0.2813(4) -0.0649(5) 0.083(2) Uani 1 1 d . . . H20 H 0.3984 0.2470 -0.0885 0.100 Uiso 1 1 calc R . . P1 P 0.0000 0.67627(11) 0.2500 0.0590(5) Uani 1 2 d SD . . F3 F 0.0320(4) 0.6732(4) 0.1754(3) 0.137(2) Uani 1 1 d . B . F1 F 0.0998(3) 0.6758(4) 0.3050(4) 0.150(3) Uani 1 1 d . B . P2 P 0.0000 0.2477(2) 0.2500 0.1254(15) Uani 1 2 d SD . . C21 C 0.4335(5) 0.3292(3) -0.0179(5) 0.0747(17) Uani 1 1 d . . . H21 H 0.4935 0.3277 -0.0091 0.090 Uiso 1 1 calc R . . F6 F 0.0298(10) 0.2486(10) 0.3436(7) 0.292(8) Uani 1 1 d . A . F5A F -0.0406(16) 0.1788(8) 0.244(2) 0.236(9) Uani 0.50 1 d PD A -1 F5B F -0.0961(14) 0.2204(11) 0.237(2) 0.236(9) Uani 0.50 1 d PD A -2 F8A F -0.0024(17) 0.5979(6) 0.2675(12) 0.082(4) Uiso 0.25 1 d PD B -1 F8B F 0.0373(12) 0.6059(7) 0.2883(11) 0.082(4) Uiso 0.25 1 d PD B -2 F9A F -0.001(4) 0.7536(6) 0.256(2) 0.088(4) Uiso 0.25 1 d PD B -1 F9B F -0.0185(13) 0.7448(7) 0.2060(11) 0.088(4) Uiso 0.25 1 d PD B -2 F7 F 0.0633(10) 0.2955(9) 0.2448(13) 0.320(9) Uani 1 1 d . A . O1W O 0.8218(15) 0.3212(11) 0.0635(13) 0.313(9) Uani 1 1 d . . . O2WA O 0.349(2) 0.7270(16) 0.9647(18) 0.204(9) Uani 0.50 1 d P C 1 O2WB O 0.335(2) 0.6722(16) 0.9920(18) 0.204(9) Uani 0.50 1 d P D 2 O3W O 0.0301(15) 0.4690(8) 0.2746(10) 0.146(8) Uani 0.50 1 d P E -1 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 0.0389(2) 0.0559(3) 0.0395(2) -0.00103(15) 0.01703(16) 0.00332(14) N9 0.044(2) 0.059(2) 0.0407(19) 0.0026(18) 0.0177(16) 0.0080(17) N4 0.044(2) 0.058(2) 0.0433(19) -0.0012(17) 0.0206(16) 0.0041(17) N8 0.049(2) 0.056(2) 0.0381(18) 0.0041(17) 0.0185(16) 0.0037(17) N6 0.044(2) 0.060(3) 0.051(2) -0.0043(18) 0.0195(18) 0.0051(17) C11 0.051(3) 0.079(4) 0.053(3) 0.001(2) 0.028(2) 0.007(2) N2 0.045(2) 0.063(3) 0.050(2) -0.001(2) 0.0182(18) 0.0009(19) C13 0.049(3) 0.101(5) 0.051(3) 0.000(3) 0.009(2) -0.013(3) C1 0.048(3) 0.062(3) 0.058(3) 0.005(2) 0.025(2) 0.008(2) C12 0.055(3) 0.075(4) 0.050(3) -0.006(2) 0.022(2) -0.005(2) N5 0.057(2) 0.063(3) 0.050(2) 0.0020(19) 0.0297(19) 0.008(2) N1 0.084(4) 0.101(5) 0.060(3) 0.030(3) 0.033(3) 0.018(3) C15 0.049(3) 0.095(4) 0.053(3) 0.016(3) 0.023(2) 0.018(3) C2 0.058(3) 0.057(3) 0.051(3) -0.002(2) 0.020(2) 0.008(2) C14 0.036(2) 0.105(5) 0.059(3) 0.009(3) 0.017(2) -0.001(3) N7 0.051(2) 0.067(3) 0.052(2) -0.002(2) 0.0259(19) 0.012(2) C17 0.058(3) 0.058(3) 0.047(2) 0.010(2) 0.028(2) 0.011(2) C16 0.046(2) 0.063(3) 0.045(2) 0.009(2) 0.023(2) 0.011(2) N3 0.042(2) 0.078(3) 0.063(3) 0.001(2) 0.027(2) 0.000(2) C19 0.098(5) 0.061(3) 0.061(3) -0.011(3) 0.029(3) -0.004(3) C18 0.061(3) 0.064(3) 0.050(3) -0.003(2) 0.017(2) 0.001(3) C10 0.051(3) 0.087(4) 0.085(4) 0.006(3) 0.034(3) -0.003(3) C8 0.048(3) 0.080(4) 0.061(3) -0.007(3) 0.013(2) 0.001(3) C4 0.075(4) 0.066(3) 0.048(3) -0.003(2) 0.028(3) -0.001(3) C3 0.082(4) 0.058(3) 0.053(3) 0.004(2) 0.024(3) 0.010(3) C6 0.073(4) 0.071(4) 0.091(5) -0.018(4) 0.032(4) 0.020(3) C5 0.055(3) 0.060(3) 0.072(3) -0.003(3) 0.024(3) 0.007(2) C7 0.066(3) 0.081(4) 0.060(3) -0.009(3) 0.027(3) 0.025(3) C9 0.048(3) 0.101(5) 0.091(5) -0.003(4) 0.016(3) -0.010(3) C20 0.108(6) 0.068(4) 0.092(5) -0.010(4) 0.058(4) 0.014(4) P1 0.0442(9) 0.0618(12) 0.0633(12) 0.000 0.0103(8) 0.000 F3 0.103(4) 0.226(7) 0.087(3) -0.004(4) 0.042(3) -0.011(4) F1 0.062(3) 0.257(8) 0.107(4) -0.024(5) 0.002(3) 0.030(4) P2 0.181(4) 0.089(2) 0.157(4) 0.000 0.122(4) 0.000 C21 0.076(4) 0.068(4) 0.095(5) -0.001(3) 0.048(4) 0.016(3) F6 0.248(14) 0.50(3) 0.154(8) 0.014(12) 0.106(9) 0.007(16) F5A 0.24(2) 0.131(12) 0.38(2) -0.071(18) 0.17(2) -0.064(12) F5B 0.24(2) 0.131(12) 0.38(2) -0.071(18) 0.17(2) -0.064(12) F7 0.243(14) 0.332(19) 0.43(2) 0.075(17) 0.174(17) -0.101(13) O1W 0.33(2) 0.32(2) 0.30(2) 0.030(17) 0.127(18) 0.026(18) O2WA 0.209(15) 0.25(3) 0.173(17) -0.012(18) 0.094(12) 0.03(2) O2WB 0.209(15) 0.25(3) 0.173(17) -0.012(18) 0.094(12) 0.03(2) O3W 0.20(3) 0.159(13) 0.109(16) -0.002(9) 0.087(15) -0.043(12) _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 C1 1.999(6) . ? Ru1 N9 2.063(4) . ? Ru1 N8 2.069(4) . ? Ru1 N6 2.083(4) . ? Ru1 N2 2.090(4) . ? Ru1 N4 2.119(4) . ? N9 C12 1.334(7) . ? N9 C16 1.375(6) . ? N4 C2 1.314(7) . ? N4 N5 1.360(5) . ? N8 C18 1.333(7) . ? N8 C17 1.359(7) . ? N6 C5 1.309(7) . ? N6 N7 1.365(6) . ? C11 N5 1.432(7) . ? C11 N7 1.433(8) . ? C11 N3 1.445(8) . ? N2 C8 1.320(7) . ? N2 N3 1.357(6) . ? C13 C12 1.377(8) . ? C13 C14 1.381(10) . ? C1 N1 1.146(8) . ? N5 C4 1.355(7) . ? C15 C14 1.366(10) . ? C15 C16 1.395(7) . ? C2 C3 1.395(8) . ? N7 C7 1.351(7) . ? C17 C21 1.391(8) . ? C17 C16 1.450(8) . ? N3 C10 1.359(7) . ? C19 C20 1.366(11) . ? C19 C18 1.370(9) . ? C10 C9 1.351(11) . ? C8 C9 1.396(9) . ? C4 C3 1.347(9) . ? C6 C7 1.341(10) . ? C6 C5 1.397(9) . ? C20 C21 1.374(11) . ? P1 F1 1.550(5) . ? P1 F1 1.550(5) 2 ? P1 F9B 1.553(14) 2 ? P1 F9B 1.553(14) . ? P1 F3 1.554(5) . ? P1 F3 1.554(5) 2 ? P1 F9A 1.565(12) 2 ? P1 F9A 1.565(12) . ? P1 F8B 1.591(13) . ? P1 F8B 1.591(13) 2 ? P1 F8A 1.612(12) 2 ? P1 F8A 1.612(12) . ? P2 F7 1.435(11) . ? P2 F7 1.435(11) 2 ? P2 F6 1.508(12) . ? P2 F6 1.508(12) 2 ? P2 F5A 1.524(14) . ? P2 F5A 1.524(14) 2 ? P2 F5B 1.590(15) . ? P2 F5B 1.590(15) 2 ? 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 C1 Ru1 N9 93.79(19) . . ? C1 Ru1 N8 90.48(19) . . ? N9 Ru1 N8 78.45(16) . . ? C1 Ru1 N6 93.4(2) . . ? N9 Ru1 N6 98.46(17) . . ? N8 Ru1 N6 175.18(16) . . ? C1 Ru1 N2 89.67(19) . . ? N9 Ru1 N2 176.26(17) . . ? N8 Ru1 N2 100.14(17) . . ? N6 Ru1 N2 82.72(17) . . ? C1 Ru1 N4 175.12(18) . . ? N9 Ru1 N4 91.08(15) . . ? N8 Ru1 N4 90.62(15) . . ? N6 Ru1 N4 85.72(17) . . ? N2 Ru1 N4 85.46(16) . . ? C12 N9 C16 118.1(5) . . ? C12 N9 Ru1 126.5(4) . . ? C16 N9 Ru1 115.4(4) . . ? C2 N4 N5 104.8(4) . . ? C2 N4 Ru1 136.9(4) . . ? N5 N4 Ru1 117.6(3) . . ? C18 N8 C17 118.5(5) . . ? C18 N8 Ru1 125.9(4) . . ? C17 N8 Ru1 115.5(3) . . ? C5 N6 N7 105.3(5) . . ? C5 N6 Ru1 137.5(4) . . ? N7 N6 Ru1 117.1(3) . . ? N5 C11 N7 110.8(5) . . ? N5 C11 N3 110.3(5) . . ? N7 C11 N3 110.6(5) . . ? C8 N2 N3 105.4(4) . . ? C8 N2 Ru1 136.6(4) . . ? N3 N2 Ru1 117.9(3) . . ? C12 C13 C14 119.3(6) . . ? N1 C1 Ru1 175.0(6) . . ? N9 C12 C13 123.0(6) . . ? C4 N5 N4 110.7(4) . . ? C4 N5 C11 129.9(5) . . ? N4 N5 C11 119.1(4) . . ? C14 C15 C16 119.9(6) . . ? N4 C2 C3 111.9(5) . . ? C15 C14 C13 119.0(5) . . ? C7 N7 N6 110.6(5) . . ? C7 N7 C11 129.0(5) . . ? N6 N7 C11 120.1(4) . . ? N8 C17 C21 121.0(6) . . ? N8 C17 C16 115.5(4) . . ? C21 C17 C16 123.5(5) . . ? N9 C16 C15 120.8(5) . . ? N9 C16 C17 114.9(4) . . ? C15 C16 C17 124.3(5) . . ? N2 N3 C10 110.8(5) . . ? N2 N3 C11 119.5(4) . . ? C10 N3 C11 129.6(5) . . ? C20 C19 C18 119.9(6) . . ? N8 C18 C19 122.3(6) . . ? C9 C10 N3 107.0(6) . . ? N2 C8 C9 110.9(6) . . ? C3 C4 N5 107.6(5) . . ? C4 C3 C2 104.9(5) . . ? C7 C6 C5 105.8(6) . . ? N6 C5 C6 111.0(6) . . ? C6 C7 N7 107.4(6) . . ? C10 C9 C8 105.8(6) . . ? C19 C20 C21 119.0(6) . . ? F1 P1 F1 179.3(7) . 2 ? F1 P1 F9B 74.5(8) . 2 ? F1 P1 F9B 106.2(8) 2 2 ? F1 P1 F9B 106.2(8) . . ? F1 P1 F9B 74.5(8) 2 . ? F9B P1 F9B 54.3(14) 2 . ? F1 P1 F3 85.3(3) . . ? F1 P1 F3 94.7(3) 2 . ? F9B P1 F3 112.2(8) 2 . ? F9B P1 F3 72.2(8) . . ? F1 P1 F3 94.7(3) . 2 ? F1 P1 F3 85.3(3) 2 2 ? F9B P1 F3 72.2(8) 2 2 ? F9B P1 F3 112.2(8) . 2 ? F3 P1 F3 175.4(6) . 2 ? F1 P1 F9A 91(2) . 2 ? F1 P1 F9A 90(2) 2 2 ? F9B P1 F9A 30.6(16) 2 2 ? F9B P1 F9A 23.8(17) . 2 ? F3 P1 F9A 88.3(17) . 2 ? F3 P1 F9A 96.3(17) 2 2 ? F1 P1 F9A 90(2) . . ? F1 P1 F9A 91(2) 2 . ? F9B P1 F9A 23.8(17) 2 . ? F9B P1 F9A 30.6(15) . . ? F3 P1 F9A 96.3(17) . . ? F3 P1 F9A 88.3(17) 2 . ? F9A P1 F9A 8(3) 2 . ? F1 P1 F8B 65.5(7) . . ? F1 P1 F8B 113.8(8) 2 . ? F9B P1 F8B 127.9(10) 2 . ? F9B P1 F8B 167.1(10) . . ? F3 P1 F8B 96.8(8) . . ? F3 P1 F8B 79.1(8) 2 . ? F9A P1 F8B 155(2) 2 . ? F9A P1 F8B 151(2) . . ? F1 P1 F8B 113.8(8) . 2 ? F1 P1 F8B 65.5(7) 2 2 ? F9B P1 F8B 167.1(10) 2 2 ? F9B P1 F8B 127.9(10) . 2 ? F3 P1 F8B 79.1(8) . 2 ? F3 P1 F8B 96.8(8) 2 2 ? F9A P1 F8B 151(2) 2 2 ? F9A P1 F8B 155(2) . 2 ? F8B P1 F8B 53.5(13) . 2 ? F1 P1 F8A 91.0(10) . 2 ? F1 P1 F8A 88.3(9) 2 2 ? F9B P1 F8A 161.9(10) 2 2 ? F9B P1 F8A 142.6(9) . 2 ? F3 P1 F8A 76.6(7) . 2 ? F3 P1 F8A 98.8(7) 2 2 ? F9A P1 F8A 164.6(16) 2 2 ? F9A P1 F8A 172.7(16) . 2 ? F8B P1 F8A 34.0(9) . 2 ? F8B P1 F8A 22.8(10) 2 2 ? F1 P1 F8A 88.3(9) . . ? F1 P1 F8A 91.0(10) 2 . ? F9B P1 F8A 142.6(9) 2 . ? F9B P1 F8A 161.9(10) . . ? F3 P1 F8A 98.8(7) . . ? F3 P1 F8A 76.6(7) 2 . ? F9A P1 F8A 172.7(16) 2 . ? F9A P1 F8A 164.6(16) . . ? F8B P1 F8A 22.8(10) . . ? F8B P1 F8A 34.0(9) 2 . ? F8A P1 F8A 22.7(12) 2 . ? F7 P2 F7 95.5(16) . 2 ? F7 P2 F6 95.8(10) . . ? F7 P2 F6 83.3(10) 2 . ? F7 P2 F6 83.3(10) . 2 ? F7 P2 F6 95.8(10) 2 2 ? F6 P2 F6 178.6(16) . 2 ? F7 P2 F5A 155.3(12) . . ? F7 P2 F5A 108.5(11) 2 . ? F6 P2 F5A 92.8(15) . . ? F6 P2 F5A 88.4(15) 2 . ? F7 P2 F5A 108.5(11) . 2 ? F7 P2 F5A 155.3(12) 2 2 ? F6 P2 F5A 88.4(15) . 2 ? F6 P2 F5A 92.8(15) 2 2 ? F5A P2 F5A 48.5(17) . 2 ? F7 P2 F5B 155.6(14) . . ? F7 P2 F5B 63.5(10) 2 . ? F6 P2 F5B 94.0(14) . . ? F6 P2 F5B 86.5(13) 2 . ? F5A P2 F5B 45.5(10) . . ? F5A P2 F5B 94.0(14) 2 . ? F7 P2 F5B 63.5(10) . 2 ? F7 P2 F5B 155.6(14) 2 2 ? F6 P2 F5B 86.5(13) . 2 ? F6 P2 F5B 94.0(14) 2 2 ? F5A P2 F5B 94.0(14) . 2 ? F5A P2 F5B 45.5(10) 2 2 ? F5B P2 F5B 139.5(18) . 2 ? C20 C21 C17 119.2(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.803 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.119 #END data_2a _database_code_depnum_ccdc_archive 'CCDC 843188' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H19 F6 N6 P Ru S' _chemical_formula_weight 693.57 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.850(5) _cell_length_b 10.115(5) _cell_length_c 16.037(5) _cell_angle_alpha 77.086(5) _cell_angle_beta 78.323(5) _cell_angle_gamma 70.776(5) _cell_volume 1308.