# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 #====================================================================== # end of cif file # Attachment '- brie8i.cif' data_global4 _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- brie8i.cif' #====================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Holdt, Hans-J\"urgen Universit\"at Potsdam Institut f\"ur Chemie Karl-Liebknecht-Str. 24-25 14476 Golm Germany ; _publ_contact_author_phone +49-331-977-5180 _publ_contact_author_fax +49-331-977-5055 _publ_contact_author_email holdt@chem.uni-potsdam.de #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Mono- and dinuclear ruthenium(II) 1,6,7,12-tetraazaperylene complexes ; loop_ _publ_author_name _publ_author_address T.Brietzke ; Universit\"at Potsdam Institut f\"ur Chemie Anorganische Chemie Karl-Liebknecht-Str. 24-25 14476 Golm Bundesrepublik Deutschland ; W.Mickler ; Universit\"at Potsdam Institut f\"ur Chemie Anorganische Chemie Karl-Liebknecht-Str. 24-25 14476 Golm Bundesrepublik Deutschland ; A.Kelling ; Universit\"at Potsdam Institut f\"ur Chemie Anorganische Chemie Karl-Liebknecht-Str. 24-25 14476 Golm Bundesrepublik Deutschland ; 'Hans-J\"urgen Holdt' ; Universit\"at Potsdam Institut f\"ur Chemie Anorganische Chemie Karl-Liebknecht-Str. 24-25 14476 Golm Bundesrepublik Deutschland ; _publ_contact_author_name 'Holdt, Hans-Jurgen' #====================================================================== data_brie2i _database_code_depnum_ccdc_archive 'CCDC 844735' #TrackingRef '- brie2i.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,6,7,12-Tetraazaperylene ; _chemical_name_common 1,6,7,12-Tetraazaperylene _chemical_melting_point ? _chemical_formula_moiety 'C16 H8 N4 , C2 H2 Cl6' _chemical_formula_sum 'C18 H10 Cl6 N4' _chemical_formula_weight 495.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.436(4) _cell_length_b 5.6121(7) _cell_length_c 19.241(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.222(17) _cell_angle_gamma 90.00 _cell_volume 1975.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 7331 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 29.39 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 1.300 _exptl_crystal_size_mid 0.533 _exptl_crystal_size_min 0.140 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method ? _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.88 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.7805 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was embedded in perfluoropolyalkylether oil. ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 210(2) _diffrn_measurement_method 'rotation method, delta omega = 1.0 deg' _diffrn_measurement_details ; 180 frames, detector distance = 100 mm ; _diffrn_reflns_number 6042 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1743 _reflns_number_gt 1460 _reflns_threshold_expression >2sigma(I) _publ_section_exptl_refinement ; All hydrogen atoms were found from the difference Fourier map. ; _computing_data_collection 'X-AREA (Stoe, 2006)' _computing_cell_refinement 'X-AREA (Stoe, 2002)' _computing_data_reduction 'X-RED32 (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0338P)^2^+4.2796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1743 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15811(17) 0.6451(6) -0.02729(16) 0.0363(7) Uani 1 1 d . . . H1 H 0.1872(19) 0.507(7) -0.0195(17) 0.044 Uiso 1 1 d . . . C2 C 0.05607(14) 0.8173(5) 0.00760(13) 0.0254(6) Uani 1 1 d . . . C3 C -0.00047(14) 0.8258(5) 0.05548(13) 0.0256(6) Uani 1 1 d . . . C4 C -0.05077(17) 0.6755(6) 0.14920(15) 0.0358(7) Uani 1 1 d . . . H4 H -0.0484(18) 0.545(6) 0.1844(18) 0.043 Uiso 1 1 d . . . C5 C -0.10559(17) 0.8401(6) 0.14453(15) 0.0345(7) Uani 1 1 d . . . H5 H -0.1433(19) 0.837(6) 0.1754(17) 0.041 Uiso 1 1 d . . . C6 C -0.10877(15) 1.0148(5) 0.09149(14) 0.0296(6) Uani 1 1 d . . . C7 C -0.05443(14) 1.0080(5) 0.04596(13) 0.0257(6) Uani 1 1 d . . . C8 C -0.16176(17) 1.1960(6) 0.08065(16) 0.0364(7) Uani 1 1 d . . . H8 H -0.1996(19) 1.206(6) 0.1085(18) 0.044 Uiso 1 1 d . . . C9 C 0.13891(17) 0.3375(5) 0.15438(16) 0.0329(6) Uani 1 1 d . . . H9 H 0.1088(19) 0.432(6) 0.1225(17) 0.040 Uiso 1 1 d . . . Cl1 Cl 0.19381(5) 0.15247(16) 0.10849(5) 0.0508(3) Uani 1 1 d . . . Cl2 Cl 0.08278(6) 0.16548(17) 0.20179(5) 0.0552(3) Uani 1 1 d . . . Cl3 Cl 0.19503(5) 0.52575(17) 0.21102(5) 0.0540(3) Uani 1 1 d . . . N1 N 0.10641(13) 0.6481(4) 0.01657(12) 0.0318(5) Uani 1 1 d . . . N2 N 0.00160(13) 0.6634(4) 0.10558(12) 0.0318(5) 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 0.0341(16) 0.0354(17) 0.0390(16) -0.0022(13) 0.0029(12) 0.0087(14) C2 0.0262(14) 0.0244(14) 0.0241(12) -0.0048(11) -0.0029(10) -0.0004(11) C3 0.0268(14) 0.0251(14) 0.0237(12) -0.0014(11) -0.0018(10) -0.0020(11) C4 0.0395(17) 0.0380(17) 0.0300(15) 0.0065(13) 0.0047(13) -0.0022(14) C5 0.0341(16) 0.0407(17) 0.0293(14) -0.0007(13) 0.0068(12) -0.0046(14) C6 0.0274(14) 0.0330(15) 0.0281(13) -0.0050(12) 0.0021(11) -0.0030(12) C7 0.0258(13) 0.0275(14) 0.0228(12) -0.0025(11) -0.0011(10) -0.0012(11) C8 0.0315(16) 0.0437(17) 0.0353(16) -0.0057(14) 0.0093(13) 0.0030(14) C9 0.0370(16) 0.0289(15) 0.0322(14) 0.0017(12) 0.0015(12) 0.0043(13) Cl1 0.0533(5) 0.0481(5) 0.0508(5) -0.0138(4) 0.0062(4) 0.0139(4) Cl2 0.0597(6) 0.0507(5) 0.0569(5) 0.0111(4) 0.0144(4) -0.0101(4) Cl3 0.0550(5) 0.0499(5) 0.0575(5) -0.0219(4) 0.0085(4) -0.0090(4) N1 0.0328(13) 0.0306(13) 0.0309(12) -0.0022(10) 0.0002(10) 0.0061(11) N2 0.0338(13) 0.0311(13) 0.0296(12) 0.0051(10) 0.0000(10) -0.0012(11) _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 1.350(4) . ? C1 C8 1.368(4) 5_575 ? C1 H1 0.94(4) . ? C2 N1 1.324(4) . ? C2 C7 1.420(4) 5_575 ? C2 C3 1.476(4) . ? C3 N2 1.324(4) . ? C3 C7 1.422(4) . ? C4 N2 1.358(4) . ? C4 C5 1.364(4) . ? C4 H4 0.99(4) . ? C5 C6 1.411(4) . ? C5 H5 0.97(3) . ? C6 C8 1.407(4) . ? C6 C7 1.412(4) . ? C7 C2 1.420(4) 5_575 ? C8 C1 1.368(4) 5_575 ? C8 H8 0.93(4) . ? C9 Cl2 1.753(3) . ? C9 Cl3 1.758(3) . ? C9 Cl1 1.763(3) . ? C9 H9 0.94(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C8 124.5(3) . 5_575 ? N1 C1 H1 110(2) . . ? C8 C1 H1 125(2) 5_575 . ? N1 C2 C7 122.7(2) . 5_575 ? N1 C2 C3 118.7(2) . . ? C7 C2 C3 118.6(2) 5_575 . ? N2 C3 C7 123.0(2) . . ? N2 C3 C2 118.3(2) . . ? C7 C3 C2 118.7(2) . . ? N2 C4 C5 124.9(3) . . ? N2 C4 H4 114(2) . . ? C5 C4 H4 121(2) . . ? C4 C5 C6 118.8(3) . . ? C4 C5 H5 122(2) . . ? C6 C5 H5 119(2) . . ? C8 C6 C5 125.0(3) . . ? C8 C6 C7 117.5(3) . . ? C5 C6 C7 117.5(3) . . ? C6 C7 C2 118.6(2) . 5_575 ? C6 C7 C3 118.6(2) . . ? C2 C7 C3 122.7(2) 5_575 . ? C1 C8 C6 118.9(3) 5_575 . ? C1 C8 H8 120(2) 5_575 . ? C6 C8 H8 121(2) . . ? Cl2 C9 Cl3 110.38(16) . . ? Cl2 C9 Cl1 110.47(17) . . ? Cl3 C9 Cl1 109.53(17) . . ? Cl2 C9 H9 108(2) . . ? Cl3 C9 H9 109(2) . . ? Cl1 C9 H9 110(2) . . ? C2 N1 C1 117.8(3) . . ? C3 N2 C4 117.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.1(4) . . . . ? C7 C2 C3 N2 -179.6(2) 5_575 . . . ? N1 C2 C3 C7 179.8(2) . . . . ? C7 C2 C3 C7 0.2(4) 5_575 . . . ? N2 C4 C5 C6 -0.9(5) . . . . ? C4 C5 C6 C8 -179.6(3) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C8 C6 C7 C2 0.2(4) . . . 5_575 ? C5 C6 C7 C2 -179.6(2) . . . 5_575 ? C8 C6 C7 C3 -179.6(2) . . . . ? C5 C6 C7 C3 0.6(4) . . . . ? N2 C3 C7 C6 -0.7(4) . . . . ? C2 C3 C7 C6 179.6(2) . . . . ? N2 C3 C7 C2 179.6(2) . . . 5_575 ? C2 C3 C7 C2 -0.2(4) . . . 5_575 ? C5 C6 C8 C1 179.6(3) . . . 5_575 ? C7 C6 C8 C1 -0.1(4) . . . 5_575 ? C7 C2 N1 C1 0.4(4) 5_575 . . . ? C3 C2 N1 C1 -179.3(3) . . . . ? C8 C1 N1 C2 -0.4(5) 5_575 . . . ? C7 C3 N2 C4 -0.1(4) . . . . ? C2 C3 N2 C4 179.7(3) . . . . ? C5 C4 N2 C3 0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.305 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.059 #====================================================================== data_brie4i _database_code_depnum_ccdc_archive 'CCDC 844736' #TrackingRef '- brie4i.