# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alain Igau' _publ_contact_author_email ALAIN.IGAU@LCC-TOULOUSE.FR _publ_section_title ; Broad HOMO-LUMO gap tuning through the coordination of a single phosphine, aminophosphine, or phosphite onto a Ru(tpy)(bpy)2+ core ; loop_ _publ_author_name 'Alain Igau' 'Isabelle Dixon' 'Alberto Juris' 'Emilie Lebon' 'Gilles Loustau' 'Pierre Sutra' 'Laure Vendier' # Attachment 'B806325G_Supp_Info.cif' data_(1.BH3) _database_code_depnum_ccdc_archive 'CCDC 665729' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H17 B1 N1 P' _chemical_formula_sum 'C16 H17 B N P' _chemical_formula_weight 265.09 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.503(2) _cell_length_b 10.494(2) _cell_length_c 15.347(3) _cell_angle_alpha 90.182(15) _cell_angle_beta 99.474(16) _cell_angle_gamma 103.301(18) _cell_volume 1467.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 1329 _cell_measurement_theta_min 2.8078 _cell_measurement_theta_max 32.1287 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description planar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.2 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 0.986 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_av_unetI/netI 0.1415 _diffrn_reflns_number 10776 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5575 _reflns_number_gt 2608 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0743P)^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_number_reflns 5575 _refine_ls_number_parameters 345 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.895 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.1392(4) 0.0361(5) 0.3061(3) 0.0407(12) Uani 1 1 d . . . H1 H 0.0616 0.0487 0.3324 0.049 Uiso 1 1 calc R . . C2 C 0.1328(6) -0.0673(5) 0.2425(4) 0.085(2) Uani 1 1 d D . . H2 H 0.0518 -0.1339 0.2197 0.102 Uiso 1 1 calc R . . C3 C 0.2861(7) -0.0444(5) 0.2205(3) 0.0617(16) Uani 1 1 d D . . H3 H 0.319 -0.0942 0.1815 0.074 Uiso 1 1 calc R . . C4 C 0.3679(5) 0.0671(4) 0.2713(3) 0.0341(10) Uani 1 1 d . . . H4 H 0.4667 0.1042 0.2712 0.041 Uiso 1 1 calc R . . C5 C 0.5177(4) 0.2600(4) 0.4389(2) 0.0243(9) Uani 1 1 d . . . C6 C 0.5410(5) 0.1722(4) 0.5039(3) 0.0353(11) Uani 1 1 d . . . H6 H 0.4616 0.1145 0.5213 0.042 Uiso 1 1 calc R . . C7 C 0.6820(5) 0.1705(5) 0.5428(3) 0.0405(11) Uani 1 1 d . . . H7 H 0.6967 0.1112 0.5864 0.049 Uiso 1 1 calc R . . C8 C 0.8001(5) 0.2541(5) 0.5186(3) 0.0476(13) Uani 1 1 d . . . H8 H 0.8947 0.2507 0.5445 0.057 Uiso 1 1 calc R . . C9 C 0.7789(5) 0.3409(5) 0.4573(3) 0.0454(12) Uani 1 1 d . . . H9 H 0.8597 0.3994 0.4421 0.054 Uiso 1 1 calc R . . C10 C 0.6391(4) 0.3457(4) 0.4159(3) 0.0339(10) Uani 1 1 d . . . H10 H 0.6269 0.4063 0.3729 0.041 Uiso 1 1 calc R . . C11 C 0.3428(4) 0.3864(4) 0.3136(2) 0.0230(9) Uani 1 1 d D . . C12 C 0.3623(5) 0.5133(4) 0.3456(3) 0.0395(11) Uani 1 1 d . . . H12 H 0.3694 0.5318 0.4057 0.047 Uiso 1 1 calc R . . C13 C 0.3710(5) 0.6108(5) 0.2871(3) 0.0444(12) Uani 1 1 d . . . H13 H 0.3871 0.6968 0.3086 0.053 Uiso 1 1 calc R . . C14 C 0.3572(6) 0.5877(6) 0.2000(4) 0.0606(15) Uani 1 1 d . . . H14 H 0.3601 0.6565 0.1618 0.073 Uiso 1 1 calc R . . C15 C 0.3399(5) 0.4696(5) 0.1692(4) 0.0547(15) Uani 1 1 d . . . H15 H 0.3315 0.4538 0.1087 0.066 Uiso 1 1 calc R . . C16 C 0.3338(4) 0.3689(4) 0.2234(3) 0.0322(10) Uani 1 1 d D . . H16 H 0.3233 0.285 0.1996 0.039 Uiso 1 1 calc R . . C17 C 0.7313(5) 0.4673(4) 0.2003(3) 0.0365(11) Uani 1 1 d . . . H17 H 0.6328 0.458 0.1764 0.044 Uiso 1 1 calc R . . C18 C 0.8191(7) 0.5656(5) 0.2644(4) 0.0677(19) Uani 1 1 d . . . H18 H 0.7886 0.6328 0.2901 0.081 Uiso 1 1 calc R . . C19 C 0.9671(5) 0.5397(4) 0.2817(3) 0.0429(12) Uani 1 1 d . . . H19 H 1.0482 0.5867 0.3205 0.052 Uiso 1 1 calc R . . C20 C 0.9608(4) 0.4335(4) 0.2296(3) 0.0355(11) Uani 1 1 d . . . H20 H 1.0396 0.3958 0.2271 0.043 Uiso 1 1 calc R . . C21 C 0.9138(4) 0.2430(4) 0.0592(2) 0.0256(9) Uani 1 1 d . . . C22 C 0.9402(5) 0.3260(4) -0.0092(3) 0.0405(12) Uani 1 1 d . . . H22 H 0.879 0.382 -0.0273 0.049 Uiso 1 1 calc R . . C23 C 1.0594(6) 0.3242(5) -0.0503(3) 0.0521(14) Uani 1 1 d . . . H23 H 1.0783 0.3808 -0.0957 0.062 Uiso 1 1 calc R . . C24 C 1.1480(5) 0.2431(5) -0.0264(3) 0.0486(13) Uani 1 1 d . . . H24 H 1.2278 0.2442 -0.0545 0.058 Uiso 1 1 calc R . . C25 C 1.1207(5) 0.1610(5) 0.0381(3) 0.0445(12) Uani 1 1 d . . . H25 H 1.1807 0.1032 0.0537 0.053 Uiso 1 1 calc R . . C26 C 1.0048(4) 0.1601(4) 0.0824(3) 0.0332(10) Uani 1 1 d . . . H26 H 0.9886 0.1032 0.128 0.04 Uiso 1 1 calc R . . C27 C 0.7431(4) 0.1162(4) 0.1855(3) 0.0236(9) Uani 1 1 d . . . C28 C 0.6802(5) -0.0083(4) 0.1493(3) 0.0391(11) Uani 1 1 d . . . H28 H 0.6501 -0.0212 0.0884 0.047 Uiso 1 1 calc R . . C29 C 0.6619(5) -0.1136(5) 0.2030(3) 0.0478(13) Uani 1 1 d . . . H29 H 0.6212 -0.1975 0.1779 0.057 Uiso 1 1 calc R . . C30 C 0.7021(5) -0.0969(5) 0.2915(4) 0.0483(13) Uani 1 1 d . . . H30 H 0.688 -0.1688 0.3271 0.058 Uiso 1 1 calc R . . C31 C 0.7627(5) 0.0240(5) 0.3284(3) 0.0411(12) Uani 1 1 d . . . H31 H 0.7904 0.0352 0.3894 0.049 Uiso 1 1 calc R . . C32 C 0.7837(4) 0.1305(4) 0.2767(3) 0.0279(10) Uani 1 1 d . . . H32 H 0.8258 0.2134 0.3031 0.034 Uiso 1 1 calc R . . N1 N 0.2819(4) 0.1142(3) 0.3215(2) 0.0348(9) Uani 1 1 d . . . N2 N 0.8223(3) 0.3886(3) 0.1809(2) 0.0299(8) Uani 1 1 d . . . P1 P 0.33286(12) 0.25628(11) 0.38786(7) 0.0286(3) Uani 1 1 d . . . P2 P 0.76150(11) 0.25013(11) 0.11335(7) 0.0277(3) Uani 1 1 d . . . B1 B 0.2031(6) 0.2615(6) 0.4698(4) 0.0481(15) Uani 1 1 d . . . H1A H 0.1092 0.268 0.4382 0.072 Uiso 1 1 calc R . . H1B H 0.243 0.3362 0.51 0.072 Uiso 1 1 calc R . . H1C H 0.1919 0.183 0.5025 0.072 Uiso 1 1 calc R . . B2 B 0.5861(6) 0.2525(6) 0.0345(4) 0.0511(16) Uani 1 1 d . . . H2A H 0.5069 0.245 0.0671 0.077 Uiso 1 1 calc R . . H2B H 0.564 0.1803 -0.008 0.077 Uiso 1 1 calc R . . H2C H 0.5986 0.3333 0.0044 0.077 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 C1 0.019(2) 0.044(3) 0.053(3) 0.017(3) -0.002(2) 0.001(2) C2 0.085(5) 0.038(4) 0.086(5) 0.028(3) -0.062(4) -0.022(3) C3 0.110(5) 0.046(3) 0.037(3) -0.002(3) -0.001(3) 0.045(3) C4 0.031(3) 0.035(3) 0.038(3) -0.001(2) 0.008(2) 0.011(2) C5 0.029(2) 0.021(2) 0.022(2) -0.0008(18) 0.0042(17) 0.0063(18) C6 0.037(3) 0.031(3) 0.039(3) 0.006(2) 0.006(2) 0.010(2) C7 0.044(3) 0.042(3) 0.034(3) -0.002(2) -0.003(2) 0.013(2) C8 0.044(3) 0.060(4) 0.041(3) -0.011(3) -0.002(2) 0.022(3) C9 0.041(3) 0.057(3) 0.039(3) -0.009(3) 0.006(2) 0.013(2) C10 0.037(3) 0.043(3) 0.022(2) 0.001(2) 0.0040(19) 0.011(2) C11 0.024(2) 0.024(2) 0.022(2) 0.0047(18) 0.0037(16) 0.0097(17) C12 0.055(3) 0.036(3) 0.028(3) 0.001(2) 0.007(2) 0.012(2) C13 0.069(3) 0.038(3) 0.034(3) 0.005(2) 0.014(2) 0.025(2) C14 0.058(4) 0.067(4) 0.057(4) 0.005(3) 0.015(3) 0.012(3) C15 0.047(3) 0.057(4) 0.071(4) 0.029(3) 0.021(3) 0.028(3) C16 0.027(2) 0.037(3) 0.036(3) 0.009(2) 0.0075(19) 0.0132(19) C17 0.039(3) 0.032(3) 0.048(3) 0.010(2) 0.022(2) 0.017(2) C18 0.123(5) 0.041(3) 0.065(4) 0.016(3) 0.070(4) 0.034(3) C19 0.050(3) 0.033(3) 0.045(3) -0.006(2) 0.013(2) 0.006(2) C20 0.027(2) 0.035(3) 0.044(3) -0.002(2) 0.003(2) 0.009(2) C21 0.025(2) 0.028(2) 0.023(2) 0.0005(18) 0.0035(17) 0.0044(18) C22 0.044(3) 0.042(3) 0.043(3) 0.013(2) 0.018(2) 0.017(2) C23 0.069(4) 0.050(3) 0.048(3) 0.011(3) 0.035(3) 0.017(3) C24 0.051(3) 0.051(3) 0.052(3) 0.001(3) 0.025(3) 0.016(3) C25 0.044(3) 0.044(3) 0.050(3) -0.006(3) 0.014(2) 0.014(2) C26 0.032(3) 0.037(3) 0.032(3) 0.006(2) 0.0098(19) 0.009(2) C27 0.017(2) 0.026(2) 0.027(2) -0.0005(18) 0.0069(16) 0.0017(17) C28 0.045(3) 0.040(3) 0.027(3) -0.002(2) 0.008(2) 0.000(2) C29 0.063(3) 0.035(3) 0.044(3) 0.001(2) 0.019(3) 0.002(2) C30 0.048(3) 0.045(3) 0.058(4) 0.010(3) 0.021(3) 0.014(3) C31 0.037(3) 0.046(3) 0.042(3) 0.015(3) 0.010(2) 0.011(2) C32 0.024(2) 0.031(2) 0.029(2) 0.0011(19) 0.0040(17) 0.0069(18) N1 0.034(2) 0.032(2) 0.039(2) 0.0016(17) 0.0067(16) 0.0077(17) N2 0.0239(19) 0.034(2) 0.030(2) -0.0004(17) 0.0040(15) 0.0052(16) P1 0.0286(6) 0.0314(7) 0.0282(6) 0.0068(5) 0.0082(5) 0.0092(5) P2 0.0240(6) 0.0331(7) 0.0250(6) 0.0029(5) 0.0034(4) 0.0051(5) B1 0.047(4) 0.058(4) 0.049(4) 0.014(3) 0.024(3) 0.018(3) B2 0.031(3) 0.069(4) 0.048(4) 0.008(3) -0.003(3) 0.006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 N1 1.395(5) . ? C1 C2 1.442(8) . ? C2 C3 1.514(6) . ? C3 C4 1.399(7) . ? C4 N1 1.378(5) . ? C5 C6 1.386(5) . ? C5 C10 1.387(5) . ? C5 P1 1.793(4) . ? C6 C7 1.379(6) . ? C7 C8 1.361(6) . ? C8 C9 1.334(6) . ? C9 C10 1.387(6) . ? C11 C12 1.379(5) . ? C11 C16 1.381(5) . ? C11 P1 1.777(4) . ? C12 C13 1.360(5) . ? C13 C14 1.338(7) . ? C14 C15 1.290(7) . ? C15 C16 1.344(6) . ? C17 N2 1.389(5) . ? C17 C18 1.434(7) . ? C18 C19 1.475(7) . ? C19 C20 1.353(6) . ? C20 N2 1.379(5) . ? C21 C26 1.370(5) . ? C21 C22 1.383(5) . ? C21 P2 1.799(4) . ? C22 C23 1.388(6) . ? C23 C24 1.341(6) . ? C24 C25 1.333(6) . ? C25 C26 1.385(6) . ? C27 C28 1.379(6) . ? C27 C32 1.388(5) . ? C27 P2 1.786(4) . ? C28 C29 1.377(6) . ? C29 C30 1.349(6) . ? C30 C31 1.346(6) . ? C31 C32 1.368(5) . ? N1 P1 1.729(4) . ? N2 P2 1.711(4) . ? P1 B1 1.910(5) . ? P2 B2 1.897(5) . ? 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 C1 C2 108.2(4) . . ? C1 C2 C3 105.3(4) . . ? C4 C3 C2 105.7(4) . . ? N1 C4 C3 110.6(4) . . ? C6 C5 C10 118.2(4) . . ? C6 C5 P1 118.6(3) . . ? C10 C5 P1 123.2(3) . . ? C7 C6 C5 120.0(4) . . ? C8 C7 C6 121.1(4) . . ? C9 C8 C7 119.5(5) . . ? C8 C9 C10 121.5(5) . . ? C5 C10 C9 119.8(4) . . ? C12 C11 C16 116.5(4) . . ? C12 C11 P1 119.8(3) . . ? C16 C11 P1 123.7(3) . . ? C13 C12 C11 118.4(4) . . ? C14 C13 C12 122.5(5) . . ? C15 C14 C13 119.7(6) . . ? C14 C15 C16 120.9(6) . . ? C15 C16 C11 121.9(5) . . ? N2 C17 C18 106.5(4) . . ? C17 C18 C19 106.7(4) . . ? C20 C19 C18 106.1(4) . . ? C19 C20 N2 111.2(4) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 P2 123.3(3) . . ? C22 C21 P2 118.1(3) . . ? C21 C22 C23 118.9(4) . . ? C24 C23 C22 121.8(4) . . ? C25 C24 C23 119.4(4) . . ? C24 C25 C26 121.3(4) . . ? C21 C26 C25 120.1(4) . . ? C28 C27 C32 117.7(4) . . ? C28 C27 P2 118.5(3) . . ? C32 C27 P2 123.8(3) . . ? C29 C28 C27 120.1(4) . . ? C30 C29 C28 120.9(5) . . ? C31 C30 C29 120.0(5) . . ? C30 C31 C32 120.5(5) . . ? C31 C32 C27 120.8(4) . . ? C4 N1 C1 110.2(4) . . ? C4 N1 P1 126.6(3) . . ? C1 N1 P1 123.0(3) . . ? C20 N2 C17 109.6(4) . . ? C20 N2 P2 126.9(3) . . ? C17 N2 P2 123.3(3) . . ? N1 P1 C11 105.32(18) . . ? N1 P1 C5 103.80(17) . . ? C11 P1 C5 106.63(18) . . ? N1 P1 B1 112.8(2) . . ? C11 P1 B1 113.3(2) . . ? C5 P1 B1 114.0(2) . . ? N2 P2 C27 105.68(18) . . ? N2 P2 C21 104.52(17) . . ? C27 P2 C21 106.17(18) . . ? N2 P2 B2 112.1(2) . . ? C27 P2 B2 113.6(2) . . ? C21 P2 B2 113.9(2) . . ? #====END data_(2Se) _database_code_depnum_ccdc_archive 'CCDC 665730' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H18 N1 P Se' _chemical_formula_sum 'C16 H18 N P Se' _chemical_formula_weight 334.24 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0551(15) _cell_length_b 17.944(4) _cell_length_c 9.1410(8) _cell_angle_alpha 90 _cell_angle_beta 97.767(10) _cell_angle_gamma 90 _cell_volume 1471.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 160 _cell_measurement_reflns_used 5795 _cell_measurement_theta_min 2.5337 _cell_measurement_theta_max 32.2947 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.764 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 160 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 0.0109835982 _diffrn_orient_matrix_ub_12 -0.0063365619 _diffrn_orient_matrix_ub_13 0.0773765523 _diffrn_orient_matrix_ub_21 -0.0273911331 _diffrn_orient_matrix_ub_22 0.0362295342 _diffrn_orient_matrix_ub_23 0.0120130386 _diffrn_orient_matrix_ub_31 -0.0734772906 _diffrn_orient_matrix_ub_32 -0.0144439051 _diffrn_orient_matrix_ub_33 -0.0045108698 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_unetI/netI 0.0804 _diffrn_reflns_number 14968 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 32.31 _diffrn_reflns_theta_full 32.31 _diffrn_measured_fraction_theta_full 0.948 _diffrn_measured_fraction_theta_max 0.948 _reflns_number_total 4970 _reflns_number_gt 3101 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0892P)^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_number_reflns 4970 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.13 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.047 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.159 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.8775(4) 0.31026(18) 0.3110(4) 0.0347(7) Uani 1 1 d . . . H1A H 0.7821 0.2852 0.2894 0.042 Uiso 1 1 calc R . . H1B H 0.8992 0.318 0.4168 0.042 Uiso 1 1 calc R . . C2 C 0.8768(6) 0.3814(3) 0.2313(8) 0.0879(19) Uani 1 1 d . . . H2A H 0.7847 0.3859 0.164 0.105 Uiso 1 1 calc R . . H2B H 0.8813 0.4223 0.3011 0.105 Uiso 1 1 calc R . . C3 C 0.9965(7) 0.3856(3) 0.1528(6) 0.0787(17) Uani 1 1 d . . . H3A H 1.0705 0.4197 0.2015 0.094 Uiso 1 1 calc R . . H3B H 0.9637 0.4044 0.0543 0.094 Uiso 1 1 calc R . . C4 C 1.0631(4) 0.31098(17) 0.1432(4) 0.0333(7) Uani 1 1 d . . . H4A H 1.1708 0.3132 0.1659 0.04 Uiso 1 1 calc R . . H4B H 1.0371 0.2899 0.0453 0.04 Uiso 1 1 calc R . . C5 C 0.9318(3) 0.13898(16) 0.3950(3) 0.0263(6) Uani 1 1 d . . . C6 C 0.9981(4) 0.17093(18) 0.5262(4) 0.0318(6) Uani 1 1 d . . . H6 H 1.0567 0.2134 0.5245 0.038 Uiso 1 1 calc R . . C7 C 0.9760(4) 0.1389(2) 0.6597(4) 0.0367(7) Uani 1 1 d . . . H7 H 1.0178 0.1607 0.748 0.044 Uiso 1 1 calc R . . C8 C 0.8927(4) 0.0752(2) 0.6617(4) 0.0405(8) Uani 1 1 d . . . H8 H 0.8797 0.0535 0.7514 0.049 Uiso 1 1 calc R . . C9 C 0.8284(4) 0.04341(19) 0.5323(4) 0.0377(7) Uani 1 1 d . . . H9 H 0.7725 0 0.5343 0.045 Uiso 1 1 calc R . . C10 C 0.8468(3) 0.07583(18) 0.3987(4) 0.0326(6) Uani 1 1 d . . . H10 H 0.8014 0.0548 0.311 0.039 Uiso 1 1 calc R . . C11 C 1.1451(3) 0.14152(16) 0.1889(3) 0.0242(5) Uani 1 1 d . . . C12 C 1.2757(3) 0.17041(19) 0.2659(4) 0.0328(7) Uani 1 1 d . . . H12 H 1.2724 0.2104 0.3301 0.039 Uiso 1 1 calc R . . C13 C 1.4108(4) 0.1386(2) 0.2454(4) 0.0399(8) Uani 1 1 d . . . H13 H 1.4986 0.1582 0.2951 0.048 Uiso 1 1 calc R . . C14 C 1.4178(4) 0.0791(2) 0.1540(4) 0.0383(7) Uani 1 1 d . . . H14 H 1.5094 0.0582 0.1422 0.046 Uiso 1 1 calc R . . C15 C 1.2885(4) 0.05026(19) 0.0792(4) 0.0390(8) Uani 1 1 d . . . H15 H 1.2924 0.009 0.0182 0.047 Uiso 1 1 calc R . . C16 C 1.1529(4) 0.08232(17) 0.0943(3) 0.0311(6) Uani 1 1 d . . . H16 H 1.0663 0.0638 0.0403 0.037 Uiso 1 1 calc R . . N1 N 0.9975(3) 0.26639(13) 0.2556(3) 0.0251(5) Uani 1 1 d . . . P1 P 0.96566(8) 0.17768(4) 0.22012(8) 0.02325(17) Uani 1 1 d . . . Se1 Se 0.79504(3) 0.152862(19) 0.04693(3) 0.03406(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0368(17) 0.0287(17) 0.0411(17) -0.0047(13) 0.0147(13) 0.0038(13) C2 0.087(4) 0.040(3) 0.154(5) 0.039(3) 0.078(4) 0.025(2) C3 0.119(4) 0.035(2) 0.097(4) 0.021(2) 0.071(3) 0.026(3) C4 0.0365(16) 0.0246(15) 0.0408(17) 0.0022(12) 0.0128(13) -0.0050(12) C5 0.0240(13) 0.0290(15) 0.0272(14) 0.0007(10) 0.0083(10) -0.0003(11) C6 0.0296(15) 0.0347(16) 0.0323(16) 0.0028(12) 0.0082(12) -0.0038(12) C7 0.0346(17) 0.049(2) 0.0274(15) 0.0057(13) 0.0079(12) 0.0006(14) C8 0.0409(18) 0.044(2) 0.0400(18) 0.0130(15) 0.0186(15) 0.0043(15) C9 0.0373(17) 0.0272(16) 0.052(2) 0.0076(14) 0.0201(15) -0.0015(13) C10 0.0317(15) 0.0302(16) 0.0374(16) 0.0001(12) 0.0105(12) -0.0016(12) C11 0.0221(12) 0.0273(14) 0.0244(13) 0.0042(10) 0.0073(10) 0.0015(10) C12 0.0275(15) 0.0378(17) 0.0335(16) -0.0076(13) 0.0053(12) 0.0006(12) C13 0.0256(15) 0.049(2) 0.0448(19) -0.0044(15) 0.0057(13) 0.0061(14) C14 0.0351(16) 0.0367(18) 0.0476(19) 0.0068(14) 0.0213(14) 0.0089(14) C15 0.047(2) 0.0245(15) 0.051(2) -0.0012(13) 0.0284(16) -0.0008(13) C16 0.0353(15) 0.0239(14) 0.0372(16) -0.0026(12) 0.0160(12) -0.0046(12) N1 0.0266(11) 0.0215(11) 0.0280(12) -0.0011(9) 0.0068(9) -0.0017(9) P1 0.0217(3) 0.0232(4) 0.0252(3) -0.0013(3) 0.0045(3) -0.0011(3) Se1 0.0314(2) 0.0353(2) 0.0333(2) -0.00234(12) -0.00378(13) -0.00443(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.469(6) . ? C1 N1 1.485(4) . ? C2 C3 1.381(7) . ? C3 C4 1.476(6) . ? C4 N1 1.488(4) . ? C5 C10 1.373(4) . ? C5 C6 1.390(4) . ? C5 P1 1.807(3) . ? C6 C7 1.387(4) . ? C7 C8 1.371(5) . ? C8 C9 1.371(5) . ? C9 C10 1.383(5) . ? C11 C16 1.377(4) . ? C11 C12 1.393(4) . ? C11 P1 1.807(3) . ? C12 C13 1.386(5) . ? C13 C14 1.362(5) . ? C14 C15 1.375(5) . ? C15 C16 1.379(4) . ? N1 P1 1.642(3) . ? P1 Se1 2.1049(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 104.2(3) . . ? C3 C2 C1 110.8(4) . . ? C2 C3 C4 109.7(4) . . ? C3 C4 N1 104.0(3) . . ? C10 C5 C6 119.8(3) . . ? C10 C5 P1 120.1(2) . . ? C6 C5 P1 120.0(2) . . ? C7 C6 C5 119.4(3) . . ? C8 C7 C6 120.1(3) . . ? C9 C8 C7 120.4(3) . . ? C8 C9 C10 119.9(3) . . ? C5 C10 C9 120.3(3) . . ? C16 C11 C12 119.5(3) . . ? C16 C11 P1 120.0(2) . . ? C12 C11 P1 120.4(2) . . ? C13 C12 C11 118.9(3) . . ? C14 C13 C12 121.4(3) . . ? C13 C14 C15 119.5(3) . . ? C14 C15 C16 120.2(3) . . ? C11 C16 C15 120.5(3) . . ? C1 N1 C4 109.2(2) . . ? C1 N1 P1 117.7(2) . . ? C4 N1 P1 117.4(2) . . ? N1 P1 C5 104.12(13) . . ? N1 P1 C11 103.99(13) . . ? C5 P1 C11 105.40(13) . . ? N1 P1 Se1 116.43(9) . . ? C5 P1 Se1 112.89(10) . . ? C11 P1 Se1 112.90(10) . . ? #====END data_([Ru]1) _database_code_depnum_ccdc_archive 'CCDC 665731' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H33 N6 P Ru, C3 H6 O, 2(F6 P)' _chemical_formula_sum 'C44 H39 F12 N6 O P3 Ru' _chemical_formula_weight 1089.