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3421 _cell_measurement_theta_min 3.6737 _cell_measurement_theta_max 28.9595 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_T_min 0.60460 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16981 _diffrn_reflns_av_R_equivalents 0.1289 _diffrn_reflns_av_sigmaI/netI 0.1931 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 26.99 _reflns_number_total 5652 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 5652 _refine_ls_number_parameters 373 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1835 _refine_ls_R_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.3574 _refine_ls_wR_factor_gt 0.3379 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45216(13) 0.39329(12) 0.79196(7) 0.0326(4) Uani 1 1 d . . . S1 S 0.2546(5) 0.1017(5) 1.0433(3) 0.0546(11) Uani 1 1 d . . . P1 P 0.1453(6) 0.0583(5) 0.6403(3) 0.0631(13) Uani 1 1 d D . . N105 N 0.5457(14) 0.4814(12) 0.6737(6) 0.041(3) Uani 1 1 d . . . C103 C 0.6391(16) 0.4852(15) 0.8840(8) 0.035(3) Uani 1 1 d . . . C110 C 0.1416(15) 0.6109(14) 0.7837(8) 0.034(3) Uani 1 1 d . . . C100 C 0.3199(17) 0.2072(16) 0.9602(9) 0.044(4) Uani 1 1 d . . . C106 C 0.4864(15) 0.5954(14) 0.8819(8) 0.033(3) Uani 1 1 d . . . C109 C 0.2337(14) 0.6599(14) 0.8314(8) 0.034(3) Uani 1 1 d . . . N104 N 0.5444(13) 0.2184(12) 0.7286(7) 0.034(3) Uani 1 1 d . . . N101 N 0.2231(14) 0.4819(11) 0.7586(7) 0.037(3) Uani 1 1 d . . . F2 F 0.0842(19) 0.040(2) 0.5628(10) 0.157(8) Uani 1 1 d . A . C102 C 0.6287(16) 0.3892(15) 0.6167(8) 0.038(3) Uani 1 1 d . . . C104 C 0.7963(18) 0.2644(17) 0.8441(10) 0.049(4) Uani 1 1 d . . . H104 H 0.8095 0.1903 0.8152 0.059 Uiso 1 1 calc R . . C107 C 0.4407(17) 0.7213(15) 0.9131(9) 0.043(3) Uani 1 1 d . . . H107 H 0.5115 0.7427 0.9399 0.051 Uiso 1 1 calc R . . C108 C 0.288(2) 0.8158(17) 0.9042(10) 0.050(4) Uani 1 1 d . . . H108 H 0.2563 0.9006 0.9255 0.060 Uiso 1 1 calc R . . N102 N 0.3796(13) 0.5689(11) 0.8417(6) 0.031(2) Uani 1 1 d . . . C105 C 0.9209(16) 0.2613(18) 0.8840(10) 0.047(4) Uani 1 1 d . . . H105 H 1.0141 0.1842 0.8846 0.056 Uiso 1 1 calc R . . N100 N 0.3644(12) 0.2789(12) 0.9028(7) 0.033(2) Uani 1 1 d . . . N103 N 0.6560(13) 0.3696(12) 0.8449(7) 0.034(2) Uani 1 1 d . . . C101 C 0.704(2) 0.4361(19) 0.5384(10) 0.060(5) Uani 1 1 d . . . H101 H 0.7629 0.3726 0.5012 0.072 Uiso 1 1 calc R . . C26 C -0.0088(18) 0.6845(17) 0.7634(10) 0.051(4) Uani 1 1 d . . . H26 H -0.0630 0.7707 0.7822 0.061 Uiso 1 1 calc R . . C27 C 0.9057(18) 0.3761(19) 0.9238(10) 0.055(4) Uani 1 1 d . . . H27 H 0.9904 0.3770 0.9496 0.066 Uiso 1 1 calc R . . C28 C 0.1458(17) 0.4295(16) 0.7151(8) 0.039(3) Uani 1 1 d . . . H28 H 0.1982 0.3405 0.6996 0.047 Uiso 1 1 calc R . . C29 C 0.7629(17) 0.4891(17) 0.9245(9) 0.045(4) Uani 1 1 d . . . H29 H 0.7505 0.5652 0.9514 0.054 Uiso 1 1 calc R . . C30 C -0.0016(19) 0.4983(18) 0.6931(10) 0.053(4) Uani 1 1 d . . . H30 H -0.0505 0.4580 0.6635 0.063 Uiso 1 1 calc R . . C31 C 0.1817(16) 0.7841(16) 0.8633(9) 0.041(3) Uani 1 1 d . . . H31 H 0.0785 0.8461 0.8580 0.050 Uiso 1 1 calc R . . C32 C -0.0806(18) 0.6332(16) 0.7160(11) 0.053(4) Uani 1 1 d . . . H32 H -0.1805 0.6863 0.6989 0.063 Uiso 1 1 calc R . . C33 C 0.692(2) 0.580(2) 0.5142(11) 0.065(5) Uani 1 1 d . . . H33 H 0.7485 0.6126 0.4625 0.078 Uiso 1 1 calc R . . C34 C 0.6235(16) 0.2423(15) 0.6485(8) 0.039(3) Uani 1 1 d . . . C35 C 0.6913(18) 0.1357(18) 0.5979(10) 0.050(4) Uani 1 1 d . . . H35 H 0.7457 0.1538 0.5426 0.060 Uiso 1 1 calc R . . F4 F -0.0014(15) 0.0191(17) 0.7010(9) 0.114(5) Uani 1 1 d . A . C37 C 0.598(2) 0.6717(19) 0.5663(10) 0.059(4) Uani 1 1 d . . . H37 H 0.5766 0.7691 0.5478 0.070 Uiso 1 1 calc R . . F6 F 0.029(2) 0.2179(17) 0.6279(13) 0.150(7) Uani 1 1 d . A . F3 F 0.2535(19) -0.0956(15) 0.6602(11) 0.153(8) Uani 1 1 d . A . C41 C 0.5330(17) 0.6200(15) 0.6468(9) 0.043(3) Uani 1 1 d . . . H41 H 0.4778 0.6833 0.6846 0.051 Uiso 1 1 calc R . . C42 C 0.675(2) 0.0033(18) 0.6324(12) 0.060(4) Uani 1 1 d . . . H42 H 0.7169 -0.0695 0.5999 0.071 Uiso 1 1 calc R . . F5 F 0.191(2) 0.083(2) 0.7243(12) 0.156(7) Uani 1 1 d . A . C44 C 0.5335(17) 0.0858(15) 0.7610(9) 0.043(3) Uani 1 1 d . . . H44 H 0.4811 0.0674 0.8168 0.051 Uiso 1 1 calc R . . C45 C 0.598(2) -0.0214(18) 0.7138(12) 0.058(4) Uani 1 1 d . . . H45 H 0.5883 -0.1116 0.7374 0.070 Uiso 1 1 calc R . . F1A F 0.280(5) 0.136(6) 0.604(2) 0.116(14) Uani 0.50 1 d PD A 1 F1B F 0.290(5) 0.077(6) 0.567(2) 0.116(14) Uani 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0297(6) 0.0250(6) 0.0424(6) -0.0101(4) -0.0045(4) -0.0046(4) S1 0.053(2) 0.055(3) 0.057(2) -0.0021(19) -0.0029(18) -0.025(2) P1 0.061(3) 0.042(3) 0.082(3) -0.005(2) -0.011(2) -0.014(2) N105 0.051(7) 0.033(7) 0.026(5) -0.008(4) -0.006(5) 0.005(5) C103 0.035(7) 0.032(8) 0.036(7) -0.005(5) -0.003(5) -0.009(6) C110 0.033(7) 0.021(7) 0.050(8) -0.013(5) -0.006(6) -0.006(6) C100 0.038(8) 0.035(8) 0.045(8) -0.016(7) -0.014(6) 0.019(7) C106 0.028(7) 0.027(7) 0.038(7) -0.008(5) -0.001(5) -0.001(5) C109 0.016(6) 0.032(7) 0.051(8) -0.016(6) 0.001(5) -0.003(5) N104 0.030(6) 0.027(6) 0.044(6) -0.006(5) -0.009(5) -0.003(5) N101 0.043(7) 0.020(6) 0.044(6) -0.008(5) -0.003(5) -0.005(5) F2 0.120(12) 0.21(2) 0.132(12) -0.108(13) -0.034(10) 0.017(13) C102 0.040(8) 0.034(8) 0.036(7) -0.010(6) -0.003(6) -0.004(6) C104 0.047(9) 0.045(10) 0.056(9) -0.010(7) -0.007(7) -0.014(8) C107 0.039(8) 0.033(8) 0.057(9) -0.018(6) -0.014(6) -0.002(6) C108 0.064(11) 0.034(9) 0.060(9) -0.023(7) -0.008(7) -0.015(8) N102 0.034(6) 0.024(6) 0.040(6) -0.012(4) -0.003(4) -0.012(5) C105 0.019(7) 0.051(10) 0.068(10) -0.008(7) -0.014(6) -0.003(7) N100 0.028(6) 0.033(6) 0.049(7) -0.010(5) -0.004(5) -0.020(5) N103 0.030(6) 0.024(6) 0.044(6) -0.002(4) -0.002(4) -0.006(5) C101 0.062(11) 0.047(11) 0.053(9) -0.016(8) 0.015(8) -0.001(9) C26 0.035(8) 0.036(9) 0.075(11) -0.018(7) -0.009(7) 0.007(7) C27 0.035(9) 0.062(12) 0.066(10) -0.004(8) -0.022(7) -0.008(8) C28 0.044(9) 0.039(8) 0.046(8) -0.019(6) -0.006(6) -0.020(7) C29 0.035(8) 0.048(10) 0.055(9) -0.012(7) -0.008(6) -0.014(7) C30 0.048(10) 0.049(10) 0.060(10) -0.016(7) -0.014(7) -0.005(8) C31 0.023(7) 0.043(9) 0.061(9) -0.019(7) -0.002(6) -0.009(6) C32 0.037(8) 0.031(9) 0.084(11) -0.015(7) -0.019(7) 0.007(7) C33 0.076(13) 0.058(12) 0.054(10) -0.007(8) 0.015(9) -0.025(10) C34 0.032(7) 0.034(8) 0.047(8) -0.016(6) -0.014(6) 0.005(6) C35 0.041(9) 0.050(10) 0.053(9) -0.022(7) -0.001(7) -0.001(7) F4 0.070(8) 0.125(13) 0.153(12) -0.018(9) -0.006(8) -0.045(9) C37 0.076(12) 0.045(10) 0.061(10) -0.001(8) -0.015(9) -0.029(9) F6 0.127(13) 0.064(10) 0.26(2) -0.011(11) -0.075(13) -0.017(9) F3 0.112(12) 0.055(9) 0.213(17) 0.003(9) 0.027(11) 0.031(8) C41 0.045(9) 0.025(8) 0.059(9) -0.006(6) -0.009(7) -0.010(7) C42 0.059(11) 0.036(10) 0.083(12) -0.034(8) -0.004(9) -0.002(8) F5 0.162(16) 0.151(18) 0.174(15) -0.052(12) -0.088(13) -0.016(13) C44 0.043(8) 0.027(8) 0.053(9) -0.006(6) -0.004(6) -0.005(6) C45 0.051(10) 0.030(9) 0.092(13) -0.024(8) -0.007(9) -0.003(7) F1A 0.083(11) 0.16(4) 0.11(2) 0.04(2) -0.022(17) -0.08(2) F1B 0.083(11) 0.16(4) 0.11(2) 0.04(2) -0.022(17) -0.08(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N102 1.970(10) . ? Ru1 N105 2.042(11) . ? Ru1 N100 2.053(11) . ? Ru1 N101 2.056(12) . ? Ru1 N103 2.068(11) . ? Ru1 N104 2.085(11) . ? S1 C100 1.646(17) . ? P1 F2 1.518(15) . ? P1 F3 1.537(14) . ? P1 F4 1.564(13) . ? P1 F5 1.574(16) . ? P1 F1A 1.584(18) . ? P1 F1B 1.584(19) . ? P1 F6 1.596(17) . ? N105 C41 1.345(18) . ? N105 C102 1.380(17) . ? C103 N103 1.398(17) . ? C103 C29 1.398(19) . ? C103 C106 1.442(18) . ? C110 C26 1.359(19) . ? C110 N101 1.372(16) . ? C110 C109 1.478(18) . ? C100 N100 1.127(18) . ? C106 N102 1.368(17) . ? C106 C107 1.378(19) . ? C109 N102 1.333(16) . ? C109 C31 1.365(19) . ? N104 C34 1.345(16) . ? N104 C44 1.353(18) . ? N101 C28 1.354(17) . ? C102 C101 1.359(19) . ? C102 C34 1.47(2) . ? C104 N103 1.343(19) . ? C104 C105 1.37(2) . ? C107 C108 1.39(2) . ? C108 C31 1.40(2) . ? C105 C27 1.40(2) . ? C101 C33 1.40(2) . ? C26 C32 1.36(2) . ? C27 C29 1.40(2) . ? C28 C30 1.34(2) . ? C30 C32 1.41(2) . ? C33 C37 1.34(2) . ? C34 C35 1.40(2) . ? C35 C42 1.37(2) . ? C37 C41 1.36(2) . ? C42 C45 1.36(2) . ? C44 C45 1.36(2) . ? 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 N102 Ru1 N105 95.4(4) . . ? N102 Ru1 N100 92.9(4) . . ? N105 Ru1 N100 171.6(4) . . ? N102 Ru1 N101 78.9(4) . . ? N105 Ru1 N101 90.2(4) . . ? N100 Ru1 N101 90.3(4) . . ? N102 Ru1 N103 80.5(4) . . ? N105 Ru1 N103 92.0(4) . . ? N100 Ru1 N103 90.5(4) . . ? N101 Ru1 N103 159.3(4) . . ? N102 Ru1 N104 173.7(4) . . ? N105 Ru1 N104 78.5(4) . . ? N100 Ru1 N104 93.2(4) . . ? N101 Ru1 N104 102.7(4) . . ? N103 Ru1 N104 97.9(4) . . ? F2 P1 F3 96.6(11) . . ? F2 P1 F4 90.0(10) . . ? F3 P1 F4 90.9(8) . . ? F2 P1 F5 174.4(10) . . ? F3 P1 F5 86.8(11) . . ? F4 P1 F5 85.6(10) . . ? F2 P1 F1A 107.3(16) . . ? F3 P1 F1A 100(2) . . ? F4 P1 F1A 158.4(17) . . ? F5 P1 F1A 76.3(16) . . ? F2 P1 F1B 79.8(16) . . ? F3 P1 F1B 84(2) . . ? F4 P1 F1B 168.2(16) . . ? F5 P1 F1B 105.0(16) . . ? F1A P1 F1B 33(2) . . ? F2 P1 F6 87.1(10) . . ? F3 P1 F6 175.3(11) . . ? F4 P1 F6 86.3(9) . . ? F5 P1 F6 89.3(10) . . ? F1A P1 F6 82(2) . . ? F1B P1 F6 99(2) . . ? C41 N105 C102 117.6(12) . . ? C41 N105 Ru1 126.0(9) . . ? C102 N105 Ru1 116.4(9) . . ? N103 C103 C29 120.9(13) . . ? N103 C103 C106 116.1(12) . . ? C29 C103 C106 123.0(13) . . ? C26 C110 N101 121.1(12) . . ? C26 C110 C109 125.0(12) . . ? N101 C110 C109 113.9(11) . . ? N100 C100 S1 179.5(15) . . ? N102 C106 C107 118.4(12) . . ? N102 C106 C103 113.8(12) . . ? C107 C106 C103 127.7(13) . . ? N102 C109 C31 120.9(12) . . ? N102 C109 C110 113.1(11) . . ? C31 C109 C110 126.0(12) . . ? C34 N104 C44 118.4(12) . . ? C34 N104 Ru1 115.4(9) . . ? C44 N104 Ru1 126.2(9) . . ? C28 N101 C110 117.3(12) . . ? C28 N101 Ru1 128.2(9) . . ? C110 N101 Ru1 114.6(9) . . ? C101 C102 N105 120.8(14) . . ? C101 C102 C34 125.3(13) . . ? N105 C102 C34 113.9(11) . . ? N103 C104 C105 122.9(15) . . ? C106 C107 C108 119.4(14) . . ? C107 C108 C31 120.4(14) . . ? C109 N102 C106 122.7(11) . . ? C109 N102 Ru1 119.5(9) . . ? C106 N102 Ru1 117.7(9) . . ? C104 C105 C27 119.0(14) . . ? C100 N100 Ru1 174.4(12) . . ? C104 N103 C103 118.7(12) . . ? C104 N103 Ru1 129.3(11) . . ? C103 N103 Ru1 111.9(8) . . ? C102 C101 C33 119.5(15) . . ? C32 C26 C110 120.5(14) . . ? C29 C27 C105 119.7(15) . . ? C30 C28 N101 123.8(14) . . ? C27 C29 C103 118.6(15) . . ? C28 C30 C32 118.2(15) . . ? C109 C31 C108 118.2(13) . . ? C26 C32 C30 118.9(14) . . ? C37 C33 C101 119.4(15) . . ? N104 C34 C35 122.0(14) . . ? N104 C34 C102 115.6(11) . . ? C35 C34 C102 122.4(13) . . ? C42 C35 C34 117.8(15) . . ? C33 C37 C41 119.2(16) . . ? N105 C41 C37 122.9(14) . . ? C45 C42 C35 120.1(15) . . ? C45 C44 N104 121.5(14) . . ? C44 C45 C42 120.1(16) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.410 _refine_diff_density_min -1.632 _refine_diff_density_rms 0.232 #END data_2b _database_code_depnum_ccdc_archive 'CCDC 843189' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 F6 N9 P Ru S' _chemical_formula_weight 674.54 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6230(2) _cell_length_b 10.4796(2) _cell_length_c 14.7558(4) _cell_angle_alpha 87.312(2) _cell_angle_beta 81.518(2) _cell_angle_gamma 73.325(2) _cell_volume 1263.36(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 12784 _cell_measurement_theta_min 3.6246 _cell_measurement_theta_max 28.7493 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.1708 _exptl_crystal_size_mid 0.1092 _exptl_crystal_size_min 0.0393 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20783 