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(2,2'-Bipyridyl)(1,6,7,12-tetraazaperylene)-ruthenium(ii) bis(hexafluorophosphate) ; _chemical_name_common ; bis(2,2'-Bipyridyl)(1,6,7,12-tetraazaperylene)-ruthenium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 N8 Ru1 2+ , F12 P2 2- , C1 H1.5 N0.5 , C3.5 H4' _chemical_formula_sum 'C40.50 H29.50 F12 N8.50 P2 Ru' _chemical_formula_weight 1026.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9023(13) _cell_length_b 12.5034(14) _cell_length_c 16.7340(18) _cell_angle_alpha 76.174(9) _cell_angle_beta 76.325(9) _cell_angle_gamma 83.086(9) _cell_volume 2147.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 17578 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 29.46 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.850 _exptl_crystal_size_mid 0.700 _exptl_crystal_size_min 0.690 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method ? _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 0.53 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.6962 _exptl_absorpt_correction_T_max 0.6994 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was embedded in perfluoropolyalkylether oil. ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 210(2) _diffrn_measurement_method 'rotation method, delta omega = 1.0 deg' _diffrn_measurement_details ; 180 frames, detector distance = 100 mm ; _diffrn_reflns_number 13509 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7096 _reflns_number_gt 5881 _reflns_threshold_expression >2sigma(I) _publ_section_exptl_refinement ; All hydrogen atoms were calculated in idealized positions and allowed to ride on their corresponding carbon atoms. ; _computing_data_collection 'X-AREA (Stoe, 2006)' _computing_cell_refinement 'X-AREA (Stoe, 2002)' _computing_data_reduction 'X-RED32 (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0568P)^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 SHELXL _refine_ls_extinction_coef 0.0023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7096 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1628(3) 1.0567(2) 0.7483(2) 0.0454(8) Uani 1 1 d . . . H1 H 0.1655 1.0491 0.8045 0.054 Uiso 1 1 calc R . . C2 C 0.1599(4) 1.1588(3) 0.6991(2) 0.0525(9) Uani 1 1 d . . . H2 H 0.1603 1.2196 0.7220 0.063 Uiso 1 1 calc R . . C3 C 0.1509(4) 1.2761(3) 0.5551(3) 0.0617(10) Uani 1 1 d . . . H3 H 0.1493 1.3421 0.5718 0.074 Uiso 1 1 calc R . . C4 C 0.1482(4) 1.2768(3) 0.4745(2) 0.0640(11) Uani 1 1 d . . . H4 H 0.1431 1.3452 0.4379 0.077 Uiso 1 1 calc R . . C5 C 0.1736(4) 0.8963(4) 0.3582(2) 0.0660(11) Uani 1 1 d . . . H5 H 0.1791 0.9006 0.3012 0.079 Uiso 1 1 calc R . . C6 C 0.1704(4) 0.7939(4) 0.4103(3) 0.0666(11) Uani 1 1 d . . . H6 H 0.1735 0.7313 0.3889 0.080 Uiso 1 1 calc R . . C7 C 0.1553(4) 0.6860(3) 0.5594(2) 0.0635(10) Uani 1 1 d . . . H7 H 0.1529 0.6192 0.5448 0.076 Uiso 1 1 calc R . . C8 C 0.1520(4) 0.6866(3) 0.6402(2) 0.0543(9) Uani 1 1 d . . . H8 H 0.1479 0.6199 0.6796 0.065 Uiso 1 1 calc R . . C9 C 0.1591(3) 0.9757(2) 0.63798(19) 0.0381(7) Uani 1 1 d . . . C10 C 0.1573(3) 1.0791(2) 0.5819(2) 0.0415(7) Uani 1 1 d . . . C11 C 0.1570(3) 1.0881(3) 0.4955(2) 0.0453(8) Uani 1 1 d . . . C12 C 0.1625(3) 0.9861(3) 0.4645(2) 0.0467(8) Uani 1 1 d . . . C13 C 0.1613(3) 0.8832(3) 0.52365(19) 0.0437(7) Uani 1 1 d . . . C14 C 0.1576(3) 0.8769(2) 0.60893(19) 0.0400(7) Uani 1 1 d . . . C15 C 0.1562(3) 1.1750(3) 0.6131(2) 0.0491(8) Uani 1 1 d . . . C16 C 0.1623(4) 0.7846(3) 0.4962(2) 0.0544(9) Uani 1 1 d . . . C17 C 0.4412(3) 0.8392(3) 0.7091(2) 0.0478(8) Uani 1 1 d . . . H17 H 0.4135 0.9126 0.6920 0.057 Uiso 1 1 calc R . . C18 C 0.5674(3) 0.8099(3) 0.6898(2) 0.0576(9) Uani 1 1 d . . . H18 H 0.6243 0.8628 0.6601 0.069 Uiso 1 1 calc R . . C19 C 0.6103(4) 0.7014(3) 0.7145(3) 0.0627(10) Uani 1 1 d . . . H19 H 0.6960 0.6798 0.7018 0.075 Uiso 1 1 calc R . . C20 C 0.5225(3) 0.6255(3) 0.7588(2) 0.0568(9) Uani 1 1 d . . . H20 H 0.5491 0.5521 0.7771 0.068 Uiso 1 1 calc R . . C21 C 0.3960(3) 0.6585(3) 0.7758(2) 0.0438(7) Uani 1 1 d . . . C22 C 0.2952(3) 0.5844(2) 0.8204(2) 0.0446(7) Uani 1 1 d . . . C23 C 0.3171(4) 0.4713(3) 0.8446(3) 0.0599(10) Uani 1 1 d . . . H23 H 0.3984 0.4381 0.8334 0.072 Uiso 1 1 calc R . . C24 C 0.2140(4) 0.4081(3) 0.8863(3) 0.0652(11) Uani 1 1 d . . . H24 H 0.2258 0.3318 0.9033 0.078 Uiso 1 1 calc R . . C25 C 0.0968(4) 0.4589(3) 0.9015(2) 0.0557(9) Uani 1 1 d . . . H25 H 0.0278 0.4176 0.9299 0.067 Uiso 1 1 calc R . . C26 C 0.0798(3) 0.5711(3) 0.8751(2) 0.0472(8) Uani 1 1 d . . . H26 H -0.0014 0.6049 0.8854 0.057 Uiso 1 1 calc R . . C27 C 0.2667(3) 0.8329(3) 0.9324(2) 0.0468(8) Uani 1 1 d . . . H27 H 0.3461 0.8286 0.8970 0.056 Uiso 1 1 calc R . . C28 C 0.2597(4) 0.8422(3) 1.0137(2) 0.0551(9) Uani 1 1 d . . . H28 H 0.3327 0.8453 1.0325 0.066 Uiso 1 1 calc R . . C29 C 0.1431(4) 0.8467(3) 1.0663(2) 0.0558(9) Uani 1 1 d . . . H29 H 0.1358 0.8502 1.1221 0.067 Uiso 1 1 calc R . . C30 C 0.0369(4) 0.8462(3) 1.0357(2) 0.0505(8) Uani 1 1 d . . . H30 H -0.0430 0.8503 1.0705 0.061 Uiso 1 1 calc R . . C31 C 0.0495(3) 0.8394(2) 0.95254(19) 0.0398(7) Uani 1 1 d . . . C32 C -0.0583(3) 0.8449(2) 0.91231(19) 0.0397(7) Uani 1 1 d . . . C33 C -0.1815(3) 0.8715(3) 0.9489(2) 0.0496(8) Uani 1 1 d . . . H33 H -0.2019 0.8809 1.0041 0.059 Uiso 1 1 calc R . . C34 C -0.2746(3) 0.8844(3) 0.9037(3) 0.0575(10) Uani 1 1 d . . . H34 H -0.3582 0.9024 0.9278 0.069 Uiso 1 1 calc R . . C35 C -0.2418(3) 0.8701(3) 0.8226(3) 0.0588(10) Uani 1 1 d . . . H35 H -0.3028 0.8807 0.7903 0.071 Uiso 1 1 calc R . . C36 C -0.1188(3) 0.8401(3) 0.7891(2) 0.0504(8) Uani 1 1 d . . . H36 H -0.0983 0.8276 0.7347 0.060 Uiso 1 1 calc R . . F1 F -0.2425(2) 1.4408(2) 0.7364(2) 0.0940(9) Uani 1 1 d . . . F2 F 0.0545(2) 1.42638(19) 0.71510(19) 0.0808(7) Uani 1 1 d . . . F3 F -0.0882(2) 1.30544(16) 0.72521(15) 0.0695(6) Uani 1 1 d . . . F4 F -0.0773(3) 1.4616(2) 0.62622(16) 0.0982(9) Uani 1 1 d . . . F5 F -0.1002(3) 1.56033(17) 0.72636(18) 0.0827(8) Uani 1 1 d . . . F6 F -0.1096(3) 1.4027(2) 0.82437(16) 0.0822(7) Uani 1 1 d . . . F7 F 0.3125(2) 1.1427(3) 0.85141(18) 0.0904(8) Uani 1 1 d . A . F8 F 0.6129(2) 1.1205(2) 0.8178(2) 0.0956(9) Uani 1 1 d . A . F9A F 0.4524(5) 1.0318(6) 0.9105(6) 0.118(3) Uani 0.70 1 d P A 1 F10A F 0.4675(7) 1.0592(10) 0.7705(8) 0.142(3) Uani 0.70 1 d P A 1 F11A F 0.4679(7) 1.2394(7) 0.7632(6) 0.132(3) Uani 0.70 1 d P A 1 F12A F 0.4517(5) 1.2085(7) 0.8993(5) 0.0970(17) Uani 0.70 1 d P A 1 F9B F 0.4680(16) 1.0040(10) 0.8349(18) 0.127(6) Uani 0.30 1 d P A 2 F10B F 0.4600(15) 1.159(2) 0.7353(7) 0.130(6) Uani 0.30 1 d P A 2 F11B F 0.4672(15) 1.2507(10) 0.831(2) 0.137(6) Uani 0.30 1 d P A 2 F12B F 0.4721(11) 1.107(2) 0.9218(6) 0.105(5) Uani 0.30 1 d P A 2 N1 N 0.1621(2) 0.96278(19) 0.71897(16) 0.0380(6) Uani 1 1 d . . . N2 N 0.1525(3) 1.1852(3) 0.44238(18) 0.0558(8) Uani 1 1 d . . . N3 N 0.1695(3) 0.9926(3) 0.38351(18) 0.0579(8) Uani 1 1 d . . . N4 N 0.1545(2) 0.7821(2) 0.66711(16) 0.0404(6) Uani 1 1 d . . . N5 N 0.3549(2) 0.7659(2) 0.75200(16) 0.0393(6) Uani 1 1 d . . . N6 N 0.1783(2) 0.6339(2) 0.83445(16) 0.0400(6) Uani 1 1 d . . . N7 N 0.1638(2) 0.82960(18) 0.90157(16) 0.0379(6) Uani 1 1 d . . . N8 N -0.0265(2) 0.82799(19) 0.83227(16) 0.0401(6) Uani 1 1 d . . . P1 P -0.09474(10) 1.43287(7) 0.72569(6) 0.0538(2) Uani 1 1 d . . . P2 P 0.46412(10) 1.13276(8) 0.83201(7) 0.0572(3) Uani 1 1 d . . . Ru1 Ru 0.16366(2) 0.801111(19) 0.784561(15) 0.03489(10) Uani 1 1 d . . . N9 N 0.5000 1.0000 0.5000 0.164(4) Uani 1 2 d S . . C41 C 0.5057(10) 1.0937(12) 0.5217(7) 0.103(4) Uani 0.50 1 d P . . C42 C 0.5025(10) 1.2112(11) 0.5329(10) 0.116(4) Uani 0.50 1 d P . . H42C H 0.5294 1.2102 0.5837 0.174 Uiso 0.50 1 calc PR . . H42B H 0.4178 1.2444 0.5364 0.174 Uiso 0.50 1 calc PR . . H42A H 0.5582 1.2531 0.4856 0.174 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0545(19) 0.0408(16) 0.0383(17) -0.0132(14) -0.0069(15) 0.0096(14) C2 0.064(2) 0.0389(16) 0.053(2) -0.0116(15) -0.0164(18) 0.0101(15) C3 0.071(2) 0.0417(17) 0.060(2) -0.0008(17) -0.007(2) 0.0118(17) C4 0.066(2) 0.052(2) 0.053(2) 0.0106(18) -0.0016(19) 0.0115(17) C5 0.069(3) 0.095(3) 0.0354(18) -0.019(2) -0.0091(18) -0.005(2) C6 0.077(3) 0.080(3) 0.052(2) -0.023(2) -0.024(2) 0.000(2) C7 0.082(3) 0.059(2) 0.057(2) -0.0199(18) -0.020(2) -0.009(2) C8 0.069(2) 