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6647(4) _cell_length_b 11.7577(5) _cell_length_c 22.6217(10) _cell_angle_alpha 76.051(4) _cell_angle_beta 85.002(4) _cell_angle_gamma 76.882(4) _cell_volume 2428.27(18) _cell_formula_units_Z 2 _cell_measurement_temperature 103 _cell_measurement_reflns_used 12020 _cell_measurement_theta_min 2.7684 _cell_measurement_theta_max 32.1289 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.91 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 -0.0209601525 _diffrn_orient_matrix_ub_12 -0.0410055744 _diffrn_orient_matrix_ub_13 -0.0139604956 _diffrn_orient_matrix_ub_21 0.0548835247 _diffrn_orient_matrix_ub_22 0.0067570817 _diffrn_orient_matrix_ub_23 -0.022632788 _diffrn_orient_matrix_ub_31 0.0471716346 _diffrn_orient_matrix_ub_32 -0.0481114413 _diffrn_orient_matrix_ub_33 0.018373621 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_number 14809 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8215 _reflns_number_gt 6780 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1726P)^2^+7.6812P] 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_number_reflns 8215 _refine_ls_number_parameters 570 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2483 _refine_ls_wR_factor_gt 0.2367 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.148 _refine_diff_density_min -1.852 _refine_diff_density_rms 0.172 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.2435(10) 0.4305(9) 0.6839(4) 0.056(2) Uani 1 1 d . A . H1 H 0.2504 0.4797 0.7096 0.067 Uiso 1 1 calc R . . C2 C 0.3327(10) 0.4098(10) 0.6371(4) 0.064(3) Uani 1 1 d . . . H2 H 0.4128 0.4421 0.6251 0.077 Uiso 1 1 calc R . . C3 C 0.2857(8) 0.3307(7) 0.6088(4) 0.047(2) Uani 1 1 d . . . H3 H 0.3276 0.3028 0.5749 0.057 Uiso 1 1 calc R . . C4 C 0.1671(7) 0.3039(6) 0.6410(3) 0.0325(15) Uani 1 1 d . A . H4 H 0.1143 0.2526 0.6331 0.039 Uiso 1 1 calc R . . C5 C 0.1290(7) 0.2661(6) 0.8102(3) 0.0288(14) Uani 1 1 d . . . C6 C 0.0791(8) 0.2712(8) 0.8692(3) 0.046(2) Uani 1 1 d . . . H6 H -0.0101 0.3175 0.8757 0.055 Uiso 1 1 calc R . . C7 C 0.1611(11) 0.2082(12) 0.9180(4) 0.080(4) Uani 1 1 d . . . H7 H 0.1261 0.2121 0.9572 0.096 Uiso 1 1 calc R . . C8 C 0.2889(13) 0.1419(12) 0.9104(5) 0.086(4) Uani 1 1 d . . . H8 H 0.3433 0.1013 0.944 0.104 Uiso 1 1 calc R . . C9 C 0.3419(9) 0.1328(8) 0.8522(5) 0.064(3) Uani 1 1 d . . . H9 H 0.4313 0.0855 0.8471 0.077 Uiso 1 1 calc R . . C10 C 0.2607(7) 0.1950(7) 0.8008(4) 0.0390(17) Uani 1 1 d . . . H10 H 0.2946 0.1884 0.7617 0.047 Uiso 1 1 calc R . . C11 C -0.0409(7) 0.4970(6) 0.7582(3) 0.0341(16) Uani 1 1 d . . . C12A C 0.007(2) 0.5255(15) 0.8115(9) 0.0446(19) Uani 0.5 1 d P A 1 H12A H 0.0679 0.4683 0.8387 0.054 Uiso 0.5 1 calc PR A 1 C13A C -0.0441(19) 0.6453(13) 0.8202(8) 0.0446(19) Uani 0.5 1 d P A 1 H13A H -0.0085 0.6697 0.8508 0.054 Uiso 0.5 1 calc PR A 1 C14A C -0.145(2) 0.7225(15) 0.7831(8) 0.0446(19) Uani 0.5 1 d P A 1 H14A H -0.1853 0.7963 0.7921 0.054 Uiso 0.5 1 calc PR A 1 C12B C 0.050(2) 0.5479(15) 0.7858(8) 0.0446(19) Uani 0.5 1 d P A 2 H12B H 0.1342 0.4994 0.802 0.054 Uiso 0.5 1 calc PR A 2 C13B C 0.0165(19) 0.6662(13) 0.7893(8) 0.0446(19) Uani 0.5 1 d P A 2 H13B H 0.0706 0.6949 0.8122 0.054 Uiso 0.5 1 calc PR A 2 C14B C -0.105(2) 0.7455(15) 0.7567(8) 0.0446(19) Uani 0.5 1 d P A 2 H14B H -0.1224 0.8278 0.7535 0.054 Uiso 0.5 1 calc PR A 2 C15 C -0.1918(9) 0.6956(7) 0.7307(4) 0.0453(19) Uani 1 1 d . . . H15 H -0.2471 0.7545 0.702 0.054 Uiso 1 1 calc R A 1 C16 C -0.1509(7) 0.5771(5) 0.7247(3) 0.0276(13) Uani 1 1 d . A . H16 H -0.198 0.5514 0.6979 0.033 Uiso 1 1 calc R . . C17 C 0.0629(7) 0.0464(5) 0.6798(3) 0.0287(14) Uani 1 1 d . B . H17 H 0.033 0.0899 0.6414 0.034 Uiso 1 1 calc R . . C18 C 0.1667(8) -0.0578(6) 0.6848(4) 0.0437(18) Uani 1 1 d . . . H18 H 0.2063 -0.0836 0.6501 0.052 Uiso 1 1 calc R . . C19 C 0.2101(11) -0.1220(7) 0.7413(5) 0.062(3) Uani 1 1 d . . . H19 H 0.2818 -0.1908 0.7451 0.074 Uiso 1 1 calc R . . C20 C 0.1498(13) -0.0866(7) 0.7914(5) 0.074(3) Uani 1 1 d . . . H20 H 0.1804 -0.1303 0.8298 0.089 Uiso 1 1 calc R . . C21 C 0.0379(10) 0.0188(6) 0.7856(3) 0.045(2) Uani 1 1 d . B . C22 C -0.0448(11) 0.0560(6) 0.8360(4) 0.052(2) Uani 1 1 d . . . C23A C -0.008(2) -0.0043(18) 0.8942(8) 0.059(3) Uani 0.52 1 d P B 1 H23A H 0.067 -0.0701 0.9033 0.071 Uiso 0.52 1 calc PR B 1 C24A C -0.094(2) 0.0421(18) 0.9375(8) 0.059(3) Uani 0.52 1 d P B 1 H24A H -0.081 0.006 0.9785 0.071 Uiso 0.52 1 calc PR B 1 C25A C -0.197(2) 0.139(2) 0.9213(9) 0.059(3) Uani 0.52 1 d P B 1 H25A H -0.2502 0.1674 0.9531 0.071 Uiso 0.52 1 calc PR B 1 C23B C -0.080(2) -0.002(2) 0.8999(9) 0.059(3) Uani 0.48 1 d P B 2 H23B H -0.0324 -0.0815 0.9141 0.071 Uiso 0.48 1 calc PR B 2 C24B C -0.171(2) 0.046(2) 0.9387(9) 0.059(3) Uani 0.48 1 d P B 2 H24B H -0.1737 0.0066 0.9796 0.071 Uiso 0.48 1 calc PR B 2 C25B C -0.262(2) 0.155(2) 0.9185(10) 0.059(3) Uani 0.48 1 d P B 2 H25B H -0.3326 0.19 0.943 0.071 Uiso 0.48 1 calc PR B 2 C26 C -0.2375(11) 0.2049(7) 0.8603(4) 0.054(2) Uani 1 1 d . . . C27 C -0.3397(8) 0.3158(6) 0.8316(3) 0.0353(16) Uani 1 1 d . B . C28 C -0.4476(10) 0.3802(9) 0.8627(4) 0.058(3) Uani 1 1 d . . . H28 H -0.4587 0.3549 0.9048 0.07 Uiso 1 1 calc R B . C29 C -0.5384(8) 0.4811(9) 0.8321(4) 0.055(2) Uani 1 1 d . B . H29 H -0.6092 0.5251 0.8531 0.066 Uiso 1 1 calc R . . C30 C -0.5225(8) 0.5157(9) 0.7698(4) 0.051(2) Uani 1 1 d . . . H30 H -0.5836 0.5826 0.7479 0.061 Uiso 1 1 calc R B . C31 C -0.4147(7) 0.4496(6) 0.7404(3) 0.0333(15) Uani 1 1 d . B . H31 H -0.4057 0.4728 0.6981 0.04 Uiso 1 1 calc R . . C32 C -0.1525(7) 0.4170(6) 0.6049(3) 0.0308(15) Uani 1 1 d . B . H32 H -0.0946 0.4528 0.6221 0.037 Uiso 1 1 calc R . . C33 C -0.1894(9) 0.4677(8) 0.5447(3) 0.046(2) Uani 1 1 d . . . H33 H -0.1597 0.5361 0.5226 0.055 Uiso 1 1 calc R . . C34 C -0.2730(10) 0.4111(12) 0.5192(4) 0.073(3) Uani 1 1 d . . . H34 H -0.2965 0.4384 0.4785 0.087 Uiso 1 1 calc R . . C35 C -0.3198(8) 0.3153(10) 0.5547(4) 0.058(3) Uani 1 1 d . . . H35 H -0.3798 0.2795 0.5387 0.07 Uiso 1 1 calc R . . C36 C -0.2798(7) 0.2713(7) 0.6135(3) 0.0345(16) Uani 1 1 d . B . C37 C -0.3311(7) 0.1712(7) 0.6542(4) 0.0374(17) Uani 1 1 d . B . C38 C -0.4114(8) 0.1050(9) 0.6338(5) 0.054(2) Uani 1 1 d . . . H38 H -0.4317 0.1208 0.5928 0.065 Uiso 1 1 calc R . . C39 C -0.4599(9) 0.0162(10) 0.6753(6) 0.075(4) Uani 1 1 d . . . H39 H -0.5147 -0.0287 0.6627 0.09 Uiso 1 1 calc R . . C40 C -0.4280(9) -0.0067(8) 0.7352(6) 0.064(3) Uani 1 1 d . . . H40 H -0.4626 -0.066 0.7637 0.077 Uiso 1 1 calc R . . C41 C -0.3442(8) 0.0585(6) 0.7534(4) 0.0439(19) Uani 1 1 d . B . H41 H -0.3206 0.0412 0.7941 0.053 Uiso 1 1 calc R . . C50 C 0.0686(8) 0.1680(7) 0.4867(3) 0.0393(17) Uani 1 1 d . . . C51 C 0.1647(11) 0.0529(9) 0.4755(6) 0.077(3) Uani 1 1 d . . . H51A H 0.1772 -0.0065 0.5132 0.116 Uiso 1 1 calc R . . H51B H 0.2555 0.0685 0.4594 0.116 Uiso 1 1 calc R . . H51C H 0.1222 0.0239 0.4469 0.116 Uiso 1 1 calc R . . O1 O 0.0437(7) 0.1857(7) 0.5365(3) 0.0660(18) Uani 1 1 d . . . N6 N 0.1376(6) 0.3646(5) 0.6872(2) 0.0312(13) Uani 1 1 d . . . N3 N 0.0042(6) 0.0864(4) 0.7290(2) 0.0264(11) Uani 1 1 d . . . N4 N -0.1428(7) 0.1588(5) 0.8198(3) 0.0371(14) Uani 1 1 d . A . N5 N -0.3212(6) 0.3527(5) 0.7697(3) 0.0288(12) Uani 1 1 d . . . N2 N -0.1940(5) 0.3208(5) 0.6400(2) 0.0253(11) Uani 1 1 d . . . N1 N -0.2966(5) 0.1458(5) 0.7136(3) 0.0290(12) Uani 1 1 d . . . C52 C 0.0044(11) 0.2573(10) 0.4313(4) 0.069(3) Uani 1 1 d . . . H52A H 0.0573 0.2401 0.3954 0.103 Uiso 1 1 calc R . . H52B H 0.0073 0.3368 0.4343 0.103 Uiso 1 1 calc R . . H52C H -0.0926 0.252 0.4288 0.103 Uiso 1 1 calc R . . F1 F 0.5501(6) 0.2498(5) 0.3426(2) 0.0622(13) Uani 1 1 d . . . F2 F 0.4470(5) 0.2384(5) 0.4823(2) 0.0585(13) Uani 1 1 d . . . F3 F 0.4795(8) 0.3847(5) 0.4025(4) 0.098(2) Uani 1 1 d . . . F4 F 0.5146(9) 0.1057(5) 0.4236(3) 0.096(2) Uani 1 1 d . . . F5 F 0.3405(6) 0.2629(7) 0.3957(3) 0.086(2) Uani 1 1 d . . . F6 F 0.6586(6) 0.2242(7) 0.4308(3) 0.097(2) Uani 1 1 d . . . Ru1 Ru -0.15369(5) 0.24213(4) 0.732683(19) 0.0189(2) Uani 1 1 d . A . P1 P 0.01438(16) 0.34449(13) 0.74639(7) 0.0198(3) Uani 1 1 d . A . P2 P 0.49971(19) 0.24670(16) 0.41281(9) 0.0331(4) Uani 1 1 d . . . P3A P 0.2086(5) 0.6312(4) 0.96402(17) 0.1068(14) Uani 1 1 d . . . F7A F 0.2361(13) 0.6650(11) 0.8928(5) 0.1612(17) Uani 1 1 d . . . F8A F 0.1888(13) 0.6055(11) 1.0335(5) 0.1612(17) Uani 1 1 d . . . F9A F 0.1530(13) 0.5118(11) 0.9578(5) 0.1612(17) Uani 1 1 d . . . F10A F 0.2566(13) 0.7653(11) 0.9605(5) 0.1612(17) Uani 1 1 d . . . F11A F 0.0598(13) 0.7074(11) 0.9512(5) 0.1612(17) Uani 1 1 d . . . F12A F 0.3570(13) 0.5459(11) 0.9703(5) 0.1612(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(6) 0.077(6) 0.041(5) -0.007(4) -0.005(4) -0.054(5) C2 0.048(5) 0.095(7) 0.055(5) 0.000(5) 0.003(4) -0.050(5) C3 0.037(4) 0.050(5) 0.047(5) 0.004(4) 0.012(3) -0.013(4) C4 0.033(4) 0.031(3) 0.031(4) -0.003(3) 0.007(3) -0.008(3) C5 0.025(3) 0.030(3) 0.027(3) -0.005(3) -0.010(3) 0.004(3) C6 0.034(4) 0.076(6) 0.026(4) -0.015(4) -0.006(3) 0.000(4) C7 0.054(6) 0.132(10) 0.035(5) -0.004(6) -0.020(4) 0.007(6) C8 0.077(8) 0.111(9) 0.049(6) 0.010(6) -0.034(6) 0.007(7) C9 0.028(4) 0.055(5) 0.097(8) -0.013(5) -0.023(5) 0.017(4) C10 0.025(4) 0.044(4) 0.045(4) -0.012(3) -0.007(3) 0.002(3) C11 0.035(4) 0.026(3) 0.045(4) -0.013(3) -0.016(3) -0.003(3) C12A 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C13A 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C14A 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C12B 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C13B 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C14B 0.060(6) 0.029(4) 0.051(6) -0.012(4) -0.011(4) -0.016(3) C15 0.046(5) 0.031(4) 0.060(5) -0.016(3) -0.013(4) 0.000(3) C16 0.029(3) 0.023(3) 0.029(3) -0.006(3) -0.002(3) -0.003(3) C17 0.029(3) 0.020(3) 0.037(4) -0.007(3) -0.001(3) -0.004(3) C18 0.041(4) 0.030(4) 0.061(5) -0.018(4) 0.001(4) -0.001(3) C19 0.072(6) 0.030(4) 0.073(6) -0.016(4) -0.020(5) 0.021(4) C20 0.112(9) 0.024(4) 0.071(7) -0.007(4) -0.038(6) 0.027(5) C21 0.074(6) 0.019(3) 0.038(4) 0.000(3) -0.018(4) -0.002(3) C22 0.094(7) 0.022(4) 0.032(4) 0.004(3) -0.002(4) -0.006(4) C23A 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C24A 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C25A 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C23B 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C24B 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C25B 0.070(9) 0.050(4) 0.027(3) 0.010(3) 0.018(6) 0.020(7) C26 0.095(7) 0.036(4) 0.030(4) -0.006(3) 0.018(4) -0.022(4) C27 0.043(4) 0.040(4) 0.030(4) -0.016(3) 0.011(3) -0.020(3) C28 0.062(6) 0.083(7) 0.044(5) -0.033(5) 0.032(4) -0.039(5) C29 0.023(4) 0.087(7) 0.061(6) -0.041(5) 0.012(4) -0.004(4) C30 0.026(4) 0.072(6) 0.061(5) -0.037(5) 0.001(4) -0.004(4) C31 0.026(3) 0.038(4) 0.040(4) -0.019(3) -0.004(3) -0.005(3) C32 0.041(4) 0.027(3) 0.017(3) -0.003(3) 0.000(3) 0.006(3) C33 0.044(4) 0.055(5) 0.023(4) -0.004(3) -0.004(3) 0.018(4) C34 0.044(5) 0.133(10) 0.028(4) -0.020(6) -0.018(4) 0.017(6) C35 0.028(4) 0.115(8) 0.040(5) -0.041(5) -0.013(3) -0.002(5) C36 0.017(3) 0.059(4) 0.033(4) -0.028(3) 0.001(3) 0.001(3) C37 0.015(3) 0.052(4) 0.053(5) -0.037(4) 0.001(3) 0.002(3) C38 0.018(4) 0.083(6) 0.084(6) -0.060(6) 0.007(4) -0.017(4) C39 0.032(5) 0.093(8) 0.137(11) -0.095(8) 0.012(6) -0.020(5) C40 0.039(5) 0.040(5) 0.129(10) -0.045(5) 0.025(5) -0.021(4) C41 0.039(4) 0.025(3) 0.072(6) -0.017(4) 0.010(4) -0.013(3) C50 0.038(4) 0.045(4) 0.039(4) -0.013(3) 0.006(3) -0.018(3) C51 0.066(7) 0.050(5) 0.114(9) -0.024(6) 0.039(6) -0.015(5) O1 0.064(4) 0.090(5) 0.039(3) -0.018(3) -0.001(3) -0.004(4) N6 0.034(3) 0.040(3) 0.026(3) -0.006(2) 0.002(2) -0.024(3) N3 0.028(3) 0.019(2) 0.031(3) -0.002(2) -0.006(2) -0.004(2) N4 0.063(4) 0.026(3) 0.021(3) 0.000(2) 0.003(3) -0.014(3) N5 0.028(3) 0.031(3) 0.034(3) -0.014(2) 0.005(2) -0.015(2) N2 0.018(3) 0.035(3) 0.022(3) -0.016(2) -0.005(2) 0.007(2) N1 0.019(3) 0.027(3) 0.048(3) -0.026(3) 0.003(2) -0.004(2) C52 0.057(6) 0.092(7) 0.041(5) 0.004(5) 0.017(4) -0.008(5) F1 0.058(3) 0.069(3) 0.054(3) -0.015(3) 0.008(2) -0.006(3) F2 0.054(3) 0.087(4) 0.034(2) -0.015(2) -0.009(2) -0.012(3) F3 0.106(5) 0.037(3) 0.143(6) -0.026(3) 0.052(5) -0.017(3) F4 0.174(7) 0.047(3) 0.071(4) -0.011(3) -0.023(4) -0.026(4) F5 0.044(3) 0.159(6) 0.056(3) -0.010(4) -0.013(3) -0.036(4) F6 0.031(3) 0.157(7) 0.127(6) -0.091(5) -0.016(3) 0.002(3) Ru1 0.0223(3) 0.0179(3) 0.0175(3) -0.00504(19) -0.00131(19) -0.00468(19) P1 0.0219(8) 0.0202(7) 0.0182(7) -0.0043(6) -0.0052(6) -0.0044(6) P2 0.0268(9) 0.0322(9) 0.0410(10) -0.0103(8) -0.0100(7) -0.0022(7) P3A 0.117(3) 0.103(3) 0.076(2) -0.020(2) -0.003(2) 0.026(2) F7A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) F8A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) F9A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) F10A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) F11A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) F12A 0.167(4) 0.182(4) 0.117(3) -0.026(3) -0.005(3) -0.010(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.340(13) . ? C1 N6 1.404(9) . ? C2 C3 1.417(13) . ? C3 C4 1.362(10) . ? C4 N6 1.378(9) . ? C5 C10 1.386(10) . ? C5 C6 1.390(10) . ? C5 P1 1.826(6) . ? C6 C7 1.373(12) . ? C7 C8 1.324(16) . ? C8 C9 1.390(15) . ? C9 C10 1.410(12) . ? C11 C16 1.390(9) . ? C11 C12B 1.425(18) . ? C11 C12A 1.464(19) . ? C11 P1 1.828(7) . ? C12A C13A 1.44(2) . ? C13A C14A 1.36(2) . ? C14A C15 1.430(19) . ? C12B C13B 1.38(2) . ? C13B C14B 1.45(2) . ? C14B C15 1.370(19) . ? C15 C16 1.395(9) . ? C17 N3 1.342(9) . ? C17 C18 1.384(10) . ? C18 C19 1.365(12) . ? C19 C20 1.342(14) . ? C20 C21 1.436(11) . ? C21 N3 1.357(9) . ? C21 C22 1.432(12) . ? C22 N4 1.349(10) . ? C22 C23A 1.37(2) . ? C22 C23B 1.491(19) . ? C23A C24A 1.36(2) . ? C24A C25A 1.33(2) . ? C25A C26 1.45(2) . ? C23B C24B 1.32(3) . ? C24B C25B 1.38(2) . ? C25B C26 1.33(2) . ? C26 N4 1.357(10) . ? C26 C27 1.489(12) . ? C27 N5 1.371(9) . ? C27 C28 1.388(11) . ? C28 C29 1.377(14) . ? C29 C30 1.374(13) . ? C30 C31 1.376(10) . ? C31 N5 1.352(9) . ? C32 N2 1.337(9) . ? C32 C33 1.390(9) . ? C33 C34 1.393(14) . ? C34 C35 1.361(15) . ? C35 C36 1.360(11) . ? C36 N2 1.365(8) . ? C36 C37 1.463(11) . ? C37 N1 1.359(9) . ? C37 C38 1.389(10) . ? C38 C39 1.365(16) . ? C39 C40 1.366(16) . ? C40 C41 1.380(11) . ? C41 N1 1.333(9) . ? C50 O1 1.187(9) . ? C50 C52 1.505(12) . ? C50 C51 1.521(12) . ? N6 P1 1.721(6) . ? N3 Ru1 2.115(5) . ? N4 Ru1 1.978(5) . ? N5 Ru1 2.085(5) . ? N2 Ru1 2.109(5) . ? N1 Ru1 2.103(5) . ? F1 P2 1.613(5) . ? F2 P2 1.598(5) . ? F3 P2 1.551(5) . ? F4 P2 1.591(6) . ? F5 P2 1.578(5) . ? F6 P2 1.570(5) . ? Ru1 P1 2.3104(15) . ? P3A F11A 1.523(12) . ? P3A F8A 1.532(11) . ? P3A F12A 1.548(12) . ? P3A F7A 1.578(11) . ? P3A F9A 1.652(13) . ? P3A F10A 1.725(14) . ? 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 C2 C1 N6 107.8(8) . . ? C1 C2 C3 109.2(7) . . ? C4 C3 C2 106.3(8) . . ? C3 C4 N6 109.4(7) . . ? C10 C5 C6 119.7(6) . . ? C10 C5 P1 120.7(5) . . ? C6 C5 P1 119.4(5) . . ? C7 C6 C5 120.2(8) . . ? C8 C7 C6 121.5(10) . . ? C7 C8 C9 120.2(8) . . ? C8 C9 C10 120.3(8) . . ? C5 C10 C9 118.0(8) . . ? C16 C11 C12B 116.4(9) . . ? C16 C11 C12A 119.4(9) . . ? C16 C11 P1 119.5(5) . . ? C12B C11 P1 121.4(9) . . ? C12A C11 P1 119.6(8) . . ? C13A C12A C11 117.6(14) . . ? C14A C13A C12A 119.3(15) . . ? C13A C14A C15 123.0(14) . . ? C13B C12B C11 122.2(16) . . ? C12B C13B C14B 118.7(14) . . ? C15 C14B C13B 118.1(13) . . ? C14B C15 C16 121.0(10) . . ? C16 C15 C14A 117.2(9) . . ? C11 C16 C15 121.0(6) . . ? N3 C17 C18 121.8(7) . . ? C19 C18 C17 119.1(8) . . ? C20 C19 C18 120.4(8) . . ? C19 C20 C21 119.8(8) . . ? N3 C21 C22 117.2(7) . . ? N3 C21 C20 118.7(8) . . ? C22 C21 C20 124.1(8) . . ? N4 C22 C23A 126.4(10) . . ? N4 C22 C21 113.8(6) . . ? C23A C22 C21 119.3(10) . . ? N4 C22 C23B 107.7(10) . . ? C21 C22 C23B 136.1(10) . . ? C24A C23A C22 112.9(15) . . ? C25A C24A C23A 120.3(16) . . ? C24A C25A C26 128.0(15) . . ? C24B C23B C22 127.0(16) . . ? C23B C24B C25B 119.9(16) . . ? C26 C25B C24B 113.2(16) . . ? C25B C26 N4 128.2(12) . . ? N4 C26 C25A 108.7(10) . . ? C25B C26 C27 117.8(11) . . ? N4 C26 C27 113.3(6) . . ? C25A C26 C27 137.5(10) . . ? N5 C27 C28 120.3(8) . . ? N5 C27 C26 114.8(6) . . ? C28 C27 C26 124.9(7) . . ? C29 C28 C27 120.8(8) . . ? C30 C29 C28 118.9(7) . . ? C29 C30 C31 118.8(8) . . ? N5 C31 C30 123.4(7) . . ? N2 C32 C33 125.1(7) . . ? C32 C33 C34 116.7(9) . . ? C35 C34 C33 119.1(7) . . ? C36 C35 C34 120.7(8) . . ? C35 C36 N2 122.6(8) . . ? C35 C36 C37 122.8(7) . . ? N2 C36 C37 114.6(6) . . ? N1 C37 C38 121.1(8) . . ? N1 C37 C36 116.6(6) . . ? C38 C37 C36 122.4(7) . . ? C39 C38 C37 118.6(9) . . ? C38 C39 C40 120.0(8) . . ? C39 C40 C41 119.8(9) . . ? N1 C41 C40 120.9(9) . . ? O1 C50 C52 121.8(8) . . ? O1 C50 C51 122.0(8) . . ? C52 C50 C51 116.2(8) . . ? C4 N6 C1 107.3(6) . . ? C4 N6 P1 126.8(4) . . ? C1 N6 P1 124.9(5) . . ? C17 N3 C21 119.8(6) . . ? C17 N3 Ru1 128.5(4) . . ? C21 N3 Ru1 111.5(5) . . ? C22 N4 C26 122.8(7) . . ? C22 N4 Ru1 118.5(5) . . ? C26 N4 Ru1 118.7(5) . . ? C31 N5 C27 117.8(6) . . ? C31 N5 Ru1 128.5(5) . . ? C27 N5 Ru1 113.6(5) . . ? C32 N2 C36 115.9(6) . . ? C32 N2 Ru1 128.2(4) . . ? C36 N2 Ru1 115.8(5) . . ? C41 N1 C37 119.5(6) . . ? C41 N1 Ru1 125.3(5) . . ? C37 N1 Ru1 115.0(5) . . ? N4 Ru1 N5 79.6(2) . . ? N4 Ru1 N1 93.9(2) . . ? N5 Ru1 N1 89.91(19) . . ? N4 Ru1 N2 171.2(2) . . ? N5 Ru1 N2 97.6(2) . . ? N1 Ru1 N2 77.6(2) . . ? N4 Ru1 N3 78.7(2) . . ? N5 Ru1 N3 157.4(2) . . ? N1 Ru1 N3 85.49(19) . . ? N2 Ru1 N3 102.96(19) . . ? N4 Ru1 P1 89.37(18) . . ? N5 Ru1 P1 94.21(14) . . ? N1 Ru1 P1 175.14(15) . . ? N2 Ru1 P1 99.22(15) . . ? N3 Ru1 P1 91.65(14) . . ? N6 P1 C5 101.4(3) . . ? N6 P1 C11 100.7(3) . . ? C5 P1 C11 103.4(3) . . ? N6 P1 Ru1 115.10(19) . . ? C5 P1 Ru1 113.5(2) . . ? C11 P1 Ru1 120.2(2) . . ? F3 P2 F6 92.6(4) . . ? F3 P2 F5 90.0(4) . . ? F6 P2 F5 177.4(4) . . ? F3 P2 F4 178.0(4) . . ? F6 P2 F4 89.3(4) . . ? F5 P2 F4 88.1(4) . . ? F3 P2 F2 90.1(4) . . ? F6 P2 F2 90.9(3) . . ? F5 P2 F2 88.7(3) . . ? F4 P2 F2 89.2(3) . . ? F3 P2 F1 92.1(3) . . ? F6 P2 F1 90.3(3) . . ? F5 P2 F1 90.0(3) . . ? F4 P2 F1 88.5(3) . . ? F2 P2 F1 177.4(3) . . ? F11A P3A F8A 95.5(6) . . ? F11A P3A F12A 172.5(7) . . ? F8A P3A F12A 90.0(6) . . ? F11A P3A F7A 85.6(6) . . ? F8A P3A F7A 175.5(8) . . ? F12A P3A F7A 89.3(6) . . ? F11A P3A F9A 89.9(7) . . ? F8A P3A F9A 94.3(7) . . ? F12A P3A F9A 84.5(7) . . ? F7A P3A F9A 90.1(6) . . ? F11A P3A F10A 85.2(7) . . ? F8A P3A F10A 92.7(6) . . ? F12A P3A F10A 99.7(7) . . ? F7A P3A F10A 83.0(6) . . ? F9A P3A F10A 171.8(6) . . ? #====END data_([Ru]2) _database_code_depnum_ccdc_archive 'CCDC 665732' _audit_creation_date 07-05-10 _audit_creation_method CRYSTALS_ver_12.84 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H37 N6 P Ru, 2(F6 P)' _chemical_formula_sum 'C41 H37 F12 N6 P3 Ru1' _chemical_formula_weight 1035.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _cell_length_a 17.7785(16) _cell_length_b 19.299(2) _cell_length_c 14.1272(12) _cell_angle_alpha 90 _cell_angle_beta 91.932(11) _cell_angle_gamma 90 _cell_volume 4844.5(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 180 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'red orange' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2088 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.504 # Sheldrick geometric approximatio 0.93 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.96 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 180 _diffrn_reflns_number 47479 _reflns_number_total 9479 _diffrn_reflns_av_R_equivalents 0.101 # Number of reflections with Friedels Law is 9479 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9523 _diffrn_reflns_theta_min 2.097 _diffrn_reflns_theta_max 26.018 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.498 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -21 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 17 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'IPDS (Stoe & Cie, 1996)' _computing_cell_refinement 'IPDS (Stoe & Cie, 1996)' _computing_data_reduction 'XRED (Stoe & Cie 1996)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.90 _refine_diff_density_max 0.67 _refine_ls_number_reflns 3531 _refine_ls_number_restraints 0 _refine_ls_number_parameters 577 #_refine_ls_R_factor_ref 0.0600 _refine_ls_wR_factor_ref 0.0694 _refine_ls_goodness_of_fit_ref 1.1155 #_reflns_number_all 9439 _refine_ls_R_factor_all 0.1295 _refine_ls_wR_factor_all 0.0697 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3531 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_gt 0.0694 _refine_ls_shift/su_max 0.000972 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 92.6 -102. 