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5148 _reflns_number_gt 4392 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.9090P] 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 5148 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.12620(3) 0.22621(2) 0.699210(18) 0.03587(10) Uani 1 1 d . . . P1 P -0.25034(13) 0.27044(10) 1.04751(8) 0.0544(2) Uani 1 1 d . . . S1 S 0.52463(14) -0.19399(11) 0.62731(9) 0.0671(3) Uani 1 1 d . . . F2 F -0.3956(4) 0.2058(3) 1.0819(2) 0.0937(9) Uani 1 1 d . . . F3 F -0.2028(4) 0.2598(3) 1.14886(19) 0.0870(8) Uani 1 1 d . . . F4 F -0.3743(3) 0.4132(2) 1.0757(2) 0.0858(8) Uani 1 1 d . . . F1 F -0.1306(4) 0.1283(3) 1.0264(2) 0.0907(9) Uani 1 1 d . . . N8 N 0.2886(3) 0.3399(3) 0.66304(18) 0.0391(6) Uani 1 1 d . . . N7 N 0.2352(3) 0.3206(3) 0.85880(18) 0.0384(6) Uani 1 1 d . . . N3 N 0.0248(3) 0.2424(3) 0.58005(19) 0.0419(6) Uani 1 1 d . . . C1 C 0.3911(4) -0.0493(4) 0.6434(2) 0.0461(8) Uani 1 1 d . . . C21 C 0.1849(4) 0.4456(3) 0.8110(2) 0.0371(6) Uani 1 1 d . . . H21 H 0.2024 0.5157 0.8466 0.045 Uiso 1 1 calc R . . N6 N 0.2224(3) 0.2081(3) 0.82206(19) 0.0404(6) Uani 1 1 d . . . N4 N -0.0397(3) 0.3968(3) 0.75314(18) 0.0373(6) Uani 1 1 d . . . F6 F -0.2982(4) 0.2851(3) 0.9484(2) 0.0909(9) Uani 1 1 d . . . N5 N 0.0139(3) 0.4796(3) 0.80058(18) 0.0383(6) Uani 1 1 d . . . C14 C -0.1096(4) 0.5843(3) 0.8350(3) 0.0495(8) Uani 1 1 d . . . H14 H -0.1013 0.6528 0.8702 0.059 Uiso 1 1 calc R . . N9 N 0.2843(3) 0.4376(2) 0.72201(18) 0.0372(6) Uani 1 1 d . . . C6 C -0.1208(4) 0.1023(3) 0.6632(3) 0.0459(8) Uani 1 1 d . . . N2 N -0.0383(3) 0.1182(3) 0.73184(19) 0.0416(6) Uani 1 1 d . . . C18 C 0.4020(4) 0.4980(4) 0.6941(3) 0.0466(8) Uani 1 1 d . . . H18 H 0.4233 0.5661 0.7239 0.056 Uiso 1 1 calc R . . F5 F -0.1117(4) 0.3415(3) 1.0173(2) 0.0979(9) Uani 1 1 d . . . N1 N 0.2977(4) 0.0554(3) 0.6542(2) 0.0533(8) Uani 1 1 d . . . C20 C 0.4097(4) 0.3420(4) 0.5972(2) 0.0504(8) Uani 1 1 d . . . H20 H 0.4416 0.2859 0.5466 0.061 Uiso 1 1 calc R . . C15 C 0.3190(4) 0.2922(4) 0.9311(2) 0.0496(8) Uani 1 1 d . . . H15 H 0.3447 0.3527 0.9662 0.060 Uiso 1 1 calc R . . C7 C -0.0845(4) 0.1715(3) 0.5777(3) 0.0448(8) Uani 1 1 d . . . C19 C 0.4832(5) 0.4398(4) 0.6137(3) 0.0578(10) Uani 1 1 d . . . H19 H 0.5701 0.4607 0.5771 0.069 Uiso 1 1 calc R . . C16 C 0.3581(5) 0.1585(4) 0.9425(3) 0.0587(10) Uani 1 1 d . . . H16 H 0.4148 0.1089 0.9874 0.070 Uiso 1 1 calc R . . C8 C -0.1529(5) 0.1674(4) 0.4987(3) 0.0566(10) Uani 1 1 d . . . H8 H -0.2249 0.1164 0.4978 0.068 Uiso 1 1 calc R . . C3 C -0.1739(5) -0.0149(5) 0.8297(3) 0.0677(12) Uani 1 1 d . . . H3 H -0.1898 -0.0541 0.8868 0.081 Uiso 1 1 calc R . . C2 C -0.0659(5) 0.0600(4) 0.8127(3) 0.0551(9) Uani 1 1 d . . . H2 H -0.0094 0.0708 0.8595 0.066 Uiso 1 1 calc R . . C13 C -0.2475(5) 0.5708(4) 0.8086(3) 0.0610(10) Uani 1 1 d . . . H13 H -0.3525 0.6282 0.8213 0.073 Uiso 1 1 calc R . . C5 C -0.2313(5) 0.0284(4) 0.6766(3) 0.0628(11) Uani 1 1 d . . . H5 H -0.2873 0.0185 0.6293 0.075 Uiso 1 1 calc R . . C11 C 0.0601(5) 0.3116(4) 0.5051(3) 0.0551(9) Uani 1 1 d . . . H11 H 0.1326 0.3620 0.5069 0.066 Uiso 1 1 calc R . . C9 C -0.1148(5) 0.2381(5) 0.4221(3) 0.0664(11) Uani 1 1 d . . . H9 H -0.1610 0.2364 0.3693 0.080 Uiso 1 1 calc R . . C12 C -0.1999(4) 0.4527(4) 0.7583(3) 0.0511(8) Uani 1 1 d . . . H12 H -0.2707 0.4181 0.7320 0.061 Uiso 1 1 calc R . . C17 C 0.2968(5) 0.1103(4) 0.8736(3) 0.0533(9) Uani 1 1 d . . . H17 H 0.3068 0.0208 0.8651 0.064 Uiso 1 1 calc R . . C4 C -0.2584(6) -0.0313(5) 0.7613(3) 0.0705(12) Uani 1 1 d . . . H4 H -0.3325 -0.0816 0.7715 0.085 Uiso 1 1 calc R . . C10 C -0.0060(6) 0.3118(5) 0.4255(3) 0.0659(11) Uani 1 1 d . . . H10 H 0.0222 0.3608 0.3748 0.079 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 0.03291(14) 0.03440(14) 0.04447(16) -0.00329(10) -0.01233(10) -0.01220(10) P1 0.0553(6) 0.0441(5) 0.0663(6) -0.0079(4) -0.0178(5) -0.0122(4) S1 0.0580(6) 0.0542(6) 0.0861(8) -0.0258(5) -0.0148(5) -0.0049(5) F2 0.089(2) 0.0686(17) 0.133(3) -0.0013(17) -0.0146(19) -0.0383(15) F3 0.103(2) 0.0856(18) 0.0688(16) -0.0106(14) -0.0299(15) -0.0099(16) F4 0.0782(18) 0.0477(13) 0.129(2) -0.0148(14) -0.0235(17) -0.0068(12) F1 0.100(2) 0.0686(16) 0.0838(19) -0.0192(14) -0.0201(16) 0.0134(15) N8 0.0352(14) 0.0432(14) 0.0414(15) -0.0052(11) -0.0086(11) -0.0128(11) N7 0.0392(14) 0.0396(14) 0.0408(14) 0.0015(11) -0.0151(11) -0.0135(11) N3 0.0376(14) 0.0406(14) 0.0489(16) -0.0069(12) -0.0119(12) -0.0090(11) C1 0.0405(18) 0.058(2) 0.0469(19) -0.0125(16) -0.0087(15) -0.0224(16) C21 0.0344(16) 0.0379(15) 0.0420(17) -0.0022(13) -0.0091(13) -0.0128(12) N6 0.0396(14) 0.0352(13) 0.0502(16) 0.0011(11) -0.0128(12) -0.0138(11) N4 0.0308(13) 0.0404(14) 0.0434(15) -0.0007(11) -0.0099(11) -0.0121(11) F6 0.109(2) 0.0849(19) 0.0818(19) 0.0001(15) -0.0434(17) -0.0177(17) N5 0.0327(13) 0.0374(13) 0.0450(15) -0.0045(11) -0.0089(11) -0.0079(10) C14 0.0463(19) 0.0440(18) 0.055(2) -0.0085(15) -0.0049(16) -0.0068(15) N9 0.0354(13) 0.0373(13) 0.0429(14) -0.0021(11) -0.0095(11) -0.0144(11) C6 0.0412(18) 0.0441(18) 0.058(2) -0.0112(15) -0.0129(16) -0.0155(14) N2 0.0402(15) 0.0397(14) 0.0493(16) -0.0042(12) -0.0110(12) -0.0152(11) C18 0.0415(18) 0.0503(19) 0.056(2) 0.0046(16) -0.0130(16) -0.0237(15) F5 0.0738(19) 0.126(3) 0.107(2) 0.001(2) -0.0088(17) -0.0515(18) N1 0.0495(18) 0.0406(16) 0.077(2) -0.0075(14) -0.0264(16) -0.0141(14) C20 0.0418(19) 0.068(2) 0.0432(19) -0.0062(16) -0.0048(15) -0.0171(17) C15 0.0453(19) 0.062(2) 0.047(2) 0.0020(16) -0.0201(16) -0.0166(16) C7 0.0388(17) 0.0401(17) 0.057(2) -0.0108(15) -0.0155(15) -0.0083(13) C19 0.047(2) 0.082(3) 0.054(2) 0.005(2) -0.0055(17) -0.034(2) C16 0.058(2) 0.062(2) 0.062(2) 0.0158(19) -0.030(2) -0.0165(19) C8 0.053(2) 0.060(2) 0.064(2) -0.0122(19) -0.0259(19) -0.0170(17) C3 0.068(3) 0.074(3) 0.073(3) 0.007(2) -0.005(2) -0.041(2) C2 0.057(2) 0.063(2) 0.056(2) -0.0023(18) -0.0126(18) -0.0309(19) C13 0.0373(19) 0.061(2) 0.078(3) -0.010(2) -0.0056(18) -0.0023(16) C5 0.057(2) 0.071(3) 0.077(3) -0.008(2) -0.021(2) -0.036(2) C11 0.056(2) 0.061(2) 0.056(2) 0.0039(18) -0.0191(18) -0.0222(18) C9 0.064(3) 0.081(3) 0.059(3) -0.007(2) -0.031(2) -0.016(2) C12 0.0354(18) 0.057(2) 0.063(2) -0.0013(17) -0.0163(16) -0.0109(15) C17 0.053(2) 0.0415(18) 0.070(2) 0.0113(17) -0.0219(19) -0.0149(16) C4 0.064(3) 0.079(3) 0.087(3) -0.003(2) -0.011(2) -0.048(2) C10 0.070(3) 0.079(3) 0.052(2) 0.006(2) -0.023(2) -0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.034(3) . ? Ru1 N2 2.048(3) . ? Ru1 N4 2.051(3) . ? Ru1 N3 2.056(3) . ? Ru1 N6 2.081(3) . ? Ru1 N8 2.084(3) . ? P1 F1 1.565(3) . ? P1 F6 1.567(3) . ? P1 F5 1.582(3) . ? P1 F2 1.597(3) . ? P1 F3 1.599(3) . ? P1 F4 1.601(3) . ? S1 C1 1.622(4) . ? N8 C20 1.322(4) . ? N8 N9 1.363(4) . ? N7 C15 1.350(4) . ? N7 N6 1.360(4) . ? N7 C21 1.441(4) . ? N3 C11 1.339(5) . ? N3 C7 1.362(4) . ? C1 N1 1.161(5) . ? C21 N5 1.444(4) . ? C21 N9 1.451(4) . ? N6 C17 1.317(4) . ? N4 C12 1.328(4) . ? N4 N5 1.357(4) . ? N5 C14 1.348(4) . ? C14 C13 1.351(5) . ? N9 C18 1.350(4) . ? C6 N2 1.362(4) . ? C6 C5 1.379(5) . ? C6 C7 1.465(5) . ? N2 C2 1.335(5) . ? C18 C19 1.359(5) . ? C20 C19 1.397(5) . ? C15 C16 1.352(5) . ? C7 C8 1.389(5) . ? C16 C17 1.389(5) . ? C8 C9 1.374(6) . ? C3 C2 1.371(5) . ? C3 C4 1.372(6) . ? C13 C12 1.398(5) . ? C5 C4 1.391(6) . ? C11 C10 1.379(5) . ? C9 C10 1.383(6) . ? 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 N2 88.69(12) . . ? N1 Ru1 N4 175.92(11) . . ? N2 Ru1 N4 91.95(10) . . ? N1 Ru1 N3 90.88(12) . . ? N2 Ru1 N3 78.78(11) . . ? N4 Ru1 N3 93.19(10) . . ? N1 Ru1 N6 89.68(12) . . ? N2 Ru1 N6 99.49(11) . . ? N4 Ru1 N6 86.24(10) . . ? N3 Ru1 N6 178.17(11) . . ? N1 Ru1 N8 92.26(11) . . ? N2 Ru1 N8 178.11(11) . . ? N4 Ru1 N8 87.22(10) . . ? N3 Ru1 N8 99.56(11) . . ? N6 Ru1 N8 82.16(10) . . ? F1 P1 F6 91.88(16) . . ? F1 P1 F5 93.00(19) . . ? F6 P1 F5 91.10(18) . . ? F1 P1 F2 89.97(18) . . ? F6 P1 F2 90.35(18) . . ? F5 P1 F2 176.65(18) . . ? F1 P1 F3 89.52(15) . . ? F6 P1 F3 178.45(16) . . ? F5 P1 F3 88.14(18) . . ? F2 P1 F3 90.34(18) . . ? F1 P1 F4 176.44(18) . . ? F6 P1 F4 91.29(16) . . ? F5 P1 F4 88.58(17) . . ? F2 P1 F4 88.38(16) . . ? F3 P1 F4 87.34(16) . . ? C20 N8 N9 104.9(3) . . ? C20 N8 Ru1 137.6(2) . . ? N9 N8 Ru1 117.40(19) . . ? C15 N7 N6 111.3(3) . . ? C15 N7 C21 128.7(3) . . ? N6 N7 C21 119.2(2) . . ? C11 N3 C7 118.1(3) . . ? C11 N3 Ru1 126.3(2) . . ? C7 N3 Ru1 115.6(2) . . ? N1 C1 S1 178.8(4) . . ? N7 C21 N5 111.4(2) . . ? N7 C21 N9 109.4(2) . . ? N5 C21 N9 110.2(3) . . ? C17 N6 N7 104.9(3) . . ? C17 N6 Ru1 136.8(2) . . ? N7 N6 Ru1 117.73(19) . . ? C12 N4 N5 104.7(3) . . ? C12 N4 Ru1 136.8(2) . . ? N5 N4 Ru1 118.47(19) . . ? C14 N5 N4 111.8(3) . . ? C14 N5 C21 128.9(3) . . ? N4 N5 C21 119.3(2) . . ? N5 C14 C13 106.9(3) . . ? C18 N9 N8 111.7(3) . . ? C18 N9 C21 127.9(3) . . ? N8 N9 C21 119.0(2) . . ? N2 C6 C5 121.1(4) . . ? N2 C6 C7 114.6(3) . . ? C5 C6 C7 124.3(3) . . ? C2 N2 C6 118.6(3) . . ? C2 N2 Ru1 125.4(2) . . ? C6 N2 Ru1 116.0(2) . . ? N9 C18 C19 106.4(3) . . ? C1 N1 Ru1 168.6(3) . . ? N8 C20 C19 110.9(3) . . ? N7 C15 C16 106.6(3) . . ? N3 C7 C8 120.9(4) . . ? N3 C7 C6 114.8(3) . . ? C8 C7 C6 124.3(3) . . ? C18 C19 C20 106.1(3) . . ? C15 C16 C17 106.1(3) . . ? C9 C8 C7 120.4(4) . . ? C2 C3 C4 119.2(4) . . ? N2 C2 C3 122.8(4) . . ? C14 C13 C12 105.9(3) . . ? C6 C5 C4 119.4(4) . . ? N3 C11 C10 123.1(4) . . ? C8 C9 C10 118.4(4) . . ? N4 C12 C13 110.8(3) . . ? N6 C17 C16 111.0(3) . . ? C3 C4 C5 118.9(4) . . ? C11 C10 C9 119.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.773 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.073 #END data_3a _database_code_depnum_ccdc_archive 'CCDC 843190' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H39 Fe N11 O4 P Ru' _chemical_formula_weight 1105.86 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9718(18) _cell_length_b 13.3882(12) _cell_length_c 17.290(2) _cell_angle_alpha 102.217(9) _cell_angle_beta 96.540(11) _cell_angle_gamma 113.410(11) _cell_volume 2626.