0.0458(17) 0.051(2) -0.0100(16) -0.0162(19) -0.0077(16) C9 0.0323(15) 0.0427(15) 0.0346(16) -0.0053(13) -0.0045(13) 0.0037(12) C10 0.0330(15) 0.0449(16) 0.0385(17) -0.0023(14) -0.0035(13) 0.0070(12) C11 0.0324(15) 0.0552(18) 0.0367(17) 0.0013(15) -0.0009(13) 0.0059(13) C12 0.0357(16) 0.063(2) 0.0360(17) -0.0050(15) -0.0060(14) 0.0012(14) C13 0.0392(17) 0.0551(18) 0.0346(16) -0.0088(14) -0.0072(14) 0.0015(14) C14 0.0311(15) 0.0483(16) 0.0371(16) -0.0068(14) -0.0043(13) 0.0000(12) C15 0.0478(19) 0.0412(16) 0.048(2) -0.0038(15) -0.0029(16) 0.0101(14) C16 0.055(2) 0.069(2) 0.0434(19) -0.0192(17) -0.0134(17) -0.0015(17) C17 0.0443(18) 0.0512(17) 0.0448(18) -0.0096(15) -0.0045(15) -0.0022(15) C18 0.0421(19) 0.072(2) 0.052(2) -0.0090(18) -0.0004(16) -0.0071(17) C19 0.0390(19) 0.079(3) 0.064(2) -0.017(2) -0.0055(18) 0.0109(17) C20 0.049(2) 0.058(2) 0.057(2) -0.0102(18) -0.0094(18) 0.0136(16) C21 0.0440(18) 0.0478(17) 0.0382(17) -0.0092(14) -0.0102(14) 0.0049(14) C22 0.0509(19) 0.0416(15) 0.0390(17) -0.0047(14) -0.0126(15) 0.0040(14) C23 0.065(2) 0.0452(18) 0.063(2) -0.0075(17) -0.013(2) 0.0118(17) C24 0.086(3) 0.0378(17) 0.066(3) 0.0006(17) -0.018(2) -0.0006(18) C25 0.066(2) 0.0426(17) 0.053(2) 0.0028(16) -0.0130(19) -0.0110(16) C26 0.0482(19) 0.0474(17) 0.0423(18) -0.0028(15) -0.0078(15) -0.0063(14) C27 0.0493(19) 0.0474(17) 0.0453(18) -0.0064(14) -0.0193(16) 0.0007(14) C28 0.072(3) 0.0473(18) 0.052(2) -0.0091(16) -0.031(2) 0.0019(17) C29 0.087(3) 0.0457(17) 0.0363(18) -0.0091(15) -0.0171(19) -0.0020(18) C30 0.066(2) 0.0426(16) 0.0380(17) -0.0065(14) -0.0034(16) -0.0037(15) C31 0.0486(18) 0.0280(13) 0.0380(16) -0.0012(12) -0.0069(14) -0.0007(12) C32 0.0461(17) 0.0286(13) 0.0381(17) -0.0007(12) -0.0052(14) 0.0012(12) C33 0.052(2) 0.0414(16) 0.0448(19) -0.0078(14) 0.0056(16) 0.0039(14) C34 0.0375(18) 0.0547(19) 0.069(3) -0.0049(18) -0.0022(17) 0.0052(15) C35 0.0421(19) 0.068(2) 0.062(2) -0.0057(19) -0.0159(18) 0.0027(16) C36 0.0459(19) 0.0587(19) 0.0444(18) -0.0055(16) -0.0136(15) 0.0008(15) F1 0.0598(15) 0.1016(19) 0.129(3) -0.0416(18) -0.0285(16) 0.0103(13) F2 0.0552(14) 0.0703(14) 0.113(2) -0.0292(14) -0.0061(14) 0.0036(11) F3 0.0869(16) 0.0475(11) 0.0770(16) -0.0164(10) -0.0239(13) 0.0025(11) F4 0.148(3) 0.0758(16) 0.0585(15) -0.0041(13) -0.0237(17) 0.0198(16) F5 0.0855(17) 0.0485(12) 0.107(2) -0.0239(12) -0.0050(15) 0.0081(11) F6 0.101(2) 0.0842(16) 0.0607(14) -0.0159(13) -0.0134(14) -0.0099(14) F7 0.0615(16) 0.131(2) 0.0916(19) -0.0516(18) -0.0215(14) 0.0079(15) F8 0.0578(15) 0.0894(18) 0.125(3) -0.0192(17) 0.0013(15) 0.0010(13) F9A 0.087(4) 0.084(3) 0.135(6) 0.041(4) -0.001(3) 0.000(3) F10A 0.122(5) 0.166(7) 0.178(8) -0.141(6) -0.011(6) 0.005(6) F11A 0.163(6) 0.092(5) 0.098(5) 0.033(4) -0.008(5) 0.012(5) F12A 0.084(3) 0.120(5) 0.108(4) -0.065(4) -0.025(3) 0.006(3) F9B 0.127(11) 0.057(6) 0.190(18) -0.047(9) 0.008(14) -0.023(6) F10B 0.129(11) 0.189(16) 0.048(6) -0.019(10) -0.001(6) 0.033(14) F11B 0.133(11) 0.044(6) 0.24(2) -0.066(12) -0.020(18) 0.016(6) F12B 0.075(7) 0.190(15) 0.045(5) -0.005(9) -0.013(4) -0.025(10) N1 0.0384(13) 0.0399(12) 0.0329(13) -0.0079(11) -0.0057(11) 0.0039(10) N2 0.0494(17) 0.0616(18) 0.0413(16) 0.0051(14) -0.0027(13) 0.0074(14) N3 0.0538(18) 0.080(2) 0.0357(15) -0.0062(15) -0.0101(13) -0.0005(15) N4 0.0403(14) 0.0419(13) 0.0384(14) -0.0081(11) -0.0091(12) -0.0001(11) N5 0.0381(14) 0.0420(13) 0.0360(13) -0.0092(11) -0.0067(11) 0.0031(11) N6 0.0409(14) 0.0415(13) 0.0374(14) -0.0059(11) -0.0127(12) 0.0012(11) N7 0.0441(14) 0.0313(11) 0.0360(13) -0.0041(10) -0.0097(11) 0.0019(10) N8 0.0418(14) 0.0380(12) 0.0362(14) -0.0015(11) -0.0103(11) 0.0044(11) P1 0.0572(6) 0.0450(5) 0.0567(6) -0.0113(4) -0.0126(5) 0.0072(4) P2 0.0573(6) 0.0505(5) 0.0602(6) -0.0123(5) -0.0085(5) 0.0033(4) Ru1 0.03545(14) 0.03539(14) 0.03102(14) -0.00395(9) -0.00706(10) 0.00166(9) N9 0.207(11) 0.110(6) 0.128(8) 0.030(6) -0.008(7) 0.000(7) C41 0.060(6) 0.132(10) 0.081(7) 0.037(8) -0.011(5) 0.000(6) C42 0.053(6) 0.128(10) 0.179(14) -0.072(9) -0.019(7) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.345(4) . ? C1 N1 1.378(4) . ? C2 C15 1.414(5) . ? C3 C4 1.354(6) . ? C3 C15 1.403(4) . ? C4 N2 1.368(5) . ? C5 N3 1.361(5) . ? C5 C6 1.365(6) . ? C6 C16 1.398(5) . ? C7 C8 1.346(5) . ? C7 C16 1.417(5) . ? C8 N4 1.378(4) . ? C9 N1 1.334(4) . ? C9 C10 1.405(4) . ? C9 C14 1.434(4) . ? C10 C15 1.415(5) . ? C10 C11 1.425(5) . ? C11 N2 1.326(4) . ? C11 C12 1.478(5) . ? C12 N3 1.323(4) . ? C12 C13 1.422(4) . ? C13 C14 1.402(4) . ? C13 C16 1.413(5) . ? C14 N4 1.340(4) . ? C17 N5 1.346(4) . ? C17 C18 1.363(5) . ? C18 C19 1.379(5) . ? C19 C20 1.383(5) . ? C20 C21 1.373(5) . ? C21 N5 1.359(4) . ? C21 C22 1.466(4) . ? C22 N6 1.342(4) . ? C22 C23 1.383(5) . ? C23 C24 1.398(5) . ? C24 C25 1.352(6) . ? C25 C26 1.370(5) . ? C26 N6 1.355(4) . ? C27 N7 1.349(4) . ? C27 C28 1.377(5) . ? C28 C29 1.368(6) . ? C29 C30 1.373(5) . ? C30 C31 1.388(5) . ? C31 N7 1.344(4) . ? C31 C32 1.474(4) . ? C32 N8 1.363(4) . ? C32 C33 1.375(4) . ? C33 C34 1.377(5) . ? C34 C35 1.368(6) . ? C35 C36 1.371(5) . ? C36 N8 1.345(4) . ? F1 P1 1.572(3) . ? F2 P1 1.589(3) . ? F3 P1 1.588(2) . ? F4 P1 1.586(3) . ? F5 P1 1.590(2) . ? F6 P1 1.577(3) . ? F7 P2 1.603(3) . ? F8 P2 1.577(3) . ? F9A P2 1.582(5) . ? F10A P2 1.528(5) . ? F11A P2 1.538(5) . ? F12A P2 1.610(5) . ? F9B P2 1.595(11) . ? F10B P2 1.584(12) . ? F11B P2 1.474(10) . ? F12B P2 1.481(9) . ? N1 Ru1 2.057(2) . ? N4 Ru1 2.062(3) . ? N5 Ru1 2.048(3) . ? N6 Ru1 2.060(2) . ? N7 Ru1 2.073(3) . ? N8 Ru1 2.056(3) . ? N9 C41 1.319(17) 2_676 ? N9 C41 1.319(17) . ? C41 C42 1.520(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 122.9(3) . . ? C1 C2 C15 120.9(3) . . ? C4 C3 C15 119.4(4) . . ? C3 C4 N2 125.5(3) . . ? N3 C5 C6 124.8(3) . . ? C5 C6 C16 119.0(4) . . ? C8 C7 C16 121.5(3) . . ? C7 C8 N4 122.8(3) . . ? N1 C9 C10 123.4(3) . . ? N1 C9 C14 116.5(2) . . ? C10 C9 C14 120.0(3) . . ? C9 C10 C15 118.5(3) . . ? C9 C10 C11 121.2(3) . . ? C15 C10 C11 120.3(3) . . ? N2 C11 C10 121.8(3) . . ? N2 C11 C12 119.4(3) . . ? C10 C11 C12 118.8(3) . . ? N3 C12 C13 122.1(3) . . ? N3 C12 C11 119.7(3) . . ? C13 C12 C11 118.2(3) . . ? C14 C13 C16 118.8(3) . . ? C14 C13 C12 121.8(3) . . ? C16 C13 C12 119.4(3) . . ? N4 C14 C13 123.9(3) . . ? N4 C14 C9 116.2(3) . . ? C13 C14 C9 119.9(3) . . ? C3 C15 C2 127.0(3) . . ? C3 C15 C10 116.2(3) . . ? C2 C15 C10 116.8(3) . . ? C6 C16 C13 117.2(3) . . ? C6 C16 C7 126.7(4) . . ? C13 C16 C7 116.1(3) . . ? N5 C17 C18 122.6(3) . . ? C17 C18 C19 119.6(3) . . ? C18 C19 C20 118.3(3) . . ? C21 C20 C19 120.1(3) . . ? N5 C21 C20 121.1(3) . . ? N5 C21 C22 114.4(3) . . ? C20 C21 C22 124.4(3) . . ? N6 C22 C23 121.8(3) . . ? N6 C22 C21 115.2(3) . . ? C23 C22 C21 123.1(3) . . ? C22 C23 C24 118.4(4) . . ? C25 C24 C23 119.4(3) . . ? C24 C25 C26 120.0(3) . . ? N6 C26 C25 121.6(3) . . ? N7 C27 C28 123.2(3) . . ? C29 C28 C27 118.5(3) . . ? C28 C29 C30 119.3(3) . . ? C29 C30 C31 119.7(3) . . ? N7 C31 C30 121.5(3) . . ? N7 C31 C32 114.7(3) . . ? C30 C31 C32 123.9(3) . . ? N8 C32 C33 121.2(3) . . ? N8 C32 C31 114.8(3) . . ? C33 C32 C31 123.9(3) . . ? C32 C33 C34 119.9(3) . . ? C35 C34 C33 118.8(3) . . ? C34 C35 C36 119.7(3) . . ? N8 C36 C35 122.2(3) . . ? C9 N1 C1 117.5(2) . . ? C9 N1 Ru1 114.2(2) . . ? C1 N1 Ru1 128.4(2) . . ? C11 N2 C4 116.8(3) . . ? C12 N3 C5 117.4(3) . . ? C14 N4 C8 116.8(3) . . ? C14 N4 Ru1 113.9(2) . . ? C8 N4 Ru1 129.2(2) . . ? C17 N5 C21 118.3(3) . . ? C17 N5 Ru1 125.7(2) . . ? C21 N5 Ru1 116.0(2) . . ? C22 N6 C26 118.8(3) . . ? C22 N6 Ru1 115.82(19) . . ? C26 N6 Ru1 125.3(2) . . ? C31 N7 C27 117.8(3) . . ? C31 N7 Ru1 115.8(2) . . ? C27 N7 Ru1 126.3(2) . . ? C36 N8 C32 118.2(3) . . ? C36 N8 Ru1 125.7(2) . . ? C32 N8 Ru1 115.8(2) . . ? F1 P1 F6 90.50(17) . . ? F1 P1 F4 90.44(18) . . ? F6 P1 F4 178.85(18) . . ? F1 P1 F3 90.62(15) . . ? F6 P1 F3 89.91(14) . . ? F4 P1 F3 89.42(14) . . ? F1 P1 F2 179.27(16) . . ? F6 P1 F2 89.34(16) . . ? F4 P1 F2 89.73(18) . . ? F3 P1 F2 90.09(14) . . ? F1 P1 F5 89.81(15) . . ? F6 P1 F5 89.93(15) . . ? F4 P1 F5 90.74(15) . . ? F3 P1 F5 179.54(16) . . ? F2 P1 F5 