62.9 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.8977(5) 0.1842(5) 0.3721(7) 0.0354 1.0000 Uani . . . . . . H2 H 0.9247 0.1706 0.3195 0.0500 1.0000 Uiso R . . . . . C3 C 0.9311(6) 0.2276(5) 0.4376(7) 0.0399 1.0000 Uani . . . . . . H4 H 0.9801 0.2434 0.4287 0.0500 1.0000 Uiso R . . . . . C5 C 0.8918(6) 0.2482(6) 0.5160(7) 0.0490 1.0000 Uani . . . . . . H6 H 0.9143 0.2770 0.5604 0.0500 1.0000 Uiso R . . . . . C7 C 0.8203(6) 0.2234(5) 0.5254(7) 0.0412 1.0000 Uani . . . . . . H8 H 0.7937 0.2388 0.5757 0.0500 1.0000 Uiso R . . . . . C9 C 0.7878(5) 0.1793(5) 0.4582(7) 0.0326 1.0000 Uani . . . . . . C10 C 0.7119(5) 0.1522(5) 0.4626(7) 0.0327 1.0000 Uani . . . . . . C11 C 0.6651(6) 0.1681(6) 0.5332(7) 0.0441 1.0000 Uani . . . . . . H12 H 0.6813 0.1955 0.5846 0.0500 1.0000 Uiso R . . . . . C13 C 0.5919(6) 0.1432(6) 0.5331(8) 0.0518 1.0000 Uani . . . . . . H14 H 0.5591 0.1561 0.5790 0.0500 1.0000 Uiso R . . . . . C15 C 0.5684(6) 0.1012(5) 0.4567(7) 0.0435 1.0000 Uani . . . . . . H16 H 0.5198 0.0847 0.4545 0.0500 1.0000 Uiso R . . . . . C17 C 0.6174(5) 0.0849(6) 0.3895(6) 0.0327 1.0000 Uani . . . . . . H18 H 0.6019 0.0570 0.3405 0.0500 1.0000 Uiso R . . . . . C19 C 0.6848(7) 0.2064(6) 0.1944(8) 0.0488 1.0000 Uani . . . . . . H20 H 0.6482 0.1995 0.2373 0.0500 1.0000 Uiso R . . . . . C21 C 0.6726(8) 0.2564(5) 0.1247(8) 0.0519 1.0000 Uani . . . . . . H22 H 0.6306 0.2838 0.1267 0.0500 1.0000 Uiso R . . . . . C23 C 0.7251(10) 0.2654(7) 0.0563(9) 0.0699 1.0000 Uani . . . . . . H24 H 0.7183 0.2993 0.0120 0.0500 1.0000 Uiso R . . . . . C25 C 0.7889(8) 0.2231(6) 0.0582(8) 0.0584 1.0000 Uani . . . . . . H26 H 0.8243 0.2298 0.0127 0.0500 1.0000 Uiso R . . . . . C27 C 0.7979(7) 0.1740(6) 0.1268(7) 0.0465 1.0000 Uani . . . . . . C28 C 0.8617(5) 0.1252(6) 0.1331(7) 0.0397 1.0000 Uani . . . . . . C29 C 0.9241(7) 0.1231(8) 0.0745(8) 0.0628 1.0000 Uani . . . . . . H30 H 0.9248 0.1536 0.0219 0.0500 1.0000 Uiso R . . . . . C31 C 0.9801(7) 0.0742(8) 0.0959(9) 0.0666 1.0000 Uani . . . . . . H32 H 1.0212 0.0730 0.0558 0.0500 1.0000 Uiso R . . . . . C33 C 0.9781(6) 0.0336(7) 0.1702(9) 0.0548 1.0000 Uani . . . . . . H34 H 1.0163 0.0011 0.1826 0.0500 1.0000 Uiso R . . . . . C35 C 0.9166(6) 0.0365(6) 0.2284(7) 0.0445 1.0000 Uani . . . . . . C36 C 0.9068(6) -0.0017(5) 0.3195(7) 0.0398 1.0000 Uani . . . . . . C37 C 0.9583(6) -0.0455(6) 0.3572(9) 0.0539 1.0000 Uani . . . . . . H38 H 1.0008 -0.0581 0.3237 0.0500 1.0000 Uiso R . . . . . C39 C 0.9472(7) -0.0761(7) 0.4419(11) 0.0682 1.0000 Uani . . . . . . H40 H 0.9822 -0.1083 0.4667 0.0500 1.0000 Uiso R . . . . . C41 C 0.8843(7) -0.0598(6) 0.4909(9) 0.0569 1.0000 Uani . . . . . . H42 H 0.8740 -0.0790 0.5517 0.0500 1.0000 Uiso R . . . . . C43 C 0.8322(6) -0.0147(5) 0.4493(8) 0.0420 1.0000 Uani . . . . . . H44 H 0.7881 -0.0030 0.4822 0.0500 1.0000 Uiso R . . . . . C45 C 0.6655(5) -0.0749(5) 0.3533(7) 0.0391 1.0000 Uani . . . . . . H46 H 0.6754 -0.0375 0.3973 0.0500 1.0000 Uiso R . . . . . H47 H 0.7100 -0.1048 0.3522 0.0500 1.0000 Uiso R . . . . . C48 C 0.5956(6) -0.1160(7) 0.3738(8) 0.0524 1.0000 Uani . . . . . . H49 H 0.6057 -0.1497 0.4248 0.0500 1.0000 Uiso R . . . . . H50 H 0.5555 -0.0851 0.3954 0.0500 1.0000 Uiso R . . . . . C51 C 0.5751(11) -0.1484(9) 0.2820(10) 0.1035 1.0000 Uani . . . . . . H52 H 0.5953 -0.1964 0.2789 0.0500 1.0000 Uiso R . . . . . H53 H 0.5197 -0.1538 0.2727 0.0500 1.0000 Uiso R . . . . . C54 C 0.6072(6) -0.1052(6) 0.2068(8) 0.0472 1.0000 Uani . . . . . . H55 H 0.6408 -0.1308 0.1670 0.0500 1.0000 Uiso R . . . . . H56 H 0.5669 -0.0857 0.1647 0.0500 1.0000 Uiso R . . . . . C57 C 0.6413(5) 0.0462(5) 0.1140(6) 0.0334 1.0000 Uani . . . . . . C58 C 0.5640(5) 0.0525(6) 0.1289(8) 0.0467 1.0000 Uani . . . . . . H59 H 0.5440 0.0325 0.1827 0.0500 1.0000 Uiso R . . . . . C60 C 0.5188(6) 0.0881(7) 0.0630(9) 0.0579 1.0000 Uani . . . . . . H61 H 0.4662 0.0919 0.0734 0.0500 1.0000 Uiso R . . . . . C62 C 0.5479(8) 0.1178(6) -0.0130(10) 0.0618 1.0000 Uani . . . . . . H63 H 0.5182 0.1400 -0.0591 0.0500 1.0000 Uiso R . . . . . C64 C 0.6243(7) 0.1149(6) -0.0297(7) 0.0476 1.0000 Uani . . . . . . H65 H 0.6446 0.1356 -0.0809 0.0500 1.0000 Uiso R . . . . . C66 C 0.6697(5) 0.0784(5) 0.0349(6) 0.0366 1.0000 Uani . . . . . . H67 H 0.7202 0.0753 0.0249 0.0500 1.0000 Uiso R . . . . . C68 C 0.7601(6) -0.0532(5) 0.1309(6) 0.0340 1.0000 Uani . . . . . . C69 C 0.7555(8) -0.0639(6) 0.0336(8) 0.0544 1.0000 Uani . . . . . . H70 H 0.7231 -0.0366 -0.0033 0.0500 1.0000 Uiso R . . . . . C71 C 0.8005(8) -0.1118(7) -0.0100(9) 0.0696 1.0000 Uani . . . . . . H72 H 0.7938 -0.1190 -0.0760 0.0500 1.0000 Uiso R . . . . . C73 C 0.8502(7) -0.1519(6) 0.0408(9) 0.0578 1.0000 Uani . . . . . . H74 H 0.8829 -0.1824 0.0119 0.0500 1.0000 Uiso R . . . . . C75 C 0.8548(6) -0.1454(6) 0.1370(9) 0.0514 1.0000 Uani . . . . . . H76 H 0.8872 -0.1733 0.1725 0.0500 1.0000 Uiso R . . . . . C77 C 0.8102(5) -0.0974(5) 0.1812(7) 0.0383 1.0000 Uani . . . . . . H78 H 0.8120 -0.0941 0.2466 0.0500 1.0000 Uiso R . . . . . N1 N 0.8264(4) 0.1596(4) 0.3813(5) 0.0295 1.0000 Uani . . . . . . N2 N 0.6899(4) 0.1077(4) 0.3909(5) 0.0286 1.0000 Uani . . . . . . N5 N 0.7451(4) 0.1643(4) 0.1963(5) 0.0361 1.0000 Uani . . . . . . N4 N 0.8586(4) 0.0810(4) 0.2082(5) 0.0333 1.0000 Uani . . . . . . N3 N 0.8408(4) 0.0146(4) 0.3622(5) 0.0303 1.0000 Uani . . . . . . N6 N 0.6474(4) -0.0478(4) 0.2578(5) 0.0321 1.0000 Uani . . . . . . F91 F 0.9674(5) -0.2633(5) 0.1407(8) 0.1102 1.0000 Uani . . . . . . F92 F 1.1187(4) -0.2578(5) 0.2574(6) 0.0966 1.0000 Uani . . . . . . F93 F 1.0004(6) -0.2315(8) 0.2821(8) 0.1493 1.0000 Uani . . . . . . F95 F 1.0345(6) -0.3342(5) 0.2297(10) 0.1389 1.0000 Uani . . . . . . F96 F 1.0509(6) -0.1817(5) 0.1677(10) 0.1360 1.0000 Uani . . . . . . F97 F 1.1903(9) 0.2146(7) 0.2008(9) 0.1711 1.0000 Uani . . . . . . F99 F 1.0710(9) 0.2109(7) 0.1928(13) 0.2033 1.0000 Uani . . . . . . F100 F 1.1906(7) 0.1788(10) 0.3454(8) 0.1755 1.0000 Uani . . . . . . F101 F 1.1212(11) 0.2810(6) 0.2847(11) 0.1979 1.0000 Uani . . . . . . F102 F 1.1377(8) 0.1242(6) 0.2469(14) 0.1742 1.0000 Uani . . . . . . P1 P 0.70485(13) 0.00505(13) 0.20008(17) 0.0286 1.0000 Uani . . . . . . P3 P 1.04507(17) -0.25819(17) 0.1954(2) 0.0532 1.0000 Uani . . . . . . P2 P 1.12984(19) 0.20166(18) 0.2732(2) 0.0548 1.0000 Uani . . . . . . Ru1 Ru 0.77317(4) 0.08648(4) 0.29148(5) 0.0257 1.0000 Uani . . . . . . F980 F 1.0596(8) 0.1606(13) 0.3130(16) 0.1139 0.5000 Uani . . . . . . F981 F 1.1018(14) 0.2102(14) 0.3787(15) 0.1323 0.5000 Uani . . . . . . F940 F 1.0882(7) -0.2854(8) 0.1107(7) 0.1567 1.0000 Uani . . . . . . 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 C1 0.037(6) 0.038(6) 0.031(5) -0.003(4) 0.001(4) -0.012(5) C3 0.037(6) 0.046(6) 0.037(6) -0.006(5) -0.002(5) -0.015(5) C5 0.065(8) 0.058(7) 0.024(5) -0.005(5) -0.003(5) -0.020(6) C7 0.047(6) 0.052(7) 0.025(5) -0.016(5) 0.007(4) -0.010(5) C9 0.037(6) 0.030(5) 0.031(5) 0.002(4) 0.001(4) 0.002(4) C10 0.030(5) 0.033(6) 0.036(5) 0.007(5) 0.005(4) 0.003(4) C11 0.050(6) 0.050(7) 0.034(6) -0.017(5) 0.017(5) -0.005(5) C13 0.045(6) 0.058(7) 0.054(7) -0.010(6) 0.023(5) -0.008(6) C15 0.038(6) 0.049(7) 0.045(6) -0.005(5) 0.015(5) 0.001(5) C17 0.026(4) 0.042(5) 0.030(4) 0.000(5) 0.003(3) 0.003(5) C19 0.061(8) 0.047(7) 0.038(6) -0.007(6) -0.013(5) 0.005(6) C21 0.086(9) 0.025(6) 0.042(7) 0.005(5) -0.020(6) 0.016(6) C23 0.124(13) 0.045(8) 0.040(7) 0.009(6) -0.023(8) -0.026(9) C25 0.095(10) 0.046(8) 0.034(6) 0.006(6) 0.011(6) -0.024(7) C27 0.060(7) 0.054(7) 0.025(6) 0.000(5) -0.006(5) -0.013(6) C28 0.035(6) 0.046(6) 0.038(6) -0.013(5) 0.003(4) -0.014(5) C29 0.065(8) 0.093(10) 0.032(6) -0.007(6) 0.029(6) -0.032(8) C31 0.052(8) 0.091(11) 0.058(8) -0.031(8) 0.026(6) -0.023(8) C33 0.032(6) 0.072(8) 0.062(8) -0.009(7) 0.023(5) -0.001(6) C35 0.048(7) 0.046(7) 0.040(6) -0.008(5) 0.006(5) -0.008(6) C36 0.042(6) 0.038(6) 0.039(6) -0.007(5) 0.002(5) -0.004(5) C37 0.040(6) 0.055(8) 0.066(8) -0.005(7) -0.006(6) 0.007(6) C39 0.046(7) 0.063(9) 0.095(10) -0.006(8) -0.016(7) 0.021(7) C41 0.075(9) 0.041(6) 0.054(7) 0.017(6) -0.026(7) -0.012(6) C43 0.042(6) 0.037(6) 0.046(7) 0.006(5) -0.009(5) -0.010(5) C45 0.038(5) 0.044(7) 0.035(5) 0.004(5) 0.000(4) -0.003(5) C48 0.052(7) 0.069(8) 0.037(6) 0.007(5) 0.009(5) -0.024(6) C51 0.148(15) 0.105(12) 0.059(9) -0.023(9) 0.028(9) -0.081(12) C54 0.051(6) 0.054(7) 0.037(6) -0.004(5) 0.001(5) -0.018(5) C57 0.033(5) 0.039(6) 0.027(5) -0.008(4) -0.006(4) -0.006(5) C58 0.031(6) 0.062(7) 0.046(6) -0.009(6) -0.001(5) 0.003(5) C60 0.048(6) 0.063(8) 0.061(7) -0.005(8) -0.015(5) 0.020(7) C62 0.074(9) 0.050(7) 0.058(8) -0.013(6) -0.031(7) 0.018(7) C64 0.067(8) 0.044(6) 0.031(6) -0.003(5) -0.012(5) 0.008(6) C66 0.047(6) 0.036(6) 0.027(5) -0.002(5) -0.001(4) 0.005(5) C68 0.044(6) 0.036(5) 0.023(5) -0.002(4) 0.006(4) -0.010(5) C69 0.087(9) 0.044(7) 0.034(6) 0.002(5) 0.017(6) 0.016(6) C71 0.106(11) 0.060(8) 0.044(7) -0.011(6) 0.023(7) 0.033(8) C73 0.070(8) 0.051(7) 0.055(8) -0.006(6) 0.026(6) 0.015(7) C75 0.050(7) 0.037(6) 0.068(8) -0.008(6) 0.017(6) 0.007(5) C77 0.040(5) 0.037(6) 0.038(5) -0.001(5) 0.003(4) 0.007(5) N1 0.031(4) 0.038(5) 0.020(4) 0.004(4) 0.004(3) 0.001(4) N2 0.035(5) 0.030(5) 0.021(4) -0.005(3) -0.001(3) -0.002(3) N5 0.042(5) 0.038(5) 0.028(5) -0.007(4) 0.002(4) -0.008(4) N4 0.036(4) 0.035(5) 0.028(4) -0.006(4) -0.003(3) -0.009(4) N3 0.031(4) 0.039(5) 0.021(4) -0.001(4) 0.002(3) -0.014(4) N6 0.033(4) 0.040(5) 0.023(4) -0.003(4) -0.001(3) -0.016(4) F91 0.077(5) 0.086(6) 0.164(9) -0.042(6) -0.059(6) 0.029(5) F92 0.066(5) 0.125(7) 0.096(6) -0.018(6) -0.034(4) 0.017(5) F93 0.121(8) 0.225(14) 0.102(8) -0.029(9) 0.018(6) 0.089(9) F95 0.104(7) 0.079(7) 0.231(14) 0.072(8) -0.017(8) -0.003(6) F96 0.107(7) 0.063(6) 0.235(14) 0.028(7) -0.024(8) -0.031(5) F97 0.235(15) 0.161(11) 0.123(9) 0.082(9) 0.103(10) 0.042(10) F99 0.199(14) 0.134(11) 0.265(19) 0.009(11) -0.167(14) -0.001(10) F100 0.135(10) 0.296(19) 0.092(8) 0.038(10) -0.042(7) 0.033(11) F101 0.31(2) 0.102(9) 0.180(14) -0.084(10) -0.006(14) 0.029(11) F102 0.158(11) 0.078(7) 0.29(2) 0.015(9) 0.000(12) 0.014(8) P1 0.0287(13) 0.0326(14) 0.0245(13) -0.0036(11) 0.0025(10) -0.0006(10) P3 0.0515(18) 0.0551(19) 0.0531(19) 0.0038(15) 0.0006(14) 0.0003(15) P2 0.058(2) 0.067(2) 0.0393(16) 0.0084(15) 0.0047(14) 0.0102(16) Ru1 0.0259(4) 0.0322(4) 0.0193(3) -0.0004(4) 0.0037(2) -0.0009(4) F980 0.037(9) 0.18(2) 0.124(16) 0.001(16) 0.034(9) -0.029(11) F981 0.137(19) 0.17(2) 0.090(14) 0.040(15) 0.072(14) 0.061(17) F940 0.137(9) 0.272(16) 0.064(6) 0.004(8) 0.043(6) 0.093(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . H2 . 0.935 no C1 . C3 . 1.369(13) yes C1 . N1 . 1.364(12) yes C3 . H4 . 0.934 no C3 . C5 . 1.387(15) yes C5 . H6 . 0.919 no C5 . C7 . 1.369(15) yes C7 . H8 . 0.916 no C7 . C9 . 1.386(13) yes C9 . C10 . 1.451(13) yes C9 . N1 . 1.358(12) yes C10 . C11 . 1.355(13) yes C10 . N2 . 1.376(12) yes C11 . H12 . 0.936 no C11 . C13 . 1.387(15) yes C13 . H14 . 0.921 no C13 . C15 . 1.403(15) yes C15 . H16 . 0.920 no C15 . C17 . 1.348(13) yes C17 . H18 . 0.912 no C17 . N2 . 1.360(11) yes C19 . H20 . 0.914 no C19 . C21 . 1.391(15) yes C19 . N5 . 1.344(14) yes C21 . H22 . 0.915 no C21 . C23 . 1.376(19) yes C23 . H24 . 0.912 no C23 . C25 . 1.40(2) yes C25 . H26 . 0.924 no C25 . C27 . 1.361(16) yes C27 . C28 . 1.477(16) yes C27 . N5 . 1.393(13) yes C28 . C29 . 1.406(14) yes C28 . N4 . 1.364(13) yes C29 . H30 . 0.949 no C29 . C31 . 1.40(2) yes C31 . H32 . 0.940 no C31 . C33 . 1.312(18) yes C33 . H34 . 0.936 no C33 . C35 . 1.392(14) yes C35 . C36 . 1.499(15) yes C35 . N4 . 1.365(13) yes C36 . C37 . 1.342(15) yes C36 . N3 . 1.374(12) yes C37 . H38 . 0.938 no C37 . C39 . 1.355(18) yes C39 . H40 . 0.939 no C39 . C41 . 1.373(18) yes C41 . H42 . 0.958 no C41 . C43 . 1.387(15) yes C43 . H44 . 0.952 no C43 . N3 . 1.367(13) yes C45 . H46 . 0.964 no C45 . H47 . 0.981 no C45 . C48 . 1.511(14) yes C45 . N6 . 1.471(12) yes C48 . H49 . 0.984 no C48 . H50 . 0.985 no C48 . C51 . 1.474(17) yes C51 . H52 . 0.994 no C51 . H53 . 0.995 no C51 . C54 . 1.480(17) yes C54 . H55 . 0.970 no C54 . H56 . 0.992 no C54 . N6 . 1.491(12) yes C57 . C58 . 1.403(14) yes C57 . C66 . 1.388(13) yes C57 . P1 . 1.816(10) yes C58 . H59 . 0.933 no C58 . C60 . 1.390(16) yes C60 . H61 . 0.954 no C60 . C62 . 1.337(18) yes C62 . H63 . 0.929 no C62 . C64 . 1.387(17) yes C64 . H65 . 0.912 no C64 . C66 . 1.389(14) yes C66 . H67 . 0.916 no C68 . C69 . 1.389(14) yes C68 . C77 . 1.408(14) yes C68 . P1 . 1.802(10) yes C69 . H70 . 0.928 no C69 . C71 . 1.380(16) yes C71 . H72 . 0.947 no C71 . C73 . 1.361(17) yes C73 . H74 . 0.931 no C73 . C75 . 1.365(17) yes C75 . H76 . 0.924 no C75 . C77 . 1.382(14) yes C77 . H78 . 0.925 no N1 . Ru1 . 2.101(8) yes N2 . Ru1 . 2.115(7) yes N5 . Ru1 . 2.065(8) yes N4 . Ru1 . 1.955(7) yes N3 . Ru1 . 2.071(8) yes N6 . P1 . 1.675(7) yes F91 . P3 . 1.563(8) yes F92 . P3 . 1.549(8) yes F93 . P3 . 1.569(10) yes F95 . P3 . 1.559(9) yes F96 . P3 . 1.531(10) yes F97 . P2 . 1.528(11) yes F99 . P2 . 1.528(12) yes F100 . P2 . 1.527(11) yes F101 . P2 . 1.547(12) yes F102 . P2 . 1.548(13) yes P1 . Ru1 . 2.347(3) yes P3 . F940 . 1.535(9) yes P2 . F980 . 1.597(16) yes P2 . F981 . 1.596(18) yes F980 . F981 . 1.51(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag H2 . C1 . C3 . 119.0 no H2 . C1 . N1 . 118.8 no C3 . C1 . N1 . 122.2(9) yes C1 . C3 . H4 . 119.6 no C1 . C3 . C5 . 119.7(9) yes H4 . C3 . C5 . 120.7 no C3 . C5 . H6 . 120.0 no C3 . C5 . C7 . 118.1(10) yes H6 . C5 . C7 . 121.9 no C5 . C7 . H8 . 117.8 no C5 . C7 . C9 . 121.0(9) yes H8 . C7 . C9 . 121.1 no C7 . C9 . C10 . 124.0(9) yes C7 . C9 . N1 . 120.7(9) yes C10 . C9 . N1 . 115.3(8) yes C9 . C10 . C11 . 123.0(9) yes C9 . C10 . N2 . 115.9(8) yes C11 . C10 . N2 . 121.1(9) yes C10 . C11 . H12 . 121.2 no C10 . C11 . C13 . 121.3(10) yes H12 . C11 . C13 . 117.4 no C11 . C13 . H14 . 121.5 no C11 . C13 . C15 . 117.2(9) yes H14 . C13 . C15 . 121.2 no C13 . C15 . H16 . 118.8 no C13 . C15 . C17 . 119.5(10) yes H16 . C15 . C17 . 121.6 no C15 . C17 . H18 . 119.0 no C15 . C17 . N2 . 123.3(9) yes H18 . C17 . N2 . 117.7 no H20 . C19 . C21 . 118.2 no H20 . C19 . N5 . 119.0 no C21 . C19 . N5 . 122.6(12) yes C19 . C21 . H22 . 119.1 no C19 . C21 . C23 . 119.4(12) yes H22 . C21 . C23 . 121.5 no C21 . C23 . H24 . 119.8 no C21 . C23 . C25 . 118.9(11) yes H24 . C23 . C25 . 121.3 no C23 . C25 . H26 . 118.5 no C23 . C25 . C27 . 119.6(12) yes H26 . C25 . C27 . 121.8 no C25 . C27 . C28 . 123.9(11) yes C25 . C27 . N5 . 122.1(12) yes C28 . C27 . N5 . 114.0(9) yes C27 . C28 . C29 . 127.1(11) yes C27 . C28 . N4 . 113.2(9) yes C29 . C28 . N4 . 119.6(11) yes C28 . C29 . H30 . 118.3 no C28 . C29 . C31 . 117.6(12) yes H30 . C29 . C31 . 124.1 no C29 . C31 . H32 . 116.7 no C29 . C31 . C33 . 122.6(11) yes H32 . C31 . C33 . 120.6 no C31 . C33 . H34 . 120.8 no C31 . C33 . C35 . 119.5(12) yes H34 . C33 . C35 . 119.7 no C33 . C35 . C36 . 127.1(11) yes C33 . C35 . N4 . 120.3(10) yes C36 . C35 . N4 . 112.4(9) yes C35 . C36 . C37 . 123.6(10) yes C35 . C36 . N3 . 112.9(9) yes C37 . C36 . N3 . 123.5(10) yes C36 . C37 . H38 . 120.9 no C36 . C37 . C39 . 120.5(11) yes H38 . C37 . C39 . 118.5 no C37 . C39 . H40 . 120.2 no C37 . C39 . C41 . 119.4(12) yes H40 . C39 . C41 . 120.4 no C39 . C41 . H42 . 123.1 no C39 . C41 . C43 . 118.3(12) yes H42 . C41 . C43 . 118.6 no C41 . C43 . H44 . 119.4 no C41 . C43 . N3 . 123.2(11) yes H44 . C43 . N3 . 117.4 no H46 . C45 . H47 . 108.7 no H46 . C45 . C48 . 113.8 no H47 . C45 . C48 . 111.2 no H46 . C45 . N6 . 110.8 no H47 . C45 . N6 . 110.2 no C48 . C45 . N6 . 101.9(8) yes C45 . C48 . H49 . 110.9 no C45 . C48 . H50 . 110.4 no H49 . C48 . H50 . 106.8 no C45 . C48 . C51 . 103.6(9) yes H49 . C48 . C51 . 113.5 no H50 . C48 . C51 . 111.8 no C48 . C51 . H52 . 110.7 no C48 . C51 . H53 . 112.0 no H52 . C51 . H53 . 104.8 no C48 . C51 . C54 . 107.6(11) yes H52 . C51 . C54 . 110.2 no H53 . C51 . C54 . 111.6 no C51 . C54 . H55 . 112.9 no C51 . C54 . H56 . 110.9 no H55 . C54 . H56 . 107.0 no C51 . C54 . N6 . 105.2(9) yes H55 . C54 . N6 . 111.3 no H56 . C54 . N6 . 109.5 no C58 . C57 . C66 . 117.9(9) yes C58 . C57 . P1 . 121.9(8) yes C66 . C57 . P1 . 120.0(7) yes C57 . C58 . H59 . 119.2 no C57 . C58 . C60 . 119.3(11) yes H59 . C58 . C60 . 121.5 no C58 . C60 . H61 . 118.8 no C58 . C60 . C62 . 121.3(11) yes H61 . C60 . C62 . 119.9 no C60 . C62 . H63 . 122.3 no C60 . C62 . C64 . 121.8(11) yes H63 . C62 . C64 . 115.9 no C62 . C64 . H65 . 122.3 no C62 . C64 . C66 . 117.3(11) yes H65 . C64 . C66 . 120.4 no C64 . C66 . C57 . 122.4(10) yes C64 . C66 . H67 . 118.9 no C57 . C66 . H67 . 118.7 no C69 . C68 . C77 . 115.1(9) yes C69 . C68 . P1 . 127.9(9) yes C77 . C68 . P1 . 116.8(7) yes C68 . C69 . H70 . 119.0 no C68 . C69 . C71 . 121.7(12) yes H70 . C69 . C71 . 119.2 no C69 . C71 . H72 . 118.8 no C69 . C71 . C73 . 121.4(12) yes H72 . C71 . C73 . 119.6 no C71 . C73 . H74 . 122.1 no C71 . C73 . C75 . 119.3(11) yes H74 . C73 . C75 . 118.5 no C73 . C75 . H76 . 120.1 no C73 . C75 . C77 . 119.7(11) yes H76 . C75 . C77 . 120.2 no C68 . C77 . C75 . 122.7(10) yes C68 . C77 . H78 . 117.6 no C75 . C77 . H78 . 119.7 no C1 . N1 . C9 . 118.3(8) yes C1 . N1 . Ru1 . 125.3(6) yes C9 . N1 . Ru1 . 116.3(6) yes C10 . N2 . C17 . 117.3(8) yes C10 . N2 . Ru1 . 114.9(6) yes C17 . N2 . Ru1 . 127.7(6) yes C27 . N5 . C19 . 117.3(9) yes C27 . N5 . Ru1 . 113.8(7) yes C19 . N5 . Ru1 . 128.9(7) yes C35 . N4 . C28 . 120.4(8) yes C35 . N4 . Ru1 . 120.3(7) yes C28 . N4 . Ru1 . 119.2(7) yes C36 . N3 . C43 . 115.0(9) yes C36 . N3 . Ru1 . 115.7(6) yes C43 . N3 . Ru1 . 129.1(7) yes C54 . N6 . C45 . 105.4(8) yes C54 . N6 . P1 . 120.5(6) yes C45 . N6 . P1 . 123.0(6) yes C57 . P1 . C68 . 104.4(4) yes C57 . P1 . N6 . 102.5(4) yes C68 . P1 . N6 . 103.7(4) yes C57 . P1 . Ru1 . 112.0(3) yes C68 . P1 . Ru1 . 115.7(3) yes N6 . P1 . Ru1 . 116.9(3) yes F93 . P3 . F91 . 86.8(6) yes F93 . P3 . F95 . 89.8(8) yes F91 . P3 . F95 . 88.9(6) yes F93 . P3 . F92 . 89.9(6) yes F91 . P3 . F92 . 174.2(6) yes F95 . P3 . F92 . 86.4(6) yes F93 . P3 . F96 . 85.6(8) yes F91 . P3 . F96 . 90.0(6) yes F95 . P3 . F96 . 175.4(8) yes F92 . P3 . F96 . 94.4(6) yes F93 . P3 . F940 . 179.1(9) yes F91 . P3 . F940 . 92.9(7) yes F95 . P3 . F940 . 89.4(8) yes F92 . P3 . F940 . 90.4(6) yes F96 . P3 . F940 . 95.2(8) yes F102 . P2 . F101 . 172.1(10) yes F102 . P2 . F99 . 89.9(9) yes F101 . P2 . F99 . 84.0(8) yes F102 . P2 . F97 . 85.8(8) yes F101 . P2 . F97 . 89.0(9) yes F99 . P2 . F97 . 87.9(10) yes F102 . P2 . F100 . 79.3(9) yes F101 . P2 . F100 . 106.6(10) yes F99 . P2 . F100 . 169.1(10) yes F97 . P2 . F100 . 89.8(8) yes F102 . P2 . F980 . 71.5(10) yes F101 . P2 . F980 . 111.9(12) yes F99 . P2 . F980 . 78.3(11) yes F97 . P2 . F980 . 153.2(11) yes F100 . P2 . F980 . 99.5(10) yes F102 . P2 . F981 . 111.0(12) yes F101 . P2 . F981 . 76.3(11) yes F99 . P2 . F981 . 117.1(12) yes F97 . P2 . F981 . 148.9(13) yes F100 . P2 . F981 . 69.0(10) yes F980 . P2 . F981 . 56.6(11) yes N2 . Ru1 . N1 . 77.3(3) yes N2 . Ru1 . N3 . 102.6(3) yes N1 . Ru1 . N3 . 85.2(3) yes N2 . Ru1 . N5 . 97.6(3) yes N1 . Ru1 . N5 . 90.0(3) yes N3 . Ru1 . N5 . 157.6(3) yes N2 . Ru1 . P1 . 97.7(2) yes N1 . Ru1 . P1 . 175.0(2) yes N3 . Ru1 . P1 . 95.7(2) yes N5 . Ru1 . P1 . 91.1(2) yes N2 . Ru1 . N4 . 170.3(3) yes N1 . Ru1 . N4 . 93.3(3) yes N3 . Ru1 . N4 . 78.7(3) yes N5 . Ru1 . N4 . 79.8(3) yes P1 . Ru1 . N4 . 91.7(2) yes P2 . F980 . F981 . 61.6(9) yes F980 . F981 . P2 . 61.7(11) yes #====END data_([Ru]3) _database_code_depnum_ccdc_archive 'CCDC 665733' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H28 N5 O3 P Ru, C3 H6 O, 2(F6 P)' _chemical_formula_sum 'C31 H34 F12 N5 O4 P3 Ru' _chemical_formula_weight 962.61 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.058(3) _cell_length_b 16.561(3) _cell_length_c 12.834(2) _cell_angle_alpha 90 _cell_angle_beta 126.380(19) _cell_angle_gamma 90 _cell_volume 3774.