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7236 _cell_measurement_theta_min 3.7013 _cell_measurement_theta_max 29.0385 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.5341 _exptl_crystal_size_mid 0.2644 _exptl_crystal_size_min 0.0917 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19780 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10667 _reflns_number_gt 7180 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+9.7927P] 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 10667 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.004 _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 0.35519(4) 0.27923(4) 0.62420(3) 0.03822(16) Uani 1 1 d . . . Fe1 Fe 0.78261(7) 0.39662(7) 0.73123(5) 0.0396(2) Uani 1 1 d . . . P1 P 0.23043(16) 0.99775(15) 0.93628(10) 0.0510(4) Uani 1 1 d . . . C9 C -0.0155(6) 0.1512(7) 0.5392(4) 0.0624(19) Uani 1 1 d . . . H9 H -0.0690 0.1126 0.4901 0.075 Uiso 1 1 calc R . . N4 N 0.3567(4) 0.2504(4) 0.5084(3) 0.0397(11) Uani 1 1 d . . . N3 N 0.3400(4) 0.1151(4) 0.5988(3) 0.0427(12) Uani 1 1 d . . . N2 N 0.1789(4) 0.2258(4) 0.6122(3) 0.0388(11) Uani 1 1 d . . . N1 N 0.3410(4) 0.3124(4) 0.7443(3) 0.0396(11) Uani 1 1 d . . . C10 C 0.0994(6) 0.1753(6) 0.5426(4) 0.0505(16) Uani 1 1 d . . . H10 H 0.1220 0.1557 0.4947 0.061 Uiso 1 1 calc R . . C15 C 0.3484(5) 0.0749(6) 0.5205(4) 0.0475(15) Uani 1 1 d . . . C2 C 0.4126(6) 0.3809(6) 0.8877(4) 0.0535(16) Uani 1 1 d . . . H2 H 0.4729 0.4046 0.9320 0.064 Uiso 1 1 calc R . . C6 C 0.1447(5) 0.2557(5) 0.6813(4) 0.0421(13) Uani 1 1 d . . . C11 C 0.3279(8) 0.0479(7) 0.6473(5) 0.068(2) Uani 1 1 d . . . H11 H 0.3204 0.0737 0.6997 0.081 Uiso 1 1 calc R . . C37 C 0.2830(6) 1.1190(6) 1.0231(4) 0.0537(16) Uani 1 1 d . . . C4 C 0.2171(7) 0.3367(6) 0.8331(4) 0.0573(17) Uani 1 1 d . . . H4 H 0.1455 0.3320 0.8402 0.069 Uiso 1 1 calc R . . C29 C 0.9377(6) 0.4375(6) 0.7882(4) 0.0548(17) Uani 1 1 d . . . C27 C 0.7401(5) 0.4197(6) 0.8361(4) 0.0475(15) Uani 1 1 d . . . N5 N 0.3650(5) 0.4301(5) 0.6044(3) 0.0517(13) Uani 1 1 d . . . C26 C 0.6256(5) 0.3576(5) 0.6801(4) 0.0433(14) Uani 1 1 d . . . C8 C -0.0504(6) 0.1837(7) 0.6073(5) 0.0615(19) Uani 1 1 d . . . H8 H -0.1268 0.1706 0.6050 0.074 Uiso 1 1 calc R . . C1 C 0.4282(5) 0.3508(5) 0.8102(4) 0.0454(14) Uani 1 1 d . . . H1 H 0.5002 0.3568 0.8029 0.054 Uiso 1 1 calc R . . N8 N 0.7102(6) 0.4291(7) 0.8960(4) 0.076(2) Uani 1 1 d . . . C22 C 0.3519(9) 0.5187(8) 0.4992(6) 0.089(3) Uani 1 1 d . . . H22 H 0.3457 0.5164 0.4447 0.107 Uiso 1 1 calc R . . C44 C 0.3470(6) 0.9919(6) 0.8909(4) 0.0554(17) Uani 1 1 d . . . C5 C 0.2352(5) 0.3047(5) 0.7562(4) 0.0421(13) Uani 1 1 d . . . C21 C 0.3578(6) 0.4287(6) 0.5242(4) 0.0544(17) Uani 1 1 d . . . C20 C 0.3540(6) 0.3268(6) 0.4698(4) 0.0531(16) Uani 1 1 d . . . N10 N 0.8542(7) 0.6464(6) 0.7308(4) 0.080(2) Uani 1 1 d . . . C16 C 0.3530(5) 0.1501(6) 0.4686(4) 0.0461(14) Uani 1 1 d . . . C7 C 0.0296(6) 0.2364(6) 0.6799(4) 0.0547(17) Uani 1 1 d . . . H7 H 0.0078 0.2590 0.7275 0.066 Uiso 1 1 calc R . . C28 C 0.7422(6) 0.2372(6) 0.7227(4) 0.0521(16) Uani 1 1 d . . . C17 C 0.3499(7) 0.1251(7) 0.3858(4) 0.067(2) Uani 1 1 d . . . H17 H 0.3506 0.0579 0.3581 0.080 Uiso 1 1 calc R . . C55 C 0.1307(6) 1.0096(7) 0.8620(4) 0.0598(18) Uani 1 1 d . . . N11 N 0.8524(7) 0.3694(7) 0.5664(4) 0.082(2) Uani 1 1 d . . . C19 C 0.3486(7) 0.3043(8) 0.3871(5) 0.075(2) Uani 1 1 d . . . H19 H 0.3471 0.3567 0.3597 0.090 Uiso 1 1 calc R . . C38 C 0.1564(6) 0.8732(6) 0.9672(4) 0.0546(17) Uani 1 1 d . . . C49 C 0.4107(7) 1.0785(7) 0.8598(4) 0.066(2) Uani 1 1 d . . . H49 H 0.3934 1.1401 0.8636 0.080 Uiso 1 1 calc R . . C32 C 0.3906(7) 1.2109(6) 1.0374(5) 0.067(2) Uani 1 1 d . . . H32 H 0.4417 1.2080 1.0043 0.080 Uiso 1 1 calc R . . C54 C 0.0758(8) 1.0776(8) 0.8828(6) 0.081(3) Uani 1 1 d . . . H54 H 0.0951 1.1242 0.9355 0.098 Uiso 1 1 calc R . . C45 C 0.3716(8) 0.8992(7) 0.8834(5) 0.071(2) Uani 1 1 d . . . H45 H 0.3303 0.8397 0.9036 0.086 Uiso 1 1 calc R . . N7 N 0.7218(7) 0.1444(6) 0.7178(4) 0.0719(18) Uani 1 1 d . . . N6 N 0.5312(5) 0.3344(5) 0.6532(3) 0.0451(12) Uani 1 1 d . . . N9 N 1.0297(6) 0.4608(8) 0.8218(4) 0.090(2) Uani 1 1 d . . . C30 C 0.8265(6) 0.3775(6) 0.6268(4) 0.0547(17) Uani 1 1 d . . . C25 C 0.3686(7) 0.5215(7) 0.6572(5) 0.070(2) Uani 1 1 d . . . H25 H 0.3747 0.5243 0.7118 0.084 Uiso 1 1 calc R . . C14 C 0.3485(7) -0.0307(7) 0.4945(5) 0.066(2) Uani 1 1 d . . . H14 H 0.3579 -0.0560 0.4425 0.080 Uiso 1 1 calc R . . C40 C 0.1542(10) 0.7624(9) 1.0605(6) 0.093(3) Uani 1 1 d . . . H40 H 0.1896 0.7531 1.1066 0.112 Uiso 1 1 calc R . . C36 C 0.2094(8) 1.1216(7) 1.0758(5) 0.074(2) Uani 1 1 d . . . H36 H 0.1388 1.0596 1.0678 0.089 Uiso 1 1 calc R . . C35 C 0.2433(9) 1.2178(9) 1.1401(6) 0.085(3) Uani 1 1 d . . . H35 H 0.1956 1.2197 1.1761 0.102 Uiso 1 1 calc R . . C31 C 0.8265(6) 0.5538(6) 0.7338(4) 0.0512(16) Uani 1 1 d . . . C3 C 0.3080(7) 0.3759(7) 0.8994(4) 0.0624(19) Uani 1 1 d . . . H3 H 0.2981 0.3987 0.9516 0.075 Uiso 1 1 calc R . . C42 C -0.0057(8) 0.6944(7) 0.9501(5) 0.080(3) Uani 1 1 d . . . H42 H -0.0781 0.6392 0.9211 0.096 Uiso 1 1 calc R . . C43 C 0.0482(7) 0.7888(7) 0.9251(4) 0.067(2) Uani 1 1 d . . . H43 H 0.0115 0.7967 0.8789 0.080 Uiso 1 1 calc R . . C48 C 0.5003(8) 1.0755(9) 0.8231(5) 0.076(2) Uani 1 1 d . . . H48 H 0.5442 1.1360 0.8047 0.091 Uiso 1 1 calc R . . C34 C 0.3450(10) 1.3091(8) 1.1511(5) 0.085(3) Uani 1 1 d . . . H34 H 0.3643 1.3745 1.1927 0.102 Uiso 1 1 calc R . . C47 C 0.5224(8) 0.9833(10) 0.8146(5) 0.083(3) Uani 1 1 d . . . H47 H 0.5799 0.9790 0.7883 0.099 Uiso 1 1 calc R . . C39 C 0.2096(8) 0.8579(8) 1.0355(5) 0.077(2) Uani 1 1 d . . . H39 H 0.2826 0.9120 1.0643 0.092 Uiso 1 1 calc R . . C50 C 0.1029(8) 0.9400(9) 0.7833(5) 0.082(3) Uani 1 1 d . . . H50 H 0.1399 0.8941 0.7690 0.099 Uiso 1 1 calc R . . C18 C 0.3456(9) 0.2023(9) 0.3460(5) 0.085(3) Uani 1 1 d . . . H18 H 0.3407 0.1858 0.2903 0.102 Uiso 1 1 calc R . . C24 C 0.3635(9) 0.6114(7) 0.6326(7) 0.092(3) Uani 1 1 d . . . H24 H 0.3658 0.6734 0.6705 0.110 Uiso 1 1 calc R . . C12 C 0.3258(10) -0.0579(8) 0.6233(6) 0.100(4) Uani 1 1 d . . . H12 H 0.3184 -0.1016 0.6595 0.120 Uiso 1 1 calc R . . C51 C 0.0185(11) 0.9410(10) 0.7268(6) 0.109(4) Uani 1 1 d . . . H51 H -0.0004 0.8958 0.6737 0.131 Uiso 1 1 calc R . . C13 C 0.3344(10) -0.0977(8) 0.5471(6) 0.102(4) Uani 1 1 d . . . H13 H 0.3310 -0.1699 0.5299 0.122 Uiso 1 1 calc R . . C41 C 0.0472(10) 0.6814(8) 1.0176(6) 0.086(3) Uani 1 1 d . . . H41 H 0.0104 0.6172 1.0347 0.103 Uiso 1 1 calc R . . C46 C 0.4603(9) 0.8968(9) 0.8445(6) 0.084(3) Uani 1 1 d . . . H46 H 0.4772 0.8347 0.8390 0.100 Uiso 1 1 calc R . . C52 C -0.0368(10) 1.0059(12) 0.7470(9) 0.119(5) Uani 1 1 d . . . H52 H -0.0945 1.0031 0.7083 0.143 Uiso 1 1 calc R . . C53 C -0.0088(9) 1.0763(11) 0.8246(9) 0.108(4) Uani 1 1 d . . . H53 H -0.0458 1.1223 0.8379 0.130 Uiso 1 1 calc R . . C33 C 0.4203(10) 1.3062(7) 1.1012(5) 0.085(3) Uani 1 1 d . . . H33 H 0.4911 1.3685 1.1106 0.102 Uiso 1 1 calc R . . C23 C 0.3552(11) 0.6097(9) 0.5535(8) 0.113(4) Uani 1 1 d . . . H23 H 0.3518 0.6701 0.5367 0.135 Uiso 1 1 calc R . . O2W O 0.1545(12) 0.7009(12) 0.7238(9) 0.226(6) Uani 1 1 d . . . O4W O 1.2522(14) 0.5993(13) 0.8128(13) 0.297(10) Uani 1 1 d . . . O1WA O -0.063(3) 0.710(2) 0.5927(13) 0.213(9) Uani 0.50 1 d P A 1 O1WB O 0.053(3) 0.659(2) 0.5796(13) 0.213(9) Uani 0.50 1 d P B 2 O3WA O 0.3687(14) 0.6690(14) 0.9832(9) 0.109(3) Uani 0.50 1 d P C 1 O3WB O 0.2836(14) 0.6272(14) 0.9385(9) 0.109(3) Uani 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0353(3) 0.0456(3) 0.0357(3) 0.0106(2) 0.00064(18) 0.0218(2) Fe1 0.0365(5) 0.0471(5) 0.0375(4) 0.0104(4) 0.0027(4) 0.0227(4) P1 0.0553(10) 0.0481(10) 0.0467(9) 0.0151(8) 0.0028(8) 0.0210(8) C9 0.037(4) 0.085(5) 0.058(4) 0.017(4) -0.007(3) 0.025(4) N4 0.033(3) 0.043(3) 0.040(3) 0.016(2) 0.004(2) 0.013(2) N3 0.039(3) 0.046(3) 0.041(3) 0.010(2) -0.005(2) 0.022(2) N2 0.038(3) 0.038(3) 0.045(3) 0.012(2) 0.003(2) 0.023(2) N1 0.043(3) 0.037(3) 0.040(3) 0.011(2) 0.003(2) 0.020(2) C10 0.044(4) 0.067(5) 0.041(3) 0.013(3) 0.002(3) 0.028(3) C15 0.040(3) 0.050(4) 0.045(3) -0.001(3) -0.009(3) 0.024(3) C2 0.059(4) 0.049(4) 0.042(3) 0.007(3) -0.002(3) 0.018(3) C6 0.041(3) 0.047(4) 0.044(3) 0.010(3) 0.004(3) 0.027(3) C11 0.091(6) 0.063(5) 0.051(4) 0.017(4) -0.001(4) 0.040(5) C37 0.058(4) 0.052(4) 0.049(4) 0.016(3) 0.008(3) 0.021(3) C4 0.061(4) 0.066(5) 0.049(4) 0.010(3) 0.017(3) 0.033(4) C29 0.048(4) 0.063(4) 0.054(4) 0.009(3) -0.002(3) 0.031(3) C27 0.041(3) 0.048(4) 0.048(4) 0.010(3) 0.002(3) 0.018(3) N5 0.046(3) 0.052(3) 0.058(3) 0.015(3) 0.001(3) 0.025(3) C26 0.042(3) 0.050(4) 0.041(3) 0.011(3) 0.000(3) 0.026(3) C8 0.041(4) 0.084(5) 0.067(5) 0.020(4) 0.008(3) 0.037(4) C1 0.041(3) 0.042(3) 0.044(3) 0.007(3) -0.002(3) 0.015(3) N8 0.073(5) 0.110(6) 0.048(4) 0.016(4) 0.013(3) 0.046(4) C22 0.105(7) 0.071(6) 0.096(7) 0.046(6) -0.006(5) 0.038(6) C44 0.055(4) 0.057(4) 0.047(4) 0.013(3) 0.000(3) 0.021(4) C5 0.042(3) 0.038(3) 0.049(3) 0.010(3) 0.008(3) 0.021(3) C21 0.049(4) 0.059(4) 0.060(4) 0.031(4) 0.002(3) 0.023(3) C20 0.047(4) 0.059(4) 0.047(4) 0.022(3) -0.001(3) 0.016(3) N10 0.110(6) 0.058(4) 0.075(5) 0.022(4) 0.017(4) 0.038(4) C16 0.037(3) 0.053(4) 0.038(3) 0.004(3) -0.001(2) 0.016(3) C7 0.049(4) 0.066(5) 0.058(4) 0.016(3) 0.012(3) 0.035(4) C28 0.070(5) 0.059(5) 0.037(3) 0.012(3) 0.013(3) 0.037(4) C17 0.064(5) 0.078(6) 0.042(4) 0.003(4) 0.006(3) 0.022(4) C55 0.054(4) 0.066(5) 0.061(4) 0.035(4) 0.005(3) 0.021(4) N11 0.096(6) 0.113(6) 0.063(4) 0.032(4) 0.030(4) 0.064(5) C19 0.079(6) 0.098(7) 0.052(4) 0.043(5) 0.007(4) 0.034(5) C38 0.065(4) 0.052(4) 0.044(3) 0.014(3) 0.002(3) 0.025(4) C49 0.073(5) 0.069(5) 0.057(4) 0.020(4) 0.011(4) 0.031(4) C32 0.080(6) 0.053(4) 0.060(4) 0.016(4) 0.013(4) 0.022(4) C54 0.070(6) 0.092(7) 0.101(7) 0.047(6) 0.015(5) 0.044(5) C45 0.078(6) 0.070(5) 0.067(5) 0.015(4) 0.008(4) 0.036(5) N7 0.097(5) 0.054(4) 0.065(4) 0.014(3) 0.025(4) 0.033(4) N6 0.048(3) 0.054(3) 0.039(3) 0.012(2) 0.005(2) 0.030(3) N9 0.057(4) 0.134(7) 0.078(5) 0.009(5) -0.010(4) 0.057(5) C30 0.057(4) 0.069(5) 0.050(4) 0.021(3) 0.011(3) 0.037(4) C25 0.071(5) 0.060(5) 0.078(5) 0.013(4) 0.004(4) 0.034(4) C14 0.063(5) 0.063(5) 0.065(5) -0.009(4) -0.014(4) 0.040(4) C40 0.136(9) 0.082(7) 0.068(6) 0.035(5) 0.000(6) 0.053(7) C36 0.070(5) 0.070(5) 0.066(5) 0.006(4) 0.004(4) 0.025(4) C35 0.099(7) 0.088(7) 0.069(6) 0.010(5) 0.013(5) 0.047(6) C31 0.057(4) 0.055(4) 0.044(3) 0.014(3) 0.007(3) 0.027(3) C3 0.074(5) 0.068(5) 0.040(4) 0.004(3) 0.011(3) 0.032(4) C42 0.091(6) 0.050(5) 0.064(5) 0.012(4) 0.001(4) 0.002(4) C43 0.085(6) 0.057(5) 0.047(4) 0.015(3) -0.001(4) 0.024(4) C48 0.066(5) 0.093(7) 0.064(5) 0.022(5) 0.013(4) 0.029(5) C34 0.126(9) 0.062(6) 0.060(5) 0.004(4) 0.000(5) 0.046(6) C47 0.068(6) 0.119(8) 0.061(5) 0.013(5) 0.007(4) 0.048(6) C39 0.083(6) 0.070(5) 0.069(5) 0.028(4) -0.008(4) 0.026(5) C50 0.089(6) 0.097(7) 0.056(5) 0.034(5) 0.005(4) 0.032(5) C18 0.100(7) 0.105(8) 0.035(4) 0.019(4) 0.007(4) 0.033(6) C24 0.100(7) 0.050(5) 0.122(8) 0.018(5) -0.009(6) 0.040(5) C12 0.154(10) 0.065(6) 0.078(6) 0.014(5) -0.026(6) 0.062(7) C51 0.113(9) 0.103(9) 0.074(6) 0.041(6) -0.023(6) 0.013(7) C13 0.138(9) 0.064(6) 0.093(7) -0.007(5) -0.035(6) 0.065(6) C41 0.122(8) 0.056(5) 0.078(6) 0.030(5) 0.030(6) 0.029(5) C46 0.089(7) 0.097(7) 0.076(6) 0.014(5) 0.005(5) 0.061(6) C52 0.074(7) 0.120(10) 0.134(11) 