89.47(14) . . ? F11B P2 F12B 88.4(12) . . ? F11B P2 F10A 139.0(13) . . ? F12B P2 F10A 132.3(10) . . ? F11B P2 F11A 45.8(11) . . ? F12B P2 F11A 134.0(10) . . ? F10A P2 F11A 93.2(6) . . ? F11B P2 F8 89.3(6) . . ? F12B P2 F8 82.5(5) . . ? F10A P2 F8 91.0(3) . . ? F11A P2 F8 91.9(3) . . ? F11B P2 F9A 128.0(13) . . ? F12B P2 F9A 40.4(8) . . ? F10A P2 F9A 92.9(5) . . ? F11A P2 F9A 173.2(5) . . ? F8 P2 F9A 90.8(2) . . ? F11B P2 F10B 92.2(12) . . ? F12B P2 F10B 178.2(8) . . ? F10A P2 F10B 47.1(8) . . ? F11A P2 F10B 46.4(9) . . ? F8 P2 F10B 95.8(6) . . ? F9A P2 F10B 139.4(11) . . ? F11B P2 F9B 176.8(11) . . ? F12B P2 F9B 89.9(11) . . ? F10A P2 F9B 42.5(8) . . ? F11A P2 F9B 135.7(10) . . ? F8 P2 F9B 87.9(6) . . ? F9A P2 F9B 50.6(8) . . ? F10B P2 F9B 89.5(12) . . ? F11B P2 F7 91.2(6) . . ? F12B P2 F7 94.6(5) . . ? F10A P2 F7 90.5(3) . . ? F11A P2 F7 90.4(3) . . ? F8 P2 F7 177.13(18) . . ? F9A P2 F7 86.7(2) . . ? F10B P2 F7 87.0(6) . . ? F9B P2 F7 91.6(6) . . ? F11B P2 F12A 42.4(11) . . ? F12B P2 F12A 47.1(9) . . ? F10A P2 F12A 176.5(4) . . ? F11A P2 F12A 87.9(4) . . ? F8 P2 F12A 92.3(2) . . ? F9A P2 F12A 85.7(4) . . ? F10B P2 F12A 133.7(10) . . ? F9B P2 F12A 136.4(10) . . ? F7 P2 F12A 86.1(2) . . ? N5 Ru1 N8 172.95(9) . . ? N5 Ru1 N1 96.89(10) . . ? N8 Ru1 N1 87.76(9) . . ? N5 Ru1 N6 78.52(10) . . ? N8 Ru1 N6 97.45(10) . . ? N1 Ru1 N6 171.98(10) . . ? N5 Ru1 N4 87.36(10) . . ? N8 Ru1 N4 98.75(10) . . ? N1 Ru1 N4 79.10(10) . . ? N6 Ru1 N4 94.04(10) . . ? N5 Ru1 N7 95.65(10) . . ? N8 Ru1 N7 78.42(10) . . ? N1 Ru1 N7 97.89(9) . . ? N6 Ru1 N7 89.15(10) . . ? N4 Ru1 N7 176.00(10) . . ? C41 N9 C41 179.998(4) 2_676 . ? N9 C41 C42 169.7(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C15 -0.2(5) . . . . ? C15 C3 C4 N2 -1.2(6) . . . . ? N3 C5 C6 C16 -0.1(7) . . . . ? C16 C7 C8 N4 0.4(6) . . . . ? N1 C9 C10 C15 -1.3(5) . . . . ? C14 C9 C10 C15 178.7(3) . . . . ? N1 C9 C10 C11 178.6(3) . . . . ? C14 C9 C10 C11 -1.4(4) . . . . ? C9 C10 C11 N2 178.5(3) . . . . ? C15 C10 C11 N2 -1.7(5) . . . . ? C9 C10 C11 C12 -1.9(4) . . . . ? C15 C10 C11 C12 178.0(3) . . . . ? N2 C11 C12 N3 3.5(5) . . . . ? C10 C11 C12 N3 -176.2(3) . . . . ? N2 C11 C12 C13 -177.1(3) . . . . ? C10 C11 C12 C13 3.2(4) . . . . ? N3 C12 C13 C14 178.1(3) . . . . ? C11 C12 C13 C14 -1.3(4) . . . . ? N3 C12 C13 C16 -2.6(5) . . . . ? C11 C12 C13 C16 177.9(3) . . . . ? C16 C13 C14 N4 -0.3(5) . . . . ? C12 C13 C14 N4 179.0(3) . . . . ? C16 C13 C14 C9 178.8(3) . . . . ? C12 C13 C14 C9 -1.9(5) . . . . ? N1 C9 C14 N4 2.5(4) . . . . ? C10 C9 C14 N4 -177.5(3) . . . . ? N1 C9 C14 C13 -176.6(3) . . . . ? C10 C9 C14 C13 3.4(4) . . . . ? C4 C3 C15 C2 179.8(4) . . . . ? C4 C3 C15 C10 -0.5(5) . . . . ? C1 C2 C15 C3 179.0(4) . . . . ? C1 C2 C15 C10 -0.8(5) . . . . ? C9 C10 C15 C3 -178.3(3) . . . . ? C11 C10 C15 C3 1.8(5) . . . . ? C9 C10 C15 C2 1.4(5) . . . . ? C11 C10 C15 C2 -178.4(3) . . . . ? C5 C6 C16 C13 -1.6(6) . . . . ? C5 C6 C16 C7 178.6(4) . . . . ? C14 C13 C16 C6 -177.8(3) . . . . ? C12 C13 C16 C6 2.8(5) . . . . ? C14 C13 C16 C7 2.0(5) . . . . ? C12 C13 C16 C7 -177.3(3) . . . . ? C8 C7 C16 C6 177.8(4) . . . . ? C8 C7 C16 C13 -2.1(6) . . . . ? N5 C17 C18 C19 0.0(6) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C19 C20 C21 N5 -2.0(6) . . . . ? C19 C20 C21 C22 178.4(3) . . . . ? N5 C21 C22 N6 -2.9(4) . . . . ? C20 C21 C22 N6 176.7(3) . . . . ? N5 C21 C22 C23 175.5(3) . . . . ? C20 C21 C22 C23 -4.9(6) . . . . ? N6 C22 C23 C24 -1.2(6) . . . . ? C21 C22 C23 C24 -179.6(3) . . . . ? C22 C23 C24 C25 0.0(6) . . . . ? C23 C24 C25 C26 0.9(6) . . . . ? C24 C25 C26 N6 -0.7(6) . . . . ? N7 C27 C28 C29 1.0(5) . . . . ? C27 C28 C29 C30 -2.5(5) . . . . ? C28 C29 C30 C31 0.9(5) . . . . ? C29 C30 C31 N7 2.3(4) . . . . ? C29 C30 C31 C32 -176.3(3) . . . . ? N7 C31 C32 N8 6.3(3) . . . . ? C30 C31 C32 N8 -175.1(3) . . . . ? N7 C31 C32 C33 -169.7(3) . . . . ? C30 C31 C32 C33 8.9(4) . . . . ? N8 C32 C33 C34 -1.7(4) . . . . ? C31 C32 C33 C34 174.1(3) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? C33 C34 C35 C36 2.1(5) . . . . ? C34 C35 C36 N8 -2.7(5) . . . . ? C10 C9 N1 C1 0.3(4) . . . . ? C14 C9 N1 C1 -179.6(3) . . . . ? C10 C9 N1 Ru1 179.9(2) . . . . ? C14 C9 N1 Ru1 -0.1(3) . . . . ? C2 C1 N1 C9 0.4(5) . . . . ? C2 C1 N1 Ru1 -179.0(3) . . . . ? C10 C11 N2 C4 0.0(5) . . . . ? C12 C11 N2 C4 -179.6(3) . . . . ? C3 C4 N2 C11 1.5(6) . . . . ? C13 C12 N3 C5 0.9(5) . . . . ? C11 C12 N3 C5 -179.6(3) . . . . ? C6 C5 N3 C12 0.4(6) . . . . ? C13 C14 N4 C8 -1.4(4) . . . . ? C9 C14 N4 C8 179.5(3) . . . . ? C13 C14 N4 Ru1 175.5(2) . . . . ? C9 C14 N4 Ru1 -3.6(3) . . . . ? C7 C8 N4 C14 1.4(5) . . . . ? C7 C8 N4 Ru1 -175.0(3) . . . . ? C18 C17 N5 C21 -0.8(5) . . . . ? C18 C17 N5 Ru1 179.8(3) . . . . ? C20 C21 N5 C17 1.8(5) . . . . ? C22 C21 N5 C17 -178.6(3) . . . . ? C20 C21 N5 Ru1 -178.8(3) . . . . ? C22 C21 N5 Ru1 0.9(4) . . . . ? C23 C22 N6 C26 1.4(5) . . . . ? C21 C22 N6 C26 179.9(3) . . . . ? C23 C22 N6 Ru1 -174.9(3) . . . . ? C21 C22 N6 Ru1 3.6(4) . . . . ? C25 C26 N6 C22 -0.4(5) . . . . ? C25 C26 N6 Ru1 175.5(3) . . . . ? C30 C31 N7 C27 -3.7(4) . . . . ? C32 C31 N7 C27 174.9(2) . . . . ? C30 C31 N7 Ru1 172.7(2) . . . . ? C32 C31 N7 Ru1 -8.7(3) . . . . ? C28 C27 N7 C31 2.1(4) . . . . ? C28 C27 N7 Ru1 -173.8(2) . . . . ? C35 C36 N8 C32 1.0(4) . . . . ? C35 C36 N8 Ru1 -172.5(3) . . . . ? C33 C32 N8 C36 1.2(4) . . . . ? C31 C32 N8 C36 -175.0(2) . . . . ? C33 C32 N8 Ru1 175.3(2) . . . . ? C31 C32 N8 Ru1 -0.9(3) . . . . ? C17 N5 Ru1 N8 -124.2(8) . . . . ? C21 N5 Ru1 N8 56.4(9) . . . . ? C17 N5 Ru1 N1 6.8(3) . . . . ? C21 N5 Ru1 N1 -172.6(2) . . . . ? C17 N5 Ru1 N6 -179.8(3) . . . . ? C21 N5 Ru1 N6 0.7(2) . . . . ? C17 N5 Ru1 N4 85.5(3) . . . . ? C21 N5 Ru1 N4 -93.9(2) . . . . ? C17 N5 Ru1 N7 -91.9(3) . . . . ? C21 N5 Ru1 N7 88.7(2) . . . . ? C36 N8 Ru1 N5 -156.2(7) . . . . ? C32 N8 Ru1 N5 30.2(9) . . . . ? C36 N8 Ru1 N1 72.3(2) . . . . ? C32 N8 Ru1 N1 -101.3(2) . . . . ? C36 N8 Ru1 N6 -101.6(2) . . . . ? C32 N8 Ru1 N6 84.8(2) . . . . ? C36 N8 Ru1 N4 -6.3(3) . . . . ? C32 N8 Ru1 N4 -179.90(18) . . . . ? C36 N8 Ru1 N7 170.8(3) . . . . ? C32 N8 Ru1 N7 -2.77(18) . . . . ? C9 N1 Ru1 N5 84.6(2) . . . . ? C1 N1 Ru1 N5 -95.9(3) . . . . ? C9 N1 Ru1 N8 -100.7(2) . . . . ? C1 N1 Ru1 N8 78.8(3) . . . . ? C9 N1 Ru1 N6 30.1(8) . . . . ? C1 N1 Ru1 N6 -150.4(6) . . . . ? C9 N1 Ru1 N4 -1.3(2) . . . . ? C1 N1 Ru1 N4 178.1(3) . . . . ? C9 N1 Ru1 N7 -178.7(2) . . . . ? C1 N1 Ru1 N7 0.8(3) . . . . ? C22 N6 Ru1 N5 -2.4(2) . . . . ? C26 N6 Ru1 N5 -178.4(3) . . . . ? C22 N6 Ru1 N8 -176.5(2) . . . . ? C26 N6 Ru1 N8 7.4(3) . . . . ? C22 N6 Ru1 N1 53.2(8) . . . . ? C26 N6 Ru1 N1 -122.9(7) . . . . ? C22 N6 Ru1 N4 84.1(2) . . . . ? C26 N6 Ru1 N4 -92.0(3) . . . . ? C22 N6 Ru1 N7 -98.3(2) . . . . ? C26 N6 Ru1 N7 85.6(3) . . . . ? C14 N4 Ru1 N5 -94.8(2) . . . . ? C8 N4 Ru1 N5 81.6(3) . . . . ? C14 N4 Ru1 N8 88.7(2) . . . . ? C8 N4 Ru1 N8 -94.8(3) . . . . ? C14 N4 Ru1 N1 2.7(2) . . . . ? C8 N4 Ru1 N1 179.2(3) . . . . ? C14 N4 Ru1 N6 -173.1(2) . . . . ? C8 N4 Ru1 N6 3.3(3) . . . . ? C14 N4 Ru1 N7 43.9(15) . . . . ? C8 N4 Ru1 N7 -139.6(13) . . . . ? C31 N7 Ru1 N5 -169.78(19) . . . . ? C27 N7 Ru1 N5 6.3(2) . . . . ? C31 N7 Ru1 N8 6.38(18) . . . . ? C27 N7 Ru1 N8 -177.6(2) . . . . ? C31 N7 Ru1 N1 92.45(19) . . . . ? C27 N7 Ru1 N1 -91.5(2) . . . . ? C31 N7 Ru1 N6 -91.40(19) . . . . ? C27 N7 Ru1 N6 84.6(2) . . . . ? C31 N7 Ru1 N4 51.6(14) . . . . ? C27 N7 Ru1 N4 -132.3(13) . . . . ? C41 N9 C41 C42 -169(48) 2_676 . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.515 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 170 53 ' ' 2 0.500 0.500 0.500 166 43 ' ' _platon_squeeze_details ; ; #====================================================================== data_brie7i _database_code_depnum_ccdc_archive 'CCDC 844737' #TrackingRef '- brie7i.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(4,4'-Dimethyl-2,2'-bipyridyl)(1,6,7,12-tetraazaperylene)-ruthenium(ii) bis(hexafluorophosphate) ; _chemical_name_common ; bis(4,4'-Dimethyl-2,2'-bipyridyl)(1,6,7,12-tetraazaperylene)- ruthenium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 N8 Ru1 2+ , F12 P2 2- , C14 H16' _chemical_formula_sum 'C54 H48 F12 N8 P2 Ru' _chemical_formula_weight 1200.