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 20340 _cell_measurement_theta_min 3.0184 _cell_measurement_theta_max 32.2032 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.275 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.125 _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8356 _exptl_absorpt_correction_T_max 0.9263 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0749 _diffrn_reflns_number 12578 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6488 _reflns_number_gt 5154 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0410P)^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_number_reflns 6488 _refine_ls_number_parameters 510 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_diff_density_max 0.628 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.4230(3) 0.8005(4) 0.5274(6) 0.0429(15) Uani 1 1 d . . . H1A H 0.3989 0.7489 0.4959 0.064 Uiso 1 1 calc R . . H1B H 0.3868 0.8425 0.4785 0.064 Uiso 1 1 calc R . . H1C H 0.4432 0.8058 0.6171 0.064 Uiso 1 1 calc R . . C2 C 0.3695(3) 0.8105(3) 0.2235(5) 0.0367(12) Uani 1 1 d . . . H2A H 0.3906 0.8562 0.2806 0.055 Uiso 1 1 calc R . . H2B H 0.3176 0.8044 0.1899 0.055 Uiso 1 1 calc R . . H2C H 0.373 0.8187 0.1532 0.055 Uiso 1 1 calc R . . C3 C 0.4359(3) 0.6055(3) 0.4522(6) 0.0445(14) Uani 1 1 d . . . H3A H 0.4271 0.6135 0.5163 0.067 Uiso 1 1 calc R . . H3B H 0.4487 0.5501 0.4528 0.067 Uiso 1 1 calc R . . H3C H 0.3912 0.619 0.3684 0.067 Uiso 1 1 calc R . . C4 C 0.7369(3) 0.8509(3) 0.4846(5) 0.0315(12) Uani 1 1 d . . . H4 H 0.7289 0.8925 0.5238 0.038 Uiso 1 1 calc R . . C5 C 0.7980(3) 0.8566(4) 0.4778(6) 0.0503(16) Uani 1 1 d . . . H5 H 0.8291 0.9017 0.5099 0.06 Uiso 1 1 calc R . . C6 C 0.8109(3) 0.7937(4) 0.4226(6) 0.0492(17) Uani 1 1 d . . . H6 H 0.851 0.7955 0.417 0.059 Uiso 1 1 calc R . . C7 C 0.7630(3) 0.7280(4) 0.3757(5) 0.0471(16) Uani 1 1 d . . . H7 H 0.7714 0.6847 0.3397 0.056 Uiso 1 1 calc R . . C8 C 0.7035(3) 0.7264(4) 0.3820(5) 0.0325(12) Uani 1 1 d . . . C9 C 0.6493(3) 0.6593(3) 0.3320(5) 0.0302(12) Uani 1 1 d . . . C10 C 0.6531(4) 0.5913(4) 0.2720(6) 0.0489(16) Uani 1 1 d . . . H10 H 0.6932 0.5857 0.2669 0.059 Uiso 1 1 calc R . . C11 C 0.5992(4) 0.5329(4) 0.2207(6) 0.0542(18) Uani 1 1 d . . . H11 H 0.6029 0.4874 0.1824 0.065 Uiso 1 1 calc R . . C12 C 0.5395(4) 0.5416(4) 0.2260(6) 0.0462(16) Uani 1 1 d . . . H12 H 0.5011 0.5034 0.1888 0.055 Uiso 1 1 calc R . . C13 C 0.5377(3) 0.6098(3) 0.2893(5) 0.0356(13) Uani 1 1 d . . . H13 H 0.4978 0.6152 0.295 0.043 Uiso 1 1 calc R . . C14 C 0.4982(3) 0.8295(4) 0.1478(5) 0.0345(14) Uani 1 1 d . . . H14 H 0.4975 0.7756 0.1268 0.041 Uiso 1 1 calc R . . C15 C 0.4603(3) 0.8858(4) 0.0474(5) 0.0412(15) Uani 1 1 d . . . H15 H 0.4347 0.8699 -0.0385 0.049 Uiso 1 1 calc R . . C16 C 0.4621(3) 0.9663(4) 0.0797(5) 0.0415(14) Uani 1 1 d . . . H16 H 0.4374 1.0052 0.015 0.05 Uiso 1 1 calc R . . C17 C 0.5007(3) 0.9883(3) 0.2082(5) 0.0369(13) Uani 1 1 d . . . H17 H 0.5023 1.042 0.2308 0.044 Uiso 1 1 calc R . . C18 C 0.5372(3) 0.9291(3) 0.3032(5) 0.0309(12) Uani 1 1 d . . . C19 C 0.5800(3) 0.9463(3) 0.4437(5) 0.0304(12) Uani 1 1 d . . . C20 C 0.5941(3) 1.0219(3) 0.5020(5) 0.0357(13) Uani 1 1 d . . . H20 H 0.5752 1.0685 0.452 0.043 Uiso 1 1 calc R . . C21 C 0.6363(3) 1.0263(3) 0.6341(6) 0.0372(14) Uani 1 1 d . . . H21 H 0.6464 1.0764 0.6739 0.045 Uiso 1 1 calc R . . C22 C 0.6643(3) 0.9569(3) 0.7095(5) 0.0329(12) Uani 1 1 d . . . H22 H 0.6933 0.9598 0.7993 0.04 Uiso 1 1 calc R . . C23 C 0.6477(3) 0.8833(3) 0.6469(5) 0.0252(11) Uani 1 1 d . . . C24 C 0.6757(3) 0.8030(3) 0.7106(5) 0.0248(12) Uani 1 1 d . . . C25 C 0.7144(3) 0.7912(3) 0.8414(5) 0.0288(12) Uani 1 1 d . . . H25 H 0.7243 0.8346 0.8953 0.035 Uiso 1 1 calc R . . C26 C 0.7383(3) 0.7151(3) 0.8925(5) 0.0333(12) Uani 1 1 d . . . H26 H 0.7646 0.7063 0.9809 0.04 Uiso 1 1 calc R . . C27 C 0.7222(3) 0.6515(3) 0.8088(5) 0.0309(12) Uani 1 1 d . . . H27 H 0.7385 0.5996 0.8415 0.037 Uiso 1 1 calc R . . C28 C 0.6823(3) 0.6650(3) 0.6776(5) 0.0253(11) Uani 1 1 d . . . H28 H 0.6715 0.6217 0.6231 0.03 Uiso 1 1 calc R . . C101 C 1.0730(4) 1.2438(5) 0.8896(6) 0.0565(19) Uani 1 1 d . . . C102 C 1.1089(6) 1.2351(5) 1.0230(8) 0.083(3) Uani 1 1 d . . . H10A H 1.1606 1.2201 1.0649 0.124 Uiso 1 1 calc R . . H10B H 1.084 1.1939 1.0373 0.124 Uiso 1 1 calc R . . H10C H 1.1068 1.2853 1.0581 0.124 Uiso 1 1 calc R . . C103 C 1.0584(4) 1.1683(4) 0.8146(6) 0.0526(16) Uani 1 1 d . . . H10D H 1.0114 1.1453 0.7885 0.079 Uiso 1 1 calc R . . H10E H 1.0983 1.1303 0.8678 0.079 Uiso 1 1 calc R . . H10F H 1.0562 1.1806 0.7393 0.079 Uiso 1 1 calc R . . N1 N 0.6904(3) 0.7886(3) 0.4372(4) 0.0306(11) Uani 1 1 d . . . N2 N 0.5910(3) 0.6678(3) 0.3421(4) 0.0312(10) Uani 1 1 d . . . N3 N 0.5349(2) 0.8489(3) 0.2708(4) 0.0310(10) Uani 1 1 d . . . N4 N 0.6067(2) 0.8794(2) 0.5169(4) 0.0231(9) Uani 1 1 d . . . N5 N 0.6583(2) 0.7402(2) 0.6258(4) 0.0248(9) Uani 1 1 d . . . O1 O 0.48326(19) 0.8071(2) 0.5135(3) 0.0304(8) Uani 1 1 d . . . O2 O 0.41005(19) 0.7394(2) 0.2928(3) 0.0320(8) Uani 1 1 d . . . O3 O 0.4975(2) 0.6570(2) 0.4813(3) 0.0334(9) Uani 1 1 d . . . O4 O 1.0574(3) 1.3110(3) 0.8387(5) 0.0708(14) Uani 1 1 d . . . F1 F 0.3288(2) 1.0639(2) 0.0760(3) 0.0556(10) Uani 1 1 d . . . F2 F 0.2767(3) 1.0118(3) 0.2486(5) 0.1065(19) Uani 1 1 d . . . F3 F 0.2817(2) 0.9507(2) 0.0983(4) 0.0758(13) Uani 1 1 d . . . F4 F 0.38596(18) 1.0077(2) 0.2737(3) 0.0442(8) Uani 1 1 d . . . F5 F 0.3207(3) 1.1259(3) 0.2216(4) 0.0807(15) Uani 1 1 d . . . F6 F 0.2191(2) 1.0687(2) 0.0505(4) 0.0642(10) Uani 1 1 d . . . F7 F 0.8930(3) 1.0126(3) 0.6994(4) 0.0864(16) Uani 1 1 d . . . F8 F 0.7787(2) 1.1449(2) 0.6622(4) 0.0733(12) Uani 1 1 d . . . F9 F 0.8994(3) 1.1124(3) 0.8198(4) 0.0889(14) Uani 1 1 d . . . F10 F 0.7701(2) 1.0437(2) 0.5419(4) 0.0667(11) Uani 1 1 d . . . F11 F 0.8613(2) 1.1352(3) 0.6166(4) 0.0853(16) Uani 1 1 d . . . F12 F 0.8094(2) 1.0183(3) 0.7425(5) 0.1038(19) Uani 1 1 d . . . P1 P 0.49207(8) 0.74471(8) 0.42834(13) 0.0259(3) Uani 1 1 d . . . P2 P 0.30169(9) 1.03792(9) 0.15957(14) 0.0343(4) Uani 1 1 d . . . P3 P 0.83514(9) 1.07782(12) 0.68106(15) 0.0450(4) Uani 1 1 d . . . Ru1 Ru 0.59318(2) 0.77429(2) 0.43363(3) 0.02394(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.043(3) 0.055(4) -0.014(3) 0.036(3) -0.010(3) C2 0.029(3) 0.033(3) 0.035(3) 0.006(3) 0.012(3) 0.009(3) C3 0.042(4) 0.037(3) 0.049(4) -0.004(3) 0.024(3) -0.011(3) C4 0.030(3) 0.031(3) 0.036(3) 0.006(2) 0.021(3) 0.008(3) C5 0.037(3) 0.058(4) 0.064(4) 0.019(3) 0.035(4) 0.010(3) C6 0.034(3) 0.082(5) 0.041(4) 0.022(3) 0.027(3) 0.020(4) C7 0.034(3) 0.075(5) 0.033(3) 0.012(3) 0.021(3) 0.022(4) C8 0.031(3) 0.053(4) 0.018(3) 0.004(3) 0.017(3) 0.009(3) C9 0.034(3) 0.031(3) 0.023(3) 0.006(2) 0.015(3) 0.017(3) C10 0.051(4) 0.053(4) 0.041(4) -0.006(3) 0.026(3) 0.015(3) C11 0.064(5) 0.045(4) 0.047(4) -0.011(3) 0.029(4) 0.014(4) C12 0.059(4) 0.035(3) 0.045(4) -0.011(3) 0.030(4) 0.002(3) C13 0.041(3) 0.033(3) 0.034(3) 0.000(2) 0.023(3) 0.005(3) C14 0.034(3) 0.044(4) 0.029(3) 0.001(3) 0.021(3) 0.009(3) C15 0.039(4) 0.057(4) 0.027(3) 0.006(3) 0.019(3) 0.007(3) C16 0.035(3) 0.054(4) 0.035(3) 0.012(3) 0.021(3) 0.014(3) C17 0.045(4) 0.039(3) 0.033(3) 0.015(3) 0.027(3) 0.016(3) C18 0.032(3) 0.024(3) 0.043(3) 0.006(2) 0.026(3) 0.003(2) C19 0.031(3) 0.032(3) 0.036(3) 0.004(2) 0.024(3) 0.005(2) C20 0.036(3) 0.034(3) 0.038(3) 0.010(2) 0.022(3) 0.011(3) C21 0.042(4) 0.031(3) 0.047(4) 0.003(3) 0.030(3) 0.007(3) C22 0.034(3) 0.033(3) 0.031(3) 0.003(2) 0.019(3) 0.006(3) C23 0.026(3) 0.028(3) 0.027(3) 0.001(2) 0.019(3) 0.002(2) C24 0.017(3) 0.026(3) 0.031(3) 0.004(2) 0.014(2) 0.004(2) C25 0.026(3) 0.032(3) 0.019(3) -0.002(2) 0.009(2) 0.000(2) C26 0.024(3) 0.044(3) 0.023(3) 0.005(2) 0.008(2) -0.001(3) C27 0.035(3) 0.027(3) 0.032(3) 0.003(2) 0.021(3) 0.004(3) C28 0.022(3) 0.026(3) 0.027(3) -0.001(2) 0.013(2) 0.001(2) C101 0.043(4) 0.073(5) 0.047(4) -0.009(3) 0.023(4) 0.006(4) C102 0.137(9) 0.049(5) 0.057(5) -0.009(4) 0.055(6) 0.018(5) C103 0.048(4) 0.050(4) 0.053(4) -0.011(3) 0.027(4) -0.003(3) N1 0.030(3) 0.036(3) 0.028(3) 0.008(2) 0.018(2) 0.007(2) N2 0.034(3) 0.034(3) 0.025(2) 0.006(2) 0.017(2) 0.009(2) N3 0.025(2) 0.037(3) 0.032(3) 0.010(2) 0.018(2) 0.011(2) N4 0.024(2) 0.026(2) 0.021(2) -0.0008(18) 0.014(2) 0.002(2) N5 0.026(2) 0.025(2) 0.026(2) 0.0027(18) 0.017(2) 0.0047(19) O1 0.031(2) 0.036(2) 0.031(2) -0.0078(16) 0.0217(18) -0.0023(17) O2 0.0281(19) 0.0254(19) 0.0329(19) 0.0004(15) 0.0128(17) 0.0035(16) O3 0.030(2) 0.032(2) 0.032(2) 0.0059(17) 0.0158(19) 0.0045(19) O4 0.085(4) 0.042(3) 0.063(3) 0.003(3) 0.032(3) 0.006(3) F1 0.059(2) 0.076(3) 0.047(2) 0.0226(19) 0.040(2) 0.021(2) F2 0.124(4) 0.126(4) 0.143(4) 0.089(3) 0.119(4) 0.073(3) F3 0.060(3) 0.0248(19) 0.076(3) -0.0034(19) 0.004(2) 0.0074(19) F4 0.038(2) 0.051(2) 0.0275(18) 0.0035(16) 0.0107(17) 0.0086(17) F5 0.114(4) 0.046(2) 0.054(3) -0.0048(19) 0.035(3) 0.031(3) F6 0.042(2) 0.062(2) 0.076(3) 0.0298(19) 0.028(2) 0.0188(18) F7 0.076(3) 0.114(4) 0.067(3) 0.011(3) 0.041(3) 0.044(3) F8 0.073(3) 0.077(3) 0.055(3) 0.003(2) 0.030(2) 0.034(2) F9 0.065(3) 0.131(4) 0.042(2) -0.011(2) 0.016(2) 0.015(3) F10 0.069(3) 0.050(2) 0.050(2) -0.0009(18) 0.018(2) 0.008(2) F11 0.057(3) 0.126(4) 0.063(3) 0.030(3) 0.031(2) -0.017(3) F12 0.054(3) 0.139(4) 0.120(4) 0.098(3) 0.053(3) 0.033(3) P1 0.0243(8) 0.0248(7) 0.0252(8) -0.0014(6) 0.0129(7) 0.0029(7) P2 0.0407(9) 0.0292(8) 0.0384(9) 0.0105(7) 0.0265(8) 0.0111(7) P3 0.0370(9) 0.0659(13) 0.0334(9) 0.0137(7) 0.0216(8) 0.0126(8) Ru1 0.0267(2) 0.02402(19) 0.02212(18) 0.0018(2) 0.01504(16) 0.0046(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.447(6) . ? C2 O2 1.427(6) . ? C3 O3 1.453(6) . ? C4 N1 1.323(7) . ? C4 C5 1.402(7) . ? C5 C6 1.381(9) . ? C6 C7 1.381(9) . ? C7 C8 1.362(7) . ? C8 N1 1.375(7) . ? C8 C9 1.471(8) . ? C9 N2 1.375(6) . ? C9 C10 1.395(7) . ? C10 C11 1.362(9) . ? C11 C12 1.365(8) . ? C12 C13 1.405(7) . ? C13 N2 1.349(7) . ? C14 N3 1.317(7) . ? C14 C15 1.398(8) . ? C15 C16 1.389(8) . ? C16 C17 1.383(8) . ? C17 C18 1.389(7) . ? C18 N3 1.384(7) . ? C18 C19 1.484(7) . ? C19 N4 1.342(6) . ? C19 C20 1.396(7) . ? C20 C21 1.369(8) . ? C21 C22 1.389(7) . ? C22 C23 1.385(7) . ? C23 N4 1.347(6) . ? C23 C24 1.489(7) . ? C24 C25 1.373(7) . ? C24 N5 1.385(6) . ? C25 C26 1.374(7) . ? C26 C27 1.392(7) . ? C27 C28 1.379(7) . ? C28 N5 1.362(6) . ? C101 O4 1.232(9) . ? C101 C102 1.404(10) . ? C101 C103 1.493(9) . ? N1 Ru1 2.130(5) . ? N2 Ru1 2.103(4) . ? N3 Ru1 2.088(4) . ? N4 Ru1 1.970(4) . ? N5 Ru1 2.064(4) . ? O1 P1 1.598(3) . ? O2 P1 1.604(4) . ? O3 P1 1.578(4) . ? F1 P2 1.567(3) . ? F2 P2 1.594(4) . ? F3 P2 1.577(4) . ? F4 P2 1.619(4) . ? F5 P2 1.593(4) . ? F6 P2 1.585(4) . ? F7 P3 1.579(4) . ? F8 P3 1.576(4) . ? F9 P3 1.586(4) . ? F10 P3 1.590(4) . ? F11 P3 1.577(4) . ? F12 P3 1.564(4) . ? P1 Ru1 2.2448(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C4 C5 122.4(5) . . ? C6 C5 C4 118.6(6) . . ? C5 C6 C7 118.7(5) . . ? C8 C7 C6 120.4(6) . . ? C7 C8 N1 121.3(6) . . ? C7 C8 C9 123.5(5) . . ? N1 C8 C9 115.2(4) . . ? N2 C9 C10 120.1(5) . . ? N2 C9 C8 116.4(4) . . ? C10 C9 C8 123.5(5) . . ? C11 C10 C9 121.2(6) . . ? C10 C11 C12 119.5(6) . . ? C11 C12 C13 118.2(6) . . ? N2 C13 C12 123.3(5) . . ? N3 C14 C15 123.2(5) . . ? C16 C15 C14 118.0(5) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 119.2(5) . . ? N3 C18 C17 120.9(5) . . ? N3 C18 C19 115.6(4) . . ? C17 C18 C19 123.4(5) . . ? N4 C19 C20 120.0(5) . . ? N4 C19 C18 113.0(4) . . ? C20 C19 C18 127.0(5) . . ? C21 C20 C19 118.9(5) . . ? C20 C21 C22 120.9(5) . . ? C23 C22 C21 117.9(5) . . ? N4 C23 C22 120.9(4) . . ? N4 C23 C24 113.1(4) . . ? C22 C23 C24 125.9(5) . . ? C25 C24 N5 122.3(5) . . ? C25 C24 C23 123.6(5) . . ? N5 C24 C23 114.0(4) . . ? C24 C25 C26 120.0(5) . . ? C25 C26 C27 118.4(5) . . ? C28 C27 C26 120.3(5) . . ? N5 C28 C27 121.8(5) . . ? O4 C101 C102 121.2(7) . . ? O4 C101 C103 122.0(6) . . ? C102 C101 C103 116.8(7) . . ? C4 N1 C8 118.6(5) . . ? C4 N1 Ru1 126.4(3) . . ? C8 N1 Ru1 115.0(4) . . ? C13 N2 C9 117.7(4) . . ? C13 N2 Ru1 127.1(3) . . ? C9 N2 Ru1 115.2(4) . . ? C14 N3 C18 118.8(5) . . ? C14 N3 Ru1 129.1(4) . . ? C18 N3 Ru1 112.1(3) . . ? C19 N4 C23 121.4(4) . . ? C19 N4 Ru1 119.2(3) . . ? C23 N4 Ru1 119.2(3) . . ? C28 N5 C24 117.2(4) . . ? C28 N5 Ru1 128.8(3) . . ? C24 N5 Ru1 113.9(3) . . ? C1 O1 P1 122.0(3) . . ? C2 O2 P1 121.2(3) . . ? C3 O3 P1 127.5(3) . . ? O3 P1 O1 108.0(2) . . ? O3 P1 O2 99.5(2) . . ? O1 P1 O2 105.10(19) . . ? O3 P1 Ru1 111.59(14) . . ? O1 P1 Ru1 111.11(15) . . ? O2 P1 Ru1 120.42(14) . . ? F1 P2 F3 91.0(2) . . ? F1 P2 F6 90.7(2) . . ? F3 P2 F6 91.1(2) . . ? F1 P2 F5 89.9(2) . . ? F3 P2 F5 179.0(3) . . ? F6 P2 F5 88.3(2) . . ? F1 P2 F2 178.2(3) . . ? F3 P2 F2 89.8(3) . . ? F6 P2 F2 90.9(2) . . ? F5 P2 F2 89.4(3) . . ? F1 P2 F4 90.26(19) . . ? F3 P2 F4 89.94(19) . . ? F6 P2 F4 178.5(2) . . ? F5 P2 F4 90.6(2) . . ? F2 P2 F4 88.1(2) . . ? F12 P3 F8 91.8(3) . . ? F12 P3 F11 177.9(3) . . ? F8 P3 F11 89.8(3) . . ? F12 P3 F7 89.8(3) . . ? F8 P3 F7 178.3(3) . . ? F11 P3 F7 88.6(3) . . ? F12 P3 F9 90.7(3) . . ? F8 P3 F9 91.0(2) . . ? F11 P3 F9 90.6(3) . . ? F7 P3 F9 88.5(3) . . ? F12 P3 F10 89.2(3) . . ? F8 P3 F10 88.5(2) . . ? F11 P3 F10 89.6(2) . . ? F7 P3 F10 92.0(2) . . ? F9 P3 F10 179.5(3) . . ? N4 Ru1 N5 79.58(16) . . ? N4 Ru1 N3 79.93(18) . . ? N5 Ru1 N3 159.45(16) . . ? N4 Ru1 N2 171.69(16) . . ? N5 Ru1 N2 101.96(16) . . ? N3 Ru1 N2 98.11(16) . . ? N4 Ru1 N1 93.68(17) . . ? N5 Ru1 N1 91.53(16) . . ? N3 Ru1 N1 88.30(16) . . ? N2 Ru1 N1 78.16(18) . . ? N4 Ru1 P1 92.11(12) . . ? N5 Ru1 P1 87.20(11) . . ? N3 Ru1 P1 95.03(12) . . ? N2 Ru1 P1 96.11(13) . . ? N1 Ru1 P1 173.76(14) . . ? #====END data_([Ru]4) _database_code_depnum_ccdc_archive 'CCDC 665734' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H34 N5 O3 P Ru, 2(F6 P)' _chemical_formula_sum 'C31 H34 F12 N5 O3 P3 Ru' _chemical_formula_weight 946.61 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.5612(6) _cell_length_b 14.9833(5) _cell_length_c 29.1467(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8979.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 10321 _cell_measurement_theta_min 2.4956 _cell_measurement_theta_max 32.1001 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'yellow ornage' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.4 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.54 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.958 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 0.0244010913 _diffrn_orient_matrix_ub_12 -0.0142161736 _diffrn_orient_matrix_ub_13 -0.018314043 _diffrn_orient_matrix_ub_21 0.016149154 _diffrn_orient_matrix_ub_22 0.0311713365 _diffrn_orient_matrix_ub_23 -0.006440146 _diffrn_orient_matrix_ub_31 0.0374289626 _diffrn_orient_matrix_ub_32 -0.0040761687 _diffrn_orient_matrix_ub_33 0.014705667 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_unetI/netI 0.1189 _diffrn_reflns_number 59297 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7915 _reflns_number_gt 3225 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Moreover, it was not possible to resolve properly diffuse electron-density residuals. Treatment with the SQUEEZE facility from PLATON, with a localized void of about 2106.3 A \^E 3 and 378 recovered electrons resulted in a smooth refinement. Since a few low order reflections are missing from the data set, the electron count is underestimated. Consequently, the values given for rcalc, F(000) and the molecular weight are only valid for the ordered part of the structure. ; _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^)+(0.1110P)^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_number_reflns 7915 _refine_ls_number_parameters 500 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.386 _refine_diff_density_min -0.8 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C7 C 0.5235(4) 0.4767(5) 0.1170(3) 0.035(2) Uani 1 1 d . . . H7 H 0.5599 0.4476 0.1055 0.041 Uiso 1 1 calc R . . C8 C 0.5217(4) 0.5653(5) 0.1142(3) 0.039(2) Uani 1 1 d . . . H8 H 0.5579 0.5966 0.1039 0.047 Uiso 1 1 calc R . . C9 C 0.4662(5) 0.6108(7) 0.1266(3) 0.056(3) Uani 1 1 d . . . H9 H 0.4622 0.6722 0.1227 0.067 Uiso 1 1 calc R . . C10 C 0.4172(4) 0.5599(6) 0.1449(3) 0.044(2) Uani 1 1 d . . . H10 H 0.3793 0.5878 0.1548 0.053 Uiso 1 1 calc R . . C11 C 0.4227(4) 0.4694(5) 0.1490(2) 0.0298(19) Uani 1 1 d . . . C12 C 0.3738(4) 0.4086(6) 0.1696(2) 0.034(2) Uani 1 1 d . . . C13A C 0.3188(4) 0.4400(6) 0.1923(3) 0.051(2) Uani 1 1 d . . . H13 H 0.3108 0.5011 0.193 0.061 Uiso 1 1 calc R . . C14 C 0.2773(4) 0.3845(6) 0.2132(3) 0.037(2) Uani 1 1 d . . . H14 H 0.2406 0.4057 0.2284 0.045 Uiso 1 1 calc R . . C15 C 0.2915(4) 0.2933(6) 0.2113(2) 0.037(2) Uani 1 1 d . . . H15 H 0.2635 0.2526 0.2251 0.044 Uiso 1 1 calc R . . C16 C 0.3466(4) 0.2630(5) 0.1891(3) 0.032(2) Uani 1 1 d . . . H16 H 0.3556 0.2022 0.1886 0.039 Uiso 1 1 calc R . . C17 C 0.5124(4) 0.2912(5) 0.2398(2) 0.033(2) Uani 1 1 d . . . H17 H 0.468 0.292 0.2459 0.04 Uiso 1 1 calc R . . C18 C 0.5552(4) 0.2917(5) 0.2765(2) 0.0286(18) Uani 1 1 d . . . H18 H 0.5393 0.2943 0.3064 0.034 Uiso 1 1 calc R . . C19 C 0.6199(4) 0.2885(5) 0.2689(3) 0.038(2) Uani 1 1 d . . . H19 H 0.6494 0.2904 0.2931 0.046 Uiso 1 1 calc R . . C20 C 0.6409(4) 0.2822(5) 0.2241(3) 0.038(2) Uani 1 1 d . . . H20 H 0.6852 0.2769 0.218 0.045 Uiso 1 1 calc R . . C21 C 0.5963(3) 0.2837(5) 0.1873(2) 0.0282(18) Uani 1 1 d . . . C22 C 0.6164(3) 0.2775(5) 0.1387(2) 0.0234(17) Uani 1 1 d . . . C23 C 0.6767(4) 0.2746(6) 0.1205(3) 0.038(2) Uani 1 1 d . . . H23 H 0.713 0.2766 0.1395 0.046 Uiso 1 1 calc R . . C24 C 0.6841(4) 0.2686(7) 0.0739(3) 0.057(3) Uani 1 1 d . . . H24 H 0.7257 0.2681 0.0613 0.068 Uiso 1 1 calc R . . C25 C 0.6317(4) 0.2635(6) 0.0459(2) 0.039(2) Uani 1 1 d . . . H25 H 0.6372 0.256 0.0144 0.046 Uiso 1 1 calc R . . C26 C 0.5685(4) 0.2695(5) 0.0648(2) 0.034(2) Uani 1 1 d . . . C27 C 0.5074(3) 0.2696(5) 0.0411(3) 0.030(2) Uani 1 1 d . . . C28 C 0.4988(5) 0.2579(7) -0.0062(3) 0.056(3) Uani 1 1 d . . . H28 H 0.5348 0.2485 -0.0249 0.067 Uiso 1 1 calc R . . C29 C 0.4391(4) 0.2602(6) -0.0247(3) 0.039(2) Uani 1 1 d . . . H29 H 0.434 0.2508 -0.056 0.047 Uiso 1 1 calc R . . C30 C 0.3848(4) 0.2765(5) 0.0023(3) 0.033(2) Uani 1 1 d . . . H30 H 0.3436 0.2811 -0.0106 0.04 Uiso 1 1 calc R . . C31 C 0.3941(4) 0.2858(5) 0.0492(2) 0.0291(19) Uani 1 1 d . . . H31 H 0.3583 0.2962 0.0679 0.035 Uiso 1 1 calc R . . N1 N 0.4769(3) 0.4279(4) 0.13497(18) 0.0252(14) Uani 1 1 d . A . N2 N 0.3876(3) 0.3205(5) 0.1683(2) 0.0342(16) Uani 1 1 d . A . N3 N 0.5320(3) 0.2897(4) 0.19596(19) 0.0267(15) Uani 1 1 d . A . N4 N 0.5628(3) 0.2743(4) 0.1109(2) 0.0332(16) Uani 1 1 d . A . N5 N 0.4535(3) 0.2802(4) 0.06845(19) 0.0244(14) Uani 1 1 d . A . O1 O 0.4060(3) 0.0828(4) 0.1468(2) 0.068(2) Uani 1 1 d . . . C1A C 0.3581(17) 0.068(3) 0.113(3) 0.069(4) Uani 0.35 1 d PD A 1 H1A1 H 0.3747 0.018 0.0953 0.083 Uiso 0.35 1 calc PR A 1 H1A2 H 0.3616 0.1194 0.0928 0.083 Uiso 0.35 1 calc PR A 1 C2A C 0.2864(15) 0.051(3) 0.1159(11) 0.069(4) Uani 0.35 1 d PD A 1 H2A1 H 0.2928 -0.0075 0.123 0.104 Uiso 0.35 1 d P B 1 H2A2 H 0.2643 0.0602 0.0873 0.104 Uiso 0.35 1 d P C 1 H2A3 H 0.2635 0.0834 0.1397 0.104 Uiso 0.35 1 d P D 1 C1B C 0.3599(11) 0.0946(15) 0.1120(13) 0.069(4) Uani 0.65 1 d P A 2 H1B1 H 0.3723 0.0664 0.0834 0.083 Uiso 0.65 1 calc PR A 2 H1B2 H 0.3488 0.1567 0.107 0.083 Uiso 0.65 1 calc PR A 2 C2B C 0.3028(8) 0.0390(13) 0.1400(6) 0.069(4) Uani 0.65 1 d P A 2 H2B1 H 0.3168 -0.009 0.1589 0.104 Uiso 0.65 1 d P E 2 H2B2 H 0.2702 0.0154 0.1182 0.104 Uiso 0.65 1 d P F 2 H2B3 H 0.2825 0.0844 0.1577 0.104 Uiso 0.65 1 d P G 2 O2 O 0.5092(4) 0.1005(5) 0.1858(2) 0.073(2) Uani 1 1 d . . . C5A C 0.5019(13) 0.0186(19) 0.2101(10) 0.067(4) Uani 0.68 1 d P A 1 H5A1 H 0.5439 -0.0054 0.2187 0.08 Uiso 0.68 1 calc PR A 1 H5A2 H 0.4793 -0.0251 0.1914 0.08 Uiso 0.68 1 calc PR A 1 C6A C 0.4618(8) 0.0420(11) 0.2528(5) 0.067(4) Uani 0.68 1 d P A 1 H6A1 H 0.4877 0.0775 0.2733 0.101 Uiso 0.68 1 calc PR A 1 H6A2 H 0.4488 -0.0119 0.2681 0.101 Uiso 0.68 1 calc PR A 1 H6A3 H 0.4239 0.0751 0.2439 0.101 Uiso 0.68 1 calc PR A 1 C5B C 0.482(3) 0.032(4) 0.210(2) 0.067(4) Uani 0.32 1 d P A 2 H5B1 H 0.4913 -0.0233 0.1937 0.08 Uiso 0.32 1 calc PR A 2 H5B2 H 0.4357 0.04 0.2106 0.08 Uiso 0.32 1 calc PR A 2 C6B C 0.5046(19) 0.024(3) 0.2543(12) 0.067(4) Uani 0.32 1 d P A 2 H6B1 H 0.5511 0.029 0.2547 0.101 Uiso 0.32 1 calc PR A 2 H6B2 H 0.4922 -0.0335 0.2663 0.101 Uiso 0.32 1 calc PR A 2 H6B3 H 0.4859 0.07 0.2729 0.101 Uiso 0.32 1 calc PR A 2 O3 O 0.5085(3) 0.0941(4) 0.09996(18) 0.0482(16) Uani 1 1 d . . . C3A C 0.526(3) 0.008(4) 0.0850(15) 0.061(5) Uani 0.39 1 d PD A 1 H3A1 H 0.4872 -0.0226 0.0753 0.074 Uiso 0.39 1 calc PR A 1 H3A2 H 0.544 -0.024 