0.087(9) -0.030(7) 0.001(7) C53 0.077(7) 0.113(9) 0.166(12) 0.093(9) 0.024(7) 0.046(7) C33 0.118(8) 0.052(5) 0.063(5) 0.014(4) 0.003(5) 0.022(5) C23 0.139(10) 0.077(7) 0.136(10) 0.043(7) -0.013(8) 0.065(7) O2W 0.175(12) 0.187(12) 0.267(16) 0.011(11) 0.010(11) 0.067(10) O4W 0.175(14) 0.174(13) 0.44(3) -0.012(15) -0.007(15) 0.041(10) O1WA 0.31(3) 0.25(2) 0.139(11) 0.121(13) 0.143(14) 0.119(17) O1WB 0.31(3) 0.25(2) 0.139(11) 0.121(13) 0.143(14) 0.119(17) O3WA 0.099(9) 0.113(9) 0.091(8) 0.023(7) 0.013(6) 0.028(7) O3WB 0.099(9) 0.113(9) 0.091(8) 0.023(7) 0.013(6) 0.028(7) _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 N4 1.961(5) . ? Ru1 N6 2.062(5) . ? Ru1 N3 2.071(5) . ? Ru1 N1 2.076(5) . ? Ru1 N2 2.077(5) . ? Ru1 N5 2.077(5) . ? Fe1 C26 1.937(6) . ? Fe1 C31 1.939(7) . ? Fe1 C29 1.940(6) . ? Fe1 C30 1.950(7) . ? Fe1 C28 1.952(7) . ? Fe1 C27 1.953(7) . ? P1 C37 1.791(7) . ? P1 C38 1.791(7) . ? P1 C55 1.795(7) . ? P1 C44 1.802(8) . ? C9 C8 1.357(10) . ? C9 C10 1.385(9) . ? N4 C20 1.344(8) . ? N4 C16 1.353(8) . ? N3 C11 1.330(8) . ? N3 C15 1.381(8) . ? N2 C10 1.337(8) . ? N2 C6 1.358(7) . ? N1 C1 1.356(7) . ? N1 C5 1.376(7) . ? C15 C14 1.390(9) . ? C15 C16 1.472(9) . ? C2 C3 1.372(10) . ? C2 C1 1.376(9) . ? C6 C7 1.407(8) . ? C6 C5 1.473(8) . ? C11 C12 1.378(11) . ? C37 C32 1.396(11) . ? C37 C36 1.398(11) . ? C4 C5 1.385(9) . ? C4 C3 1.387(10) . ? C29 N9 1.152(9) . ? C27 N8 1.146(8) . ? N5 C25 1.344(9) . ? N5 C21 1.373(8) . ? C26 N6 1.149(8) . ? C8 C7 1.377(10) . ? C22 C23 1.353(14) . ? C22 C21 1.390(10) . ? C44 C45 1.384(10) . ? C44 C49 1.385(10) . ? C21 C20 1.463(10) . ? C20 C19 1.385(10) . ? N10 C31 1.160(9) . ? C16 C17 1.392(9) . ? C28 N7 1.145(9) . ? C17 C18 1.371(12) . ? C55 C54 1.379(11) . ? C55 C50 1.390(11) . ? N11 C30 1.130(9) . ? C19 C18 1.382(13) . ? C38 C43 1.392(11) . ? C38 C39 1.394(10) . ? C49 C48 1.395(11) . ? C32 C33 1.382(11) . ? C54 C53 1.393(13) . ? C45 C46 1.405(12) . ? C25 C24 1.382(11) . ? C14 C13 1.386(13) . ? C40 C41 1.372(14) . ? C40 C39 1.383(12) . ? C36 C35 1.386(12) . ? C35 C34 1.354(14) . ? C42 C41 1.365(12) . ? C42 C43 1.367(11) . ? C48 C47 1.358(13) . ? C34 C33 1.382(14) . ? C47 C46 1.365(13) . ? C50 C51 1.389(13) . ? C24 C23 1.354(15) . ? C12 C13 1.348(14) . ? C51 C52 1.347(18) . ? C52 C53 1.378(18) . ? 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 N4 Ru1 N6 90.36(19) . . ? N4 Ru1 N3 80.1(2) . . ? N6 Ru1 N3 87.5(2) . . ? N4 Ru1 N1 174.95(19) . . ? N6 Ru1 N1 94.05(19) . . ? N3 Ru1 N1 102.54(19) . . ? N4 Ru1 N2 97.61(19) . . ? N6 Ru1 N2 171.97(19) . . ? N3 Ru1 N2 92.95(19) . . ? N1 Ru1 N2 78.03(19) . . ? N4 Ru1 N5 79.1(2) . . ? N6 Ru1 N5 94.5(2) . . ? N3 Ru1 N5 159.1(2) . . ? N1 Ru1 N5 98.1(2) . . ? N2 Ru1 N5 87.9(2) . . ? C26 Fe1 C31 90.2(3) . . ? C26 Fe1 C29 176.8(3) . . ? C31 Fe1 C29 89.7(3) . . ? C26 Fe1 C30 92.0(3) . . ? C31 Fe1 C30 86.9(3) . . ? C29 Fe1 C30 91.2(3) . . ? C26 Fe1 C28 90.4(3) . . ? C31 Fe1 C28 176.5(3) . . ? C29 Fe1 C28 89.9(3) . . ? C30 Fe1 C28 89.7(3) . . ? C26 Fe1 C27 88.2(3) . . ? C31 Fe1 C27 91.7(3) . . ? C29 Fe1 C27 88.6(3) . . ? C30 Fe1 C27 178.6(3) . . ? C28 Fe1 C27 91.7(3) . . ? C37 P1 C38 108.6(3) . . ? C37 P1 C55 109.1(4) . . ? C38 P1 C55 108.8(3) . . ? C37 P1 C44 110.5(3) . . ? C38 P1 C44 112.1(3) . . ? C55 P1 C44 107.8(3) . . ? C8 C9 C10 120.2(6) . . ? C20 N4 C16 121.9(5) . . ? C20 N4 Ru1 119.6(4) . . ? C16 N4 Ru1 118.4(4) . . ? C11 N3 C15 117.9(6) . . ? C11 N3 Ru1 129.4(5) . . ? C15 N3 Ru1 112.7(4) . . ? C10 N2 C6 118.0(5) . . ? C10 N2 Ru1 126.1(4) . . ? C6 N2 Ru1 115.6(4) . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Ru1 125.8(4) . . ? C5 N1 Ru1 115.4(4) . . ? N2 C10 C9 122.4(6) . . ? N3 C15 C14 120.7(6) . . ? N3 C15 C16 114.9(5) . . ? C14 C15 C16 124.4(6) . . ? C3 C2 C1 120.0(6) . . ? N2 C6 C7 121.2(5) . . ? N2 C6 C5 115.1(5) . . ? C7 C6 C5 123.6(6) . . ? N3 C11 C12 123.1(8) . . ? C32 C37 C36 119.9(7) . . ? C32 C37 P1 122.8(6) . . ? C36 C37 P1 117.2(6) . . ? C5 C4 C3 118.6(7) . . ? N9 C29 Fe1 179.4(8) . . ? N8 C27 Fe1 176.8(7) . . ? C25 N5 C21 118.1(6) . . ? C25 N5 Ru1 128.9(5) . . ? C21 N5 Ru1 112.9(4) . . ? N6 C26 Fe1 176.9(6) . . ? C9 C8 C7 118.7(6) . . ? N1 C1 C2 121.5(6) . . ? C23 C22 C21 120.7(9) . . ? C45 C44 C49 118.8(8) . . ? C45 C44 P1 120.9(6) . . ? C49 C44 P1 120.3(6) . . ? N1 C5 C4 121.6(6) . . ? N1 C5 C6 114.2(5) . . ? C4 C5 C6 124.1(6) . . ? N5 C21 C22 120.3(8) . . ? N5 C21 C20 115.4(6) . . ? C22 C21 C20 124.3(7) . . ? N4 C20 C19 119.9(7) . . ? N4 C20 C21 112.7(6) . . ? C19 C20 C21 127.3(7) . . ? N4 C16 C17 120.0(6) . . ? N4 C16 C15 113.6(5) . . ? C17 C16 C15 126.4(6) . . ? C8 C7 C6 119.3(6) . . ? N7 C28 Fe1 178.0(7) . . ? C18 C17 C16 118.2(8) . . ? C54 C55 C50 120.7(8) . . ? C54 C55 P1 121.7(7) . . ? C50 C55 P1 117.4(6) . . ? C18 C19 C20 118.6(7) . . ? C43 C38 C39 117.7(7) . . ? C43 C38 P1 123.1(5) . . ? C39 C38 P1 119.2(6) . . ? C44 C49 C48 121.7(8) . . ? C33 C32 C37 119.3(8) . . ? C55 C54 C53 119.7(10) . . ? C44 C45 C46 118.5(9) . . ? C26 N6 Ru1 168.5(5) . . ? N11 C30 Fe1 178.1(7) . . ? N5 C25 C24 121.7(8) . . ? C13 C14 C15 119.0(8) . . ? C41 C40 C39 120.2(8) . . ? C35 C36 C37 119.0(9) . . ? C34 C35 C36 120.9(10) . . ? N10 C31 Fe1 175.8(6) . . ? C2 C3 C4 119.7(6) . . ? C41 C42 C43 119.9(9) . . ? C42 C43 C38 121.6(7) . . ? C47 C48 C49 119.1(9) . . ? C35 C34 C33 120.7(9) . . ? C48 C47 C46 120.0(9) . . ? C40 C39 C38 120.2(8) . . ? C51 C50 C55 118.1(10) . . ? C17 C18 C19 121.3(7) . . ? C23 C24 C25 120.3(9) . . ? C13 C12 C11 119.5(9) . . ? C52 C51 C50 121.6(11) . . ? C12 C13 C14 119.8(8) . . ? C42 C41 C40 120.3(8) . . ? C47 C46 C45 121.7(9) . . ? C51 C52 C53 120.7(10) . . ? C52 C53 C54 119.2(11) . . ? C34 C33 C32 120.1(10) . . ? C24 C23 C22 118.9(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.404 _refine_diff_density_min -1.706 _refine_diff_density_rms 0.105 #END data_3b _database_code_depnum_ccdc_archive 'CCDC 843191' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H38 Fe N14 O9 P Ru' _chemical_formula_weight 1166.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 '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 11.1358(2) _cell_length_b 13.3970(2) _cell_length_c 19.2367(3) _cell_angle_alpha 88.0570(10) _cell_angle_beta 76.1420(10) _cell_angle_gamma 81.9810(10) _cell_volume 2759.07(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 29954 _cell_measurement_theta_min 3.5896 _cell_measurement_theta_max 28.9618 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1186 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_T_min 0.97891 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47395 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 27.00 _reflns_number_total 11963 _reflns_number_gt 10065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.4415P] 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 11963 _refine_ls_number_parameters 675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.694947(15) 0.211981(12) 0.052388(9) 0.02470(7) Uani 1 1 d . . . Fe1 Fe 0.88470(3) 0.28937(2) -0.205878(17) 0.02961(9) Uani 1 1 d . . . P1 P 0.61335(7) 0.28333(6) 0.43025(4) 0.04745(18) Uani 1 1 d . . . N11 N 0.66373(16) 0.09172(14) -0.00444(10) 0.0281(4) Uani 1 1 d . . . N6 N 0.79582(17) 0.25986(14) -0.04242(10) 0.0291(4) Uani 1 1 d . . . N8 N 0.54588(17) 0.31574(14) 0.04315(10) 0.0298(4) Uani 1 1 d . . . N9 N 0.84409(17) 0.11091(14) 0.06970(10) 0.0312(4) Uani 1 1 d . . . C6 C 0.8353(2) 0.27351(17) -0.10230(12) 0.0291(4) Uani 1 1 d . . . N12 N 0.67193(18) -0.00096(14) 0.02730(11) 0.0336(4) Uani 1 1 d . . . N13 N 0.58779(17) 0.15022(15) 0.14151(10) 0.0322(4) Uani 1 1 d . . . C3 C 0.7081(2) 0.30149(18) -0.20345(13) 0.0357(5) Uani 1 1 d . . . N10 N 0.82132(18) 0.01680(15) 0.09316(11) 0.0350(4) Uani 1 1 d . . . C2 C 0.8898(2) 0.1459(2) -0.22077(13) 0.0385(5) Uani 1 1 d . . . N14 N 0.60552(19) 0.04849(15) 0.14947(11) 0.0374(5) Uani 1 1 d . . . C23 C 0.6530(2) 0.07463(19) -0.06996(13) 0.0350(5) Uani 1 1 d . . . H23 H 0.6451 0.1243 -0.1042 0.042 Uiso 1 1 calc R . . C12 C 0.5253(2) 0.39918(18) 0.08444(12) 0.0341(5) Uani 1 1 d . . . C5 C 0.8816(2) 0.4341(2) -0.19824(13) 0.0380(5) Uani 1 1 d . . . C24 C 0.6553(2) -0.0284(2) -0.08056(15) 0.0452(6) Uani 1 1 d . . . H24 H 0.6492 -0.0593 -0.1219 0.054 Uiso 1 1 calc R . . C15 C 0.3639(2) 0.3773(2) 0.00145(15) 0.0450(6) Uani 1 1 d . . . H15 H 0.3112 0.3694 -0.0283 0.054 Uiso 1 1 calc R . . C22 C 0.5245(3) 0.0181(2) 0.20779(14) 0.0470(6) Uani 1 1 d . . . H22 H 0.5192 -0.0478 0.2237 0.056 Uiso 1 1 calc R . . N2 N 0.8888(3) 0.0628(2) -0.23231(15) 0.0624(7) Uani 1 1 d . . . C1 C 1.0588(2) 0.2731(2) -0.20181(14) 0.0432(6) Uani 1 1 d . . . C26 C 0.6999(2) -0.01155(18) 0.09680(13) 0.0366(5) Uani 1 1 d . . . H26 H 0.7010 -0.0825 0.1112 0.044 Uiso 1 1 calc R . . C17 C 0.9647(2) 0.1113(2) 0.06638(13) 0.0400(6) Uani 1 1 d . . . H17 H 1.0078 0.1658 0.0512 0.048 Uiso 1 1 calc R . . N5 N 0.8816(2) 0.51859(19) -0.19402(15) 0.0564(6) Uani 1 1 d . . . N3 N 0.6030(2) 0.30256(19) -0.19781(14) 0.0538(6) Uani 1 1 d . . . C7 C 0.6236(2) 0.40826(18) 0.12191(12) 0.0352(5) Uani 1 1 d . . . C4 C 0.9288(3) 0.3000(2) -0.30902(15) 0.0565(8) Uani 1 1 d . . . C21 C 0.4522(3) 0.1028(2) 0.23865(15) 0.0533(7) Uani 1 1 d . . . H21 H 0.3878 0.1063 0.2798 0.064 Uiso 1 1 calc R . . C20 C 0.4941(2) 0.1830(2) 0.19637(13) 0.0439(6) Uani 1 1 d . . . H20 H 0.4611 0.2503 0.2052 0.053 Uiso 1 1 calc R . . C25 C 0.6680(2) -0.0742(2) -0.01816(15) 0.0431(6) Uani 1 1 d . . . H25 H 0.6731 -0.1430 -0.0086 0.052 Uiso 1 1 calc R . . C18 C 1.0178(3) 0.0194(2) 0.08865(15) 0.0497(7) Uani 1 1 d . . . H18 H 1.1000 0.0020 0.0921 0.060 Uiso 1 1 calc R . . C13 C 0.4209(3) 0.4710(2) 0.08757(15) 0.0456(6) Uani 1 1 d . . . H13 H 0.4062 0.5263 0.1178 0.055 Uiso 1 1 calc R . . C14 C 0.3402(2) 0.4595(2) 0.04582(16) 0.0489(7) Uani 1 1 d . . . H14 H 0.2700 0.5068 0.0475 0.059 Uiso 1 1 calc R . . C16 C 0.4667(2) 0.30672(19) 0.00155(14) 0.0363(5) Uani 1 1 d . . . H16 H 0.4818 0.2509 -0.0283 0.044 Uiso 1 1 calc R . . C19 C 0.9252(3) -0.0397(2) 0.10434(15) 0.0464(7) Uani 1 1 d . . . H19 H 0.9321 -0.1064 0.1198 0.056 Uiso 1 1 calc R . . C29 C 0.5044(3) 0.3503(3) 0.38358(15) 0.0529(7) Uani 1 1 d . . . C36 C 0.5362(3) 0.2700(2) 0.52253(15) 0.0561(8) Uani 1 1 d . . . C11 C 0.8128(3) 0.3355(2) 0.14231(15) 0.0467(6) Uani 1 1 d . . . H11 H 0.8766 0.2815 0.1368 0.056 Uiso 1 1 calc R . . C10 C 0.8211(3) 0.4172(3) 0.18116(17) 0.0586(8) Uani 1 1 d . . . H10 H 0.8902 0.4190 0.2000 0.070 Uiso 1 1 calc R . . C8 C 0.6258(3) 0.4912(2) 0.16255(16) 0.0530(7) Uani 1 1 d . . . H8 H 0.5595 0.5433 0.1699 0.064 Uiso 1 1 calc R . . C34 C 0.7399(3) 0.3548(3) 0.42461(16) 0.0552(7) Uani 1 1 d . . . C9 C 0.7256(3) 0.4968(2) 0.19191(17) 0.0602(8) Uani 1 1 d . . . H9 