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4919(8) _cell_length_b 13.2643(9) _cell_length_c 18.5610(12) _cell_angle_alpha 99.299(5) _cell_angle_beta 98.447(5) _cell_angle_gamma 107.099(5) _cell_volume 2611.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 19661 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.10 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 1.000 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.070 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method ? _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.9007 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was embedded in perfluoropolyalkylether oil. ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 210(2) _diffrn_measurement_method 'rotation method, delta omega = 1.0 deg' _diffrn_measurement_details ; 180 frames, detector distance = 120 mm ; _diffrn_reflns_number 17073 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8669 _reflns_number_gt 7207 _reflns_threshold_expression >2sigma(I) _publ_section_exptl_refinement ; All hydrogen atoms were calculated in idealized positions and allowed to ride on their corresponding carbon atoms. ; _computing_data_collection 'X-AREA (Stoe, 2006)' _computing_cell_refinement 'X-AREA (Stoe, 2002)' _computing_data_reduction 'X-RED32 (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0786P)^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 SHELXL _refine_ls_extinction_coef 0.0017(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8669 _refine_ls_number_parameters 803 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0853(3) 0.0037(3) 0.2416(2) 0.0511(8) Uani 1 1 d . . . H1 H -0.0683 0.0014 0.2918 0.061 Uiso 1 1 calc R . . C2 C -0.1880(3) -0.0725(3) 0.1961(2) 0.0549(9) Uani 1 1 d . . . H2 H -0.2397 -0.1244 0.2157 0.066 Uiso 1 1 calc R . . C3 C -0.3188(3) -0.1468(3) 0.0667(2) 0.0529(8) Uani 1 1 d . . . H3 H -0.3761 -0.2017 0.0809 0.063 Uiso 1 1 calc R . . C4 C -0.3323(3) -0.1361(3) -0.0058(2) 0.0532(9) Uani 1 1 d . . . H4 H -0.3995 -0.1868 -0.0400 0.064 Uiso 1 1 calc R . . C5 C -0.0176(4) 0.1934(4) -0.0990(2) 0.0632(10) Uani 1 1 d . . . H5 H -0.0354 0.2004 -0.1481 0.076 Uiso 1 1 calc R . . C6 C 0.0871(4) 0.2672(3) -0.0533(2) 0.0603(10) Uani 1 1 d . . . H6 H 0.1388 0.3211 -0.0714 0.072 Uiso 1 1 calc R . . C7 C 0.2207(3) 0.3281(3) 0.0765(2) 0.0504(8) Uani 1 1 d . . . H7 H 0.2803 0.3826 0.0634 0.060 Uiso 1 1 calc R . . C8 C 0.2353(3) 0.3145(3) 0.14761(19) 0.0446(7) Uani 1 1 d . . . H8 H 0.3049 0.3612 0.1822 0.053 Uiso 1 1 calc R . . C9 C -0.0307(3) 0.0848(2) 0.14417(17) 0.0381(6) Uani 1 1 d . . . C10 C -0.1348(3) 0.0089(2) 0.09306(17) 0.0405(7) Uani 1 1 d . . . C11 C -0.1587(3) 0.0138(3) 0.01737(18) 0.0417(7) Uani 1 1 d . . . C12 C -0.0737(3) 0.1027(3) -0.00821(18) 0.0435(7) Uani 1 1 d . . . C13 C 0.0314(3) 0.1763(2) 0.04440(17) 0.0400(7) Uani 1 1 d . . . C14 C 0.0537(3) 0.1683(2) 0.11906(17) 0.0372(6) Uani 1 1 d . . . C15 C -0.2162(3) -0.0729(3) 0.11950(19) 0.0463(8) Uani 1 1 d . . . C16 C 0.1155(3) 0.2602(3) 0.02168(19) 0.0475(8) Uani 1 1 d . . . C17 C -0.0561(3) 0.3060(3) 0.2871(2) 0.0493(8) Uani 1 1 d . . . H17 H -0.1089 0.2433 0.2541 0.059 Uiso 1 1 calc R . . C18 C -0.1064(3) 0.3797(3) 0.3184(2) 0.0553(9) Uani 1 1 d . . . H18 H -0.1920 0.3657 0.3067 0.066 Uiso 1 1 calc R . . C19 C -0.0320(3) 0.4741(3) 0.3668(2) 0.0527(8) Uani 1 1 d . . . C20 C 0.0954(3) 0.4924(3) 0.3793(2) 0.0488(8) Uani 1 1 d . . . H20 H 0.1495 0.5567 0.4099 0.059 Uiso 1 1 calc R . . C21 C 0.1426(3) 0.4160(2) 0.34658(18) 0.0405(7) Uani 1 1 d . . . C22 C 0.2775(3) 0.4290(2) 0.35941(17) 0.0395(7) Uani 1 1 d . . . C23 C 0.3702(3) 0.5227(3) 0.39686(19) 0.0466(8) Uani 1 1 d . . . H23 H 0.3496 0.5832 0.4156 0.056 Uiso 1 1 calc R . . C24 C 0.4944(3) 0.5281(3) 0.40709(19) 0.0495(8) Uani 1 1 d . . . C25 C 0.5187(3) 0.4341(3) 0.3802(2) 0.0524(8) Uani 1 1 d . . . H25 H 0.6002 0.4332 0.3878 0.063 Uiso 1 1 calc R . . C26 C 0.4235(3) 0.3426(3) 0.34259(19) 0.0448(7) Uani 1 1 d . . . H26 H 0.4423 0.2809 0.3244 0.054 Uiso 1 1 calc R . . C27 C -0.0856(4) 0.5525(3) 0.4062(3) 0.0714(12) Uani 1 1 d . . . H27A H -0.0534 0.6216 0.3940 0.107 Uiso 1 1 calc R . . H27B H -0.0629 0.5597 0.4592 0.107 Uiso 1 1 calc R . . H27C H -0.1746 0.5262 0.3908 0.107 Uiso 1 1 calc R . . C28 C 0.5970(4) 0.6309(3) 0.4460(2) 0.0665(11) Uani 1 1 d . . . H28A H 0.6520 0.6524 0.4129 0.100 Uiso 1 1 calc R . . H28B H 0.6427 0.6193 0.4897 0.100 Uiso 1 1 calc R . . H28C H 0.5620 0.6867 0.4601 0.100 Uiso 1 1 calc R . . C29 C 0.0802(3) 0.1926(3) 0.42873(18) 0.0429(7) Uani 1 1 d . . . H29 H 0.0292 0.2328 0.4164 0.051 Uiso 1 1 calc R . . C30 C 0.0874(3) 0.1657(3) 0.49722(18) 0.0460(8) Uani 1 1 d . . . H30 H 0.0409 0.1872 0.5300 0.055 Uiso 1 1 calc R . . C31 C 0.1632(3) 0.1071(3) 0.51798(18) 0.0456(7) Uani 1 1 d . . . C32 C 0.2276(3) 0.0748(3) 0.46599(18) 0.0450(7) Uani 1 1 d . . . H32 H 0.2788 0.0344 0.4776 0.054 Uiso 1 1 calc R . . C33 C 0.2163(3) 0.1020(2) 0.39704(17) 0.0376(6) Uani 1 1 d . . . C34 C 0.2768(3) 0.0660(2) 0.33745(18) 0.0406(7) Uani 1 1 d . . . C35 C 0.3519(3) 0.0023(3) 0.3449(2) 0.0509(8) Uani 1 1 d . . . H35 H 0.3691 -0.0185 0.3897 0.061 Uiso 1 1 calc R . . C36 C 0.4019(3) -0.0308(3) 0.2845(2) 0.0572(10) Uani 1 1 d . . . C37 C 0.3694(4) 0.0000(3) 0.2193(2) 0.0579(10) Uani 1 1 d . . . H37 H 0.3978 -0.0234 0.1774 0.070 Uiso 1 1 calc R . . C38 C 0.2960(3) 0.0641(3) 0.21469(19) 0.0485(8) Uani 1 1 d . . . H38 H 0.2763 0.0839 0.1698 0.058 Uiso 1 1 calc R . . C39 C 0.1757(4) 0.0800(3) 0.5931(2) 0.0644(10) Uani 1 1 d . . . H39A H 0.2612 0.1099 0.6188 0.097 Uiso 1 1 calc R . . H39B H 0.1487 0.0029 0.5874 0.097 Uiso 1 1 calc R . . H39C H 0.1253 0.1096 0.6213 0.097 Uiso 1 1 calc R . . C40 C 0.4878(4) -0.0963(4) 0.2926(3) 0.0823(14) Uani 1 1 d . . . H40A H 0.4455 -0.1623 0.3061 0.123 Uiso 1 1 calc R . . H40B H 0.5600 -0.0558 0.3308 0.123 Uiso 1 1 calc R . . H40C H 0.5127 -0.1127 0.2462 0.123 Uiso 1 1 calc R . . C41A C 1.0324(6) 0.5649(5) 0.1843(4) 0.091(3) Uani 0.70 1 d PGD A 1 C42A C 1.1551(5) 0.6167(7) 0.2219(5) 0.107(4) Uani 0.70 1 d PG A 1 H42A H 1.2180 0.5924 0.2075 0.128 Uiso 0.70 1 calc PR A 1 C43A C 1.1836(6) 0.7050(8) 0.2809(5) 0.155(10) Uani 0.70 1 d PG A 1 H43A H 1.2657 0.7397 0.3060 0.186 Uiso 0.70 1 calc PR A 1 C44A C 1.0896(8) 0.7414(6) 0.3024(4) 0.129(5) Uani 0.70 1 d PG A 1 H44A H 1.1087 0.8005 0.3418 0.155 Uiso 0.70 1 calc PR A 1 C45A C 0.9669(7) 0.6895(5) 0.2648(4) 0.097(3) Uani 0.70 1 d PG A 1 H45A H 0.9040 0.7139 0.2791 0.117 Uiso 0.70 1 calc PR A 1 C46A C 0.9383(5) 0.6013(6) 0.2058(4) 0.090(5) Uani 0.70 1 d PG A 1 H46A H 0.8563 0.5666 0.1807 0.108 Uiso 0.70 1 calc PR A 1 C47A C 0.9942(11) 0.4659(8) 0.1192(6) 0.141(4) Uani 0.70 1 d PD A 1 H55A H 1.0222 0.4102 0.1352 0.212 Uiso 0.70 1 calc PR A 1 H56A H 1.0312 0.4863 0.0783 0.212 Uiso 0.70 1 calc PR A 1 H57A H 0.9052 0.4395 0.1033 0.212 Uiso 0.70 1 calc PR A 1 C41B C 1.0499(11) 0.6884(8) 0.2632(6) 0.065(4) Uani 0.30 1 d PGD B 2 C42B C 0.9540(11) 0.6037(11) 0.2152(9) 0.063(7) Uani 0.30 1 d PG B 2 H42B H 0.8717 0.6004 0.2140 0.076 Uiso 0.30 1 calc PR B 2 C43B C 0.9809(19) 0.5238(12) 0.1689(10) 0.115(10) Uani 0.30 1 d PG B 2 H43B H 0.9168 0.4671 0.1368 0.138 Uiso 0.30 1 calc PR B 2 C44B C 1.104(2) 0.5287(14) 0.1707(11) 0.166(18) Uani 0.30 1 d PG B 2 H44B H 1.1219 0.4753 0.1397 0.199 Uiso 0.30 1 calc PR B 2 C45B C 1.1998(15) 0.6135(18) 0.2187(14) 0.19(2) Uani 0.30 1 d PG B 2 H45B H 1.2820 0.6167 0.2199 0.223 Uiso 0.30 1 calc PR B 2 C46B C 1.1728(10) 0.6933(14) 0.2650(12) 0.092(10) Uani 0.30 1 d PG B 2 H46B H 1.2370 0.7500 0.2971 0.111 Uiso 0.30 1 calc PR B 2 C47B C 1.0170(19) 0.7791(12) 0.3108(10) 0.129(10) Uani 0.30 1 d PGD B 2 H55B H 1.0919 0.8318 0.3411 0.194 Uiso 0.30 1 calc PR B 2 H56B H 0.9634 0.7488 0.3424 0.194 Uiso 0.30 1 calc PR B 2 H57B H 0.9754 0.8132 0.2786 0.194 Uiso 0.30 1 calc PR B 2 C48A C 0.6646(8) 0.2683(10) 0.0369(4) 0.168(8) Uani 0.80 1 d PGD C 1 C49A C 0.6530(10) 0.1624(9) 0.0416(8) 0.167(12) Uani 0.70 1 d PG C 1 H49A H 0.6650 0.1158 0.0023 