0.1109 0.074 Uiso 0.39 1 calc PR A 1 C4A C 0.575(3) 0.005(3) 0.0464(16) 0.061(5) Uani 0.39 1 d PD A 1 H4A1 H 0.5524 0.0075 0.0176 0.092 Uiso 0.39 1 calc PR A 1 H4A2 H 0.5994 -0.0493 0.0483 0.092 Uiso 0.39 1 calc PR A 1 H4A3 H 0.6039 0.0552 0.0488 0.092 Uiso 0.39 1 calc PR A 1 C3B C 0.524(2) 0.004(2) 0.0976(9) 0.061(5) Uani 0.61 1 d P A 2 H3B1 H 0.4839 -0.0308 0.0948 0.074 Uiso 0.61 1 calc PR A 2 H3B2 H 0.5457 -0.0144 0.1254 0.074 Uiso 0.61 1 calc PR A 2 C4B C 0.5651(16) -0.0123(18) 0.0581(9) 0.061(5) Uani 0.61 1 d P A 2 H4B1 H 0.5453 0.0127 0.0312 0.092 Uiso 0.61 1 calc PR A 2 H4B2 H 0.5707 -0.0754 0.0541 0.092 Uiso 0.61 1 calc PR A 2 H4B3 H 0.6067 0.0152 0.0631 0.092 Uiso 0.61 1 calc PR A 2 F1 F 0.2111(4) 0.2099(4) 0.1215(3) 0.111(3) Uani 1 1 d . . . F2 F 0.1701(3) 0.3581(4) 0.0507(2) 0.086(2) Uani 1 1 d . . . F3 F 0.2529(2) 0.3403(4) 0.10096(17) 0.0702(17) Uani 1 1 d . . . F4 F 0.1325(3) 0.2235(4) 0.06828(16) 0.0680(16) Uani 1 1 d . . . F5 F 0.2339(3) 0.2402(6) 0.0465(2) 0.115(3) Uani 1 1 d . . . F6 F 0.1490(3) 0.3269(6) 0.1249(2) 0.117(3) Uani 1 1 d . . . F7 F 0.3917(2) 0.3587(3) 0.30371(15) 0.0510(13) Uani 1 1 d . . . F8 F 0.3483(2) 0.2141(3) 0.37799(15) 0.0506(13) Uani 1 1 d . . . F9 F 0.4379(2) 0.2967(3) 0.36525(14) 0.0526(14) Uani 1 1 d . . . F10 F 0.3018(2) 0.2761(4) 0.31585(16) 0.0696(18) Uani 1 1 d . . . F11 F 0.3406(3) 0.3633(4) 0.37239(17) 0.0676(16) Uani 1 1 d . . . F12 F 0.3998(2) 0.2115(3) 0.30937(16) 0.0528(14) Uani 1 1 d . . . P1 P 0.47151(10) 0.13673(14) 0.14114(6) 0.0289(5) Uani 1 1 d . A . P2 P 0.19160(11) 0.28489(17) 0.08547(7) 0.0423(6) Uani 1 1 d . . . P3 P 0.36968(10) 0.28676(16) 0.34073(7) 0.0351(6) Uani 1 1 d . . . Ru1 Ru 0.47608(3) 0.28584(4) 0.137659(19) 0.0242(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C7 0.035(5) 0.038(5) 0.031(5) -0.001(4) 0.006(4) 0.011(4) C8 0.048(6) 0.029(5) 0.040(5) 0.002(4) -0.002(4) -0.010(5) C9 0.085(8) 0.045(6) 0.039(5) 0.014(5) 0.003(5) -0.021(6) C10 0.046(6) 0.047(6) 0.039(5) 0.002(4) -0.003(4) 0.014(5) C11 0.037(5) 0.026(5) 0.026(4) -0.009(3) -0.006(4) -0.007(4) C12 0.039(5) 0.038(5) 0.024(4) -0.015(4) -0.008(4) 0.003(4) C13A 0.044(5) 0.045(6) 0.064(7) 0.004(5) 0.009(5) 0.002(5) C14 0.034(5) 0.040(6) 0.037(5) -0.011(4) 0.006(4) 0.000(4) C15 0.028(4) 0.066(6) 0.017(4) -0.007(4) 0.003(3) -0.030(5) C16 0.042(5) 0.030(5) 0.025(4) -0.003(4) -0.006(4) -0.007(4) C17 0.021(4) 0.058(6) 0.020(4) 0.003(4) 0.005(3) -0.003(4) C18 0.039(5) 0.036(5) 0.011(4) -0.003(3) -0.002(3) -0.002(4) C19 0.046(6) 0.043(5) 0.025(5) 0.010(4) -0.008(4) 0.001(5) C20 0.030(5) 0.051(6) 0.032(5) -0.005(4) -0.006(4) -0.001(4) C21 0.027(4) 0.032(5) 0.026(4) 0.008(3) 0.000(3) 0.007(4) C22 0.013(4) 0.031(5) 0.025(4) -0.001(3) 0.004(3) -0.008(3) C23 0.026(5) 0.064(6) 0.025(4) -0.002(4) -0.013(4) 0.010(4) C24 0.040(5) 0.097(8) 0.033(5) -0.006(5) 0.003(4) 0.000(5) C25 0.030(5) 0.074(6) 0.012(4) -0.004(4) 0.010(4) -0.007(4) C26 0.042(5) 0.042(6) 0.017(4) -0.004(4) 0.006(4) -0.006(4) C27 0.016(4) 0.049(6) 0.026(4) -0.005(4) 0.012(3) -0.008(4) C28 0.060(6) 0.085(8) 0.022(5) 0.011(5) -0.003(5) -0.009(6) C29 0.048(6) 0.060(6) 0.010(4) -0.003(4) 0.001(4) -0.015(5) C30 0.026(4) 0.039(5) 0.034(5) -0.005(4) -0.001(4) -0.025(4) C31 0.042(5) 0.027(4) 0.018(4) -0.001(3) -0.011(3) -0.014(4) N1 0.019(3) 0.038(4) 0.019(3) -0.002(3) -0.001(3) -0.001(3) N2 0.033(4) 0.046(4) 0.024(4) -0.005(3) -0.008(3) -0.004(4) N3 0.017(3) 0.047(4) 0.016(3) -0.001(3) 0.009(2) 0.003(3) N4 0.028(4) 0.041(4) 0.031(4) 0.002(3) 0.008(3) 0.002(3) N5 0.037(4) 0.014(3) 0.022(3) 0.010(3) -0.009(3) -0.012(3) O1 0.075(5) 0.057(5) 0.070(5) 0.004(4) 0.023(4) -0.013(4) C1A 0.073(7) 0.077(10) 0.057(7) -0.014(10) -0.028(5) -0.002(6) C2A 0.073(7) 0.077(10) 0.057(7) -0.014(10) -0.028(5) -0.002(6) C1B 0.073(7) 0.077(10) 0.057(7) -0.014(10) -0.028(5) -0.002(6) C2B 0.073(7) 0.077(10) 0.057(7) -0.014(10) -0.028(5) -0.002(6) O2 0.109(6) 0.064(5) 0.046(4) 0.009(4) 0.010(4) 0.018(5) C5A 0.103(15) 0.055(8) 0.043(5) 0.007(5) -0.001(9) 0.030(8) C6A 0.103(15) 0.055(8) 0.043(5) 0.007(5) -0.001(9) 0.030(8) C5B 0.103(15) 0.055(8) 0.043(5) 0.007(5) -0.001(9) 0.030(8) C6B 0.103(15) 0.055(8) 0.043(5) 0.007(5) -0.001(9) 0.030(8) O3 0.075(4) 0.032(4) 0.038(3) -0.007(3) 0.014(3) 0.003(3) C3A 0.104(10) 0.037(7) 0.044(14) 0.004(9) 0.034(10) 0.008(6) C4A 0.104(10) 0.037(7) 0.044(14) 0.004(9) 0.034(10) 0.008(6) C3B 0.104(10) 0.037(7) 0.044(14) 0.004(9) 0.034(10) 0.008(6) C4B 0.104(10) 0.037(7) 0.044(14) 0.004(9) 0.034(10) 0.008(6) F1 0.138(7) 0.085(5) 0.109(6) 0.031(4) -0.076(5) -0.019(5) F2 0.116(5) 0.072(4) 0.071(4) 0.026(3) -0.033(4) -0.010(4) F3 0.053(3) 0.099(4) 0.059(3) -0.018(3) -0.001(3) -0.033(3) F4 0.077(4) 0.087(4) 0.040(3) 0.009(3) -0.017(3) -0.034(3) F5 0.068(4) 0.191(7) 0.085(5) -0.076(5) 0.008(4) -0.013(5) F6 0.082(5) 0.208(8) 0.060(4) -0.033(5) 0.016(4) -0.029(5) F7 0.048(3) 0.069(3) 0.037(3) 0.020(2) 0.012(2) 0.006(3) F8 0.047(3) 0.071(4) 0.034(3) 0.013(2) 0.006(2) -0.006(3) F9 0.035(3) 0.093(4) 0.030(3) -0.008(3) -0.005(2) -0.008(3) F10 0.036(3) 0.143(6) 0.030(3) 0.012(3) -0.007(2) -0.007(3) F11 0.076(4) 0.082(4) 0.044(3) -0.004(3) 0.031(3) 0.014(3) F12 0.059(3) 0.058(3) 0.042(3) -0.007(2) 0.016(2) -0.010(3) P1 0.0372(12) 0.0264(12) 0.0230(11) 0.0006(9) 0.0072(9) 0.0046(10) P2 0.0412(14) 0.0617(17) 0.0238(12) 0.0009(11) -0.0078(10) -0.0050(13) P3 0.0293(12) 0.0599(16) 0.0161(10) -0.0030(10) 0.0017(9) -0.0032(12) Ru1 0.0220(4) 0.0350(4) 0.0154(3) 0.0030(3) 0.0014(3) 0.0000(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C7 N1 1.314(9) . ? C7 C8 1.331(11) . ? C8 C9 1.376(12) . ? C9 C10 1.371(11) . ? C10 C11 1.367(11) . ? C11 N1 1.340(9) . ? C11 C12 1.484(10) . ? C12 N2 1.351(10) . ? C12 C13A 1.392(11) . ? C13A C14 1.339(11) . ? C14 C15 1.398(11) . ? C15 C16 1.380(11) . ? C16 N2 1.350(9) . ? C17 N3 1.340(9) . ? C17 C18 1.386(10) . ? C18 C19 1.350(11) . ? C19 C20 1.380(10) . ? C20 C21 1.412(10) . ? C21 N3 1.349(9) . ? C21 C22 1.477(9) . ? C22 C23 1.349(10) . ? C22 N4 1.370(9) . ? C23 C24 1.370(11) . ? C24 C25 1.355(11) . ? C25 C26 1.415(10) . ? C26 N4 1.349(9) . ? C26 C27 1.434(11) . ? C27 N5 1.373(9) . ? C27 C28 1.401(11) . ? C28 C29 1.341(11) . ? C29 C30 1.387(10) . ? C30 C31 1.386(10) . ? C31 N5 1.348(9) . ? N1 Ru1 2.130(6) . ? N2 Ru1 2.092(6) . ? N3 Ru1 2.053(6) . ? N4 Ru1 1.953(6) . ? N5 Ru1 2.071(6) . ? O1 C1B 1.40(3) . ? O1 C1A 1.41(6) . ? O1 P1 1.579(7) . ? C1A C2A 1.497(10) . ? C1B C2B 1.65(3) . ? O2 C5B 1.36(8) . ? O2 C5A 1.43(3) . ? O2 P1 1.609(7) . ? C5A C6A 1.53(3) . ? C5B C6B 1.38(8) . ? O3 C3B 1.39(4) . ? O3 C3A 1.40(6) . ? O3 P1 1.558(6) . ? C3A C4A 1.507(10) . ? C3B C4B 1.45(2) . ? F1 P2 1.590(6) . ? F2 P2 1.558(6) . ? F3 P2 1.575(5) . ? F4 P2 1.604(5) . ? F5 P2 1.580(6) . ? F6 P2 1.577(7) . ? F7 P3 1.590(5) . ? F8 P3 1.600(5) . ? F9 P3 1.582(5) . ? F10 P3 1.581(5) . ? F11 P3 1.589(5) . ? F12 P3 1.578(5) . ? P1 Ru1 2.238(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 N1 C7 C8 124.0(8) . . ? C7 C8 C9 120.1(8) . . ? C10 C9 C8 115.8(9) . . ? C11 C10 C9 121.7(8) . . ? N1 C11 C10 120.2(7) . . ? N1 C11 C12 113.7(7) . . ? C10 C11 C12 126.1(8) . . ? N2 C12 C13A 121.0(8) . . ? N2 C12 C11 116.5(7) . . ? C13A C12 C11 122.3(8) . . ? C14 C13A C12 121.7(9) . . ? C13A C14 C15 117.0(8) . . ? C16 C15 C14 120.9(7) . . ? N2 C16 C15 120.8(7) . . ? N3 C17 C18 123.1(7) . . ? C19 C18 C17 119.9(7) . . ? C18 C19 C20 117.8(7) . . ? C19 C20 C21 121.0(7) . . ? N3 C21 C20 119.7(7) . . ? N3 C21 C22 117.3(6) . . ? C20 C21 C22 123.1(7) . . ? C23 C22 N4 120.4(6) . . ? C23 C22 C21 129.4(7) . . ? N4 C22 C21 110.1(6) . . ? C22 C23 C24 119.6(7) . . ? C25 C24 C23 120.9(8) . . ? C24 C25 C26 119.4(7) . . ? N4 C26 C25 118.2(7) . . ? N4 C26 C27 113.7(7) . . ? C25 C26 C27 128.0(7) . . ? N5 C27 C28 119.0(7) . . ? N5 C27 C26 115.3(7) . . ? C28 C27 C26 125.8(7) . . ? C29 C28 C27 120.4(9) . . ? C28 C29 C30 120.9(7) . . ? C31 C30 C29 117.7(7) . . ? N5 C31 C30 122.0(7) . . ? C7 N1 C11 118.0(7) . . ? C7 N1 Ru1 125.2(5) . . ? C11 N1 Ru1 116.5(5) . . ? C16 N2 C12 118.7(7) . . ? C16 N2 Ru1 125.2(6) . . ? C12 N2 Ru1 115.9(5) . . ? C17 N3 C21 118.4(6) . . ? C17 N3 Ru1 128.4(5) . . ? C21 N3 Ru1 113.1(5) . . ? C26 N4 C22 121.3(7) . . ? C26 N4 Ru1 118.8(6) . . ? C22 N4 Ru1 119.7(5) . . ? C31 N5 C27 119.7(6) . . ? C31 N5 Ru1 127.3(5) . . ? C27 N5 Ru1 112.9(5) . . ? C1B O1 P1 115.9(10) . . ? C1A O1 P1 127(2) . . ? O1 C1A C2A 132(5) . . ? O1 C1B C2B 93(2) . . ? C5B O2 P1 118(3) . . ? C5A O2 P1 129.9(14) . . ? O2 C5A C6A 105.3(16) . . ? O2 C5B C6B 115(6) . . ? C3B O3 P1 123.1(12) . . ? C3A O3 P1 137.7(19) . . ? O3 C3A C4A 116(3) . . ? O3 C3B C4B 109(2) . . ? O3 P1 O1 106.7(3) . . ? O3 P1 O2 104.4(3) . . ? O1 P1 O2 98.8(4) . . ? O3 P1 Ru1 110.7(2) . . ? O1 P1 Ru1 123.5(3) . . ? O2 P1 Ru1 110.7(3) . . ? F2 P2 F3 92.4(3) . . ? F2 P2 F6 92.0(4) . . ? F3 P2 F6 91.4(3) . . ? F2 P2 F5 89.2(4) . . ? F3 P2 F5 89.4(3) . . ? F6 P2 F5 178.5(5) . . ? F2 P2 F1 178.2(4) . . ? F3 P2 F1 88.9(3) . . ? F6 P2 F1 86.6(5) . . ? F5 P2 F1 92.1(5) . . ? F2 P2 F4 89.2(3) . . ? F3 P2 F4 176.1(4) . . ? F6 P2 F4 92.1(3) . . ? F5 P2 F4 87.1(3) . . ? F1 P2 F4 89.6(3) . . ? F12 P3 F10 90.5(3) . . ? F12 P3 F9 88.9(3) . . ? F10 P3 F9 179.4(3) . . ? F12 P3 F11 179.0(3) . . ? F10 P3 F11 90.4(3) . . ? F9 P3 F11 90.2(3) . . ? F12 P3 F7 88.8(3) . . ? F10 P3 F7 90.5(3) . . ? F9 P3 F7 89.5(3) . . ? F11 P3 F7 90.7(3) . . ? F12 P3 F8 90.8(3) . . ? F10 P3 F8 90.0(3) . . ? F9 P3 F8 90.1(3) . . ? F11 P3 F8 89.6(3) . . ? F7 P3 F8 179.4(3) . . ? N4 Ru1 N3 79.7(2) . . ? N4 Ru1 N5 79.1(3) . . ? N3 Ru1 N5 158.8(2) . . ? N4 Ru1 N2 170.4(3) . . ? N3 Ru1 N2 97.3(2) . . ? N5 Ru1 N2 103.3(2) . . ? N4 Ru1 N1 93.8(2) . . ? N3 Ru1 N1 89.9(2) . . ? N5 Ru1 N1 90.4(2) . . ? N2 Ru1 N1 77.0(2) . . ? N4 Ru1 P1 88.16(18) . . ? N3 Ru1 P1 90.83(18) . . ? N5 Ru1 P1 89.66(16) . . ? N2 Ru1 P1 101.1(2) . . ? N1 Ru1 P1 177.98(17) . . ? #====END data_([Ru]5) _database_code_depnum_ccdc_archive 'CCDC 665735' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H40 N5 O3 P Ru, 2(F6 P), 2(C3 H6 O)' _chemical_formula_sum 'C40 H52 F12 N5 O5 P3 Ru' _chemical_formula_weight 1104.85 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 22.5924(9) _cell_length_b 13.7879(7) _cell_length_c 15.3670(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4786.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used 9730 _cell_measurement_theta_min 2.6993 _cell_measurement_theta_max 32.1231 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8691 _exptl_absorpt_correction_T_max 0.9656 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_unetI/netI 0.0494 _diffrn_reflns_number 33474 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8910 _reflns_number_gt 7450 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0894P)^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_number_reflns 8910 _refine_ls_number_parameters 622 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_diff_density_max 0.798 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.7007(3) 0.4685(5) 0.5962(4) 0.0443(15) Uani 1 1 d . . . H1 H 0.7242 0.4927 0.5472 0.053 Uiso 1 1 calc R . . C2 C 0.6463(3) 0.5292(6) 0.6069(5) 0.065(2) Uani 1 1 d . . . H2A H 0.6175 0.494 0.6402 0.097 Uiso 1 1 calc R . . H2B H 0.6303 0.5444 0.5507 0.097 Uiso 1 1 calc R . . H2C H 0.6564 0.5882 0.6367 0.097 Uiso 1 1 calc R . . C3 C 0.6871(4) 0.3619(5) 0.5832(5) 0.068(2) Uani 1 1 d . . . H3A H 0.7225 0.3246 0.5915 0.102 Uiso 1 1 calc R . . H3B H 0.6723 0.3518 0.5253 0.102 Uiso 1 1 calc R . . H3C H 0.6577 0.3418 0.6246 0.102 Uiso 1 1 calc R . . C4 C 0.7927(3) 0.7305(4) 0.6479(4) 0.0477(15) Uani 1 1 d . . . H4 H 0.8047 0.7407 0.7085 0.057 Uiso 1 1 calc R . . C5 C 0.7422(4) 0.7967(5) 0.6273(5) 0.069(2) Uani 1 1 d . . . H5A H 0.7277 0.7829 0.57 0.103 Uiso 1 1 calc R . . H5B H 0.7554 0.8628 0.6299 0.103 Uiso 1 1 calc R . . H5C H 0.711 0.787 0.6689 0.103 Uiso 1 1 calc R . . C6 C 0.8451(4) 0.7457(7) 0.5899(5) 0.082(3) Uani 1 1 d . . . H6A H 0.871 0.6907 0.5937 0.122 Uiso 1 1 calc R . . H6B H 0.866 0.803 0.6078 0.122 Uiso 1 1 calc R . . H6C H 0.8319 0.7533 0.5309 0.122 Uiso 1 1 calc R . . C10 C 0.9030(2) 0.6395(4) 0.8275(4) 0.0380(13) Uani 1 1 d . . . H10 H 0.8945 0.6381 0.7683 0.046 Uiso 1 1 calc R . . C11 C 0.9597(2) 0.6648(4) 0.8533(5) 0.0432(12) Uani 1 1 d . . . H11 H 0.989 0.6774 0.8123 0.052 Uiso 1 1 calc R . . C12 C 0.9714(3) 0.6708(4) 0.9398(4) 0.0460(15) Uani 1 1 d . . . H12 H 1.009 0.6891 0.9584 0.055 Uiso 1 1 calc R . . C13 C 0.9279(2) 0.6499(4) 1.0005(4) 0.0405(13) Uani 1 1 d . . . H13 H 0.9357 0.6538 1.0598 0.049 Uiso 1 1 calc R . . C14 C 0.8722(2) 0.6230(3) 0.9702(3) 0.0271(10) Uani 1 1 d . . . C15 C 0.8238(2) 0.6016(3) 1.0296(3) 0.0268(11) Uani 1 1 d . . . C16 C 0.8280(3) 0.6029(4) 1.1194(4) 0.0403(13) Uani 1 1 d . . . H16 H 0.8646 0.6138 1.1455 0.048 Uiso 1 1 calc R . . C17 C 0.7789(3) 0.5883(4) 1.1705(4) 0.0429(15) Uani 1 1 d . . . H17 H 0.7821 0.5879 1.2309 0.051 Uiso 1 1 calc R . . C18 C 0.7246(3) 0.5741(4) 1.1308(4) 0.0425(15) Uani 1 1 d . . . H18 H 0.6902 0.5671 1.1634 0.051 Uiso 1 1 calc R . . C19 C 0.7235(2) 0.5709(4) 1.0415(4) 0.0357(13) Uani 1 1 d . . . H19 H 0.6873 0.5597 1.0144 0.043 Uiso 1 1 calc R . . C20 C 0.7479(2) 0.7930(4) 0.8595(5) 0.0362(11) Uani 1 1 d . . . H20 H 0.7885 0.8019 0.8651 0.043 Uiso 1 1 calc R . . C21 C 0.7124(3) 0.8728(4) 0.8601(6) 0.0551(16) Uani 1 1 d . . . H21 H 0.7288 0.9345 0.8642 0.066 Uiso 1 1 calc R . . C22 C 0.6527(3) 0.8617(4) 0.8547(6) 0.0595(17) Uani 1 1 d . . . H22 H 0.6278 0.9155 0.8571 0.071 Uiso 1 1 calc R . . C23 C 0.6292(2) 0.7690(4) 0.8456(5) 0.0466(14) Uani 1 1 d . . . H23 H 0.5886 0.7596 0.8399 0.056 Uiso 1 1 calc R . . C24 C 0.6676(2) 0.6915(4) 0.8452(4) 0.0343(12) Uani 1 1 d . . . C25 C 0.6462(2) 0.5905(4) 0.8398(4) 0.0339(13) Uani 1 1 d . . . C26 C 0.5880(2) 0.5579(5) 0.8347(4) 0.0463(17) Uani 1 1 d . . . H26 H 0.557 0.602 0.8299 0.056 Uiso 1 1 calc R . . C27 C 0.5768(2) 0.4598(5) 0.8370(4) 0.0500(17) Uani 1 1 d . . . H27 H 0.5381 0.4374 0.8328 0.06 Uiso 1 1 calc R . . C28 C 0.6233(2) 0.3939(5) 0.8455(5) 0.0475(14) Uani 1 1 d . . . H28 H 0.616 0.3275 0.8473 0.057 Uiso 1 1 calc R . . C29 C 0.6805(2) 0.4294(3) 0.8511(6) 0.0320(9) Uani 1 1 d . . . C30 C 0.7357(2) 0.3709(3) 0.8558(5) 0.0359(11) Uani 1 1 d . . . C31 C 0.7356(3) 0.2699(4) 0.8591(6) 0.0505(15) Uani 1 1 d . . . H31 H 0.7003 0.2353 0.8577 0.061 Uiso 1 1 calc R . . C32 C 0.7890(4) 0.2228(4) 0.8643(6) 0.064(2) Uani 1 1 d . . . H32 H 0.7901 0.1555 0.8666 0.077 Uiso 1 1 calc R . . C33 C 0.8414(3) 0.2753(4) 0.8661(5) 0.0539(17) Uani 1 1 d . . . H33 H 0.8777 0.2436 0.8676 0.065 Uiso 1 1 calc R . . C34 C 0.8389(2) 0.3750(4) 0.8658(4) 0.0422(14) Uani 1 1 d . . . H34 H 0.874 0.4101 0.8684 0.051 Uiso 1 1 calc R . . C50 C 0.9516(3) 0.1054(5) 0.5698(4) 0.0509(16) Uani 1 1 d . . . C51 C 0.9552(4) 0.0003(6) 0.5667(6) 0.080(2) Uani 1 1 d . . . H51A H 0.925 -0.0244 0.5287 0.119 Uiso 1 1 calc R . . H51B H 0.9497 -0.0256 0.6241 0.119 Uiso 1 1 calc R . . H51C H 0.9934 -0.0186 0.5451 0.119 Uiso 1 1 calc R . . C52 C 0.9939(4) 0.1546(7) 0.6271(6) 0.083(3) Uani 1 1 d . . . H52A H 0.983 0.2216 0.6328 0.124 Uiso 1 1 calc R . . H52B H 1.0329 0.15 0.6026 0.124 Uiso 1 1 calc R . . H52C H 0.9934 0.1243 0.6833 0.124 Uiso 1 1 calc R . . C53 C 0.0516(3) 0.7027(6) 0.6142(5) 0.0601(18) Uani 1 1 d . . . C54 C 0.0779(5) 0.6110(7) 0.5878(8) 0.112(4) Uani 1 1 d . . . H54A H 0.1196 0.6196 0.5785 0.168 Uiso 1 1 calc R . . H54B H 0.0596 0.5891 0.5349 0.168 Uiso 1 1 calc R . . H54C H 0.0717 0.5636 0.6327 0.168 Uiso 1 1 calc R . . C55 C 0.0378(8) 0.7702(8) 0.5366(8) 0.155(6) Uani 1 1 d . . . H55A H 0.0021 0.8058 0.5484 0.232 Uiso 1 1 calc R . . H55B H 0.0326 0.732 0.4849 0.232 Uiso 1 1 calc R . . H55C H 0.07 0.8147 0.5284 0.232 Uiso 1 1 calc R . . N2 N 0.85970(17) 0.6169(3) 0.8840(3) 0.0279(9) Uani 1 1 d . A . N1 N 0.77135(18) 0.5828(3) 0.9910(4) 0.0272(12) Uani 1 1 d . A . N3 N 0.72749(15) 0.7030(3) 0.8512(4) 0.0285(8) Uani 1 1 d . A . N4 N 0.69082(15) 0.5254(3) 0.8461(3) 0.0279(8) Uani 1 1 d . A . N5 N 0.78643(18) 0.4243(3) 0.8617(4) 0.0305(10) Uani 1 1 d . A . O1 O 0.73584(17) 0.4714(3) 0.6758(2) 0.0393(9) Uani 1 1 d . . . O2 O 0.77163(17) 0.6327(3) 0.6383(3) 0.0391(9) Uani 1 1 d . . . O3 O 0.84514(17) 0.5056(3) 0.6883(2) 0.0425(10) Uani 1 1 d . . . C7A C 0.8581(6) 0.4464(11) 0.6106(8) 0.033(3) Uani 0.54 1 d PU A 1 H7A H 0.83 0.4639 0.5646 0.039 Uiso 0.54 1 calc PR A 1 C8A C 0.8508(9) 0.3376(11) 0.6313(11) 0.060(4) Uani 0.54 1 d PU A 1 H8A1 H 0.8783 0.3194 0.676 0.09 Uiso 0.54 1 calc PR A 1 H8A2 H 0.8584 0.3002 0.5798 0.09 Uiso 0.54 1 calc PR A 1 H8A3 H 0.8112 0.3255 0.651 0.09 Uiso 0.54 1 calc PR A 1 C9A C 0.9169(8) 0.4702(14) 0.5817(13) 0.069(5) Uani 0.54 1 d PU A 1 H9A1 H 0.944 0.4645 0.6296 0.103 Uiso 0.54 1 calc PR A 1 H9A2 H 0.9175 0.5356 0.5602 0.103 Uiso 0.54 1 calc PR A 1 H9A3 H 0.9285 0.4265 0.5362 0.103 Uiso 0.54 1 calc PR A 1 C7B C 0.8679(9) 0.4798(18) 0.598(2) 0.083(9) Uani 0.46 1 d PDU A 2 H7B H 0.8439 0.5025 0.5492 0.1 Uiso 0.46 1 calc PR A 2 C8B C 0.8655(15) 0.3739(19) 0.617(2) 0.112(12) Uani 0.46 1 d PDU A 2 H8B1 H 0.8241 0.334 0.5999 0.169 Uiso 0.46 1 d P B 2 H8B2 H 0.8739 0.3359 0.6708 0.169 Uiso 0.46 1 d P C 2 H8B3 H 0.8907 0.3273 0.5721 0.169 Uiso 0.46 1 d P D 2 C9B C 0.9316(9) 0.5074(18) 0.5966(18) 0.077(7) Uani 0.46 1 d PDU A 2 H9B1 H 0.9351 0.5767 0.5996 0.116 Uiso 0.46 1 calc PR A 2 H9B2 H 0.9493 0.4846 0.5436 0.116 Uiso 0.46 1 calc PR A 2 H9B3 H 0.9515 0.4787 0.6454 0.116 Uiso 0.46 1 calc PR A 2 O4 O 0.9176(2) 0.1500(4) 0.5249(4) 0.0675(14) Uani 1 1 d . . . O5 O 0.0443(5) 0.7318(7) 0.6826(5) 0.144(3) Uani 1 1 d . . . F1 F 0.83471(17) 0.9989(3) 0.8800(3) 0.0766(14) Uani 1 1 d . . . F2 F 0.95331(17) 0.9340(3) 0.7844(3) 0.0722(12) Uani 1 1 d . . . F3 F 0.8567(2) 0.9115(4) 0.7595(3) 0.0873(15) Uani 1 1 d . . . F4 F 0.9306(2) 1.0253(6) 0.9007(4) 0.116(2) Uani 1 1 d . . . F5 F 0.8927(2) 0.8720(3) 0.8885(3) 0.0902(16) Uani 1 1 d . . . F6 F 0.8923(2) 1.0594(3) 0.7741(4) 0.0879(15) Uani 1 1 d . . . P1 P 0.78164(7) 0.55029(12) 0.70834(10) 0.0289(3) Uani 1 1 d . A . P2 P 0.89479(7) 0.96591(12) 0.83180(10) 0.0428(4) Uani 1 1 d . . . P3 P 0.04593(8) 0.37760(12) 0.81874(12) 0.0499(4) Uani 1 1 d D . . F7A F 0.0621(5) 0.3119(9) 0.7416(9) 0.1069(11) Uani 0.55 1 d P E 1 F8A F 0.0435(5) 0.4697(7) 0.8811(7) 0.1069(11) Uani 0.55 1 d PD E 1 F9A F 0.0217(4) 0.2741(5) 0.8436(9) 0.1069(11) Uani 0.55 1 d PD E 1 F10A F 0.0564(5) 0.4727(6) 0.7665(8) 0.1069(11) Uani 0.55 1 d PD E 1 F11A F -0.0232(3) 0.3949(9) 0.8154(8) 0.1069(11) Uani 0.55 1 d PD E 1 F12A F 0.1153(3) 0.3718(8) 0.8291(9) 0.1069(11) Uani 0.55 1 d PD E 1 F7B F 0.0801(6) 0.2938(9) 0.7633(10) 0.1069(11) Uani 0.45 1 d PD E 2 F8B F 0.0178(7) 0.4360(9) 0.8962(8) 0.1069(11) Uani 0.45 1 d PD E 2 F9B F 0.0615(6) 0.3149(8) 0.9024(7) 0.1069(11) Uani 0.45 1 d PD E 2 F10B F 0.0372(6) 0.4178(9) 0.7253(7) 0.1069(11) Uani 0.45 1 d PD E 2 F11B F -0.0177(4) 0.3398(10) 0.8047(10) 0.1069(11) Uani 0.45 1 d PD E 2 F12B F 0.1135(4) 0.4169(8) 0.8250(11) 0.1069(11) Uani 0.45 1 d PD E 2 Ru1 Ru 0.772961(14) 0.57181(2) 0.85386(3) 0.02312(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.051(3) 0.058(4) 0.024(3) -0.012(3) -0.010(3) -0.010(3) C2 0.062(4) 0.085(5) 0.048(4) -0.010(4) -0.019(4) 0.013(4) C3 0.088(6) 0.058(4) 0.059(5) -0.011(4) -0.022(4) -0.022(4) C4 0.069(4) 0.038(3) 0.037(3) 0.001(3) 0.005(3) -0.014(3) C5 0.108(6) 0.034(4) 0.064(5) 0.010(3) -0.004(5) 0.012(4) C6 0.103(6) 0.092(6) 0.049(4) 0.013(4) 0.021(4) -0.029(5) C10 0.029(3) 0.050(3) 0.035(3) -0.009(2) 0.002(2) 0.000(2) C11 0.027(2) 0.059(3) 0.043(3) 0.000(4) 0.002(4) -0.004(2) C12 0.029(3) 0.050(4) 0.059(4) 0.006(3) -0.008(3) -0.010(3) C13 0.033(3) 0.050(3) 0.039(3) -0.002(3) -0.010(2) -0.002(3) C14 0.027(2) 0.030(3) 