H 0.7287 0.5528 0.2184 0.072 Uiso 1 1 calc R . . C37 C 0.4102(4) 0.2946(3) 0.54658(18) 0.0717(10) Uani 1 1 d . . . H37 H 0.3619 0.3187 0.5147 0.086 Uiso 1 1 calc R . . C50 C 0.3247(4) 0.3529(4) 0.3361(2) 0.0867(13) Uani 1 1 d . . . H50 H 0.2627 0.3200 0.3259 0.104 Uiso 1 1 calc R . . C27 C 0.6705(3) 0.1617(3) 0.38950(17) 0.0586(8) Uani 1 1 d . . . C28 C 0.7196(4) 0.1528(4) 0.3185(2) 0.0899(13) Uani 1 1 d . . . H28 H 0.7157 0.2093 0.2893 0.108 Uiso 1 1 calc R . . C30 C 0.4117(3) 0.3013(3) 0.36914(19) 0.0681(9) Uani 1 1 d . . . H30 H 0.4081 0.2339 0.3816 0.082 Uiso 1 1 calc R . . C33 C 0.5094(4) 0.4510(3) 0.36495(18) 0.0708(10) Uani 1 1 d . . . H33 H 0.5715 0.4844 0.3745 0.085 Uiso 1 1 calc R . . N1 N 1.1587(2) 0.2640(2) -0.19551(18) 0.0705(8) Uani 1 1 d . . . C32 C 0.3291(4) 0.4525(4) 0.3183(2) 0.0911(14) Uani 1 1 d . . . H32 H 0.2693 0.4872 0.2968 0.109 Uiso 1 1 calc R . . C35 C 0.8433(5) 0.3435(5) 0.3675(2) 0.114(2) Uani 1 1 d . . . H35 H 0.8535 0.2934 0.3335 0.137 Uiso 1 1 calc R . . N7B N 0.71762(18) 0.32940(15) 0.11193(10) 0.0319(4) Uani 1 1 d . . . N4 N 0.9557(4) 0.3032(3) -0.37050(15) 0.0993(13) Uani 1 1 d . . . C46 C 0.4207(4) 0.5007(4) 0.3321(2) 0.0866(12) Uani 1 1 d . . . H46 H 0.4235 0.5680 0.3192 0.104 Uiso 1 1 calc R . . C38 C 0.3539(5) 0.2838(4) 0.6189(2) 0.0920(14) Uani 1 1 d . . . H38 H 0.2684 0.3025 0.6358 0.110 Uiso 1 1 calc R . . C41 C 0.6073(5) 0.2332(3) 0.5701(2) 0.0897(14) Uani 1 1 d . . . H41 H 0.6933 0.2164 0.5542 0.108 Uiso 1 1 calc R . . C39 C 0.4251(6) 0.2455(4) 0.6647(2) 0.1064(17) Uani 1 1 d . . . H39 H 0.3872 0.2358 0.7126 0.128 Uiso 1 1 calc R . . C42 C 0.7373(4) 0.4206(4) 0.4771(3) 0.1001(15) Uani 1 1 d . . . H42 H 0.6734 0.4245 0.5185 0.120 Uiso 1 1 calc R . . C44 C 0.9258(5) 0.4741(4) 0.4132(4) 0.1090(18) Uani 1 1 d . . . H44 H 0.9890 0.5139 0.4097 0.131 Uiso 1 1 calc R . . C51 C 0.7753(5) 0.0614(6) 0.2890(3) 0.1138(19) Uani 1 1 d . . . H51 H 0.8164 0.0587 0.2408 0.137 Uiso 1 1 calc R . . C45 C 0.9318(6) 0.4090(6) 0.3622(3) 0.143(3) Uani 1 1 d . . . H45 H 0.9970 0.4068 0.3215 0.171 Uiso 1 1 calc R . . C40 C 0.5497(6) 0.2214(4) 0.6413(2) 0.117(2) Uani 1 1 d . . . H40 H 0.5972 0.1967 0.6735 0.141 Uiso 1 1 calc R . . C43 C 0.8307(6) 0.4824(4) 0.4687(4) 0.124(2) Uani 1 1 d . . . H43 H 0.8251 0.5306 0.5034 0.149 Uiso 1 1 calc R . . C49 C 0.7730(6) -0.0203(5) 0.3250(4) 0.134(2) Uani 1 1 d . . . H49 H 0.8037 -0.0822 0.3026 0.161 Uiso 1 1 calc R . . C47 C 0.6752(7) 0.0755(4) 0.4299(3) 0.146(3) Uani 1 1 d . . . H47 H 0.6453 0.0769 0.4794 0.175 Uiso 1 1 calc R . . C48 C 0.7274(10) -0.0150(5) 0.3931(5) 0.213(5) Uani 1 1 d . . . H48 H 0.7289 -0.0745 0.4194 0.255 Uiso 1 1 calc R . . O3W O 0.3739(2) 0.22237(17) 0.86139(12) 0.0651(6) Uani 1 1 d . . . O4W O 0.8533(5) 0.7187(3) 0.8671(2) 0.1477(17) Uani 1 1 d . . . O2W O 0.0924(6) 0.3125(7) 0.9903(4) 0.226(3) Uani 1 1 d . . . O8W O 0.1269(10) 0.2616(8) 0.4949(4) 0.326(5) Uani 1 1 d . . . O9WA O 0.9804(19) 0.2078(14) 0.5058(9) 0.251(5) Uiso 0.50 1 d P A 1 O9WB O 0.9025(16) 0.1431(14) 0.5176(9) 0.251(5) Uiso 0.50 1 d P B 2 O1WA O 0.9527(7) 0.8390(6) 0.7565(4) 0.1051(15) Uiso 0.50 1 d P C 1 O1WB O 0.8910(7) 0.8511(6) 0.7420(4) 0.1051(15) Uiso 0.50 1 d P D 2 O7WA O 0.8942(12) 0.0567(9) 0.6033(6) 0.185(3) Uiso 0.50 1 d P E 1 O7WB O 0.7914(12) 0.0393(9) 0.6354(6) 0.185(3) Uiso 0.50 1 d P F 2 O6WA O 0.8869(12) 0.8379(10) 0.6257(7) 0.197(3) Uiso 0.50 1 d P G 1 O6WB O 0.7936(12) 0.8759(10) 0.6119(7) 0.197(3) Uiso 0.50 1 d P H 2 O5WA O 0.0470(17) 0.4093(17) 0.9677(11) 0.262(6) Uiso 0.50 1 d P I 1 O5WB O -0.0287(18) 0.4812(15) 0.9600(9) 0.262(6) Uiso 0.50 1 d P J 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02444(10) 0.02436(10) 0.02453(10) -0.00112(6) -0.00402(6) -0.00351(6) Fe1 0.02958(17) 0.03099(18) 0.02665(17) 0.00151(13) -0.00360(13) -0.00430(13) P1 0.0545(4) 0.0515(4) 0.0339(3) -0.0019(3) -0.0034(3) -0.0109(3) N11 0.0269(9) 0.0265(9) 0.0306(9) -0.0003(7) -0.0057(7) -0.0041(7) N6 0.0284(9) 0.0276(9) 0.0313(10) -0.0014(7) -0.0065(8) -0.0043(7) N8 0.0286(9) 0.0274(9) 0.0309(10) 0.0000(7) -0.0025(7) -0.0037(7) N9 0.0294(9) 0.0312(10) 0.0331(10) 0.0001(8) -0.0073(8) -0.0042(8) C6 0.0278(11) 0.0278(11) 0.0324(12) 0.0005(9) -0.0082(9) -0.0041(8) N12 0.0331(10) 0.0266(10) 0.0399(11) -0.0008(8) -0.0044(8) -0.0069(8) N13 0.0316(10) 0.0331(10) 0.0302(10) 0.0001(8) -0.0037(8) -0.0048(8) C3 0.0388(13) 0.0315(12) 0.0380(13) -0.0012(10) -0.0136(10) -0.0009(10) N10 0.0339(10) 0.0329(11) 0.0363(11) 0.0060(8) -0.0084(8) 0.0004(8) C2 0.0407(13) 0.0378(14) 0.0353(13) -0.0015(10) -0.0080(10) -0.0006(10) N14 0.0384(11) 0.0354(11) 0.0344(10) 0.0060(8) -0.0013(8) -0.0059(8) C23 0.0270(11) 0.0419(13) 0.0371(12) -0.0066(10) -0.0094(9) -0.0038(9) C12 0.0380(12) 0.0294(12) 0.0311(12) -0.0025(9) -0.0013(9) -0.0029(9) C5 0.0380(13) 0.0402(15) 0.0350(13) 0.0003(10) -0.0046(10) -0.0095(10) C24 0.0365(13) 0.0517(16) 0.0504(16) -0.0201(13) -0.0123(11) -0.0079(11) C15 0.0333(13) 0.0481(16) 0.0525(16) 0.0025(12) -0.0122(11) 0.0015(11) C22 0.0498(15) 0.0511(16) 0.0369(14) 0.0112(12) -0.0005(12) -0.0161(13) N2 0.084(2) 0.0405(15) 0.0621(17) -0.0063(12) -0.0172(14) -0.0047(13) C1 0.0350(14) 0.0442(15) 0.0473(15) 0.0045(12) -0.0025(11) -0.0083(11) C26 0.0377(12) 0.0291(12) 0.0404(13) 0.0059(10) -0.0036(10) -0.0068(9) C17 0.0280(12) 0.0530(16) 0.0385(13) -0.0058(11) -0.0076(10) -0.0027(11) N5 0.0617(16) 0.0404(14) 0.0633(16) -0.0022(12) -0.0037(12) -0.0125(11) N3 0.0431(14) 0.0514(15) 0.0698(17) -0.0070(12) -0.0215(12) -0.0006(11) C7 0.0434(13) 0.0295(12) 0.0305(12) -0.0024(9) -0.0045(10) -0.0038(10) C4 0.080(2) 0.0499(17) 0.0374(15) 0.0027(13) -0.0060(14) -0.0154(15) C21 0.0515(16) 0.068(2) 0.0338(14) 0.0044(13) 0.0070(12) -0.0165(14) C20 0.0416(14) 0.0517(16) 0.0331(13) -0.0056(11) 0.0024(10) -0.0068(12) C25 0.0363(13) 0.0325(13) 0.0604(17) -0.0112(12) -0.0062(12) -0.0106(10) C18 0.0341(13) 0.0641(19) 0.0479(16) -0.0008(13) -0.0128(11) 0.0095(12) C13 0.0469(15) 0.0346(14) 0.0477(15) -0.0076(11) -0.0019(12) 0.0055(11) C14 0.0354(13) 0.0457(16) 0.0576(17) 0.0023(13) -0.0045(12) 0.0100(11) C16 0.0328(12) 0.0339(13) 0.0427(13) -0.0003(10) -0.0096(10) -0.0046(10) C19 0.0446(15) 0.0478(16) 0.0410(14) 0.0070(12) -0.0111(11) 0.0130(12) C29 0.0593(18) 0.064(2) 0.0330(14) -0.0024(13) -0.0060(12) -0.0088(15) C36 0.079(2) 0.0481(17) 0.0355(14) -0.0016(12) -0.0010(14) -0.0102(15) C11 0.0441(14) 0.0506(16) 0.0481(15) -0.0114(12) -0.0137(12) -0.0082(12) C10 0.0603(19) 0.066(2) 0.0568(18) -0.0168(15) -0.0210(15) -0.0176(16) C8 0.072(2) 0.0358(14) 0.0501(16) -0.0121(12) -0.0163(15) 0.0014(13) C34 0.0617(18) 0.0610(19) 0.0465(16) 0.0074(14) -0.0153(14) -0.0181(15) C9 0.086(2) 0.0455(17) 0.0560(18) -0.0171(14) -0.0254(17) -0.0147(16) C37 0.076(2) 0.082(3) 0.0490(18) -0.0055(17) 0.0091(16) -0.0214(19) C50 0.061(2) 0.124(4) 0.077(3) -0.030(3) -0.024(2) 0.001(2) C27 0.0581(18) 0.062(2) 0.0533(18) -0.0139(15) -0.0059(14) -0.0086(15) C28 0.091(3) 0.102(3) 0.068(2) -0.031(2) 0.001(2) -0.007(2) C30 0.063(2) 0.079(2) 0.062(2) -0.0165(18) -0.0128(17) -0.0092(18) C33 0.084(2) 0.075(2) 0.0536(19) 0.0114(17) -0.0175(18) -0.0144(19) N1 0.0349(14) 0.080(2) 0.097(2) 0.0073(17) -0.0142(14) -0.0113(13) C32 0.087(3) 0.122(4) 0.061(2) -0.006(2) -0.027(2) 0.018(3) C35 0.113(4) 0.184(5) 0.056(2) -0.004(3) 0.000(2) -0.095(4) N7B 0.0329(10) 0.0359(11) 0.0267(9) -0.0016(8) -0.0050(8) -0.0072(8) N4 0.161(4) 0.099(3) 0.0348(16) 0.0054(16) -0.0045(18) -0.043(3) C46 0.103(3) 0.086(3) 0.067(2) 0.014(2) -0.024(2) 0.001(2) C38 0.103(3) 0.096(3) 0.059(2) -0.009(2) 0.021(2) -0.024(3) C41 0.107(3) 0.100(3) 0.049(2) 0.010(2) -0.008(2) 0.012(3) C39 0.145(5) 0.107(4) 0.046(2) -0.001(2) 0.017(3) -0.016(3) C42 0.081(3) 0.111(4) 0.108(4) -0.044(3) -0.006(3) -0.031(3) C44 0.102(4) 0.111(4) 0.140(5) 0.041(4) -0.058(4) -0.063(3) C51 0.086(3) 0.141(5) 0.102(4) -0.069(4) 0.007(3) -0.006(3) C45 0.130(5) 0.248(8) 0.077(3) 0.035(4) -0.021(3) -0.130(5) C40 0.174(6) 0.113(4) 0.050(2) 0.019(2) -0.017(3) 0.012(4) C43 0.102(4) 0.111(4) 0.168(6) -0.052(4) -0.027(4) -0.039(3) C49 0.145(5) 0.100(5) 0.143(6) -0.072(4) -0.016(4) 0.015(4) C47 0.242(8) 0.061(3) 0.102(4) -0.018(3) 0.023(4) -0.015(4) C48 0.353(14) 0.063(4) 0.165(7) -0.025(4) 0.037(8) 0.001(5) O3W 0.0804(15) 0.0580(14) 0.0710(15) 0.0218(11) -0.0345(12) -0.0335(12) O4W 0.201(4) 0.066(2) 0.151(3) -0.022(2) 0.024(3) -0.044(2) O2W 0.202(6) 0.255(8) 0.257(7) 0.051(6) -0.067(5) -0.147(6) O8W 0.407(13) 0.346(12) 0.177(7) -0.099(7) 0.081(7) -0.128(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 N6 2.0346(19) . ? Ru1 N8 2.0494(18) . ? Ru1 N7B 2.055(2) . ? Ru1 N13 2.0608(18) . ? Ru1 N9 2.0760(18) . ? Ru1 N11 2.0902(19) . ? Fe1 C4 1.932(3) . ? Fe1 C3 1.940(2) . ? Fe1 C1 1.941(3) . ? Fe1 C5 1.944(3) . ? Fe1 C2 1.944(3) . ? Fe1 C6 1.949(2) . ? P1 C34 1.791(3) . ? P1 C36 1.792(3) . ? P1 C27 1.798(3) . ? P1 C29 1.801(3) . ? N11 C23 1.325(3) . ? N11 N12 1.366(3) . ? N6 C6 1.148(3) . ? N8 C16 1.344(3) . ? N8 C12 1.354(3) . ? N9 C17 1.330(3) . ? N9 N10 1.361(3) . ? N12 C25 1.348(3) . ? N12 C26 1.442(3) . ? N13 C20 1.331(3) . ? N13 N14 1.358(3) . ? C3 N3 1.147(3) . ? N10 C19 1.350(3) . ? N10 C26 1.440(3) . ? C2 N2 1.145(4) . ? N14 C22 1.351(3) . ? N14 C26 1.445(3) . ? C23 C24 1.398(4) . ? C12 C13 1.392(3) . ? C12 C7 1.468(3) . ? C5 N5 1.138(3) . ? C24 C25 1.358(4) . ? C15 C14 1.372(4) . ? C15 C16 1.381(3) . ? C22 C21 1.360(4) . ? C1 N1 1.136(4) . ? C17 C18 1.389(4) . ? C7 N7B 1.363(3) . ? C7 C8 1.387(4) . ? C4 N4 1.149(4) . ? C21 C20 1.390(4) . ? C18 C19 1.358(4) . ? C13 C14 1.368(4) . ? C29 C30 1.383(5) . ? C29 C33 1.390(5) . ? C36 C37 1.365(5) . ? C36 C41 1.385(5) . ? C11 N7B 1.340(3) . ? C11 C10 1.372(4) . ? C10 C9 1.379(5) . ? C8 C9 1.373(4) . ? C34 C42 1.355(5) . ? C34 C35 1.383(5) . ? C37 C38 1.394(5) . ? C50 C32 1.371(7) . ? C50 C30 1.377(5) . ? C27 C28 1.346(5) . ? C27 C47 1.372(6) . ? C28 C51 1.369(7) . ? C33 C46 1.380(5) . ? C32 C46 1.361(7) . ? C35 C45 1.393(7) . ? C38 C39 1.363(7) . ? C41 C40 1.380(6) . ? C39 C40 1.348(8) . ? C42 C43 1.394(7) . ? C44 C43 1.307(7) . ? C44 C45 1.318(8) . ? C51 C49 1.275(8) . ? C49 C48 1.286(9) . ? C47 C48 1.406(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ru1 N8 89.89(7) . . ? N6 Ru1 N7B 95.51(7) . . ? N8 Ru1 N7B 78.67(8) . . ? N6 Ru1 N13 173.17(7) . . ? N8 Ru1 N13 90.80(7) . . ? N7B Ru1 N13 91.28(8) . . ? N6 Ru1 N9 92.97(7) . . ? N8 Ru1 N9 175.59(7) . . ? N7B Ru1 N9 97.70(8) . . ? N13 Ru1 N9 86.76(7) . . ? N6 Ru1 N11 87.04(7) . . ? N8 Ru1 N11 100.15(7) . . ? N7B Ru1 N11 177.17(7) . . ? N13 Ru1 N11 86.15(7) . . ? N9 Ru1 N11 83.36(7) . . ? C4 Fe1 C3 92.04(13) . . ? C4 Fe1 C1 91.66(13) . . ? C3 Fe1 C1 176.06(11) . . ? C4 Fe1 C5 89.96(12) . . ? C3 Fe1 C5 