0.200 Uiso 0.70 1 calc PR C 1 C50A C 0.6234(11) 0.1260(7) 0.1048(10) 0.255(16) Uani 0.80 1 d PG C 1 H50A H 0.6157 0.0551 0.1080 0.306 Uiso 0.80 1 calc PR C 1 C51A C 0.6055(11) 0.1956(10) 0.1635(7) 0.137(7) Uani 0.70 1 d PG C 1 H51A H 0.5857 0.1712 0.2058 0.164 Uiso 0.70 1 calc PR C 1 C52A C 0.6171(9) 0.3015(9) 0.1588(5) 0.093(4) Uani 0.70 1 d PG C 1 H52A H 0.6050 0.3480 0.1981 0.112 Uiso 0.70 1 calc PR C 1 C53A C 0.6466(7) 0.3379(6) 0.0956(6) 0.088(3) Uani 0.70 1 d PG C 1 H53A H 0.6544 0.4088 0.0924 0.105 Uiso 0.70 1 calc PR C 1 C54A C 0.7004(11) 0.3009(15) -0.0348(6) 0.214(8) Uani 0.80 1 d PD C 1 H58A H 0.6365 0.2576 -0.0771 0.321 Uiso 0.80 1 calc PR C 1 H59A H 0.7777 0.2898 -0.0402 0.321 Uiso 0.80 1 calc PR C 1 H60A H 0.7091 0.3758 -0.0319 0.321 Uiso 0.80 1 calc PR C 1 C48B C 0.664(2) 0.3420(13) 0.0673(14) 0.20(4) Uani 0.20 1 d PGD D 2 C49B C 0.668(2) 0.2611(17) 0.0106(12) 0.20(3) Uani 0.30 1 d PG D 2 H49B H 0.6802 0.2761 -0.0355 0.241 Uiso 0.30 1 calc PR D 2 C50B C 0.653(3) 0.1577(16) 0.0228(12) 0.23(5) Uani 0.20 1 d PG D 2 H50B H 0.6550 0.1036 -0.0151 0.270 Uiso 0.20 1 calc PR D 2 C51B C 0.634(3) 0.1354(14) 0.0917(11) 0.081(7) Uani 0.30 1 d PG D 2 H51B H 0.6241 0.0662 0.0998 0.097 Uiso 0.30 1 calc PR D 2 C52B C 0.631(2) 0.2163(15) 0.1483(10) 0.093(8) Uani 0.30 1 d PG D 2 H52B H 0.6185 0.2013 0.1944 0.112 Uiso 0.30 1 calc PR D 2 C53B C 0.646(3) 0.3196(14) 0.1361(12) 0.113(13) Uani 0.30 1 d PG D 2 H53B H 0.6437 0.3738 0.1740 0.136 Uiso 0.30 1 calc PR D 2 C54B C 0.661(4) 0.4342(18) 0.027(2) 0.22(3) Uani 0.20 1 d PGD D 2 H58B H 0.7228 0.5003 0.0551 0.334 Uiso 0.20 1 calc PR D 2 H59B H 0.5804 0.4423 0.0221 0.334 Uiso 0.20 1 calc PR D 2 H60B H 0.6789 0.4174 -0.0218 0.334 Uiso 0.20 1 calc PR D 2 F1 F 0.6671(3) 0.6329(4) 0.1571(2) 0.1269(13) Uani 1 1 d . . . F2 F 0.4649(4) 0.5993(5) 0.2540(3) 0.168(2) Uani 1 1 d . . . F3 F 0.6314(4) 0.5470(3) 0.2479(2) 0.1280(13) Uani 1 1 d . . . F4 F 0.4825(5) 0.5170(4) 0.1455(3) 0.174(2) Uani 1 1 d . . . F5 F 0.5114(4) 0.6945(3) 0.1682(2) 0.1298(14) Uani 1 1 d . . . F6 F 0.6501(5) 0.7172(3) 0.2663(2) 0.165(2) Uani 1 1 d . . . F7 F 0.3745(3) 0.9206(2) 0.54836(19) 0.0930(9) Uani 1 1 d . E . F8 F 0.2450(4) 0.6722(2) 0.5404(2) 0.1275(14) Uani 1 1 d . E . F9A F 0.2335(15) 0.8358(8) 0.6093(7) 0.121(3) Uani 0.50 1 d P E 1 F10A F 0.1920(8) 0.8159(7) 0.4926(7) 0.129(3) Uani 0.60 1 d P E 1 F11A F 0.3512(18) 0.7627(10) 0.4779(11) 0.170(8) Uani 0.50 1 d P E 1 F12A F 0.4470(6) 0.7853(5) 0.5467(8) 0.118(2) Uani 0.60 1 d P E 1 F9B F 0.3437(17) 0.8175(10) 0.6299(5) 0.136(5) Uani 0.50 1 d P E 2 F10B F 0.1824(9) 0.7979(10) 0.5506(14) 0.126(4) Uani 0.40 1 d P E 2 F11B F 0.2846(17) 0.7688(12) 0.4582(6) 0.156(7) Uani 0.50 1 d P E 2 F12B F 0.3981(14) 0.7917(10) 0.6092(11) 0.125(6) Uani 0.40 1 d P E 2 N1 N -0.0052(2) 0.0843(2) 0.21653(14) 0.0395(6) Uani 1 1 d . . . N2 N -0.2556(3) -0.0576(2) -0.03206(16) 0.0489(7) Uani 1 1 d . . . N3 N -0.0978(3) 0.1106(3) -0.07837(16) 0.0544(7) Uani 1 1 d . . . N4 N 0.1521(2) 0.2349(2) 0.17114(15) 0.0399(6) Uani 1 1 d . . . N5 N 0.0667(2) 0.3205(2) 0.30212(15) 0.0401(6) Uani 1 1 d . . . N6 N 0.3028(2) 0.3391(2) 0.33095(14) 0.0377(5) Uani 1 1 d . . . N7 N 0.1447(2) 0.16259(19) 0.37821(14) 0.0375(5) Uani 1 1 d . . . N8 N 0.2513(2) 0.0998(2) 0.27369(15) 0.0421(6) Uani 1 1 d . . . P1 P 0.56649(12) 0.61705(9) 0.20679(7) 0.0720(3) Uani 1 1 d . . . P2 P 0.30759(11) 0.79673(9) 0.54482(7) 0.0676(3) Uani 1 1 d . . . Ru1 Ru 0.15108(2) 0.205709(18) 0.276560(13) 0.03474(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 0.0527(19) 0.0458(17) 0.0400(18) 0.0118(14) 0.0011(15) -0.0034(15) C2 0.053(2) 0.0471(18) 0.051(2) 0.0127(16) 0.0066(16) -0.0028(15) C3 0.0461(18) 0.0467(18) 0.055(2) 0.0049(16) 0.0031(16) 0.0049(15) C4 0.0422(18) 0.0513(19) 0.050(2) -0.0053(16) -0.0056(15) 0.0073(15) C5 0.069(2) 0.081(3) 0.040(2) 0.0222(19) 0.0088(18) 0.022(2) C6 0.069(2) 0.068(2) 0.047(2) 0.0264(18) 0.0161(19) 0.018(2) C7 0.0477(18) 0.0486(18) 0.052(2) 0.0172(15) 0.0118(16) 0.0075(15) C8 0.0400(16) 0.0423(16) 0.0458(18) 0.0128(14) 0.0069(14) 0.0042(13) C9 0.0360(15) 0.0384(15) 0.0360(16) 0.0066(12) 0.0037(12) 0.0091(12) C10 0.0396(16) 0.0398(15) 0.0367(17) 0.0022(13) 0.0020(13) 0.0109(13) C11 0.0393(16) 0.0462(17) 0.0358(17) 0.0017(13) -0.0001(13) 0.0158(13) C12 0.0434(16) 0.0516(18) 0.0356(17) 0.0081(14) 0.0033(13) 0.0189(14) C13 0.0444(16) 0.0445(16) 0.0340(16) 0.0106(13) 0.0079(13) 0.0177(14) C14 0.0380(15) 0.0362(14) 0.0355(16) 0.0069(12) 0.0053(12) 0.0107(12) C15 0.0417(17) 0.0415(16) 0.0456(19) 0.0051(14) -0.0014(14) 0.0062(14) C16 0.0501(18) 0.0526(19) 0.0445(19) 0.0172(15) 0.0122(15) 0.0187(15) C17 0.0417(17) 0.0499(18) 0.050(2) 0.0087(15) -0.0033(15) 0.0132(15) C18 0.0392(17) 0.057(2) 0.070(3) 0.0149(18) 0.0037(16) 0.0188(16) C19 0.054(2) 0.0500(19) 0.062(2) 0.0172(16) 0.0139(17) 0.0242(16) C20 0.0473(18) 0.0402(17) 0.057(2) 0.0083(15) 0.0093(16) 0.0130(14) C21 0.0400(16) 0.0387(15) 0.0409(17) 0.0105(13) 0.0038(13) 0.0113(13) C22 0.0407(16) 0.0373(15) 0.0368(16) 0.0068(13) 0.0022(13) 0.0107(13) C23 0.0485(18) 0.0378(16) 0.0458(19) 0.0033(14) 0.0056(15) 0.0078(14) C24 0.0464(18) 0.0446(17) 0.0431(18) 0.0047(15) 0.0006(15) 0.0000(14) C25 0.0360(16) 0.058(2) 0.054(2) 0.0079(17) 0.0028(15) 0.0067(15) C26 0.0349(15) 0.0445(17) 0.0490(19) 0.0041(14) 0.0018(14) 0.0107(13) C27 0.062(2) 0.061(2) 0.100(4) 0.015(2) 0.027(2) 0.031(2) C28 0.051(2) 0.054(2) 0.071(3) -0.0034(19) 0.0009(19) -0.0034(17) C29 0.0416(16) 0.0416(16) 0.0423(18) 0.0038(13) 0.0060(14) 0.0131(13) C30 0.0485(18) 0.0465(17) 0.0366(17) 0.0033(14) 0.0119(14) 0.0074(14) C31 0.0515(18) 0.0397(16) 0.0360(17) 0.0077(13) 0.0023(14) 0.0041(14) C32 0.0505(18) 0.0393(16) 0.0419(18) 0.0097(13) 0.0018(14) 0.0129(14) C33 0.0380(15) 0.0313(14) 0.0355(16) 0.0025(12) 0.0005(12) 0.0055(12) C34 0.0413(16) 0.0339(14) 0.0395(17) 0.0005(13) 0.0024(13) 0.0084(13) C35 0.0517(19) 0.0435(17) 0.054(2) 0.0043(15) 0.0036(16) 0.0167(15) C36 0.0505(19) 0.052(2) 0.061(2) -0.0071(17) 0.0017(17) 0.0194(17) C37 0.059(2) 0.056(2) 0.053(2) -0.0090(17) 0.0118(17) 0.0198(17) C38 0.0524(19) 0.0477(18) 0.0396(18) -0.0019(14) 0.0100(15) 0.0135(15) C39 0.085(3) 0.064(2) 0.045(2) 0.0198(18) 0.013(2) 0.021(2) C40 0.080(3) 0.077(3) 0.095(4) -0.004(3) 0.014(3) 0.046(3) C41A 0.081(6) 0.090(7) 0.104(8) 0.045(6) 0.014(5) 0.021(5) C42A 0.065(5) 0.134(10) 0.119(9) 0.075(8) 0.003(5) 0.012(6) C43A 0.090(10) 0.200(19) 0.146(13) 0.100(13) 0.000(10) -0.019(12) C44A 0.134(11) 0.112(9) 0.092(8) 0.041(7) -0.004(8) -0.031(9) C45A 0.118(7) 0.085(5) 0.081(5) 0.034(5) 0.024(5) 0.010(5) C46A 0.076(7) 0.090(10) 0.105(10) 0.052(8) 0.009(6) 0.018(6) C47A 0.136(9) 0.147(10) 0.150(11) -0.003(8) 0.036(8) 0.076(9) C41B 0.066(10) 0.066(10) 0.069(11) 0.036(8) 0.009(9) 0.023(8) C42B 0.063(12) 0.088(19) 0.054(11) 0.021(12) 0.012(9) 0.046(13) C43B 0.18(3) 0.060(14) 0.103(19) 0.025(12) 0.03(2) 0.027(16) C44B 0.29(5) 0.18(4) 0.14(3) 0.07(3) 0.11(3) 0.18(4) C45B 0.18(4) 0.25(6) 0.23(5) 0.12(4) 0.13(4) 0.14(4) C46B 0.060(15) 0.064(12) 0.13(2) 0.041(14) -0.022(16) -0.002(11) C47B 0.18(3) 0.13(2) 0.089(17) 0.036(15) 0.024(18) 0.06(2) C48A 0.054(5) 0.30(3) 0.118(9) 0.017(12) -0.007(5) 0.044(10) C49A 0.067(9) 0.109(11) 0.30(3) -0.042(15) -0.007(11) 0.052(9) C50A 0.069(9) 0.109(12) 0.56(4) 0.001(17) 0.004(15) 0.047(9) C51A 0.048(6) 0.126(12) 0.228(17) 0.080(12) 0.006(7) 0.004(7) C52A 0.064(6) 0.077(8) 0.105(8) -0.008(6) -0.005(5) -0.001(5) C53A 0.067(5) 0.073(6) 0.100(7) 0.002(5) 0.002(5) 0.004(4) C54A 0.131(10) 0.37(3) 0.137(11) 0.032(13) 0.014(8) 0.101(13) C48B 0.14(4) 0.10(3) 0.40(11) -0.01(4) 0.16(5) 0.07(3) C49B 0.12(2) 0.26(5) 0.38(7) 0.27(5) 0.13(4) 0.13(3) C50B 0.05(3) 0.34(10) 0.34(10) 0.29(9) 0.03(4) 0.03(4) C51B 0.070(16) 0.056(13) 0.116(18) 0.034(13) -0.006(13) 0.022(11) C52B 0.051(13) 0.054(12) 0.14(2) 0.017(12) -0.022(12) -0.014(9) C53B 0.09(2) 0.069(13) 0.18(4) 0.04(2) 0.04(2) 0.011(13) C54B 0.34(8) 0.11(3) 0.14(4) 0.03(3) -0.01(5) -0.01(4) F1 0.107(2) 0.186(4) 0.119(3) 0.057(3) 0.055(2) 0.066(3) F2 0.128(3) 0.275(6) 0.161(4) 0.136(4) 0.083(3) 0.084(4) F3 0.145(3) 0.125(3) 0.143(3) 0.069(3) 