0.025(3) -0.002(2) -0.002(2) 0.000(2) C15 0.029(3) 0.022(2) 0.029(3) -0.006(2) -0.004(2) 0.003(2) C16 0.050(3) 0.037(3) 0.034(3) -0.002(2) -0.008(3) 0.003(3) C17 0.053(4) 0.049(4) 0.026(3) 0.001(3) 0.001(3) -0.004(3) C18 0.049(4) 0.048(4) 0.031(3) -0.003(3) 0.010(3) 0.000(3) C19 0.036(3) 0.044(3) 0.027(3) -0.003(2) 0.001(2) 0.000(2) C20 0.044(2) 0.035(3) 0.030(3) 0.001(3) -0.004(3) 0.004(2) C21 0.073(4) 0.032(3) 0.061(4) 0.009(4) 0.016(5) 0.013(3) C22 0.069(4) 0.046(3) 0.063(4) 0.001(4) 0.017(5) 0.028(3) C23 0.038(3) 0.058(3) 0.043(3) 0.003(3) -0.005(3) 0.021(2) C24 0.035(2) 0.047(3) 0.021(3) 0.003(3) 0.004(3) 0.010(2) C25 0.027(2) 0.048(3) 0.027(4) -0.008(2) 0.000(2) 0.002(2) C26 0.025(2) 0.075(4) 0.039(4) -0.014(3) 0.000(2) 0.004(3) C27 0.027(3) 0.074(4) 0.048(5) -0.009(3) -0.005(3) -0.019(3) C28 0.046(3) 0.056(3) 0.040(3) -0.014(3) 0.000(3) -0.023(3) C29 0.033(2) 0.035(2) 0.028(2) -0.001(3) -0.004(4) -0.004(2) C30 0.050(3) 0.030(2) 0.028(2) -0.003(3) -0.006(3) 0.001(2) C31 0.075(4) 0.027(3) 0.050(4) -0.001(4) 0.000(4) -0.009(3) C32 0.104(5) 0.026(3) 0.063(5) -0.003(3) -0.011(5) 0.012(3) C33 0.073(4) 0.040(3) 0.049(5) -0.007(3) -0.009(4) 0.021(3) C34 0.042(3) 0.040(3) 0.044(4) -0.008(3) -0.007(3) 0.011(2) C50 0.043(3) 0.071(4) 0.040(4) 0.002(3) 0.009(3) 0.006(3) C51 0.113(7) 0.074(5) 0.051(5) 0.011(4) 0.019(5) 0.008(5) C52 0.072(5) 0.099(7) 0.078(6) 0.036(5) -0.034(4) -0.029(5) C53 0.064(4) 0.071(5) 0.045(4) 0.003(4) 0.008(3) -0.005(4) C54 0.134(10) 0.077(6) 0.126(9) 0.008(7) 0.029(8) 0.019(7) C55 0.269(18) 0.066(6) 0.129(11) -0.005(7) -0.067(12) 0.038(9) N2 0.026(2) 0.027(2) 0.031(2) -0.0054(16) -0.0011(17) 0.0012(18) N1 0.025(2) 0.029(2) 0.028(3) -0.0016(19) 0.0046(18) 0.0001(18) N3 0.0295(17) 0.0320(19) 0.0240(18) -0.006(3) -0.002(2) 0.0026(16) N4 0.0242(18) 0.037(2) 0.022(2) 0.002(2) -0.009(2) -0.0060(15) N5 0.037(2) 0.0289(19) 0.025(3) 0.003(2) -0.006(3) 0.0044(16) O1 0.052(2) 0.035(2) 0.031(2) -0.0029(17) -0.0108(18) -0.0052(19) O2 0.058(3) 0.033(2) 0.026(2) 0.0012(16) -0.0025(17) 0.0011(18) O3 0.039(2) 0.065(3) 0.023(2) -0.0134(18) 0.0006(16) 0.017(2) C7A 0.047(6) 0.033(6) 0.018(5) 0.001(5) 0.003(4) 0.021(5) C8A 0.084(8) 0.042(6) 0.054(7) -0.020(6) -0.001(6) 0.014(6) C9A 0.061(8) 0.076(9) 0.069(8) -0.010(7) 0.022(7) 0.015(7) C7B 0.084(12) 0.081(12) 0.086(12) -0.006(9) 0.021(8) 0.015(8) C8B 0.112(14) 0.112(15) 0.114(14) -0.015(9) 0.009(9) 0.002(9) C9B 0.073(10) 0.081(11) 0.077(10) 0.001(8) 0.015(8) 0.004(8) O4 0.060(3) 0.078(3) 0.065(3) -0.018(3) -0.019(3) 0.019(3) O5 0.203(9) 0.167(8) 0.060(5) -0.015(5) 0.019(5) 0.027(7) F1 0.062(2) 0.061(3) 0.107(4) 0.001(2) 0.031(2) 0.0092(19) F2 0.048(2) 0.114(4) 0.055(2) -0.007(2) 0.007(2) 0.012(2) F3 0.072(3) 0.107(4) 0.082(4) -0.017(3) -0.008(3) -0.032(3) F4 0.072(3) 0.199(7) 0.077(3) -0.067(4) 0.007(3) -0.043(4) F5 0.120(4) 0.070(3) 0.080(3) 0.038(2) 0.020(3) 0.038(3) F6 0.105(4) 0.067(3) 0.092(4) 0.035(3) 0.007(3) -0.004(3) P1 0.0316(7) 0.0335(7) 0.0214(7) -0.0020(6) -0.0016(6) 0.0024(6) P2 0.0375(7) 0.0457(8) 0.0452(10) 0.0058(7) 0.0017(6) 0.0028(7) P3 0.0594(10) 0.0413(9) 0.0488(9) 0.0003(7) 0.0056(8) 0.0042(8) F7A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F8A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F9A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F10A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F11A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F12A 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F7B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F8B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F9B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F10B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F11B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) F12B 0.105(3) 0.080(2) 0.135(3) 0.007(2) 0.016(2) 0.0118(18) Ru1 0.02024(16) 0.02682(18) 0.02232(18) -0.0020(2) -0.0009(2) 0.00076(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.460(7) . ? C1 C2 1.494(10) . ? C1 C3 1.515(10) . ? C4 O2 1.436(7) . ? C4 C5 1.495(11) . ? C4 C6 1.498(10) . ? C10 N2 1.345(7) . ? C10 C11 1.384(7) . ? C11 C12 1.358(10) . ? C12 C13 1.386(9) . ? C13 C14 1.392(7) . ? C14 N2 1.356(7) . ? C14 C15 1.455(7) . ? C15 N1 1.350(6) . ? C15 C16 1.384(8) . ? C16 C17 1.374(8) . ? C17 C18 1.385(8) . ? C18 C19 1.374(9) . ? C19 N1 1.341(7) . ? C20 N3 1.331(6) . ? C20 C21 1.362(7) . ? C21 C22 1.360(9) . ? C22 C23 1.392(9) . ? C23 C24 1.376(7) . ? C24 N3 1.366(6) . ? C24 C25 1.477(7) . ? C25 N4 1.353(6) . ? C25 C26 1.392(7) . ? C26 C27 1.377(9) . ? C27 C28 1.396(9) . ? C28 C29 1.386(7) . ? C29 N4 1.346(6) . ? C29 C30 1.487(7) . ? C30 N5 1.366(6) . ? C30 C31 1.393(7) . ? C31 C32 1.372(9) . ? C32 C33 1.387(10) . ? C33 C34 1.376(8) . ? C34 N5 1.367(6) . ? C50 O4 1.202(8) . ? C50 C51 1.452(11) . ? C50 C52 1.465(10) . ? C53 O5 1.138(9) . ? C53 C54 1.455(12) . ? C53 C55 1.544(13) . ? N2 Ru1 2.108(4) . ? N1 Ru1 2.113(5) . ? N3 Ru1 2.080(4) . ? N4 Ru1 1.966(3) . ? N5 Ru1 2.060(4) . ? O1 P1 1.582(4) . ? O2 P1 1.582(4) . ? O3 C7A 1.476(13) . ? O3 C7B 1.52(3) . ? O3 P1 1.592(4) . ? C7A C9A 1.44(2) . ? C7A C8A 1.54(2) . ? C7B C8B 1.488(10) . ? C7B C9B 1.489(10) . ? F1 P2 1.612(4) . ? F2 P2 1.572(4) . ? F3 P2 1.593(5) . ? F4 P2 1.564(5) . ? F5 P2 1.561(4) . ? F6 P2 1.565(5) . ? P1 Ru1 2.2644(16) . ? P3 F7A 1.536(13) . ? P3 F11B 1.544(8) . ? P3 F10B 1.551(9) . ? P3 F10A 1.555(8) . ? P3 F8B 1.571(9) . ? P3 F9A 1.575(7) . ? P3 F12A 1.578(8) . ? P3 F11A 1.580(8) . ? P3 F9B 1.589(8) . ? P3 F8A 1.593(8) . ? P3 F12B 1.622(9) . ? P3 F7B 1.631(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.8(5) . . ? O1 C1 C3 104.3(5) . . ? C2 C1 C3 113.0(6) . . ? O2 C4 C5 107.4(6) . . ? O2 C4 C6 109.4(6) . . ? C5 C4 C6 113.0(6) . . ? N2 C10 C11 123.1(5) . . ? C12 C11 C10 118.4(6) . . ? C11 C12 C13 120.5(5) . . ? C12 C13 C14 118.2(5) . . ? N2 C14 C13 122.1(5) . . ? N2 C14 C15 116.3(4) . . ? C13 C14 C15 121.6(5) . . ? N1 C15 C16 120.1(5) . . ? N1 C15 C14 115.0(5) . . ? C16 C15 C14 124.8(5) . . ? C17 C16 C15 120.8(6) . . ? C16 C17 C18 119.0(6) . . ? C19 C18 C17 117.5(6) . . ? N1 C19 C18 124.1(6) . . ? N3 C20 C21 123.4(5) . . ? C22 C21 C20 119.6(6) . . ? C21 C22 C23 119.2(5) . . ? C24 C23 C22 118.3(5) . . ? N3 C24 C23 122.3(5) . . ? N3 C24 C25 115.9(4) . . ? C23 C24 C25 121.7(5) . . ? N4 C25 C26 119.6(5) . . ? N4 C25 C24 112.2(4) . . ? C26 C25 C24 128.0(5) . . ? C27 C26 C25 119.3(5) . . ? C26 C27 C28 120.3(5) . . ? C29 C28 C27 118.5(5) . . ? N4 C29 C28 120.4(5) . . ? N4 C29 C30 113.0(4) . . ? C28 C29 C30 126.3(5) . . ? N5 C30 C31 122.5(5) . . ? N5 C30 C29 114.4(4) . . ? C31 C30 C29 122.9(5) . . ? C32 C31 C30 118.3(6) . . ? C31 C32 C33 120.3(5) . . ? C34 C33 C32 119.1(6) . . ? N5 C34 C33 122.1(6) . . ? O4 C50 C51 121.8(7) . . ? O4 C50 C52 121.7(7) . . ? C51 C50 C52 116.4(7) . . ? O5 C53 C54 128.5(10) . . ? O5 C53 C55 118.1(9) . . ? C54 C53 C55 113.1(8) . . ? C10 N2 C14 117.7(4) . . ? C10 N2 Ru1 127.1(3) . . ? C14 N2 Ru1 115.2(3) . . ? C19 N1 C15 118.4(5) . . ? C19 N1 Ru1 125.6(4) . . ? C15 N1 Ru1 115.9(4) . . ? C20 N3 C24 117.2(4) . . ? C20 N3 Ru1 129.7(3) . . ? C24 N3 Ru1 113.0(3) . . ? C29 N4 C25 121.8(4) . . ? C29 N4 Ru1 118.7(3) . . ? C25 N4 Ru1 119.5(3) . . ? C30 N5 C34 117.5(4) . . ? C30 N5 Ru1 113.9(3) . . ? C34 N5 Ru1 128.4(4) . . ? C1 O1 P1 129.8(4) . . ? C4 O2 P1 123.8(4) . . ? C7A O3 P1 123.3(6) . . ? C7B O3 P1 125.0(10) . . ? C9A C7A O3 107.8(13) . . ? C9A C7A C8A 112.6(13) . . ? O3 C7A C8A 110.5(11) . . ? C8B C7B C9B 107(2) . . ? C8B C7B O3 93(2) . . ? C9B C7B O3 106(2) . . ? O2 P1 O1 100.7(2) . . ? O2 P1 O3 106.0(2) . . ? O1 P1 O3 105.2(2) . . ? O2 P1 Ru1 124.44(17) . . ? O1 P1 Ru1 110.21(17) . . ? O3 P1 Ru1 108.67(16) . . ? F5 P2 F4 94.1(4) . . ? F5 P2 F6 176.2(3) . . ? F4 P2 F6 88.3(4) . . ? F5 P2 F2 92.9(3) . . ? F4 P2 F2 91.5(3) . . ? F6 P2 F2 89.9(3) . . ? F5 P2 F3 89.0(3) . . ? F4 P2 F3 176.5(4) . . ? F6 P2 F3 88.5(3) . . ? F2 P2 F3 90.0(3) . . ? F5 P2 F1 87.3(3) . . ? F4 P2 F1 88.6(3) . . ? F6 P2 F1 89.9(3) . . ? F2 P2 F1 179.7(3) . . ? F3 P2 F1 89.9(3) . . ? F7A P3 F11B 85.1(8) . . ? F7A P3 F10B 61.8(6) . . ? F11B P3 F10B 82.7(8) . . ? F7A P3 F10A 93.6(7) . . ? F11B P3 F10A 110.7(7) . . ? F7A P3 F8B 169.4(8) . . ? F11B P3 F8B 84.4(8) . . ? F10B P3 F8B 117.9(7) . . ? F10A P3 F8B 91.2(6) . . ? F7A P3 F9A 74.7(7) . . ? F11B P3 F9A 53.5(6) . . ? F10B P3 F9A 120.3(7) . . ? F10A P3 F9A 160.3(7) . . ? F8B P3 F9A 98.0(7) . . ? F7A P3 F12A 79.1(7) . . ? F11B P3 F12A 157.2(7) . . ? F10B P3 F12A 103.7(7) . . ? F10A P3 F12A 86.7(6) . . ? F8B P3 F12A 110.6(8) . . ? F9A P3 F12A 106.0(5) . . ? F7A P3 F11A 107.4(7) . . ? F10B P3 F11A 77.9(7) . . ? F10A P3 F11A 90.4(6) . . ? F8B P3 F11A 63.1(7) . . ? F9A P3 F11A 78.5(5) . . ? F12A P3 F11A 173.0(7) . . ? F7A P3 F9B 104.5(6) . . ? F11B P3 F9B 97.8(7) . . ? F10B P3 F9B 166.2(7) . . ? F10A P3 F9B 147.4(7) . . ? F8B P3 F9B 75.8(7) . . ? F9A P3 F9B 52.2(6) . . ? F12A P3 F9B 70.8(6) . . ? F11A P3 F9B 109.1(7) . . ? F7A P3 F8A 160.7(7) . . ? F11B P3 F8A 108.7(7) . . ? F10B P3 F8A 105.6(6) . . ? F10A P3 F8A 69.1(6) . . ? F9A P3 F8A 124.3(7) . . ? F12A P3 F8A 90.8(6) . . ? F11A P3 F8A 82.2(6) . . ? F9B P3 F8A 87.4(6) . . ? F7A P3 F12B 91.1(7) . . ? F11B P3 F12B 175.3(8) . . ? F10B P3 F12B 93.1(8) . . ? F10A P3 F12B 66.8(6) . . ? F8B P3 F12B 99.5(8) . . ? F9A P3 F12B 128.0(6) . . ? F11A P3 F12B 151.7(6) . . ? F9B P3 F12B 85.7(7) . . ? F8A P3 F12B 74.4(7) . . ? F11B P3 F7B 97.4(8) . . ? F10B P3 F7B 80.2(7) . . ? F10A P3 F7B 104.8(7) . . ? F8B P3 F7B 161.9(8) . . ? F9A P3 F7B 69.5(7) . . ? F12A P3 F7B 63.0(7) . . ? F11A P3 F7B 123.9(7) . . ? F9B P3 F7B 86.1(7) . . ? F8A P3 F7B 153.7(7) . . ? F12B P3 F7B 79.7(7) . . ? N4 Ru1 N5 79.74(16) . . ? N4 Ru1 N3 79.37(15) . . ? N5 Ru1 N3 158.81(16) . . ? N4 Ru1 N2 170.66(18) . . ? N5 Ru1 N2 98.12(16) . . ? N3 Ru1 N2 101.93(15) . . ? N4 Ru1 N1 93.86(18) . . ? N5 Ru1 N1 90.9(2) . . ? N3 Ru1 N1 87.1(2) . . ? N2 Ru1 N1 77.03(16) . . ? N4 Ru1 P1 88.82(15) . . ? N5 Ru1 P1 85.16(19) . . ? N3 Ru1 P1 97.90(18) . . ? N2 Ru1 P1 100.10(12) . . ? N1 Ru1 P1 174.74(13) . . ? #====END data_([Ru]6) _database_code_depnum_ccdc_archive 'CCDC 665736' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H34 N5 O3 P Ru, 2(F6 P)' _chemical_formula_sum 'C43 H34 F12 N5 O3 P3 Ru' _chemical_formula_weight 1090.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.609(3) _cell_length_b 14.272(3) _cell_length_c 39.990(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8338(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 3959 _cell_measurement_theta_min 2.7829 _cell_measurement_theta_max 32.1361 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.960 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 0.0015073588 _diffrn_orient_matrix_ub_12 0.0466846938 _diffrn_orient_matrix_ub_13 -0.0048251304 _diffrn_orient_matrix_ub_21 -0.0180979054 _diffrn_orient_matrix_ub_22 -0.0117781234 _diffrn_orient_matrix_ub_23 -0.0159340781 _diffrn_orient_matrix_ub_31 -0.0462630774 _diffrn_orient_matrix_ub_32 0.0062459476 _diffrn_orient_matrix_ub_33 0.0061171661 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_unetI/netI 0.1206 _diffrn_reflns_number 52199 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8501 _reflns_number_gt 5105 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0092P)^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_number_reflns 8501 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 0.95 _refine_ls_restrained_S_all 0.95 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.608 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.1767(3) 0.3205(2) 0.41011(10) 0.0131(10) Uani 1 1 d . . . C2 C 0.1619(3) 0.3060(2) 0.44366(10) 0.0163(10) Uani 1 1 d . . . H2 H 0.1027 0.3072 0.4522 0.02 Uiso 1 1 calc R . . C3 C 0.2356(3) 0.2895(3) 0.46458(10) 0.0206(11) Uani 1 1 d . . . H3 H 0.2262 0.2801 0.4873 0.025 Uiso 1 1 calc R . . C4 C 0.3236(3) 0.2870(3) 0.45155(11) 0.0230(11) Uani 1 1 d . . . H4 H 0.3732 0.2753 0.4655 0.028 Uiso 1 1 calc R . . C5 C 0.3372(3) 0.3020(3) 0.41797(11) 0.0221(11) Uani 1 1 d . . . H5 H 0.3962 0.3005 0.4093 0.027 Uiso 1 1 calc R . . C6 C 0.2642(3) 0.3191(3) 0.39696(10) 0.0184(11) Uani 1 1 d . . . H6 H 0.2737 0.3296 0.3743 0.022 Uiso 1 1 calc R . . C7 C -0.0611(3) 0.3749(3) 0.43470(9) 0.0156(10) Uani 1 1 d . . . C8 C -0.1060(3) 0.3580(3) 0.46428(10) 0.0251(11) Uani 1 1 d . . . H8 H -0.1225 0.2974 0.4704 0.03 Uiso 1 1 calc R . . C9 C -0.1260(3) 0.4326(3) 0.48464(11) 0.0299(12) Uani 1 1 d . . . H9 H -0.1569 0.422 0.5046 0.036 Uiso 1 1 calc R . . C10 C -0.1020(3) 0.5216(3) 0.47642(11) 0.0266(12) Uani 1 1 d . . . H10 H -0.1151 0.5711 0.4908 0.032 Uiso 1 1 calc R . . C11 C -0.0580(3) 0.5375(3) 0.44654(11) 0.0248(11) Uani 1 1 d . . . H11 H -0.0422 0.5983 0.4405 0.03 Uiso 1 1 calc R . . C12 C -0.0368(3) 0.4635(3) 0.42515(9) 0.0185(11) Uani 1 1 d . . . H12 H -0.0069 0.4741 0.405 0.022 Uiso 1 1 calc R . . C13 C -0.1139(3) 0.3561(3) 0.34203(10) 0.0142(9) Uani 1 1 d . . . C14 C -0.1925(3) 0.3433(2) 0.36095(10) 0.0153(10) Uani 1 1 d . . . H14 H -0.1894 0.3335 0.3839 0.018 Uiso 1 1 calc R . . C15 C -0.2755(3) 0.3457(2) 0.34450(10) 0.0190(11) Uani 1 1 d . . . H15 H -0.3289 0.3357 0.3566 0.023 Uiso 1 1 calc R . . C16 C -0.2814(3) 0.3625(3) 0.31082(10) 0.0198(10) Uani 1 1 d . . . H16 H -0.3383 0.3656 0.3004 0.024 Uiso 1 1 calc R . . C17 C -0.2020(3) 0.3747(3) 0.29246(10) 0.0217(11) Uani 1 1 d . . . H17 H -0.2057 0.3845 0.2695 0.026 Uiso 1 1 calc R . . C18 C -0.1173(3) 0.3724(3) 0.30778(10) 0.0196(10) Uani 1 1 d . . . H18 H -0.064 0.3815 0.2955 0.024 Uiso 1 1 calc R . . C19 C -0.1599(3) 0.1247(3) 0.32611(10) 0.0193(10) Uani 1 1 d . . . H19 H -0.1264 0.1379 0.3069 0.023 Uiso 1 1 calc R . . C20 C -0.2519(3) 0.1046(3) 0.32318(11) 0.0267(11) Uani 1 1 d . . . H20 H -0.279 0.102 0.3021 0.032 Uiso 1 1 calc R . . C21 C -0.3032(3) 0.0885(3) 0.35107(12) 0.0284(13) Uani 1 1 d . . . H21 H -0.3658 0.0775 0.3494 0.034 Uiso 1 1 calc R . . C22 C -0.2603(3) 0.0888(2) 0.38205(11) 0.0200(11) Uani 1 1 d . . . H22 H -0.2939 0.0781 0.4014 0.024 Uiso 1 1 calc R . . C23 C -0.1674(3) 0.1053(2) 0.38384(10) 0.0129(10) Uani 1 1 d . . . C24 C -0.1133(3) 0.0977(2) 0.41490(10) 0.0135(10) Uani 1 1 d . . . C25 C -0.1457(3) 0.0909(2) 0.44741(10) 0.0186(11) Uani 1 1 d . . . H25 H -0.2082 0.0893 0.4517 0.022 Uiso 1 1 calc R . . C26 C -0.0832(3) 0.0867(2) 0.47312(11) 0.0198(11) Uani 1 1 d . . . H26 H -0.104 0.0848 0.4951 0.024 Uiso 1 1 calc R . . C27 C 0.0092(3) 0.0850(2) 0.46700(9) 0.0163(10) Uani 1 1 d . . . H27 H 0.0509 0.0819 0.4845 0.02 Uiso 1 1 calc R . . C28 C 0.0390(3) 0.0881(2) 0.43410(10) 0.0128(10) Uani 1 1 d . . . C29 C 0.1331(3) 0.0828(2) 0.42198(10) 0.0123(10) Uani 1 1 d . . . C30 C 0.2074(3) 0.0524(2) 0.44094(10) 0.0173(10) Uani 1 1 d . . . H30 H 0.2 0.0386 0.4635 0.021 Uiso 1 1 calc R . . C31 C 0.2919(3) 0.0428(3) 0.42608(11) 0.0234(11) Uani 1 1 d . . . H31 H 0.3419 0.0226 0.4385 0.028 Uiso 1 1 calc R . . C32 C 0.3018(3) 0.0631(3) 0.39280(11) 0.0221(11) Uani 1 1 d . . . H32 H 0.3584 0.0557 0.3824 0.027 Uiso 1 1 calc R . . C33 C 0.2277(3) 0.0945(2) 0.37478(11) 0.0175(11) Uani 1 1 d . . . H33 H 0.2353 0.1087 0.3523 0.021 Uiso 1 1 calc R . . C34 C 0.0982(3) 0.2512(3) 0.30559(10) 0.0162(10) Uani 1 1 d . . . H34 H 0.0975 0.3014 0.3204 0.019 Uiso 1 1 calc R . . C35 C 0.1248(3) 0.2677(3) 0.27279(10) 0.0256(12) Uani 1 1 d . . . H35 H 0.1424 0.3273 0.2659 0.031 Uiso 1 1 calc R . . C36 C 0.1246(3) 0.1949(3) 0.25092(11) 0.0273(12) Uani 1 1 d . . . H36 H 0.1391 0.2047 0.2285 0.033 Uiso 1 1 calc R . . C37 C 0.1028(3) 0.1066(3) 0.26213(10) 0.0213(11) Uani 1 1 d . . . H37 H 0.1044 0.0559 0.2476 0.026 Uiso 1 1 calc R . . C38 C 0.0783(3) 0.0940(3) 0.29522(10) 0.0154(10) Uani 1 1 d . . . C39 C 0.0576(3) 0.0010(3) 0.30979(10) 0.0137(10) Uani 1 1 d . . . C40 C 0.0674(3) -0.0815(3) 0.29230(10) 0.0194(11) Uani 1 1 d . . . H40 H 0.0852 -0.0809 0.27 0.023 Uiso 1 1 calc R . . C41 C 0.0504(3) -0.1650(2) 0.30850(10) 0.0197(11) Uani 1 1 d . . . H41 H 0.0567 -0.2216 0.2972 0.024 Uiso 1 1 calc R . . C42 C 0.0238(3) -0.1636(2) 0.34191(9) 0.0171(10) Uani 1 1 d . . . H42 H 0.0124 -0.2192 0.3533 0.02 Uiso 1 1 calc R . . C43 C 0.0148(3) -0.0796(2) 0.35759(9) 0.0161(10) Uani 1 1 d . . . H43 H -0.0046 -0.079 0.3797 0.019 Uiso 1 1 calc R . . N5 N -0.1175(2) 0.1256(2) 0.35561(7) 0.0133(8) Uani 1 1 d . . . N4 N -0.0231(2) 0.09829(17) 0.40931(7) 0.0099(7) Uani 1 1 d . . . N3 N 0.1443(2) 0.10532(19) 0.38874(8) 0.0125(8) Uani 1 1 d . . . N2 N 0.0735(2) 0.1669(2) 0.31685(7) 0.0128(8) Uani 1 1 d . . . N1 N 0.0325(2) 0.00249(19) 0.34261(7) 0.0111(7) Uani 1 1 d . . . O1 O 0.10609(17) 0.34404(16) 0.38779(6) 0.0152(7) Uani 1 1 d . . . O2 O -0.04284(17) 0.29398(15) 0.41558(6) 0.0132(7) Uani 1 1 d . . . O3 O -0.02672(17) 0.36136(16) 0.35723(5) 0.0127(6) Uani 1 1 d . . . F1 F 0.44247(17) -0.01575(15) 0.26773(6) 0.0388(7) Uani 1 1 d . . . F2 F 0.31074(18) 0.13215(16) 0.30324(6) 0.0456(7) Uani 1 1 d . . . F3 F 0.39439(17) 0.13150(18) 0.25624(6) 0.0422(7) Uani 1 1 d . . . F4 F 0.3586(2) -0.01423(16) 0.31485(7) 0.0599(9) Uani 1 1 d . . . F5 F 0.29225(19) 0.01568(17) 0.26578(7) 0.0606(9) Uani 1 1 d . . . F6 F 0.4617(2) 0.09983(15) 0.30526(6) 0.0529(8) Uani 1 1 d . . . F7 F -0.07054(16) -0.23930(14) 0.41417(5) 0.0270(6) Uani 1 1 d . . . F8 F -0.16167(14) -0.12799(15) 0.47556(5) 0.0236(6) Uani 1 1 d . . . F9 F -0.16856(16) -0.11732(14) 0.41917(5) 0.0305(6) Uani 1 1 d . . . F10 F -0.06354(16) -0.24951(14) 0.47097(5) 0.0289(7) Uani 1 1 d . . . F11 F -0.03120(15) -0.11324(12) 0.44514(5) 0.0249(6) Uani 1 1 d . . . F12 F -0.20065(16) -0.25521(14) 0.44458(6) 0.0301(6) Uani 1 1 d . . . P1 P 0.01483(8) 0.28385(6) 0.38181(2) 0.0121(2) Uani 1 1 d . . . P2 P 0.37640(9) 0.05832(8) 0.28556(3) 0.0268(3) Uani 1 1 d . . . P3 P -0.11648(8) -0.18405(7) 0.44493(3) 0.0188(3) Uani 1 1 d . . . Ru1 Ru 0.02286(2) 0.13568(2) 0.364600(7) 0.01178(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(3) 0.009(2) 0.014(3) 0.0015(19) -0.005(2) 0.0029(19) C2 0.009(3) 0.016(2) 0.024(3) 0.001(2) 0.003(2) -0.0008(19) C3 0.030(3) 0.018(2) 0.013(3) -0.001(2) 0.000(2) 0.000(2) C4 0.016(3) 0.023(2) 0.029(3) -0.011(2) -0.007(2) -0.002(2) C5 0.014(3) 0.030(3) 0.022(3) -0.005(2) 0.001(2) -0.003(2) C6 0.017(3) 0.026(2) 0.013(3) -0.003(2) 0.001(2) -0.003(2) C7 0.012(3) 0.016(2) 0.018(2) -0.008(2) -0.0005(18) 0.004(2) C8 0.022(3) 0.026(2) 0.027(3) -0.007(2) 0.006(2) -0.006(2) C9 0.031(3) 0.038(3) 0.021(3) -0.014(2) 0.009(2) -0.003(3) C10 0.021(3) 0.029(3) 0.030(3) -0.019(2) 0.000(2) 0.006(2) C11 0.028(3) 0.013(2) 0.034(3) -0.006(2) -0.005(2) 0.001(2) C12 0.019(3) 0.016(2) 0.020(3) 0.0024(19) 0.005(2) 0.003(2) C13 0.014(3) 0.012(2) 0.017(2) -0.002(2) -0.0019(19) 0.004(2) C14 0.016(3) 0.012(2) 0.017(3) 0.0013(19) 0.001(2) 0.0028(18) C15 0.018(3) 0.014(2) 0.025(3) 0.002(2) 0.002(2) -0.002(2) C16 0.020(3) 0.017(2) 0.023(3) -0.002(2) -0.005(2) -0.001(2) C17 0.025(3) 0.027(3) 0.013(2) 0.002(2) -0.001(2) -0.001(2) C18 0.016(3) 0.024(2) 0.019(3) 0.002(2) 0.004(2) -0.001(2) C19 0.027(3) 0.012(2) 0.019(3) 0.001(2) -0.003(2) 0.003(2) C20 0.033(3) 0.016(2) 0.031(3) -0.002(2) -0.015(3) 0.004(2) C21 0.016(3) 0.017(2) 0.052(4) -0.005(2) -0.011(3) 0.007(2) C22 0.016(3) 0.016(2) 0.028(3) 0.002(2) 0.004(2) 0.002(2) C23 0.015(3) 0.007(2) 0.017(3) -0.0056(18) 0.001(2) 0.0037(18) C24 0.014(3) 0.006(2) 0.020(3) 0.0004(18) 0.001(2) 0.0000(19) C25 0.022(3) 0.011(2) 0.023(3) 0.005(2) 0.009(2) 0.001(2) C26 0.032(3) 0.013(2) 0.015(3) 0.0010(19) 0.006(2) 0.005(2) C27 0.028(3) 0.010(2) 0.011(2) -0.0004(17) -0.001(2) 0.005(2) C28 0.014(3) 0.008(2) 0.016(2) -0.0025(18) -0.001(2) 0.0002(19) C29 0.019(3) 0.008(2) 0.010(2) -0.0037(18) -0.001(2) -0.0008(19) C30 0.022(3) 0.013(2) 0.017(3) 0.0004(19) -0.009(2) 0.002(2) C31 0.019(3) 0.018(2) 