93.16(10) . . ? C1 Fe1 C5 88.19(11) . . ? C4 Fe1 C2 86.03(12) . . ? C3 Fe1 C2 86.62(10) . . ? C1 Fe1 C2 92.29(11) . . ? C5 Fe1 C2 175.97(10) . . ? C4 Fe1 C6 177.17(12) . . ? C3 Fe1 C6 86.17(10) . . ? C1 Fe1 C6 90.08(10) . . ? C5 Fe1 C6 92.33(10) . . ? C2 Fe1 C6 91.67(10) . . ? C34 P1 C36 108.96(15) . . ? C34 P1 C27 110.24(16) . . ? C36 P1 C27 110.52(15) . . ? C34 P1 C29 108.86(15) . . ? C36 P1 C29 109.18(15) . . ? C27 P1 C29 109.04(15) . . ? C23 N11 N12 105.22(19) . . ? C23 N11 Ru1 137.45(16) . . ? N12 N11 Ru1 116.61(14) . . ? C6 N6 Ru1 163.58(17) . . ? C16 N8 C12 118.2(2) . . ? C16 N8 Ru1 125.85(16) . . ? C12 N8 Ru1 115.96(16) . . ? C17 N9 N10 104.72(19) . . ? C17 N9 Ru1 137.49(18) . . ? N10 N9 Ru1 117.76(14) . . ? N6 C6 Fe1 172.89(19) . . ? C25 N12 N11 111.2(2) . . ? C25 N12 C26 128.3(2) . . ? N11 N12 C26 119.86(19) . . ? C20 N13 N14 105.0(2) . . ? C20 N13 Ru1 136.92(18) . . ? N14 N13 Ru1 117.96(14) . . ? N3 C3 Fe1 174.4(2) . . ? C19 N10 N9 111.5(2) . . ? C19 N10 C26 129.4(2) . . ? N9 N10 C26 118.83(18) . . ? N2 C2 Fe1 176.1(3) . . ? C22 N14 N13 111.6(2) . . ? C22 N14 C26 129.1(2) . . ? N13 N14 C26 119.28(18) . . ? N11 C23 C24 110.6(2) . . ? N8 C12 C13 121.4(2) . . ? N8 C12 C7 114.5(2) . . ? C13 C12 C7 124.1(2) . . ? N5 C5 Fe1 179.0(2) . . ? C25 C24 C23 106.0(2) . . ? C14 C15 C16 119.2(3) . . ? N14 C22 C21 106.5(2) . . ? N1 C1 Fe1 176.3(3) . . ? N10 C26 N12 109.95(19) . . ? N10 C26 N14 110.6(2) . . ? N12 C26 N14 110.80(19) . . ? N9 C17 C18 111.0(3) . . ? N7B C7 C8 121.3(2) . . ? N7B C7 C12 114.8(2) . . ? C8 C7 C12 123.9(2) . . ? N4 C4 Fe1 178.0(3) . . ? C22 C21 C20 106.2(2) . . ? N13 C20 C21 110.6(3) . . ? N12 C25 C24 106.9(2) . . ? C19 C18 C17 106.0(2) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 119.3(2) . . ? N8 C16 C15 122.4(2) . . ? N10 C19 C18 106.8(2) . . ? C30 C29 C33 120.0(3) . . ? C30 C29 P1 119.1(3) . . ? C33 C29 P1 120.8(3) . . ? C37 C36 C41 119.7(3) . . ? C37 C36 P1 121.8(3) . . ? C41 C36 P1 118.6(3) . . ? N7B C11 C10 123.4(3) . . ? C11 C10 C9 119.2(3) . . ? C9 C8 C7 120.2(3) . . ? C42 C34 C35 118.2(4) . . ? C42 C34 P1 120.6(3) . . ? C35 C34 P1 121.3(3) . . ? C8 C9 C10 118.3(3) . . ? C36 C37 C38 120.0(4) . . ? C32 C50 C30 120.2(4) . . ? C28 C27 C47 117.3(4) . . ? C28 C27 P1 121.0(3) . . ? C47 C27 P1 121.5(3) . . ? C27 C28 C51 120.7(5) . . ? C50 C30 C29 119.7(4) . . ? C46 C33 C29 119.0(4) . . ? C46 C32 C50 120.2(4) . . ? C34 C35 C45 118.4(5) . . ? C11 N7B C7 117.5(2) . . ? C11 N7B Ru1 127.10(17) . . ? C7 N7B Ru1 115.39(16) . . ? C32 C46 C33 120.9(4) . . ? C39 C38 C37 119.5(4) . . ? C40 C41 C36 119.5(4) . . ? C40 C39 C38 120.8(4) . . ? C34 C42 C43 119.8(5) . . ? C43 C44 C45 119.8(5) . . ? C49 C51 C28 122.5(6) . . ? C44 C45 C35 121.9(5) . . ? C39 C40 C41 120.5(5) . . ? C44 C43 C42 121.5(5) . . ? C51 C49 C48 118.4(6) . . ? C27 C47 C48 116.9(6) . . ? C49 C48 C47 123.8(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.793 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.068 #END data_4a _database_code_depnum_ccdc_archive 'CCDC 843192' #TrackingRef 'cadranel_etal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H39 Cr N11 O5 P Ru' _chemical_formula_weight 1118.01 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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_space_group_name_H-M 'P -1' _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9762(2) _cell_length_b 13.3785(2) _cell_length_c 17.4059(3) _cell_angle_alpha 101.840(2) _cell_angle_beta 96.3190(10) _cell_angle_gamma 114.081(2) _cell_volume 2635.77(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16335 _cell_measurement_theta_min 3.6828 _cell_measurement_theta_max 28.9621 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_T_min 0.78370 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET) (compiled Oct 27 2009,12:04:35) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1158 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33560 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 26.75 _reflns_number_total 11131 _reflns_number_gt 7759 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^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 11131 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.647907(18) 0.221916(18) 0.376446(12) 0.03939(8) Uani 1 1 d . . . Cr1 Cr 0.21117(4) 0.09975(4) 0.26618(2) 0.04278(12) Uani 1 1 d . . . P1 P 0.76788(7) 0.50036(7) 0.06371(5) 0.0528(2) Uani 1 1 d . . . N6 N 0.4736(2) 0.16705(19) 0.34801(13) 0.0439(5) Uani 1 1 d . . . C23 C 0.6927(3) 0.1256(3) 0.10311(19) 0.0646(9) Uani 1 1 d . . . H23 H 0.7034 0.1041 0.0514 0.078 Uiso 1 1 calc R . . C27 C 0.2628(3) 0.0792(3) 0.15728(19) 0.0542(7) Uani 1 1 d . . . C26 C 0.3789(2) 0.1435(2) 0.32325(16) 0.0455(6) Uani 1 1 d . . . C29 C 0.1675(3) -0.0669(3) 0.26544(18) 0.0564(8) Uani 1 1 d . . . C35 C 0.5400(4) 0.6015(4) 0.1546(2) 0.0856(12) Uani 1 1 d . . . H35 H 0.5231 0.6635 0.1601 0.103 Uiso 1 1 calc R . . N5 N 0.66053(19) 0.18808(18) 0.25689(12) 0.0412(5) Uani 1 1 d . . . N1 N 0.66264(19) 0.38514(19) 0.40199(13) 0.0463(6) Uani 1 1 d . . . N4 N 0.82213(18) 0.27382(18) 0.38774(13) 0.0423(5) Uani 1 1 d . . . N2 N 0.64755(19) 0.2514(2) 0.49181(13) 0.0471(6) Uani 1 1 d . . . N9 N -0.0446(3) 0.0294(3) 0.1706(2) 0.0936(11) Uani 1 1 d . . . N8 N 0.2941(3) 0.0697(3) 0.09842(18) 0.0799(9) Uani 1 1 d . . . C17 C 1.0166(3) 0.3486(3) 0.4600(2) 0.0637(9) Uani 1 1 d . . . H17 H 1.0704 0.3856 0.5087 0.076 Uiso 1 1 calc R . . C11 C 0.6545(2) 0.4253(3) 0.47948(17) 0.0504(7) Uani 1 1 d . . . C20 C 0.8557(2) 0.2449(2) 0.31860(16) 0.0443(6) Uani 1 1 d . . . C24 C 0.5878(3) 0.1192(3) 0.11485(17) 0.0571(8) Uani 1 1 d . . . H24 H 0.5267 0.0943 0.0712 0.069 Uiso 1 1 calc R . . C12 C 0.6548(3) 0.5302(3) 0.5056(2) 0.0725(10) Uani 1 1 d . . . H12 H 0.6464 0.5551 0.5574 0.087 Uiso 1 1 calc R . . C25 C 0.5739(2) 0.1498(2) 0.19160(16) 0.0480(7) Uani 1 1 d . . . H25 H 0.5020 0.1442 0.1991 0.058 Uiso 1 1 calc R . . C21 C 0.7649(2) 0.1967(2) 0.24460(16) 0.0450(6) Uani 1 1 d . . . C18 C 1.0495(3) 0.3170(3) 0.3917(2) 0.0649(9) Uani 1 1 d . . . H18 H 1.1261 0.3306 0.3933 0.078 Uiso 1 1 calc R . . C19 C 0.9696(3) 0.2646(3) 0.31962(19) 0.0582(8) Uani 1 1 d . . . H19 H 0.9916 0.2428 0.2724 0.070 Uiso 1 1 calc R . . C34 C 0.4777(4) 0.5135(4) 0.1841(2) 0.0810(11) Uani 1 1 d . . . H34 H 0.4191 0.5163 0.2095 0.097 Uiso 1 1 calc R . . N3 N 0.6369(2) 0.0704(2) 0.39662(16) 0.0554(6) Uani 1 1 d . . . C22 C 0.7816(3) 0.1640(3) 0.16820(18) 0.0593(8) Uani 1 1 d . . . H22 H 0.8531 0.1682 0.1611 0.071 Uiso 1 1 calc R . . N7 N 0.2738(3) 0.3619(3) 0.27931(18) 0.0798(9) Uani 1 1 d . . . C15 C 0.6745(3) 0.4529(3) 0.3537(2) 0.0659(9) Uani 1 1 d . . . H15 H 0.6804 0.4271 0.3013 0.079 Uiso 1 1 calc R . . C33 C 0.5005(3) 0.4216(4) 0.1768(2) 0.0773(10) Uani 1 1 d . . . H33 H 0.4567 0.3613 0.1961 0.093 Uiso 1 1 calc R . . N10 N 0.1440(3) -0.1564(3) 0.2696(2) 0.0875(10) Uani 1 1 d . . . C30 C 0.2531(3) 0.2693(3) 0.27412(17) 0.0520(7) Uani 1 1 d . . . C10 C 0.6500(2) 0.3507(3) 0.53113(17) 0.0527(7) Uani 1 1 d . . . C16 C 0.9022(3) 0.3251(3) 0.45649(18) 0.0535(7) Uani 1 1 d . . . H16 H 0.8797 0.3456 0.5038 0.064 Uiso 1 1 calc R . . C31 C 0.6531(3) 0.5071(3) 0.10938(18) 0.0565(8) Uani 1 1 d . . . C37 C 0.7144(3) 0.3803(3) -0.02282(18) 0.0569(8) Uani 1 1 d . . . C36 C 0.6284(3) 0.5997(3) 0.1164(2) 0.0718(10) Uani 1 1 d . . . H36 H 0.6701 0.6595 0.0959 0.086 Uiso 1 1 calc R . . C39 C 0.8430(3) 0.6266(2) 0.03358(17) 0.0544(7) Uani 1 1 d . . . C5 C 0.6450(3) 0.0719(3) 0.4757(2) 0.0678(9) Uani 1 1 d . . . C40 C 0.7901(4) 0.6437(3) -0.0330(2) 0.0786(11) Uani 1 1 d . . . H40 H 0.7166 0.5897 -0.0616 0.094 Uiso 1 1 calc R . . C9 C 0.6531(3) 0.3745(4) 0.6131(2) 0.0770(10) Uani 1 1 d . . . H9 H 0.6538 0.4421 0.6410 0.092 Uiso 1 1 calc R . . C13 C 0.6679(4) 0.5973(3) 0.4535(3) 0.0998(16) Uani 1 1 d . . . H13 H 0.6696 0.6687 0.4704 0.120 Uiso 1 1 calc R . . C41 C 0.8465(4) 0.7409(4) -0.0566(2) 0.0896(13) Uani 1 1 d . . . H41 H 0.8106 0.7530 -0.1007 0.108 Uiso 1 1 calc R . . C4 C 0.6489(4) -0.0172(4) 0.5022(3) 0.1030(15) Uani 1 1 d . . . H4 H 0.6525 -0.0154 0.5562 0.124 Uiso 1 1 calc R . . C32 C 0.5888(3) 0.4187(3) 0.1407(2) 0.0680(9) Uani 1 1 d . . . H32 H 0.6059 0.3570 0.1372 0.082 Uiso 1 1 calc R . . C7 C 0.6535(4) 0.1961(4) 0.6120(2) 0.0900(13) Uani 1 1 d . . . H7 H 0.6565 0.1442 0.6394 0.108 Uiso 1 1 calc R . . C42 C 0.9518(3) 0.7073(3) 0.0757(2) 0.0675(9) Uani 1 1 d . . . H42 H 0.9875 0.6970 0.1208 0.081 Uiso 1 1 calc R . . C38 C 0.7860(3) 0.3774(3) -0.0758(2) 0.0759(10) Uani 1 1 d . . . H38 H 0.8567 0.4402 -0.0687 0.091 Uiso 1 1 calc R . . C8 C 0.6549(4) 0.2947(5) 0.6521(2) 0.0999(15) Uani 1 1 d . . . H8 H 0.6572 0.3093 0.7070 0.120 Uiso 1 1 calc R . . C1 C 0.6342(3) -0.0192(3) 0.3435(3) 0.0788(11) Uani 1 1 d . . . H1 H 0.6287 -0.0208 0.2895 0.095 Uiso 1 1 calc R . . C6 C 0.6477(3) 0.1729(3) 0.52977(19) 0.0628(9) Uani 1 1 d . . . C14 C 0.6783(4) 0.5597(3) 0.3781(3) 0.0979(15) Uani 1 1 d . . . H14 H 0.6880 0.6050 0.3429 0.117 Uiso 1 1 calc R . . C28 C 0.0462(3) 0.0536(3) 0.20545(18) 0.0585(8) Uani 1 1 d . . . C2 C 0.6396(4) -0.1106(4) 0.3686(4) 0.1128(18) Uani 1 1 d . . . H2 H 0.6379 -0.1727 0.3317 0.135 Uiso 1 1 calc R . . C3 C 0.6476(5) -0.1066(4) 0.4491(4) 0.128(2) Uani 1 1 d . . . H3 H 0.6520 -0.1662 0.4667 0.154 Uiso 1 1 calc R . . C54 C 0.1643(3) 0.1190(3) 0.3761(2) 0.0545(7) Uani 1 1 d . . . N11 N 0.1388(3) 0.1267(3) 0.43667(19) 0.0832(9) Uani 1 1 d . . . C49 C 0.8677(3) 0.4870(3) 0.13647(19) 0.0584(8) Uani 1 1 d . . . C48 C 0.6070(3) 0.2876(3) -0.0369(2) 0.0688(9) Uani 1 1 d . . . H48 H 0.5562 0.2889 -0.0034 0.083 Uiso 1 1 calc R . . C50 C 0.9224(3) 0.4198(3) 0.1139(3) 0.0783(11) Uani 1 1 d . . . H50 H 0.9016 0.3735 0.0616 0.094 Uiso 1 1 calc R . . C53 C 0.8964(4) 0.5536(3) 0.2145(2) 0.0811(11) Uani 1 1 d . . . H53 H 0.8597 0.5990 0.2300 0.097 Uiso 1 1 calc R . . C43 C 1.0077(4) 0.8034(3) 0.0506(2) 0.0838(11) Uani 1 1 d . . . H43 H 1.0815 0.8576 0.0786 0.101 Uiso 1 1 calc R . . C47 C 0.5762(4) 0.1932(3) -0.1012(2) 0.0805(11) Uani 1 1 d . . . H47 H 0.5044 0.1309 -0.1106 0.097 Uiso 1 1 calc R . . C46 C 0.6491(5) 0.1904(4) -0.1505(2) 0.0877(13) Uani 1 1 d . . . H46 H 0.6280 0.1253 -0.1923 0.105 Uiso 1 1 calc R . . C44 C 0.9548(4) 0.8189(3) -0.0153(2) 0.0885(13) Uani 1 1 d . . . H44 H 0.9932 0.8836 -0.0320 0.106 Uiso 1 1 calc R . . C45 C 0.7529(4) 0.2818(4) -0.1394(2) 0.0893(12) Uani 1 1 d . . . H45 H 0.8015 0.2799 -0.1745 0.107 Uiso 1 1 calc R . . C52 C 1.0372(4) 0.4876(5) 0.2465(4) 0.119(2) Uani 1 1 d . . . H52 H 1.0955 0.4889 0.2835 0.143 Uiso 1 1 calc R . . C55 C 0.9818(4) 0.5517(4) 0.2699(3) 0.1077(17) Uani 1 1 d . . . H55 H 1.0006 0.5946 0.3232 0.129 Uiso 1 1 calc R . . C51 C 1.0085(4) 0.4219(4) 