0.034(3) -0.009(2) -0.008(2) 0.007(2) C32 0.014(3) 0.022(2) 0.030(3) -0.007(2) 0.000(2) 0.002(2) C33 0.014(3) 0.017(2) 0.022(3) -0.0048(19) 0.006(2) -0.001(2) C34 0.020(3) 0.015(2) 0.014(2) -0.0011(19) 0.004(2) 0.002(2) C35 0.031(3) 0.019(3) 0.027(3) 0.006(2) 0.013(2) 0.004(2) C36 0.041(3) 0.025(3) 0.016(3) 0.008(2) 0.014(2) 0.011(2) C37 0.033(3) 0.017(3) 0.014(3) -0.0038(19) 0.003(2) 0.008(2) C38 0.013(3) 0.016(2) 0.017(3) 0.000(2) 0.0019(19) 0.0018(19) C39 0.008(2) 0.017(2) 0.016(3) -0.001(2) -0.0011(19) 0.0007(18) C40 0.018(3) 0.021(2) 0.019(3) -0.004(2) 0.002(2) 0.002(2) C41 0.026(3) 0.009(2) 0.024(3) -0.0056(19) 0.002(2) 0.0029(19) C42 0.019(3) 0.009(2) 0.023(2) 0.0011(17) -0.001(2) 0.001(2) C43 0.018(3) 0.012(2) 0.018(3) 0.0017(18) 0.004(2) 0.002(2) N5 0.016(2) 0.0091(17) 0.015(2) -0.0022(15) -0.0019(15) 0.0043(17) N4 0.013(2) 0.0053(15) 0.0115(19) -0.0024(13) 0.0026(17) 0.0038(16) N3 0.010(2) 0.0128(19) 0.015(2) -0.0017(15) 0.0019(15) -0.0004(15) N2 0.012(2) 0.0140(19) 0.012(2) 0.0008(15) 0.0018(15) 0.0026(15) N1 0.009(2) 0.0141(17) 0.0104(19) 0.0009(14) -0.0017(16) 0.0032(16) O1 0.0098(17) 0.0196(16) 0.0163(16) 0.0016(12) -0.0020(12) -0.0056(13) O2 0.0151(18) 0.0102(13) 0.0142(16) 0.0001(12) 0.0056(13) 0.0004(13) O3 0.0118(14) 0.0114(12) 0.0147(15) 0.0041(13) -0.0014(13) 0.0003(15) F1 0.0339(19) 0.0245(14) 0.058(2) -0.0094(13) 0.0081(13) 0.0069(13) F2 0.062(2) 0.0272(14) 0.0481(18) -0.0048(14) 0.0291(14) 0.0058(16) F3 0.055(2) 0.0402(15) 0.0311(17) 0.0116(14) 0.0127(13) 0.0157(16) F4 0.101(3) 0.0282(16) 0.051(2) 0.0163(14) 0.0260(18) 0.0008(17) F5 0.036(2) 0.0563(19) 0.090(3) -0.0338(17) -0.0193(16) 0.0006(16) F6 0.067(2) 0.0332(16) 0.0581(19) -0.0065(13) -0.0341(17) -0.0046(15) F7 0.0358(18) 0.0209(13) 0.0242(16) -0.0066(12) 0.0116(12) -0.0043(12) F8 0.0266(15) 0.0226(12) 0.0215(14) -0.0076(12) 0.0050(11) -0.0004(12) F9 0.0419(18) 0.0266(15) 0.0229(15) 0.0011(12) -0.0116(12) 0.0056(13) F10 0.0414(19) 0.0210(13) 0.0245(16) 0.0033(11) -0.0071(12) 0.0083(12) F11 0.0178(14) 0.0184(13) 0.0384(15) -0.0051(10) 0.0037(12) -0.0076(12) F12 0.0286(17) 0.0259(13) 0.0359(17) -0.0103(12) 0.0085(13) -0.0166(12) P1 0.0123(7) 0.0130(5) 0.0109(6) -0.0002(4) 0.0011(5) 0.0002(5) P2 0.0325(9) 0.0215(7) 0.0264(8) -0.0032(6) 0.0025(6) -0.0010(6) P3 0.0209(8) 0.0169(6) 0.0188(7) -0.0020(5) 0.0011(6) -0.0022(6) Ru1 0.01268(17) 0.01233(14) 0.01033(16) -0.00021(17) 0.00106(17) 0.00088(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.375(5) . ? C1 C6 1.383(5) . ? C1 O1 1.404(4) . ? C2 C3 1.384(5) . ? C3 C4 1.387(5) . ? C4 C5 1.374(5) . ? C5 C6 1.379(5) . ? C7 C12 1.368(5) . ? C7 C8 1.374(5) . ? C7 O2 1.410(4) . ? C8 C9 1.371(5) . ? C9 C10 1.358(5) . ? C10 C11 1.375(5) . ? C11 C12 1.394(5) . ? C13 C14 1.387(5) . ? C13 C18 1.390(5) . ? C13 O3 1.414(4) . ? C14 C15 1.380(5) . ? C15 C16 1.370(5) . ? C16 C17 1.384(5) . ? C17 C18 1.381(5) . ? C19 N5 1.332(4) . ? C19 C20 1.380(5) . ? C20 C21 1.363(6) . ? C21 C22 1.389(5) . ? C22 C23 1.379(5) . ? C23 N5 1.375(4) . ? C23 C24 1.477(5) . ? C24 N4 1.337(5) . ? C24 C25 1.387(5) . ? C25 C26 1.377(5) . ? C26 C27 1.372(5) . ? C27 C28 1.386(5) . ? C28 N4 1.351(4) . ? C28 C29 1.460(5) . ? C29 N3 1.377(4) . ? C29 C30 1.394(5) . ? C30 C31 1.377(5) . ? C31 C32 1.370(5) . ? C32 C33 1.376(5) . ? C33 N3 1.350(5) . ? C34 N2 1.334(4) . ? C34 C35 1.388(5) . ? C35 C36 1.357(5) . ? C36 C37 1.375(5) . ? C37 C38 1.383(5) . ? C38 N2 1.355(4) . ? C38 C39 1.480(5) . ? C39 N1 1.363(4) . ? C39 C40 1.377(5) . ? C40 C41 1.378(5) . ? C41 C42 1.392(5) . ? C42 C43 1.359(4) . ? C43 N1 1.341(4) . ? N5 Ru1 2.087(3) . ? N4 Ru1 1.983(3) . ? N3 Ru1 2.065(3) . ? N2 Ru1 2.096(3) . ? N1 Ru1 2.099(3) . ? O1 P1 1.604(3) . ? O2 P1 1.598(3) . ? O3 P1 1.600(2) . ? F1 P2 1.599(2) . ? F2 P2 1.591(2) . ? F3 P2 1.592(3) . ? F4 P2 1.585(3) . ? F5 P2 1.583(3) . ? F6 P2 1.589(3) . ? F7 P3 1.608(2) . ? F8 P3 1.605(2) . ? F9 P3 1.596(2) . ? F10 P3 1.599(2) . ? F11 P3 1.604(2) . ? F12 P3 1.595(2) . ? P1 Ru1 2.2268(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.9(4) . . ? C2 C1 O1 122.8(4) . . ? C6 C1 O1 116.2(4) . . ? C1 C2 C3 119.6(4) . . ? C2 C3 C4 119.9(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 120.7(4) . . ? C5 C6 C1 119.1(4) . . ? C12 C7 C8 121.8(4) . . ? C12 C7 O2 123.8(3) . . ? C8 C7 O2 114.4(4) . . ? C9 C8 C7 118.5(4) . . ? C10 C9 C8 121.8(4) . . ? C9 C10 C11 119.0(4) . . ? C10 C11 C12 120.9(4) . . ? C7 C12 C11 118.1(4) . . ? C14 C13 C18 122.0(4) . . ? C14 C13 O3 121.2(3) . . ? C18 C13 O3 116.6(3) . . ? C15 C14 C13 117.6(4) . . ? C16 C15 C14 121.9(4) . . ? C15 C16 C17 119.3(4) . . ? C18 C17 C16 120.8(4) . . ? C17 C18 C13 118.2(4) . . ? N5 C19 C20 122.0(4) . . ? C21 C20 C19 120.1(4) . . ? C20 C21 C22 118.7(5) . . ? C23 C22 C21 119.4(4) . . ? N5 C23 C22 121.0(4) . . ? N5 C23 C24 115.0(4) . . ? C22 C23 C24 123.9(4) . . ? N4 C24 C25 119.6(4) . . ? N4 C24 C23 112.8(4) . . ? C25 C24 C23 127.7(4) . . ? C26 C25 C24 118.5(4) . . ? C27 C26 C25 121.3(4) . . ? C26 C27 C28 118.6(4) . . ? N4 C28 C27 119.3(4) . . ? N4 C28 C29 113.2(4) . . ? C27 C28 C29 127.5(4) . . ? N3 C29 C30 120.4(4) . . ? N3 C29 C28 114.8(3) . . ? C30 C29 C28 124.7(4) . . ? C31 C30 C29 119.6(4) . . ? C32 C31 C30 119.5(4) . . ? C31 C32 C33 119.6(4) . . ? N3 C33 C32 122.1(4) . . ? N2 C34 C35 123.2(4) . . ? C36 C35 C34 118.6(4) . . ? C35 C36 C37 119.4(4) . . ? C36 C37 C38 119.5(4) . . ? N2 C38 C37 121.6(3) . . ? N2 C38 C39 115.3(3) . . ? C37 C38 C39 123.1(4) . . ? N1 C39 C40 122.0(3) . . ? N1 C39 C38 114.9(3) . . ? C40 C39 C38 123.1(4) . . ? C39 C40 C41 118.8(4) . . ? C40 C41 C42 119.3(3) . . ? C43 C42 C41 118.8(3) . . ? N1 C43 C42 123.1(3) . . ? C19 N5 C23 118.6(4) . . ? C19 N5 Ru1 127.6(3) . . ? C23 N5 Ru1 113.2(3) . . ? C24 N4 C28 122.6(3) . . ? C24 N4 Ru1 119.1(3) . . ? C28 N4 Ru1 117.6(3) . . ? C33 N3 C29 118.7(3) . . ? C33 N3 Ru1 127.3(3) . . ? C29 N3 Ru1 113.5(3) . . ? C34 N2 C38 117.6(3) . . ? C34 N2 Ru1 126.5(3) . . ? C38 N2 Ru1 115.8(2) . . ? C43 N1 C39 117.9(3) . . ? C43 N1 Ru1 126.2(2) . . ? C39 N1 Ru1 115.8(2) . . ? C1 O1 P1 125.2(2) . . ? C7 O2 P1 129.2(2) . . ? C13 O3 P1 124.7(2) . . ? O2 P1 O3 104.88(13) . . ? O2 P1 O1 105.29(13) . . ? O3 P1 O1 92.10(13) . . ? O2 P1 Ru1 112.02(9) . . ? O3 P1 Ru1 119.13(10) . . ? O1 P1 Ru1 120.72(11) . . ? F5 P2 F4 89.46(16) . . ? F5 P2 F6 179.17(17) . . ? F4 P2 F6 90.35(16) . . ? F5 P2 F2 90.48(16) . . ? F4 P2 F2 90.30(14) . . ? F6 P2 F2 90.33(15) . . ? F5 P2 F3 90.71(16) . . ? F4 P2 F3 179.78(18) . . ? F6 P2 F3 89.48(15) . . ? F2 P2 F3 89.55(13) . . ? F5 P2 F1 89.53(14) . . ? F4 P2 F1 89.83(14) . . ? F6 P2 F1 89.66(15) . . ? F2 P2 F1 179.87(18) . . ? F3 P2 F1 90.32(14) . . ? F12 P3 F9 90.39(13) . . ? F12 P3 F10 90.38(13) . . ? F9 P3 F10 179.12(15) . . ? F12 P3 F11 179.46(15) . . ? F9 P3 F11 89.87(12) . . ? F10 P3 F11 89.37(13) . . ? F12 P3 F8 90.40(13) . . ? F9 P3 F8 89.95(13) . . ? F10 P3 F8 89.60(12) . . ? F11 P3 F8 90.08(12) . . ? F12 P3 F7 90.16(12) . . ? F9 P3 F7 89.88(13) . . ? F10 P3 F7 90.56(13) . . ? F11 P3 F7 89.36(12) . . ? F8 P3 F7 179.42(15) . . ? N4 Ru1 N3 79.20(14) . . ? N4 Ru1 N5 78.72(13) . . ? N3 Ru1 N5 155.50(12) . . ? N4 Ru1 N2 176.62(11) . . ? N3 Ru1 N2 99.63(12) . . ? N5 Ru1 N2 101.81(12) . . ? N4 Ru1 N1 99.02(11) . . ? N3 Ru1 N1 87.04(12) . . ? N5 Ru1 N1 86.07(12) . . ? N2 Ru1 N1 77.72(12) . . ? N4 Ru1 P1 87.65(8) . . ? N3 Ru1 P1 95.74(8) . . ? N5 Ru1 P1 93.82(9) . . ? N2 Ru1 P1 95.63(9) . . ? N1 Ru1 P1 173.16(9) . . ? #====END data_([Ru]7) _database_code_depnum_ccdc_archive 'CCDC 665737' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H40 N5 P Ru, 2(F6 P)' _chemical_formula_sum 'C34 H40 F12 N5 P3 Ru' _chemical_formula_weight 940.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9512(9) _cell_length_b 15.1059(10) _cell_length_c 20.1824(14) _cell_angle_alpha 103.205(6) _cell_angle_beta 97.589(5) _cell_angle_gamma 102.186(5) _cell_volume 4259.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 6527 _cell_measurement_theta_min 2.7436 _cell_measurement_theta_max 32.1391 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8523 _exptl_absorpt_correction_T_max 0.9448 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_orient_matrix_ub_11 0.0014591661 _diffrn_orient_matrix_ub_12 -0.0477693061 _diffrn_orient_matrix_ub_13 -0.0099488202 _diffrn_orient_matrix_ub_21 0.0440451431 _diffrn_orient_matrix_ub_22 0.0111671263 _diffrn_orient_matrix_ub_23 0.0221694276 _diffrn_orient_matrix_ub_31 -0.0223875558 _diffrn_orient_matrix_ub_32 -0.0086393996 _diffrn_orient_matrix_ub_33 0.0275895937 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_unetI/netI 0.1262 _diffrn_reflns_number 30391 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 15520 _reflns_number_gt 9055 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Moreover, it was not possible to resolve properly diffuse electron-density residuals. Treatment with the SQUEEZE facility from PLATON, with a localized void of about 624.3 A \^E 3 and 109 recovered electrons resulted in a smooth refinement. Since a few low order reflections are missing from the data set, the electron count is underestimated. Consequently, the values given for rcalc, F(000) and the molecular weight are only valid for the ordered part of the structure. ; _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^)+(0.1430P)^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_number_reflns 15520 _refine_ls_number_parameters 933 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2527 _refine_ls_wR_factor_gt 0.2326 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.726 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.153 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ru Ru -1.2594 0.8363 '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' 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 C1 C 0.8461(5) 0.6529(5) 0.9241(4) 0.0301(17) Uani 1 1 d . . . H1 H 0.8283 0.6226 0.9602 0.036 Uiso 1 1 calc R . . C2 C 0.8828(6) 0.7574(6) 0.9609(5) 0.047(2) Uani 1 1 d . . . H2A H 0.9346 0.7662 0.9974 0.071 Uiso 1 1 calc R . . H2B H 0.8342 0.7807 0.9801 0.071 Uiso 1 1 calc R . . H2C H 0.9026 0.7911 0.9282 0.071 Uiso 1 1 calc R . . C3 C 0.9245(5) 0.6121(6) 0.8991(4) 0.0370(19) Uani 1 1 d . . . H3A H 0.9422 0.636 0.8613 0.055 Uiso 1 1 calc R . . H3B H 0.9035 0.5449 0.8839 0.055 Uiso 1 1 calc R . . H3C H 0.9772 0.6298 0.9364 0.055 Uiso 1 1 calc R . . C4 C 0.6459(6) 0.6355(6) 0.9058(4) 0.038(2) Uani 1 1 d . . . H4 H 0.5872 0.6078 0.8722 0.045 Uiso 1 1 calc R . . C5 C 0.6419(6) 0.5789(7) 0.9593(4) 0.045(2) Uani 1 1 d . . . H5A H 0.6908 0.6105 0.9987 0.067 Uiso 1 1 calc R . . H5B H 0.6497 0.5176 0.9393 0.067 Uiso 1 1 calc R . . H5C H 0.5827 0.5731 0.9736 0.067 Uiso 1 1 calc R . . C6 C 0.6425(7) 0.7379(6) 0.9397(5) 0.056(3) Uani 1 1 d . . . H6A H 0.5824 0.7378 0.9516 0.084 Uiso 1 1 calc R . . H6B H 0.6533 0.7754 0.9076 0.084 Uiso 1 1 calc R . . H6C H 0.6898 0.7638 0.9808 0.084 Uiso 1 1 calc R . . C7 C 0.7531(6) 0.7220(6) 0.8189(4) 0.0375(19) Uani 1 1 d . . . H7 H 0.7655 0.7762 0.8593 0.045 Uiso 1 1 calc R . . C8 C 0.8391(7) 0.7403(6) 0.7844(5) 0.050(2) Uani 1 1 d . . . H8A H 0.8262 0.6981 0.7389 0.075 Uiso 1 1 calc R . . H8B H 0.8916 0.7304 0.812 0.075 Uiso 1 1 calc R . . H8C H 0.8528 0.8039 0.7809 0.075 Uiso 1 1 calc R . . C9 C 0.6661(7) 0.7289(6) 0.7729(5) 0.049(2) Uani 1 1 d . . . H9A H 0.6704 0.7934 0.7733 0.074 Uiso 1 1 calc R . . H9B H 0.6117 0.705 0.7902 0.074 Uiso 1 1 calc R . . H9C H 0.6616 0.6926 0.7263 0.074 Uiso 1 1 calc R . . C10 C 0.7909(5) 0.4179(5) 0.9103(4) 0.0309(17) Uani 1 1 d . . . H10 H 0.7823 0.4745 0.9352 0.037 Uiso 1 1 calc R . . C11 C 0.8394(6) 0.3683(5) 0.9458(4) 0.0355(19) Uani 1 1 d . . . H11 H 0.8623 0.3917 0.9932 0.043 Uiso 1 1 calc R . . C12 C 0.8531(7) 0.2863(6) 0.9111(5) 0.048(2) Uani 1 1 d . . . H12 H 0.8886 0.2545 0.9338 0.057 Uiso 1 1 calc R . . C13 C 0.8135(6) 0.2494(6) 0.8407(5) 0.042(2) Uani 1 1 d . . . H13 H 0.819 0.1912 0.8164 0.05 Uiso 1 1 calc R . . C14 C 0.7648(6) 0.3026(5) 0.8073(4) 0.0348(19) Uani 1 1 d . . . C15 C 0.7176(5) 0.2677(5) 0.7348(4) 0.0335(18) Uani 1 1 d . . . C16 C 0.7142(6) 0.1787(6) 0.6923(4) 0.041(2) Uani 1 1 d . . . H16 H 0.7482 0.1402 0.7081 0.049 Uiso 1 1 calc R . . C17 C 0.6604(7) 0.1497(6) 0.6277(5) 0.050(2) Uani 1 1 d . . . H17 H 0.657 0.0908 0.5992 0.06 Uiso 1 1 calc R . . C18 C 0.6123(6) 0.2062(6) 0.6051(4) 0.037(2) Uani 1 1 d . . . H18 H 0.5733 0.1854 0.5618 0.045 Uiso 1 1 calc R . . C19 C 0.6209(6) 0.2950(6) 0.6463(4) 0.0360(19) Uani 1 1 d . . . H19 H 0.5905 0.3351 0.629 0.043 Uiso 1 1 calc R . . C20 C 0.8981(5) 0.4682(5) 0.7423(4) 0.0286(17) Uani 1 1 d . . . H20 H 0.9095 0.4419 0.779 0.034 Uiso 1 1 calc R . . C21 C 0.9666(6) 0.4846(6) 0.7036(4) 0.042(2) Uani 1 1 d . . . H21 H 1.0233 0.4702 0.7146 0.05 Uiso 1 1 calc R . . C22 C 0.9501(6) 0.5220(7) 0.6495(5) 0.048(2) Uani 1 1 d . . . H22 H 0.996 0.5355 0.6238 0.058 Uiso 1 1 calc R . . C23 C 0.8631(6) 0.5400(6) 0.6327(4) 0.042(2) Uani 1 1 d . . . H23 H 0.8499 0.5634 0.5948 0.051 Uiso 1 1 calc R . . C24 C 0.7975(5) 0.5229(5) 0.6727(4) 0.0289(17) Uani 1 1 d . . . C25 C 0.7022(6) 0.5328(5) 0.6557(4) 0.0331(18) Uani 1 1 d . . . C26 C 0.6625(6) 0.5597(6) 0.5997(4) 0.042(2) Uani 1 1 d . . . H26 H 0.699 0.5775 0.5688 0.051 Uiso 1 1 calc R . . C27 C 0.5729(7) 0.5603(7) 0.5896(5) 0.051(2) Uani 1 1 d . . . H27 H 0.5482 0.5795 0.5521 0.061 Uiso 1 1 calc R . . C28 C 0.5154(7) 0.5331(6) 0.6338(5) 0.047(2) Uani 1 1 d . . . H28 H 0.4524 0.5321 0.6261 0.056 Uiso 1 1 calc R . . C29 C 0.5561(5) 0.5075(6) 0.6897(4) 0.0334(18) Uani 1 1 d . . . C30 C 0.5077(5) 0.4703(6) 0.7405(4) 0.038(2) Uani 1 1 d . . . C31 C 0.4149(6) 0.4611(7) 0.7398(5) 0.049(2) Uani 1 1 d . . . H31 H 0.379 0.4799 0.7069 0.059 Uiso 1 1 calc R . . C32 C 0.3748(6) 0.4236(7) 0.7882(6) 0.057(3) Uani 1 1 d . . . H32 H 0.3126 0.4207 0.7907 0.069 Uiso 1 1 calc R . . C33 C 0.4288(6) 0.3902(6) 0.8331(5) 0.050(2) Uani 1 1 d . . . H33 H 0.4022 0.3613 0.8643 0.06 Uiso 1 1 calc R . . C34 C 0.5205(6) 0.3997(5) 0.8315(4) 0.0358(19) Uani 1 1 d . . . H34 H 0.5561 0.3779 0.8627 0.043 Uiso 1 1 calc R . . C44 C 0.3058(7) 0.8023(6) 0.5972(5) 0.048(2) Uani 1 1 d . . . H44 H 0.3614 0.8366 0.627 0.058 Uiso 1 1 calc R . . C45 C 0.3097(7) 0.7371(6) 0.5383(5) 0.052(2) Uani 1 1 d . . . H45 H 0.3672 0.729 0.529 0.062 Uiso 1 1 calc R . . C46 C 0.2305(8) 0.6846(8) 0.4938(5) 0.069(3) Uani 1 1 d . . . H46 H 0.2323 0.6388 0.4547 0.082 Uiso 1 1 calc R . . C47 C 0.1464(8) 0.7015(7) 0.5084(5) 0.068(3) Uani 1 1 d . . . H47 H 0.0907 0.6683 0.4784 0.082 Uiso 1 1 calc R . . C48 C 0.1467(7) 0.7699(6) 0.5695(4) 0.045(2) Uani 1 1 d . . . C49 C 0.0600(6) 0.7894(6) 0.5879(4) 0.040(2) Uani 1 1 d . . . C50 C -0.0284(7) 0.7474(7) 0.5460(5) 0.054(3) Uani 1 1 d . . . H50 H -0.034 0.7042 0.5037 0.065 Uiso 1 1 calc R . . C51 C -0.1056(7) 0.7691(7) 0.5663(5) 0.053(2) Uani 1 1 d . . . H51 H -0.1642 0.7421 0.5384 0.063 Uiso 1 1 calc R . . C52 C -0.0947(7) 0.8321(7) 0.6294(5) 0.054(2) Uani 1 1 d . . . H52 H -0.1462 0.848 0.6455 0.065 Uiso 1 1 calc R . . C53 C -0.0073(6) 0.8714(6) 0.6685(5) 0.047(2) Uani 1 1 d . . . H53 H -0.0008 0.9134 0.7115 0.056 Uiso 1 1 calc R . . C54 C 0.1914(6) 0.7219(5) 0.7466(4) 0.0375(19) Uani 1 1 d . . . H54 H 0.2135 0.6996 0.7066 0.045 Uiso 1 1 calc R . . C55 C 0.1717(6) 0.6639(6) 0.7881(5) 0.041(2) Uani 1 1 d . . . H55 H 0.1781 0.6026 0.7757 0.05 Uiso 1 1 calc R . . C56 C 0.1423(6) 0.6966(6) 0.8485(5) 0.046(2) Uani 1 1 d . . . H56 H 0.1332 0.6596 0.8792 0.055 Uiso 1 1 calc R . . C57 C 0.1262(6) 0.7863(7) 0.8633(5) 0.046(2) Uani 1 1 d . . . H57 H 0.1022 0.8081 0.9024 0.055 Uiso 1 1 calc R . . C58 C 0.1466(5) 0.8425(5) 0.8187(4) 0.0297(17) Uani 1 1 d . . . C59 C 0.1301(6) 0.9370(6) 0.8289(4) 0.042(2) Uani 1 1 d . . . C60 C 0.0842(6) 0.9793(6) 0.8762(4) 0.040(2) Uani 1 1 d . . . H60 H 0.0627 0.9495 0.9087 0.048 Uiso 1 1 calc R . . C61 C 0.0703(7) 1.0650(7) 0.8755(5) 0.058(3) Uani 1 1 d . . . H61 H 0.0402 1.0947 0.9081 0.069 Uiso 1 1 calc R . . C62 C 0.1011(8) 1.1086(7) 0.8256(6) 0.062(3) Uani 1 1 d . . . H62 H 0.0918 1.1674 0.8251 0.074 Uiso 1 1 calc R . . C63 C 0.1442(7) 1.0650(6) 0.7785(5) 0.047(2) Uani 1 1 d . . . C64 C 0.1745(7) 1.0958(6) 0.7181(5) 0.051(2) Uani 1 1 d . . . C65 C 0.2213(8) 1.0518(8) 0.6135(6) 0.070(3) Uani 1 1 d . . . H65 H 0.2345 1.006 0.5795 0.083 Uiso 1 1 calc R . . C66 C 0.2208(9) 1.1380(9) 0.6014(7) 0.080(4) Uani 1 1 d . . . H66 H 0.2352 1.1502 0.5605 0.096 Uiso 1 1 calc R . . C67 C 0.1991(9) 1.2045(9) 0.6493(7) 0.085(4) Uani 1 1 d . . . H67 H 0.202 1.2641 0.6431 0.102 Uiso 1 1 calc R . . C68 C 0.1722(8) 1.1814(7) 0.7087(6) 0.068(3) Uani 1 1 d . . . H68 H 0.1531 1.2243 0.7411 0.082 Uiso 1 1 calc R . . N2 N 0.7557(4) 0.3881(4) 0.8418(3) 0.0261(14) Uani 1 1 d . . . N1 N 0.6722(4) 0.3252(4) 0.7108(3) 0.0246(13) Uani 1 1 d . . . N5 N 0.8156(4) 0.4891(4) 0.7288(3) 0.0230(13) Uani 1 1 d . . . N4 N 0.6478(4) 0.5091(4) 0.7011(3) 0.0272(14) Uani 1 1 d . . . N3 N 0.5620(4) 0.4394(4) 0.7867(3) 0.0296(14) Uani 1 1 d . . . N7 N 0.2262(5) 0.8186(4) 0.6138(3) 0.0370(16) Uani 1 1 d . B . N6 N 0.0681(5) 0.8523(4) 0.6480(3) 0.0347(16) Uani 1 1 d . B . N8 N 0.1802(4) 0.8124(4) 0.7609(3) 0.0315(15) Uani 1 1 d . B . N9 N 0.1615(5) 0.9802(4) 0.7818(3) 0.0374(17) Uani 1 1 d . B . N10 N 0.2036(6) 1.0316(5) 0.6722(4) 0.053(2) Uani 1 1 d . B . P1 P 0.73912(13) 0.61895(13) 0.85533(10) 0.0240(4) Uani 1 1 d . . . P3 P 0.11750(15) 0.40258(15) 0.86760(11) 0.0328(5) Uani 1 1 d . . . P4 P 0.20284(16) 0.48004(17) 0.60010(12) 0.0418(6) Uani 1 1 d . . . Ru1 Ru 0.70094(4) 0.46289(4) 0.77640(3) 0.02321(18) Uani 1 1 d . . . Ru2 Ru 0.20760(5) 0.90966(4) 0.70501(3) 0.0348(2) Uani 1 1 d . . . C38 C 0.3964(7) 1.0534(6) 0.8516(5) 0.0586(16) Uani 1 1 d D . . H38 H 0.4613 1.0531 0.8668 0.07 Uiso 1 1 calc R A 1 P2A P 0.3617(6) 0.9846(5) 0.7570(4) 0.0350(12) Uani 0.5 1 d P B 1 C35A C 0.4111(11) 1.0823(13) 0.7208(8) 0.0586(16) Uani 0.5 1 d PD B 1 H35A H 0.3624 1.1164 0.7175 0.07 Uiso 0.5 1 calc PR B 1 C36A C 0.4227(14) 1.0470(14) 0.6464(7) 0.0586(16) Uani 0.5 1 d PD B 1 H36A H 0.4137 1.092 0.6214 0.088 Uiso 0.5 1 d P C 1 H36B H 0.378 0.9882 0.625 0.088 Uiso 0.5 1 d P D 1 H36C H 0.4846 1.038 0.6464 0.088 Uiso 0.5 1 d P E 1 C37A C 0.4975(12) 1.1566(13) 0.7620(8) 0.0586(16) Uani 0.5 1 d PD B 1 H37A H 0.5496 1.1289 0.7651 0.088 Uiso 0.5 1 calc PR B 1 H37B H 0.4875 1.182 0.8078 0.088 Uiso 0.5 1 calc PR B 1 H37C H 0.5102 1.206 0.7393 0.088 Uiso 0.5 1 calc PR B 1 C39A C 0.3982(14) 1.1486(9) 0.8371(9) 0.0586(16) Uani 0.5 1 d PD B 1 H39A H 0.3357 1.1555 0.8284 0.088 Uiso 0.5 1 calc PR B 1 H39B H 0.426 1.1523 0.7973 0.088 Uiso 0.5 1 calc PR B 1 H39C H 0.434 1.1978 0.8765 0.088 Uiso 0.5 1 calc PR B 1 C40A C 0.3471(13) 1.0426(13) 0.9112(8) 0.0586(16) Uani 0.5 1 d PD B 1 H40A H 0.3875 1.079 0.9541 0.088 Uiso 0.5 1 calc PR B 1 H40B H 0.3312 0.9776 0.9113 0.088 Uiso 0.5 1 calc PR B 1 H40C H 0.2914 1.0643 0.906 0.088 Uiso 0.5 1 calc PR B 1 C41A C 0.4492(12) 0.9118(11) 0.7549(9) 0.0586(16) Uani 0.5 1 d PD B 1 H41A H 0.4784 0.9152 0.7145 0.07 Uiso 0.5 1 calc PR B 1 C42A C 0.4120(15) 0.8088(10) 0.7518(10) 0.0586(16) Uani 0.5 1 d PD B 1 H42A H 0.4624 0.784 0.7677 0.088 Uiso 0.5 1 calc PR B 1 H42B H 0.3838 0.7744 0.7049 0.088 Uiso 0.5 1 calc PR B 1 H42C H 0.3664 0.8031 0.7809 0.088 Uiso 0.5 1 calc PR B 1 C43A C 0.5252(12) 0.9573(12) 0.8209(9) 0.0586(16) Uani 0.5 1 d PD B 1 H43A H 0.497 0.9812 0.859 0.088 Uiso 0.5 1 calc PR B 1 H43B H 0.57 1.0079 0.8132 0.088 Uiso 0.5 1 calc PR B 1 H43C H 0.5559 0.9111 0.8316 0.088 Uiso 0.5 1 calc PR B 1 P2B P 0.3737(6) 0.9595(5) 0.7752(4) 0.0350(12) Uani 0.5 1 d P B 2 C35B C 0.4077(12) 0.8649(13) 0.8164(9) 0.063(2) Uani 0.5 1 d PD B 2 H35B H 0.3527 0.8399 0.8344 0.076 Uiso 0.5 1 calc PR B 2 C36B C 0.4184(15) 0.7815(13) 0.7629(9) 0.063(2) Uani 0.5 1 d PD B 2 H36D H 0.4623 0.8027 0.7357 0.095 Uiso 0.5 1 calc PR B 2 H36E H 0.3592 0.7499 0.7331 0.095 Uiso 0.5 1 calc PR B 2 H36F H 0.4404 0.7389 0.7858 0.095 Uiso 0.5 1 calc PR B 2 C37B C 0.4875(12) 0.8947(14) 0.8786(8) 0.063(2) Uani 0.5 1 d PD B 2 H37D H 0.4848 0.8453 0.9015 0.095 Uiso 0.5 1 calc PR B 2 H37E H 0.4822 0.9505 0.9103 0.095 Uiso 0.5 1 calc PR B 2 H37F H 0.5459 0.907 0.8633 0.095 Uiso 0.5 1 calc PR B 2 C39B C 0.3397(14) 1.1204(15) 0.8703(12) 0.063(2) Uani 0.5 1 d P B 2 H39D H 0.2832 1.0888 0.8815 0.095 Uiso 0.5 1 calc PR B 2 H39E H 0.3249 1.1458 0.832 0.095 Uiso 0.5 1 calc PR B 2 H39F H 0.3741 1.1704 0.9098 0.095 Uiso 0.5 1 calc PR B 2 C40B C 0.3689(14) 0.9759(15) 0.8967(12) 0.063(2) Uani 0.5 1 d P B 2 H40D H 0.3062 0.9716 0.9041 0.095 Uiso 0.5 1 calc PR B 2 H40E H 0.4108 0.9956 0.9407 0.095 Uiso 0.5 1 calc PR B 2 H40F H 0.3739 0.9156 0.8715 0.095 Uiso 0.5 1 calc PR B 2 C41B C 0.4721(12) 0.9930(12) 0.7279(9) 0.063(2) Uani 0.5 1 d PD B 2 H41B H 0.4906 0.9352 0.709 0.076 Uiso 0.5 1 calc PR B 2 C42B C 0.4466(14) 1.0320(15) 0.6668(9) 0.063(2) Uani 0.5 1 d PD B 2 H42D H 0.4362 1.0931 0.6835 0.095 Uiso 0.5 1 calc PR B 2 H42E H 0.3909 0.9908 0.6369 0.095 Uiso 0.5 1 calc PR B 2 H42F H 0.4966 1.0368 0.6414 0.095 Uiso 0.5 1 calc PR B 2 C43B C 0.5583(11) 1.0612(14) 0.7773(9) 0.063(2) Uani 0.5 1 d PD B 2 H43D H 0.6113 1.0629 0.755 0.095 Uiso 0.5 1 calc PR B 2 H43E H 0.5699 1.0405 0.8185 0.095 Uiso 0.5 1 calc PR B 2 H43F H 0.5477 1.1228 0.7895 0.095 Uiso 0.5 1 calc PR B 2 F1 F 0.1635(5) 0.4539(7) 0.8173(5) 0.122(3) Uani 1 1 d . . . F2A F 0.0753(6) 0.3465(9) 0.9161(5) 0.169(5) Uani 1 1 d . . . F3 F 0.0475(5) 0.4662(6) 0.8711(4) 0.100(2) Uani 1 1 d . . . F4 F 0.1927(4) 0.3417(4) 0.8629(4) 0.0794(19) Uani 1 1 d . . . F5A F 0.0461(5) 0.3305(5) 0.8063(4) 0.110(3) Uani 1 1 d . . . F6 F 0.1902(5) 0.4740(5) 0.9309(4) 0.114(3) Uani 1 1 d . . . F7 F 0.1052(5) 0.4107(5) 0.6017(3) 0.0809(19) Uani 1 1 d . . . F8 F 0.2958(4) 0.5480(5) 0.6029(5) 0.099(3) Uani 1 1 d . . . F9 F 0.1546(4) 0.5654(4) 0.6079(3) 0.0654(16) Uani 1 1 d . . . F10 F 0.2519(5) 0.3958(4) 0.5925(3) 0.0746(18) Uani 1 1 d . . . F11 F 0.1710(5) 0.4548(5) 0.5200(3) 0.086(2) Uani 1 1 d . . . F12 F 0.2245(6) 0.4989(6) 0.6825(3) 0.107(3) Uani 1 1 d . . . P5 P 0.6086(2) 0.8333(2) 0.57239(17) 0.0616(7) Uani 1 1 d . . . F13 F 0.5486(7) 0.7882(6) 0.6209(5) 0.1337(13) Uani 1 1 d . . . F14 F 0.6755(7) 0.8805(7) 0.5340(5) 0.1337(13) Uani 1 1 d . . . F15 F 0.5341(7) 0.8890(6) 0.5578(5) 0.1337(13) Uani 1 1 d . . . F16 F 0.6774(7) 0.7774(6) 0.5939(5) 0.1337(13) Uani 1 1 d . . . F17 F 0.5562(7) 0.7483(7) 0.5121(5) 0.1337(13) Uani 1 1 d . . . F18 F 0.6560(7) 0.9158(7) 0.6399(5) 0.1337(13) Uani 1 1 d . . . P6 P 0.19003(19) 0.98121(16) 0.07315(14) 0.0501(6) Uani 1 1 d . . . F19A F 0.2186(7) 1.0266(6) 0.0166(6) 0.1429(14) Uani 1 1 d . . . F20 F 0.1447(7) 0.9367(6) 0.1305(6) 0.1429(14) Uani 1 1 d . . . F21 F 0.1126(7) 0.9013(6) 0.0250(6) 0.1429(14) Uani 1 1 d . . . F22A F 0.2745(7) 1.0616(6) 0.1196(6) 0.1429(14) Uani 1 1 d . . . F23 F 0.1164(7) 1.0426(6) 0.0766(6) 0.1429(14) Uani 1 1 d . . . F24A F 0.2573(7) 0.9221(6) 0.0900(6) 0.1429(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(4) 0.027(4) 0.026(4) 0.004(3) -0.005(3) 0.011(3) C2 0.040(5) 0.043(5) 0.047(5) 0.007(4) -0.016(4) 0.005(4) C3 0.020(4) 0.049(5) 0.039(5) 0.010(4) -0.001(3) 0.008(4) C4 0.031(4) 0.038(5) 0.039(5) -0.001(4) 0.007(4) 0.013(4) C5 0.032(5) 0.065(6) 0.037(5) 0.012(4) 0.012(4) 0.012(4) C6 0.059(6) 0.044(6) 0.062(6) -0.004(5) 0.027(5) 0.016(5) C7 0.045(5) 0.039(5) 0.032(4) 0.018(4) 0.000(4) 0.011(4) C8 0.067(7) 0.041(5) 0.046(5) 0.016(4) 0.017(5) 0.010(5) C9 0.065(6) 0.039(5) 0.046(5) 0.015(4) -0.002(5) 0.021(5) C10 0.040(5) 0.029(4) 0.027(4) 0.012(3) 0.007(3) 0.011(3) C11 0.045(5) 0.034(5) 0.025(4) 0.005(3) -0.001(4) 0.012(4) C12 0.060(6) 0.042(5) 0.050(6) 0.025(5) 0.003(5) 0.021(5) C13 0.053(6) 0.028(4) 0.050(6) 0.018(4) 0.009(4) 0.015(4) C14 0.037(5) 0.025(4) 0.040(5) 0.012(4) 0.002(4) 0.001(3) C15 0.034(4) 0.026(4) 0.038(5) 0.008(4) 0.012(4) 0.000(3) C16 0.041(5) 0.033(5) 0.044(5) 0.001(4) 0.005(4) 0.009(4) C17 0.066(7) 0.029(5) 0.042(5) -0.005(4) 0.013(5) -0.002(4) C18 0.045(5) 0.036(5) 0.022(4) 0.000(4) 0.006(4) 0.000(4) C19 0.034(5) 0.041(5) 0.028(4) 0.005(4) 0.004(4) 0.004(4) C20 0.031(4) 0.029(4) 0.022(4) 0.002(3) 0.004(3) 0.005(3) C21 0.035(5) 0.046(5) 0.041(5) 0.000(4) 0.012(4) 0.011(4) C22 0.039(5) 0.063(6) 0.040(5) 0.006(5) 0.024(4) 0.004(4) C23 0.056(6) 0.043(5) 0.026(4) 0.011(4) 0.011(4) 0.006(4) C24 0.033(4) 0.021(4) 0.031(4) 0.005(3) 0.008(3) 0.005(3) C25 0.055(5) 0.023(4) 0.022(4) 0.005(3) 0.006(4) 0.014(4) C26 0.047(6) 0.050(5) 0.028(4) 0.011(4) 0.002(4) 0.010(4) C27 0.064(7) 0.053(6) 0.037(5) 0.018(4) -0.004(5) 0.019(5) C28 0.044(5) 0.053(6) 0.047(5) 0.018(5) -0.002(4) 0.018(4) C29 0.028(4) 0.039(5) 0.029(4) 0.004(4) -0.004(3) 0.011(4) C30 0.027(4) 0.043(5) 0.039(5) 0.009(4) -0.003(4) 0.007(4) C31 0.039(5) 0.056(6) 0.047(6) 0.005(5) 0.007(4) 0.009(4) C32 0.027(5) 0.064(7) 0.073(7) 0.009(6) 0.005(5) 0.008(5) C33 0.043(6) 0.048(6) 0.052(6) 0.001(5) 0.023(5) -0.001(4) C34 0.038(5) 0.028(4) 0.042(5) 0.009(4) 0.015(4) 0.004(4) C44 0.059(6) 0.041(5) 0.042(5) 0.008(4) 0.021(5) 0.002(4) C45 0.059(6) 0.048(6) 0.053(6) 0.015(5) 0.023(5) 0.014(5) C46 0.075(8) 0.071(7) 0.040(6) -0.012(5) 0.021(6) -0.002(6) C47 0.074(8) 0.065(7) 0.036(5) -0.018(5) 0.013(5) -0.011(6) C48 0.063(6) 0.036(5) 0.033(5) 0.005(4) 0.018(4) 0.004(4) C49 0.049(5) 0.041(5) 0.031(5) 0.010(4) 0.014(4) 0.008(4) C50 0.067(7) 0.048(6) 0.033(5) 0.001(4) 0.001(5) 0.000(5) C51 0.048(6) 0.056(6) 0.050(6) 0.013(5) 0.005(5) 0.008(5) C52 0.047(6) 0.059(6) 0.061(7) 0.020(5) 0.007(5) 0.017(5) C53 0.051(6) 0.051(6) 0.040(5) 0.005(4) 0.007(4) 0.025(5) C54 0.034(5) 0.032(5) 0.043(5) 0.003(4) 0.000(4) 0.011(4) C55 0.037(5) 0.043(5) 0.050(5) 0.020(4) 0.012(4) 0.012(4) C56 0.038(5) 0.047(5) 0.060(6) 0.031(5) 0.005(4) 0.010(4) C57 0.031(5) 0.066(6) 0.039(5) 0.022(5) 0.007(4) 0.001(4) C58 0.028(4) 0.029(4) 0.028(4) 0.006(3) 0.004(3) 0.001(3) C59 0.046(5) 0.027(4) 0.042(5) 0.001(4) 0.010(4) -0.004(4) C60 0.044(5) 0.042(5) 0.027(4) -0.001(4) 0.011(4) 0.004(4) C61 0.064(7) 0.052(6) 0.042(6) -0.014(5) 0.020(5) 0.008(5) C62 0.077(8) 0.035(5) 0.068(7) 0.001(5) 0.026(6) 0.007(5) C63 0.064(6) 0.025(4) 0.049(6) 0.003(4) 0.029(5) 0.000(4) C64 0.069(7) 0.029(5) 0.058(6) 0.015(4) 0.024(5) 0.007(4) C65 0.093(9) 0.063(7) 0.070(7) 0.032(6) 0.040(7) 0.024(6) C66 0.100(10) 0.068(8) 0.090(9) 0.048(7) 0.041(8) 0.015(7) C67 0.114(11) 0.057(7) 0.104(10) 0.041(7) 0.051(9) 0.023(7) C68 0.089(9) 0.043(6) 0.077(8) 0.017(5) 0.026(7) 0.019(6) N2 0.031(4) 0.022(3) 0.026(3) 0.008(3) 0.008(3) 0.007(3) N1 0.028(3) 0.023(3) 0.025(3) 0.009(3) 0.007(3) 0.007(3) N5 0.025(3) 0.024(3) 0.019(3) 0.006(3) 0.005(2) 0.004(3) N4 0.026(3) 0.024(3) 0.031(3) 0.009(3) 0.004(3) 0.005(3) N3 0.032(4) 0.026(3) 0.030(4) 0.006(3) 0.005(3) 0.008(3) N7 0.046(4) 0.027(4) 0.033(4) 0.007(3) 0.012(3) -0.002(3) N6 0.045(4) 0.030(4) 0.025(4) 0.004(3) 0.006(3) 0.007(3) N8 0.019(3) 0.038(4) 0.031(4) 0.004(3) -0.001(3) 0.002(3) N9 0.051(4) 0.027(4) 0.028(4) 0.003(3) 0.012(3) -0.002(3) N10 0.066(5) 0.042(5) 0.055(5) 0.016(4) 0.029(4) 0.004(4) P1 0.0256(10) 0.0248(10) 0.0239(10) 0.0090(8) 0.0030(8) 0.0092(8) P3 0.0378(12) 0.0348(12) 0.0292(11) 0.0120(9) 0.0039(9) 0.0144(9) P4 0.0408(13) 0.0526(14) 0.0336(12) 0.0087(11) 0.0039(10) 0.0197(11) Ru1 0.0248(3) 0.0241(3) 0.0207(3) 0.0067(2) 0.0030(2) 0.0059(2) Ru2 0.0427(4) 0.0271(4) 0.0310(4) 0.0034(3) 0.0135(3) 0.0015(3) C38 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) P2A 0.033(2) 0.039(4) 0.029(3) 0.0070(18) 0.007(2) 0.001(2) C35A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C36A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C37A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C39A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C40A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C41A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C42A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) C43A 0.054(4) 0.060(4) 0.058(4) 0.009(3) 0.012(3) 0.013(3) P2B 0.033(2) 0.039(4) 0.029(3) 0.0070(18) 0.007(2) 0.001(2) C35B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C36B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C37B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C39B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C40B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C41B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C42B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) C43B 0.048(4) 0.067(5) 0.071(5) 0.017(4) 0.011(4) 0.007(4) F1 0.091(6) 0.194(9) 0.145(7) 0.138(7) 0.055(5) 0.053(6) F2A 0.091(6) 0.325(15) 0.187(9) 0.217(11) 0.063(6) 0.070(7) F3 0.092(5) 0.132(6) 0.093(5) 0.011(5) 0.011(4) 0.084(5) F4 0.071(4) 0.063(4) 0.109(5) 0.020(4) 0.001(4) 0.041(3) F5A 0.068(5) 0.073(5) 0.143(7) -0.024(4) -0.032(4) 0.006(4) F6 0.105(6) 0.103(6) 0.091(5) -0.046(4) -0.035(4) 0.044(5) F7 0.077(4) 0.087(5) 0.091(5) 0.038(4) 0.035(4) 0.018(4) F8 0.049(4) 0.076(5) 0.178(8) 0.044(5) 0.013(4) 0.021(3) F9 0.052(3) 0.060(4) 0.082(4) 0.007(3) 0.005(3) 0.028(3) F10 0.097(5) 0.071(4) 0.088(5) 0.036(3) 0.044(4) 0.056(4) F11 0.130(6) 0.096(5) 0.034(3) 0.013(3) 0.001(3) 0.047(4) F12 0.125(6) 0.153(7) 0.052(4) 0.012(4) 0.001(4) 0.077(6) P5 0.0491(16) 0.0589(18) 0.080(2) 0.0225(16) 0.0113(15) 0.0151(14) F13 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) F14 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) F15 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) F16 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) F17 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) F18 0.140(3) 0.116(3) 0.143(3) 0.025(3) 0.012(3) 0.045(2) P6 0.0615(17) 0.0292(12) 0.0559(16) 0.0089(11) -0.0019(13) 0.0139(12) F19A 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) F20 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) F21 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) F22A 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) F23 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) F24A 0.144(3) 0.093(3) 0.176(4) 0.041(3) 0.001(3) 0.009(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C3 1.527(11) . ? C1 C2 1.529(11) . ? C1 P1 1.868(7) . ? C4 C5 1.522(11) . ? C4 C6 1.558(11) . ? C4 P1 1.857(8) . ? C7 C9 1.533(11) . ? C7 C8 1.544(12) . ? C7 P1 1.854(8) . ? C10 N2 1.347(9) . ? C10 C11 1.393(11) . ? C11 C12 1.346(11) . ? C12 C13 1.400(12) . ? C13 C14 1.412(11) . ? C14 N2 1.363(10) . ? C14 C15 1.461(11) . ? C15 N1 1.343(10) . ? C15 C16 1.407(11) . ? C16 C17 1.361(12) . ? C17 C18 1.343(13) . ? C18 C19 1.377(11) . ? C19 N1 1.346(9) . ? C20 N5 1.346(9) . ? C20 C21 1.382(11) . ? C21 C22 1.359(12) . ? C22 C23 1.397(13) . ? C23 C24 1.370(11) . ? C24 N5 1.362(9) . ? C24 C25 1.467(11) . ? C25 N4 1.360(9) . ? C25 C26 1.391(11) . ? C26 C27 1.330(12) . ? C27 C28 1.386(13) . ? C28 C29 1.382(11) . ? C29 N4 1.355(9) . ? C29 C30 1.476(11) . ? C30 C31 1.363(12) . ? C30 N3 1.380(10) . ? C31 C32 1.379(13) . ? C32 C33 1.383(14) . ? C33 C34 1.353(12) . ? C34 N3 1.343(9) . ? C44 N7 1.335(11) . ? C44 C45 1.377(12) . ? C45 C46 1.355(14) . ? C46 C47 1.390(15) . ? C47 C48 1.414(12) . ? C48 N7 1.342(11) . ? C48 C49 1.465(12) . ? C49 N6 1.331(10) . ? C49 C50 1.404(13) . ? C50 C51 1.354(13) . ? C51 C52 1.371(13) . ? C52 C53 1.367(13) . ? C53 N6 1.316(11) . ? C54 C55 1.360(11) . ? C54 N8 1.383(10) . ? C55 C56 1.371(12) . ? C56 C57 1.399(13) . ? C57 C58 1.391(11) . ? C58 N8 1.352(9) . ? C58 C59 1.473(11) . ? C59 N9 1.351(10) . ? C59 C60 1.367(11) . ? C60 C61 1.357(13) . ? C61 C62 1.398(14) . ? C62 C63 1.346(13) . ? C63 N9 1.374(11) . ? C63 C64 1.491(12) . ? C64 C68 1.355(13) . ? C64 N10 1.365(12) . ? C65 N10 1.333(12) . ? C65 C66 1.381(15) . ? C66 C67 1.349(16) . ? C67 C68 1.408(15) . ? N2 Ru1 2.116(6) . ? N1 Ru1 2.116(6) . ? N5 Ru1 2.084(5) . ? N4 Ru1 1.957(6) . ? N3 Ru1 2.079(6) . ? N7 Ru2 2.121(7) . ? N6 Ru2 2.138(7) . ? N8 Ru2 2.055(6) . ? N9 Ru2 1.962(6) . ? N10 Ru2 2.105(8) . ? P1 Ru1 2.4284(19) . ? P3 F2A 1.547(7) . ? P3 F5A 1.550(7) . ? P3 F1 1.557(6) . ? P3 F3 1.561(6) . ? P3 F6 1.577(7) . ? P3 F4 1.595(6) . ? P4 F8 1.529(7) . ? P4 F11 1.557(6) . ? P4 F10 1.586(6) . ? P4 F9 1.594(6) . ? P4 F12 1.599(7) . ? P4 F7 1.616(7) . ? Ru2 P2A 2.325(9) . ? Ru2 P2B 2.556(8) . ? C38 C39B 1.47(2) . ? C38 C40A 1.513(7) . ? C38 C39A 1.527(7) . ? C38 C40B 1.66(2) . ? C38 P2B 1.779(12) . ? C38 P2A 1.898(12) . ? P2A C35A 1.853(19) . ? P2A C41A 1.88(2) . ? C35A C37A 1.516(10) . ? C35A C36A 1.521(10) . ? C41A C42A 1.522(10) . ? C41A C43A 1.546(10) . ? P2B C41B 1.90(2) . ? P2B C35B 1.93(2) . ? C35B C36B 1.513(10) . ? C35B C37B 1.525(10) . ? C41B C42B 1.522(7) . ? C41B C43B 1.532(7) . ? P5 F14 1.504(11) . ? P5 F17 1.533(10) . ? P5 F16 1.540(9) . ? P5 F15 1.568(10) . ? P5 F18 1.583(10) . ? P5 F13 1.583(11) . ? P6 F21 1.523(10) . ? P6 F19A 1.523(11) . ? P6 F24A 1.534(10) . ? P6 F22A 1.571(10) . ? P6 F23 1.581(11) . ? P6 F20 1.620(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C1 C2 110.4(7) . . ? C3 C1 P1 112.4(5) . . ? C2 C1 P1 116.6(5) . . ? C5 C4 C6 109.8(7) . . ? C5 C4 P1 112.1(6) . . ? C6 C4 P1 117.7(6) . . ? C9 C7 C8 110.7(7) . . ? C9 C7 P1 115.9(6) . . ? C8 C7 P1 115.1(6) . . ? N2 C10 C11 123.2(7) . . ? C12 C11 C10 119.7(8) . . ? C11 C12 C13 119.4(8) . . ? C12 C13 C14 118.5(8) . . ? N2 C14 C13 121.8(7) . . ? N2 C14 C15 116.0(7) . . ? C13 C14 C15 122.1(7) . . ? N1 C15 C16 120.5(7) . . ? N1 C15 C14 115.3(7) . . ? C16 C15 C14 124.1(8) . . ? C17 C16 C15 119.1(8) . . ? C18 C17 C16 120.0(8) . . ? C17 C18 C19 119.8(8) . . ? N1 C19 C18 121.5(8) . . ? N5 C20 C21 122.3(7) . . ? C22 C21 C20 119.2(8) . . ? C21 C22 C23 119.2(8) . . ? C24 C23 C22 119.5(8) . . ? N5 C24 C23 121.2(7) . . ? N5 C24 C25 115.6(6) . . ? C23 C24 C25 123.1(7) . . ? N4 C25 C26 118.4(8) . . ? N4 C25 C24 113.2(6) . . ? C26 C25 C24 128.4(7) . . ? C27 C26 C25 121.0(8) . . ? C26 C27 C28 121.5(8) . . ? C29 C28 C27 116.9(8) . . ? N4 C29 C28 121.8(7) . . ? N4 C29 C30 111.8(6) . . ? C28 C29 C30 126.3(7) . . ? C31 C30 N3 121.6(8) . . ? C31 C30 C29 123.1(8) . . ? N3 C30 C29 115.2(7) . . ? C30 C31 C32 119.3(9) . . ? C31 C32 C33 118.7(9) . . ? C34 C33 C32 120.0(9) . . ? N3 C34 C33 122.3(8) . . ? N7 C44 C45 123.3(9) . . ? C46 C45 C44 120.5(10) . . ? C45 C46 C47 117.8(9) . . ? C46 C47 C48 119.2(10) . . ? N7 C48 C47 121.6(9) . . ? N7 C48 C49 116.9(7) . . ? C47 C48 C49 121.4(9) . . ? N6 C49 C50 119.6(8) . . ? N6 C49 C48 116.4(8) . . ? C50 C49 C48 124.0(8) . . ? C51 C50 C49 120.7(9) . . ? C50 C51 C52 117.9(9) . . ? C53 C52 C51 119.4(9) . . ? N6 C53 C52 122.9(9) . . ? C55 C54 N8 123.1(8) . . ? C54 C55 C56 119.3(8) . . ? C55 C56 C57 119.2(8) . . ? C58 C57 C56 119.0(8) . . ? N8 C58 C57 122.0(8) . . ? N8 C58 C59 114.9(7) . . ? C57 C58 C59 123.1(7) . . ? N9 C59 C60 120.3(8) . . ? N9 C59 C58 112.1(7) . . ? C60 C59 C58 127.5(8) . . ? C61 C60 C59 119.5(8) . . ? C60 C61 C62 120.0(9) . . ? C63 C62 C61 119.7(9) . . ? C62 C63 N9 119.6(8) . . ? C62 C63 C64 127.7(9) . . ? N9 C63 C64 112.7(7) . . ? C68 C64 N10 122.0(9) . . ? C68 C64 C63 122.4(9) . . ? N10 C64 C63 115.6(7) . . ? N10 C65 C66 122.5(11) . . ? C67 C66 C65 119.8(11) . . ? C66 C67 C68 118.4(11) . . ? C64 C68 C67 119.2(11) . . ? C10 N2 C14 117.3(6) . . ? C10 N2 Ru1 128.5(5) . . ? C14 N2 Ru1 113.8(5) . . ? C15 N1 C19 118.9(7) . . ? C15 N1 Ru1 115.1(5) . . ? C19 N1 Ru1 125.6(5) . . ? C20 N5 C24 118.5(6) . . ? C20 N5 Ru1 128.3(5) . . ? C24 N5 Ru1 112.8(5) . . ? C29 N4 C25 120.4(7) . . ? C29 N4 Ru1 120.6(5) . . ? C25 N4 Ru1 118.6(5) . . ? C34 N3 C30 117.9(7) . . ? C34 N3 Ru1 128.7(5) . . ? C30 N3 Ru1 113.4(5) . . ? C44 N7 C48 117.6(7) . . ? C44 N7 Ru2 127.9(6) . . ? C48 N7 Ru2 114.5(6) . . ? C53 N6 C49 119.5(8) . . ? C53 N6 Ru2 125.8(6) . . ? C49 N6 Ru2 114.7(6) . . ? C58 N8 C54 117.2(7) . . ? C58 N8 Ru2 114.4(5) . . ? C54 N8 Ru2 128.3(5) . . ? C59 N9 C63 120.7(7) . . ? C59 N9 Ru2 119.3(6) . . ? C63 N9 Ru2 118.7(5) . . ? C65 N10 C64 117.7(8) . . ? C65 N10 Ru2 129.6(7) . . ? C64 N10 Ru2 112.6(6) . . ? C7 P1 C4 101.6(4) . . ? C7 P1 C1 102.1(4) . . ? C4 P1 C1 103.0(4) . . ? C7 P1 Ru1 118.8(3) . . ? C4 P1 Ru1 111.5(3) . . ? C1 P1 Ru1 117.6(2) . . ? F2A P3 F5A 87.9(6) . . ? F2A P3 F1 176.2(6) . . ? F5A P3 F1 91.3(5) . . ? F2A P3 F3 94.9(5) . . ? F5A P3 F3 87.9(4) . . ? F1 P3 F3 88.9(4) . . ? F2A P3 F6 90.9(6) . . ? F5A P3 F6 178.6(5) . . ? F1 P3 F6 89.8(5) . . ? F3 P3 F6 92.9(4) . . ? F2A P3 F4 87.9(5) . . ? F5A P3 F4 93.3(4) . . ? F1 P3 F4 88.4(4) . . ? F3 P3 F4 177.0(4) . . ? F6 P3 F4 85.9(4) . . ? F8 P4 F11 95.9(4) . . ? F8 P4 F10 90.2(4) . . ? F11 P4 F10 90.4(4) . . ? F8 P4 F9 89.3(3) . . ? F11 P4 F9 89.7(4) . . ? F10 P4 F9 179.4(4) . . ? F8 P4 F12 90.5(5) . . ? F11 P4 F12 173.6(5) . . ? F10 P4 F12 90.0(4) . . ? F9 P4 F12 90.0(4) . . ? F8 P4 F7 176.8(4) . . ? F11 P4 F7 87.1(4) . . ? F10 P4 F7 90.7(4) . . ? F9 P4 F7 89.8(3) . . ? F12 P4 F7 86.5(4) . . ? N4 Ru1 N3 78.9(2) . . ? N4 Ru1 N5 79.8(2) . . ? N3 Ru1 N5 157.7(2) . . ? N4 Ru1 N1 91.7(2) . . ? N3 Ru1 N1 89.3(2) . . ? N5 Ru1 N1 84.7(2) . . ? N4 Ru1 N2 168.4(2) . . ? N3 Ru1 N2 102.6(2) . . ? N5 Ru1 N2 97.0(2) . . ? N1 Ru1 N2 76.9(2) . . ? N4 Ru1 P1 90.87(18) . . ? N3 Ru1 P1 92.00(17) . . ? N5 Ru1 P1 94.92(16) . . ? N1 Ru1 P1 177.32(17) . . ? N2 Ru1 P1 100.49(17) . . ? N9 Ru2 N8 78.9(3) . . ? N9 Ru2 N10 80.0(3) . . ? N8 Ru2 N10 158.1(3) . . ? N9 Ru2 N7 167.5(3) . . ? N8 Ru2 N7 98.0(2) . . ? N10 Ru2 N7 101.4(3) . . ? N9 Ru2 N6 90.2(3) . . ? N8 Ru2 N6 87.5(2) . . ? N10 Ru2 N6 86.8(3) . . ? N7 Ru2 N6 77.4(3) . . ? N9 Ru2 P2A 91.8(3) . . ? N8 Ru2 P2A 100.1(2) . . ? N10 Ru2 P2A 86.3(3) . . ? N7 Ru2 P2A 100.7(3) . . ? N6 Ru2 P2A 172.4(2) . . ? N9 Ru2 P2B 91.8(3) . . ? N8 Ru2 P2B 86.7(2) . . ? N10 Ru2 P2B 99.7(3) . . ? N7 Ru2 P2B 100.2(3) . . ? N6 Ru2 P2B 173.4(2) . . ? P2A Ru2 P2B 13.59(19) . . ? C39B C38 C40A 64.7(10) . . ? C39B C38 C39A 48.6(10) . . ? C40A C38 C39A 110.9(6) . . ? C39B C38 C40B 104.3(12) . . ? C39A C38 C40B 151.6(10) . . ? C39B C38 P2B 127.5(11) . . ? C40A C38 P2B 120.6(9) . . ? C39A C38 P2B 113.5(9) . . ? C40B C38 P2B 89.4(9) . . ? C39B C38 P2A 112.5(11) . . ? C40A C38 P2A 129.2(10) . . ? C39A C38 P2A 94.8(9) . . ? C40B C38 P2A 105.9(9) . . ? C35A P2A C41A 105.0(9) . . ? C35A P2A C38 96.6(7) . . ? C41A P2A C38 98.8(7) . . ? C35A P2A Ru2 112.8(6) . . ? C41A P2A Ru2 118.1(6) . . ? C38 P2A Ru2 122.2(5) . . ? C37A C35A C36A 110.2(9) . . ? C37A C35A P2A 119.3(14) . . ? C36A C35A P2A 111.8(13) . . ? C42A C41A C43A 108.3(9) . . ? C42A C41A P2A 116.3(14) . . ? C43A C41A P2A 107.4(12) . . ? C38 P2B C41B 104.7(7) . . ? C38 P2B C35B 98.9(6) . . ? C41B P2B C35B 104.0(9) . . ? C38 P2B Ru2 116.1(5) . . ? C41B P2B Ru2 117.2(5) . . ? C35B P2B Ru2 113.7(6) . . ? C36B C35B C37B 110.7(9) . . ? C36B C35B P2B 112.3(13) . . ? C37B C35B P2B 119.0(13) . . ? C42B C41B C43B 109.5(7) . . ? C42B C41B P2B 115.3(14) . . ? C43B C41B P2B 111.8(13) . . ? F14 P5 F17 97.9(6) . . ? F14 P5 F16 91.4(5) . . ? F17 P5 F16 90.2(5) . . ? F14 P5 F15 94.2(5) . . ? F17 P5 F15 91.8(5) . . ? F16 P5 F15 173.7(6) . . ? F14 P5 F18 88.4(5) . . ? F17 P5 F18 173.6(6) . . ? F16 P5 F18 89.1(5) . . ? F15 P5 F18 88.3(5) . . ? F14 P5 F13 172.8(6) . . ? F17 P5 F13 88.0(5) . . ? F16 P5 F13 84.3(5) . . ? F15 P5 F13 89.7(5) . . ? F18 P5 F13 85.6(5) . . ? F21 P6 F19A 95.4(6) . . ? F21 P6 F24A 97.4(5) . . ? F19A P6 F24A 109.7(6) . . ? F21 P6 F22A 176.2(6) . . ? F19A P6 F22A 82.4(5) . . ? F24A P6 F22A 80.5(5) . . ? F21 P6 F23 87.0(5) . . ? F19A P6 F23 84.7(6) . . ? F24A P6 F23 164.3(6) . . ? F22A P6 F23 95.9(5) . . ? F21 P6 F20 80.8(5) . . ? F19A P6 F20 171.3(6) . . ? F24A P6 F20 78.6(5) . . ? F22A P6 F20 101.8(5) . . ? F23 P6 F20 87.3(5) . . ? #====END