0.1698(4) 0.1022(15) Uani 1 1 d . . . H51 H 1.0468 0.3780 0.1546 0.123 Uiso 1 1 calc R . . O4W O 0.8378(5) 0.7924(5) 0.2729(4) 0.248(3) Uani 1 1 d . . . O1W O 0.0510(9) 0.7884(7) 0.4068(4) 0.307(4) Uani 1 1 d . . . O5W O 0.7398(10) 0.8971(7) 0.1999(10) 0.432(8) Uani 1 1 d . . . O3WA O 0.9103(11) 0.0481(13) 0.4541(8) 0.247(4) Uani 0.50 1 d P A 1 O3WB O 1.0604(12) 0.1412(15) 0.5798(9) 0.247(4) Uani 0.50 1 d P B 2 O2WA O 0.305(4) 0.131(3) 0.9311(13) 0.167(5) Uani 0.50 1 d P C 1 O2WB O 0.310(4) 0.146(3) 0.9622(14) 0.167(5) Uani 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03425(12) 0.04361(13) 0.04018(13) 0.01192(9) -0.00045(8) 0.01904(10) Cr1 0.0354(2) 0.0475(3) 0.0432(2) 0.0112(2) -0.00033(18) 0.0189(2) P1 0.0562(5) 0.0478(4) 0.0499(4) 0.0169(3) 0.0027(4) 0.0192(4) N6 0.0409(13) 0.0466(13) 0.0434(12) 0.0137(10) 0.0032(10) 0.0196(11) C23 0.079(2) 0.069(2) 0.0441(17) 0.0086(15) 0.0140(16) 0.033(2) C27 0.0492(17) 0.0588(19) 0.0503(18) 0.0086(14) -0.0022(14) 0.0261(15) C26 0.0374(15) 0.0493(16) 0.0444(15) 0.0115(12) 0.0021(12) 0.0163(13) C29 0.061(2) 0.0529(19) 0.0541(18) 0.0107(15) 0.0048(15) 0.0283(16) C35 0.091(3) 0.093(3) 0.083(3) 0.012(2) 0.004(2) 0.060(3) N5 0.0413(12) 0.0384(12) 0.0426(12) 0.0096(10) 0.0019(10) 0.0189(10) N1 0.0406(13) 0.0473(13) 0.0460(13) 0.0086(11) -0.0062(10) 0.0206(11) N4 0.0373(12) 0.0443(13) 0.0482(13) 0.0137(10) 0.0023(10) 0.0220(11) N2 0.0360(12) 0.0609(15) 0.0423(12) 0.0184(11) -0.0005(10) 0.0196(12) N9 0.0597(19) 0.124(3) 0.091(2) 0.007(2) -0.0089(17) 0.052(2) N8 0.074(2) 0.117(3) 0.0532(17) 0.0198(17) 0.0103(15) 0.048(2) C17 0.0397(16) 0.079(2) 0.065(2) 0.0156(17) -0.0064(15) 0.0254(17) C11 0.0367(15) 0.0560(18) 0.0500(17) 0.0015(14) -0.0047(12) 0.0219(14) C20 0.0410(15) 0.0434(15) 0.0523(16) 0.0121(12) 0.0068(12) 0.0238(13) C24 0.066(2) 0.0529(18) 0.0427(16) 0.0058(13) -0.0030(14) 0.0237(16) C12 0.068(2) 0.069(2) 0.066(2) -0.0139(18) -0.0155(17) 0.0391(19) C25 0.0445(16) 0.0462(16) 0.0466(16) 0.0082(13) -0.0029(12) 0.0189(14) C21 0.0448(16) 0.0427(15) 0.0508(16) 0.0129(12) 0.0094(12) 0.0228(13) C18 0.0385(16) 0.083(2) 0.080(2) 0.0259(19) 0.0080(16) 0.0327(17) C19 0.0501(18) 0.067(2) 0.066(2) 0.0166(16) 0.0122(15) 0.0342(17) C34 0.068(2) 0.109(3) 0.066(2) 0.021(2) 0.0095(19) 0.042(3) N3 0.0476(14) 0.0519(15) 0.0685(16) 0.0215(13) -0.0003(12) 0.0246(12) C22 0.0586(19) 0.066(2) 0.0571(19) 0.0117(16) 0.0158(15) 0.0326(17) N7 0.107(3) 0.0602(19) 0.073(2) 0.0181(15) 0.0340(18) 0.0347(19) C15 0.080(2) 0.0552(19) 0.0583(19) 0.0174(16) -0.0045(17) 0.0299(18) C33 0.068(2) 0.088(3) 0.069(2) 0.027(2) 0.0139(19) 0.026(2) N10 0.116(3) 0.061(2) 0.085(2) 0.0210(17) 0.018(2) 0.040(2) C30 0.0567(18) 0.0565(19) 0.0433(16) 0.0126(14) 0.0131(13) 0.0255(16) C10 0.0397(15) 0.066(2) 0.0422(16) 0.0068(14) -0.0003(12) 0.0197(15) C16 0.0449(16) 0.0645(19) 0.0487(16) 0.0114(14) 0.0017(13) 0.0259(16) C31 0.0544(18) 0.0555(18) 0.0526(17) 0.0130(14) 0.0003(14) 0.0212(16) C37 0.064(2) 0.0507(18) 0.0550(18) 0.0162(14) 0.0044(15) 0.0257(17) C36 0.080(3) 0.066(2) 0.071(2) 0.0190(18) 0.0077(19) 0.036(2) C39 0.065(2) 0.0450(16) 0.0453(16) 0.0145(13) 0.0012(14) 0.0192(15) C5 0.056(2) 0.069(2) 0.079(2) 0.0389(19) -0.0032(17) 0.0250(18) C40 0.088(3) 0.068(2) 0.070(2) 0.0274(19) -0.0106(19) 0.027(2) C9 0.075(2) 0.093(3) 0.0466(19) 0.0040(19) 0.0067(17) 0.030(2) C13 0.118(4) 0.060(2) 0.107(3) -0.007(2) -0.030(3) 0.053(3) C41 0.129(4) 0.080(3) 0.067(2) 0.037(2) 0.006(2) 0.049(3) C4 0.110(4) 0.087(3) 0.118(4) 0.058(3) -0.010(3) 0.043(3) C32 0.078(2) 0.064(2) 0.064(2) 0.0240(17) 0.0179(18) 0.030(2) C7 0.095(3) 0.113(3) 0.063(2) 0.050(2) 0.009(2) 0.038(3) C42 0.077(2) 0.0536(19) 0.0572(19) 0.0173(16) 0.0005(17) 0.0175(18) C38 0.072(2) 0.074(2) 0.067(2) 0.0100(19) 0.0057(19) 0.024(2) C8 0.114(4) 0.126(4) 0.041(2) 0.025(2) 0.006(2) 0.038(3) C1 0.075(2) 0.057(2) 0.100(3) 0.010(2) -0.009(2) 0.037(2) C6 0.0545(19) 0.077(2) 0.0552(18) 0.0335(17) -0.0018(15) 0.0230(18) C14 0.132(4) 0.057(2) 0.093(3) 0.016(2) -0.027(3) 0.045(3) C28 0.0485(18) 0.070(2) 0.0560(18) 0.0104(15) -0.0026(14) 0.0325(17) C2 0.121(4) 0.068(3) 0.149(5) 0.020(3) -0.012(3) 0.056(3) C3 0.153(5) 0.085(3) 0.156(5) 0.050(3) -0.021(4) 0.067(4) C54 0.0469(17) 0.0606(19) 0.0568(19) 0.0210(15) 0.0080(14) 0.0233(16) N11 0.091(2) 0.103(2) 0.066(2) 0.0334(18) 0.0272(18) 0.045(2) C49 0.0546(18) 0.0589(19) 0.062(2) 0.0327(16) 0.0074(15) 0.0196(16) C48 0.079(2) 0.053(2) 0.065(2) 0.0163(16) 0.0078(18) 0.0219(19) C50 0.072(2) 0.079(3) 0.094(3) 0.047(2) 0.015(2) 0.033(2) C53 0.088(3) 0.082(3) 0.062(2) 0.031(2) -0.0023(19) 0.027(2) C43 0.089(3) 0.056(2) 0.072(2) 0.0160(18) 0.005(2) 0.004(2) C47 0.100(3) 0.051(2) 0.067(2) 0.0108(18) 0.001(2) 0.017(2) C46 0.121(4) 0.062(2) 0.066(2) 0.0023(19) -0.003(3) 0.041(3) C44 0.135(4) 0.056(2) 0.073(2) 0.031(2) 0.026(3) 0.034(3) C45 0.103(3) 0.103(3) 0.063(2) 0.010(2) 0.013(2) 0.054(3) C52 0.074(3) 0.125(4) 0.143(5) 0.093(4) -0.020(3) 0.014(3) C55 0.106(4) 0.108(4) 0.077(3) 0.047(3) -0.021(3) 0.017(3) C51 0.070(3) 0.113(4) 0.147(4) 0.082(4) 0.019(3) 0.042(3) O4W 0.174(5) 0.189(5) 0.330(9) 0.001(5) -0.006(5) 0.079(4) O1W 0.404(13) 0.279(8) 0.202(6) 0.137(6) 0.088(7) 0.078(8) O5W 0.384(14) 0.214(8) 0.76(3) 0.159(11) 0.300(16) 0.131(9) O3WA 0.190(8) 0.338(12) 0.261(10) 0.159(9) 0.118(7) 0.110(9) O3WB 0.190(8) 0.338(12) 0.261(10) 0.159(9) 0.118(7) 0.110(9) O2WA 0.274(7) 0.169(9) 0.136(15) 0.079(13) 0.148(16) 0.130(7) O2WB 0.274(7) 0.169(9) 0.136(15) 0.079(13) 0.148(16) 0.130(7) _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 N2 1.966(2) . ? Ru1 N6 2.037(2) . ? Ru1 N4 2.049(2) . ? Ru1 N1 2.060(2) . ? Ru1 N5 2.076(2) . ? Ru1 N3 2.078(2) . ? Cr1 C28 2.058(3) . ? Cr1 C29 2.061(3) . ? Cr1 C54 2.068(3) . ? Cr1 C30 2.075(3) . ? Cr1 C26 2.076(3) . ? Cr1 C27 2.082(3) . ? P1 C37 1.789(3) . ? P1 C31 1.789(3) . ? P1 C39 1.792(3) . ? P1 C49 1.799(3) . ? N6 C26 1.144(3) . ? C23 C22 1.366(4) . ? C23 C24 1.370(5) . ? C27 N8 1.145(4) . ? C29 N10 1.129(4) . ? C35 C34 1.367(6) . ? C35 C36 1.395(5) . ? N5 C25 1.352(3) . ? N5 C21 1.357(3) . ? N1 C15 1.334(4) . ? N1 C11 1.378(4) . ? N4 C16 1.338(3) . ? N4 C20 1.360(3) . ? N2 C10 1.350(4) . ? N2 C6 1.351(4) . ? N9 C28 1.145(4) . ? C17 C18 1.353(5) . ? C17 C16 1.378(4) . ? C11 C12 1.382(4) . ? C11 C10 1.462(4) . ? C20 C19 1.388(4) . ? C20 C21 1.473(4) . ? C24 C25 1.369(4) . ? C12 C13 1.379(6) . ? C21 C22 1.381(4) . ? C18 C19 1.378(4) . ? C34 C33 1.362(5) . ? N3 C1 1.340(4) . ? N3 C5 1.364(4) . ? N7 C30 1.136(4) . ? C15 C14 1.384(5) . ? C33 C32 1.376(5) . ? C10 C9 1.389(4) . ? C31 C36 1.386(4) . ? C31 C32 1.398(4) . ? C37 C38 1.385(5) . ? C37 C48 1.389(5) . ? C39 C42 1.379(4) . ? C39 C40 1.388(4) . ? C5 C4 1.381(5) . ? C5 C6 1.465(5) . ? C40 C41 1.380(5) . ? C9 C8 1.384(6) . ? C13 C14 1.348(6) . ? C41 C44 1.362(6) . ? C4 C3 1.347(7) . ? C7 C8 1.352(6) . ? C7 C6 1.388(5) . ? C42 C43 1.381(5) . ? C38 C45 1.383(5) . ? C1 C2 1.406(5) . ? C2 C3 1.382(7) . ? C54 N11 1.136(4) . ? C49 C53 1.378(5) . ? C49 C50 1.379(5) . ? C48 C47 1.385(5) . ? C50 C51 1.386(5) . ? C53 C55 1.399(5) . ? C43 C44 1.369(5) . ? C47 C46 1.351(6) . ? C46 C45 1.360(6) . ? C52 C51 1.355(7) . ? C52 C55 1.358(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N6 90.97(9) . . ? N2 Ru1 N4 97.21(9) . . ? N6 Ru1 N4 171.79(8) . . ? N2 Ru1 N1 79.33(9) . . ? N6 Ru1 N1 86.90(9) . . ? N4 Ru1 N1 94.06(9) . . ? N2 Ru1 N5 175.07(8) . . ? N6 Ru1 N5 93.33(8) . . ? N4 Ru1 N5 78.52(8) . . ? N1 Ru1 N5 103.29(9) . . ? N2 Ru1 N3 79.23(10) . . ? N6 Ru1 N3 94.72(9) . . ? N4 Ru1 N3 87.37(9) . . ? N1 Ru1 N3 158.53(10) . . ? N5 Ru1 N3 97.99(9) . . ? C28 Cr1 C29 90.56(13) . . ? C28 Cr1 C54 91.74(12) . . ? C29 Cr1 C54 86.69(12) . . ? C28 Cr1 C30 89.86(13) . . ? C29 Cr1 C30 176.41(12) . . ? C54 Cr1 C30 89.73(12) . . ? C28 Cr1 C26 177.75(12) . . ? C29 Cr1 C26 88.86(12) . . ? C54 Cr1 C26 90.40(11) . . ? C30 Cr1 C26 90.86(12) . . ? C28 Cr1 C27 90.00(12) . . ? C29 Cr1 C27 92.42(12) . . ? C54 Cr1 C27 178.05(11) . . ? C30 Cr1 C27 91.14(12) . . ? C26 Cr1 C27 87.85(11) . . ? C37 P1 C31 111.20(15) . . ? C37 P1 C39 108.42(14) . . ? C31 P1 C39 111.25(15) . . ? C37 P1 C49 108.99(15) . . ? C31 P1 C49 108.03(15) . . ? C39 P1 C49 108.91(14) . . ? C26 N6 Ru1 170.1(2) . . ? C22 C23 C24 119.2(3) . . ? N8 C27 Cr1 178.2(3) . . ? N6 C26 Cr1 173.8(3) . . ? N10 C29 Cr1 176.1(3) . . ? C34 C35 C36 120.9(4) . . ? C25 N5 C21 117.8(2) . . ? C25 N5 Ru1 126.7(2) . . ? C21 N5 Ru1 115.23(17) . . ? C15 N1 C11 117.5(3) . . ? C15 N1 Ru1 129.0(2) . . ? C11 N1 Ru1 113.42(18) . . ? C16 N4 C20 118.4(2) . . ? C16 N4 Ru1 126.1(2) . . ? C20 N4 Ru1 115.30(17) . . ? C10 N2 C6 122.0(3) . . ? C10 N2 Ru1 119.00(18) . . ? C6 N2 Ru1 119.0(2) . . ? C18 C17 C16 119.0(3) . . ? N1 C11 C12 121.4(3) . . ? N1 C11 C10 114.9(2) . . ? C12 C11 C10 123.7(3) . . ? N4 C20 C19 120.9(3) . . ? N4 C20 C21 115.4(2) . . ? C19 C20 C21 123.7(3) . . ? C25 C24 C23 119.2(3) . . ? C13 C12 C11 118.8(3) . . ? N5 C25 C24 122.5(3) . . ? N5 C21 C22 121.3(3) . . ? N5 C21 C20 114.1(2) . . ? C22 C21 C20 124.6(3) . . ? C17 C18 C19 120.0(3) . . ? C18 C19 C20 119.1(3) . . ? C33 C34 C35 120.7(4) . . ? C1 N3 C5 119.1(3) . . ? C1 N3 Ru1 127.6(2) . . ? C5 N3 Ru1 112.9(2) . . ? C23 C22 C21 119.8(3) . . ? N1 C15 C14 122.9(3) . . ? C34 C33 C32 119.5(4) . . ? N7 C30 Cr1 178.3(3) . . ? N2 C10 C9 119.8(3) . . ? N2 C10 C11 113.0(2) . . ? C9 C10 C11 127.1(3) . . ? N4 C16 C17 122.7(3) . . ? C36 C31 C32 119.2(3) . . ? C36 C31 P1 121.5(3) . . ? C32 C31 P1 119.4(3) . . ? C38 C37 C48 118.8(3) . . ? C38 C37 P1 118.2(3) . . ? C48 C37 P1 122.9(3) . . ? C31 C36 C35 118.8(4) . . ? C42 C39 C40 119.6(3) . . ? C42 C39 P1 121.1(2) . . ? C40 C39 P1 119.3(3) . . ? N3 C5 C4 121.7(4) . . ? N3 C5 C6 115.7(3) . . ? C4 C5 C6 122.6(4) . . ? C41 C40 C39 120.0(4) . . ? C8 C9 C10 118.1(4) . . ? C14 C13 C12 120.1(3) . . ? C44 C41 C40 119.8(3) . . ? C3 C4 C5 119.2(4) . . ? C33 C32 C31 120.9(3) . . ? C8 C7 C6 119.6(4) . . ? C39 C42 C43 119.7(3) . . ? C45 C38 C37 120.3(4) . . ? C7 C8 C9 121.3(4) . . ? N3 C1 C2 120.7(4) . . ? N2 C6 C7 119.1(4) . . ? N2 C6 C5 112.8(3) . . ? C7 C6 C5 128.1(3) . . ? C13 C14 C15 119.2(4) . . ? N9 C28 Cr1 178.5(4) . . ? C3 C2 C1 118.8(4) . . ? C4 C3 C2 120.5(4) . . ? N11 C54 Cr1 178.0(3) . . ? C53 C49 C50 120.3(3) . . ? C53 C49 P1 118.2(3) . . ? C50 C49 P1 121.2(3) . . ? C47 C48 C37 119.5(4) . . ? C49 C50 C51 119.6(4) . . ? C49 C53 C55 118.7(4) . . ? C44 C43 C42 120.1(4) . . ? C46 C47 C48 120.8(4) . . ? C47 C46 C45 120.6(4) . . ? C41 C44 C43 120.8(3) . . ? C46 C45 C38 120.0(4) . . ? C51 C52 C55 120.7(4) . . ? C52 C55 C53 120.4(5) . . ? C52 C51 C50 120.3(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.752 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.058