0.037(3) 0.064(3) F4 0.152(4) 0.123(3) 0.162(4) -0.016(3) -0.018(3) -0.033(3) F5 0.174(4) 0.146(3) 0.124(3) 0.068(3) 0.069(3) 0.094(3) F6 0.213(5) 0.107(3) 0.120(3) -0.018(2) -0.014(3) 0.016(3) F7 0.0894(18) 0.0546(14) 0.124(3) 0.0167(15) -0.0034(17) 0.0203(13) F8 0.166(3) 0.0602(17) 0.110(3) 0.0075(17) 0.001(2) -0.0135(19) F9A 0.148(9) 0.104(6) 0.114(8) 0.015(5) 0.052(7) 0.037(6) F10A 0.087(5) 0.125(6) 0.153(8) 0.013(6) -0.017(5) 0.031(4) F11A 0.201(15) 0.094(6) 0.219(18) -0.021(10) 0.141(14) 0.038(9) F12A 0.078(4) 0.086(4) 0.193(8) 0.022(5) 0.024(5) 0.036(3) F9B 0.182(13) 0.105(8) 0.062(4) -0.011(4) 0.031(7) -0.026(8) F10B 0.056(5) 0.135(9) 0.207(15) 0.038(11) 0.046(8) 0.050(6) F11B 0.220(16) 0.114(8) 0.070(5) 0.024(5) -0.039(8) -0.007(10) F12B 0.111(10) 0.098(7) 0.147(14) 0.044(9) -0.062(9) 0.041(6) N1 0.0427(14) 0.0361(13) 0.0335(14) 0.0046(10) 0.0051(11) 0.0067(11) N2 0.0413(14) 0.0551(16) 0.0406(15) -0.0013(13) -0.0037(12) 0.0136(13) N3 0.0588(17) 0.0684(19) 0.0340(15) 0.0117(14) 0.0015(13) 0.0214(15) N4 0.0361(13) 0.0362(13) 0.0402(14) 0.0046(11) 0.0021(11) 0.0059(10) N5 0.0367(13) 0.0405(13) 0.0402(14) 0.0109(11) 0.0009(11) 0.0104(11) N6 0.0369(13) 0.0379(13) 0.0349(13) 0.0053(10) 0.0026(10) 0.0109(11) N7 0.0369(13) 0.0314(12) 0.0361(14) 0.0003(10) 0.0005(10) 0.0061(10) N8 0.0452(14) 0.0372(13) 0.0350(14) 0.0002(11) 0.0013(11) 0.0078(11) P1 0.0727(7) 0.0590(6) 0.0800(8) 0.0167(6) 0.0196(6) 0.0122(5) P2 0.0686(7) 0.0511(6) 0.0725(7) 0.0055(5) -0.0001(6) 0.0151(5) Ru1 0.03462(14) 0.03255(14) 0.03056(15) 0.00367(9) 0.00050(9) 0.00597(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.362(5) . ? C1 N1 1.384(4) . ? C1 H1 0.9300 . ? C2 C15 1.411(5) . ? C2 H2 0.9300 . ? C3 C4 1.367(5) . ? C3 C15 1.407(5) . ? C3 H3 0.9300 . ? C4 N2 1.360(5) . ? C4 H4 0.9300 . ? C5 N3 1.359(5) . ? C5 C6 1.366(6) . ? C5 H5 0.9300 . ? C6 C16 1.406(5) . ? C6 H6 0.9300 . ? C7 C8 1.354(5) . ? C7 C16 1.417(5) . ? C7 H7 0.9300 . ? C8 N4 1.378(4) . ? C8 H8 0.9300 . ? C9 N1 1.334(4) . ? C9 C10 1.412(4) . ? C9 C14 1.432(4) . ? C10 C11 1.407(5) . ? C10 C15 1.415(5) . ? C11 N2 1.333(4) . ? C11 C12 1.487(5) . ? C12 N3 1.319(4) . ? C12 C13 1.421(4) . ? C13 C14 1.399(4) . ? C13 C16 1.410(5) . ? C14 N4 1.345(4) . ? C17 N5 1.347(4) . ? C17 C18 1.369(5) . ? C17 H17 0.9300 . ? C18 C19 1.375(5) . ? C18 H18 0.9300 . ? C19 C20 1.389(5) . ? C19 C27 1.503(5) . ? C20 C21 1.382(5) . ? C20 H20 0.9300 . ? C21 N5 1.359(4) . ? C21 C22 1.487(4) . ? C22 N6 1.353(4) . ? C22 C23 1.374(4) . ? C23 C24 1.391(5) . ? C23 H23 0.9300 . ? C24 C25 1.388(5) . ? C24 C28 1.502(5) . ? C25 C26 1.370(5) . ? C25 H25 0.9300 . ? C26 N6 1.358(4) . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N7 1.358(4) . ? C29 C30 1.372(5) . ? C29 H29 0.9300 . ? C30 C31 1.381(5) . ? C30 H30 0.9300 . ? C31 C32 1.388(5) . ? C31 C39 1.492(5) . ? C32 C33 1.383(5) . ? C32 H32 0.9300 . ? C33 N7 1.357(4) . ? C33 C34 1.478(4) . ? C34 N8 1.354(4) . ? C34 C35 1.383(5) . ? C35 C36 1.399(5) . ? C35 H35 0.9300 . ? C36 C37 1.374(6) . ? C36 C40 1.502(5) . ? C37 C38 1.366(5) . ? C37 H37 0.9300 . ? C38 N8 1.352(4) . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41A C42A 1.3900 . ? C41A C46A 1.3900 . ? C41A C47A 1.5397(11) . ? C42A C43A 1.3900 . ? C42A H42A 0.9300 . ? C43A C44A 1.3900 . ? C43A H43A 0.9300 . ? C44A C45A 1.3900 . ? C44A H44A 0.9300 . ? C45A C46A 1.3900 . ? C45A H45A 0.9300 . ? C46A H46A 0.9300 . ? C47A H55A 0.9600 . ? C47A H56A 0.9600 . ? C47A H57A 0.9600 . ? C41B C42B 1.3900 . ? C41B C46B 1.3900 . ? C41B C47B 1.5476 . ? C42B C43B 1.3900 . ? C42B H42B 0.9300 . ? C43B C44B 1.3900 . ? C43B H43B 0.9300 . ? C44B C45B 1.3900 . ? C44B H44B 0.9300 . ? C45B C46B 1.3900 . ? C45B H45B 0.9300 . ? C46B H46B 0.9300 . ? C47B H55B 0.9600 . ? C47B H56B 0.9600 . ? C47B H57B 0.9600 . ? C48A C49A 1.3900 . ? C48A C53A 1.3900 . ? C48A C54A 1.5400(11) . ? C49A C50A 1.3900 . ? C49A H49A 0.9300 . ? C50A C51A 1.3900 . ? C50A H50A 0.9300 . ? C51A C52A 1.3900 . ? C51A H51A 0.9300 . ? C52A C53A 1.3900 . ? C52A H52A 0.9300 . ? C53A H53A 0.9300 . ? C54A H58A 0.9600 . ? C54A H59A 0.9600 . ? C54A H60A 0.9600 . ? C48B C49B 1.3900 . ? C48B C53B 1.3900 . ? C48B C54B 1.5400 . ? C49B C50B 1.3900 . ? C49B H49B 0.9300 . ? C50B C51B 1.3900 . ? C50B H50B 0.9300 . ? C51B C52B 1.3900 . ? C51B H51B 0.9300 . ? C52B C53B 1.3900 . ? C52B H52B 0.9300 . ? C53B H53B 0.9300 . ? C54B H58B 0.9600 . ? C54B H59B 0.9600 . ? C54B H60B 0.9600 . ? F1 P1 1.570(3) . ? F2 P1 1.546(4) . ? F3 P1 1.572(4) . ? F4 P1 1.556(4) . ? F5 P1 1.567(4) . ? F6 P1 1.540(4) . ? F7 P2 1.581(3) . ? F8 P2 1.579(3) . ? F9A P2 1.668(9) . ? F10A P2 1.633(8) . ? F11A P2 1.461(10) . ? F11A F12A 1.484(19) . ? F12A P2 1.649(6) . ? F9B F12B 0.900(15) . ? F9B P2 1.530(10) . ? F10B P2 1.463(8) . ? F11B P2 1.555(11) . ? F12B P2 1.488(10) . ? N1 Ru1 2.047(2) . ? N4 Ru1 2.056(3) . ? N5 Ru1 2.062(3) . ? N6 Ru1 2.069(2) . ? N7 Ru1 2.063(3) . ? N8 Ru1 2.061(3) . ? 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 123.0(3) . . ? C2 C1 H1 118.5 . . ? N1 C1 H1 118.5 . . ? C1 C2 C15 120.4(3) . . ? C1 C2 H2 119.8 . . ? C15 C2 H2 119.8 . . ? C4 C3 C15 118.6(3) . . ? C4 C3 H3 120.7 . . ? C15 C3 H3 120.7 . . ? N2 C4 C3 125.5(3) . . ? N2 C4 H4 117.3 . . ? C3 C4 H4 117.2 . . ? N3 C5 C6 125.1(4) . . ? N3 C5 H5 117.4 . . ? C6 C5 H5 117.4 . . ? C5 C6 C16 118.9(4) . . ? C5 C6 H6 120.6 . . ? C16 C6 H6 120.6 . . ? C8 C7 C16 120.8(3) . . ? C8 C7 H7 119.6 . . ? C16 C7 H7 119.6 . . ? C7 C8 N4 123.1(3) . . ? C7 C8 H8 118.4 . . ? N4 C8 H8 118.4 . . ? N1 C9 C10 123.5(3) . . ? N1 C9 C14 116.6(3) . . ? C10 C9 C14 120.0(3) . . ? C11 C10 C9 121.3(3) . . ? C11 C10 C15 120.1(3) . . ? C9 C10 C15 118.6(3) . . ? N2 C11 C10 122.4(3) . . ? N2 C11 C12 118.8(3) . . ? C10 C11 C12 118.8(3) . . ? N3 C12 C13 122.3(3) . . ? N3 C12 C11 119.3(3) . . ? C13 C12 C11 118.3(3) . . ? C14 C13 C16 118.7(3) . . ? C14 C13 C12 121.5(3) . . ? C16 C13 C12 119.8(3) . . ? N4 C14 C13 124.1(3) . . ? N4 C14 C9 115.8(3) . . ? C13 C14 C9 120.1(3) . . ? C3 C15 C2 126.0(3) . . ? C3 C15 C10 116.8(3) . . ? C2 C15 C10 117.3(3) . . ? C6 C16 C13 116.6(3) . . ? C6 C16 C7 126.7(3) . . ? C13 C16 C7 116.7(3) . . ? N5 C17 C18 122.8(3) . . ? N5 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C17 C18 C19 120.7(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 116.7(3) . . ? C18 C19 C27 121.8(3) . . ? C20 C19 C27 121.4(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N5 C21 C20 121.5(3) . . ? N5 C21 C22 115.0(3) . . ? C20 C21 C22 123.4(3) . . ? N6 C22 C23 121.8(3) . . ? N6 C22 C21 114.0(2) . . ? C23 C22 C21 124.1(3) . . ? C22 C23 C24 120.7(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 116.9(3) . . ? C25 C24 C28 121.8(3) . . ? C23 C24 C28 121.4(3) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? N6 C26 C25 122.2(3) . . ? N6 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 C30 122.5(3) . . ? N7 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C31 120.6(3) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 117.1(3) . . ? C30 C31 C39 121.6(3) . . ? C32 C31 C39 121.4(3) . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? N7 C33 C32 121.7(3) . . ? N7 C33 C34 114.4(3) . . ? C32 C33 C34 123.8(3) . . ? N8 C34 C35 122.2(3) . . ? N8 C34 C33 114.3(3) . . ? C35 C34 C33 123.6(3) . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C37 C36 C35 117.0(3) . . ? C37 C36 C40 122.8(4) . . ? C35 C36 C40 120.2(4) . . ? C38 C37 C36 121.4(3) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? N8 C38 C37 121.8(4) . . ? N8 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C31 C39 H39A 109.5 . . ? C31 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C31 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42A C41A C46A 120.0 . . ? C42A C41A C47A 122.7(6) . . ? C46A C41A C47A 117.3(6) . . ? C41A C42A C43A 120.0 . . ? C41A C42A H42A 120.0 . . ? C43A C42A H42A 120.0 . . ? C44A C43A C42A 120.0 . . ? C44A C43A H43A 120.0 . . ? C42A C43A H43A 120.0 . . ? C45A C44A C43A 120.0 . . ? C45A C44A H44A 120.0 . . ? C43A C44A H44A 120.0 . . ? C46A C45A C44A 120.0 . . ? C46A C45A H45A 120.0 . . ? C44A C45A H45A 120.0 . . ? C45A C46A C41A 120.0 . . ? C45A C46A H46A 120.0 . . ? C41A C46A H46A 120.0 . . ? C41A C47A H55A 109.5 . . ? C41A C47A H56A 109.5 . . ? H55A C47A H56A 109.5 . . ? C41A C47A H57A 109.5 . . ? H55A C47A H57A 109.5 . . ? H56A C47A H57A 109.5 . . ? C42B C41B C46B 120.0 . . ? C42B C41B C47B 118.6 . . ? C46B C41B C47B 121.3 . . ? C43B C42B C41B 120.0 . . ? C43B C42B H42B 120.0 . . ? C41B C42B H42B 120.0 . . ? C42B C43B C44B 120.0 . . ? C42B C43B H43B 120.0 . . ? C44B C43B H43B 120.0 . . ? C43B C44B C45B 120.0 . . ? C43B C44B H44B 120.0 . . ? C45B C44B H44B 120.0 . . ? C46B C45B C44B 120.0 . . ? C46B C45B H45B 120.0 . . ? C44B C45B H45B 120.0 . . ? C45B C46B C41B 120.0 . . ? C45B C46B H46B 120.0 . . ? C41B C46B H46B 120.0 . . ? C41B C47B H55B 109.5 . . ? C41B C47B H56B 109.5 . . ? H55B C47B H56B 109.5 . . ? C41B C47B H57B 109.5 . . ? H55B C47B H57B 109.5 . . ? H56B C47B H57B 109.5 . . ? C49A C48A C53A 120.0 . . ? C49A C48A C54A 115.8(11) . . ? C53A C48A C54A 124.2(11) . . ? C48A C49A C50A 120.0 . . ? C48A C49A H49A 120.0 . . ? C50A C49A H49A 120.0 . . ? C51A C50A C49A 120.0 . . ? C51A C50A H50A 120.0 . . ? C49A C50A H50A 120.0 . . ? C50A C51A C52A 120.0 . . ? C50A C51A H51A 120.0 . . ? C52A C51A H51A 120.0 . . ? C51A C52A C53A 120.0 . . ? C51A C52A H52A 120.0 . . ? C53A C52A H52A 120.0 . . ? C52A C53A C48A 120.0 . . ? C52A C53A H53A 120.0 . . ? C48A C53A H53A 120.0 . . ? C48A C54A H58A 109.5 . . ? C48A C54A H59A 109.5 . . ? H58A C54A H59A 109.5 . . ? C48A C54A H60A 109.5 . . ? H58A C54A H60A 109.5 . . ? H59A C54A H60A 109.5 . . ? C49B C48B C53B 120.0 . . ? C49B C48B C54B 102.8 . . ? C53B C48B C54B 136.2 . . ? C50B C49B C48B 120.0 . . ? C50B C49B H49B 120.0 . . ? C48B C49B H49B 120.0 . . ? C49B C50B C51B 120.0 . . ? C49B C50B H50B 120.0 . . ? C51B C50B H50B 120.0 . . ? C50B C51B C52B 120.0 . . ? C50B C51B H51B 120.0 . . ? C52B C51B H51B 120.0 . . ? C53B C52B C51B 120.0 . . ? C53B C52B H52B 120.0 . . ? C51B C52B H52B 120.0 . . ? C52B C53B C48B 120.0 . . ? C52B C53B H53B 120.0 . . ? C48B C53B H53B 120.0 . . ? C48B C54B H58B 109.5 . . ? C48B C54B H59B 109.5 . . ? H58B C54B H59B 109.5 . . ? C48B C54B H60B 109.5 . . ? H58B C54B H60B 109.5 . . ? H59B C54B H60B 109.5 . . ? P2 F11A F12A 68.1(7) . . ? F11A F12A P2 55.3(4) . . ? F12B F9B P2 70.1(10) . . ? F9B F12B P2 75.2(10) . . ? C9 N1 C1 117.3(3) . . ? C9 N1 Ru1 114.36(19) . . ? C1 N1 Ru1 128.3(2) . . ? C11 N2 C4 116.7(3) . . ? C12 N3 C5 117.1(3) . . ? C14 N4 C8 116.5(3) . . ? C14 N4 Ru1 114.0(2) . . ? C8 N4 Ru1 129.4(2) . . ? C17 N5 C21 117.3(3) . . ? C17 N5 Ru1 126.8(2) . . ? C21 N5 Ru1 115.4(2) . . ? C22 N6 C26 117.9(3) . . ? C22 N6 Ru1 116.2(2) . . ? C26 N6 Ru1 125.8(2) . . ? C33 N7 C29 117.5(3) . . ? C33 N7 Ru1 116.15(19) . . ? C29 N7 Ru1 126.3(2) . . ? C38 N8 C34 117.9(3) . . ? C38 N8 Ru1 125.6(3) . . ? C34 N8 Ru1 116.4(2) . . ? F6 P1 F2 90.6(3) . . ? F6 P1 F4 179.0(3) . . ? F2 P1 F4 90.1(3) . . ? F6 P1 F5 87.7(3) . . ? F2 P1 F5 90.9(2) . . ? F4 P1 F5 91.5(3) . . ? F6 P1 F1 90.9(3) . . ? F2 P1 F1 178.5(3) . . ? F4 P1 F1 88.4(3) . . ? F5 P1 F1 88.9(2) . . ? F6 P1 F3 88.3(3) . . ? F2 P1 F3 91.3(2) . . ? F4 P1 F3 92.4(3) . . ? F5 P1 F3 175.5(3) . . ? F1 P1 F3 89.0(2) . . ? F11A P2 F10B 127.9(11) . . ? F11A P2 F12B 106.3(10) . . ? F10B P2 F12B 122.5(10) . . ? F11A P2 F9B 140.9(10) . . ? F10B P2 F9B 89.7(9) . . ? F12B P2 F9B 34.7(6) . . ? F11A P2 F11B 31.8(8) . . ? F10B P2 F11B 97.0(10) . . ? F12B P2 F11B 137.9(10) . . ? F9B P2 F11B 172.5(9) . . ? F11A P2 F8 85.8(6) . . ? F10B P2 F8 81.8(5) . . ? F12B P2 F8 84.8(5) . . ? F9B P2 F8 90.6(4) . . ? F11B P2 F8 87.3(6) . . ? F11A P2 F7 92.7(6) . . ? F10B P2 F7 100.2(5) . . ? F12B P2 F7 94.4(5) . . ? F9B P2 F7 89.8(4) . . ? F11B P2 F7 92.1(6) . . ? F8 P2 F7 177.9(2) . . ? F11A P2 F10A 89.5(9) . . ? F10B P2 F10A 43.3(7) . . ? F12B P2 F10A 164.1(9) . . ? F9B P2 F10A 129.5(8) . . ? F11B P2 F10A 58.0(7) . . ? F8 P2 F10A 97.8(3) . . ? F7 P2 F10A 83.5(3) . . ? F11A P2 F12A 56.6(8) . . ? F10B P2 F12A 172.4(8) . . ? F12B P2 F12A 51.2(7) . . ? F9B P2 F12A 84.8(7) . . ? F11B P2 F12A 88.2(7) . . ? F8 P2 F12A 92.9(3) . . ? F7 P2 F12A 85.2(3) . . ? F10A P2 F12A 143.6(6) . . ? F11A P2 F9A 168.6(9) . . ? F10B P2 F9A 41.1(7) . . ? F12B P2 F9A 85.1(8) . . ? F9B P2 F9A 50.5(6) . . ? F11B P2 F9A 136.8(8) . . ? F8 P2 F9A 94.4(4) . . ? F7 P2 F9A 87.4(4) . . ? F10A P2 F9A 79.1(5) . . ? F12A P2 F9A 134.7(7) . . ? N1 Ru1 N4 79.16(10) . . ? N1 Ru1 N8 90.46(10) . . ? N4 Ru1 N8 99.00(10) . . ? N1 Ru1 N5 97.24(10) . . ? N4 Ru1 N5 90.98(10) . . ? N8 Ru1 N5 168.41(10) . . ? N1 Ru1 N7 96.97(10) . . ? N4 Ru1 N7 175.13(9) . . ? N8 Ru1 N7 77.97(10) . . ? N5 Ru1 N7 92.45(10) . . ? N1 Ru1 N6 173.98(10) . . ? N4 Ru1 N6 96.47(10) . . ? N8 Ru1 N6 94.34(10) . . ? N5 Ru1 N6 78.59(10) . . ? N7 Ru1 N6 87.60(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C15 0.9(6) . . . . ? C15 C3 C4 N2 -1.5(6) . . . . ? N3 C5 C6 C16 -1.2(7) . . . . ? C16 C7 C8 N4 0.9(5) . . . . ? N1 C9 C10 C11 179.1(3) . . . . ? C14 C9 C10 C11 -0.7(4) . . . . ? N1 C9 C10 C15 -0.5(5) . . . . ? C14 C9 C10 C15 179.7(3) . . . . ? C9 C10 C11 N2 179.4(3) . . . . ? C15 C10 C11 N2 -1.0(5) . . . . ? C9 C10 C11 C12 -1.5(4) . . . . ? C15 C10 C11 C12 178.1(3) . . . . ? N2 C11 C12 N3 1.9(5) . . . . ? C10 C11 C12 N3 -177.3(3) . . . . ? N2 C11 C12 C13 -178.2(3) . . . . ? C10 C11 C12 C13 2.7(4) . . . . ? N3 C12 C13 C14 178.3(3) . . . . ? C11 C12 C13 C14 -1.7(4) . . . . ? N3 C12 C13 C16 -1.4(5) . . . . ? C11 C12 C13 C16 178.6(3) . . . . ? C16 C13 C14 N4 -1.0(5) . . . . ? C12 C13 C14 N4 179.3(3) . . . . ? C16 C13 C14 C9 179.2(3) . . . . ? C12 C13 C14 C9 -0.4(4) . . . . ? N1 C9 C14 N4 2.1(4) . . . . ? C10 C9 C14 N4 -178.1(3) . . . . ? N1 C9 C14 C13 -178.1(3) . . . . ? C10 C9 C14 C13 1.7(4) . . . . ? C4 C3 C15 C2 -179.7(4) . . . . ? C4 C3 C15 C10 0.9(5) . . . . ? C1 C2 C15 C3 179.9(4) . . . . ? C1 C2 C15 C10 -0.7(5) . . . . ? C11 C10 C15 C3 0.3(5) . . . . ? C9 C10 C15 C3 179.9(3) . . . . ? C11 C10 C15 C2 -179.2(3) . . . . ? C9 C10 C15 C2 0.5(5) . . . . ? C5 C6 C16 C13 -0.5(5) . . . . ? C5 C6 C16 C7 178.8(4) . . . . ? C14 C13 C16 C6 -178.0(3) . . . . ? C12 C13 C16 C6 1.7(5) . . . . ? C14 C13 C16 C7 2.7(4) . . . . ? C12 C13 C16 C7 -177.7(3) . . . . ? C8 C7 C16 C6 178.1(4) . . . . ? C8 C7 C16 C13 -2.6(5) . . . . ? N5 C17 C18 C19 0.7(6) . . . . ? C17 C18 C19 C20 2.8(6) . . . . ? C17 C18 C19 C27 -175.4(4) . . . . ? C18 C19 C20 C21 -2.8(6) . . . . ? C27 C19 C20 C21 175.4(4) . . . . ? C19 C20 C21 N5 -0.8(5) . . . . ? C19 C20 C21 C22 -178.1(3) . . . . ? N5 C21 C22 N6 -6.4(4) . . . . ? C20 C21 C22 N6 171.1(3) . . . . ? N5 C21 C22 C23 173.9(3) . . . . ? C20 C21 C22 C23 -8.7(5) . . . . ? N6 C22 C23 C24 -0.2(5) . . . . ? C21 C22 C23 C24 179.5(3) . . . . ? C22 C23 C24 C25 -2.2(5) . . . . ? C22 C23 C24 C28 178.2(4) . . . . ? C23 C24 C25 C26 2.8(5) . . . . ? C28 C24 C25 C26 -177.6(4) . . . . ? C24 C25 C26 N6 -1.0(6) . . . . ? N7 C29 C30 C31 0.7(5) . . . . ? C29 C30 C31 C32 -1.8(5) . . . . ? C29 C30 C31 C39 178.0(3) . . . . ? C30 C31 C32 C33 0.8(5) . . . . ? C39 C31 C32 C33 -179.0(3) . . . . ? C31 C32 C33 N7 1.4(5) . . . . ? C31 C32 C33 C34 -176.9(3) . . . . ? N7 C33 C34 N8 0.2(4) . . . . ? C32 C33 C34 N8 178.5(3) . . . . ? N7 C33 C34 C35 -179.0(3) . . . . ? C32 C33 C34 C35 -0.6(5) . . . . ? N8 C34 C35 C36 -1.3(5) . . . . ? C33 C34 C35 C36 177.9(3) . . . . ? C34 C35 C36 C37 -2.1(5) . . . . ? C34 C35 C36 C40 177.6(3) . . . . ? C35 C36 C37 C38 2.9(5) . . . . ? C40 C36 C37 C38 -176.7(4) . . . . ? C36 C37 C38 N8 -0.5(6) . . . . ? C46A C41A C42A C43A 0.0 . . . . ? C47A C41A C42A C43A -179.3(10) . . . . ? C41A C42A C43A C44A 0.0 . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C43A C44A C45A C46A 0.0 . . . . ? C44A C45A C46A C41A 0.0 . . . . ? C42A C41A C46A C45A 0.0 . . . . ? C47A C41A C46A C45A 179.3(9) . . . . ? C46B C41B C42B C43B 0.0 . . . . ? C47B C41B C42B C43B 176.7 . . . . ? C41B C42B C43B C44B 0.0 . . . . ? C42B C43B C44B C45B 0.0 . . . . ? C43B C44B C45B C46B 0.0 . . . . ? C44B C45B C46B C41B 0.0 . . . . ? C42B C41B C46B C45B 0.0 . . . . ? C47B C41B C46B C45B -176.6 . . . . ? C53A C48A C49A C50A 0.0 . . . . ? C54A C48A C49A C50A 178.7(9) . . . . ? C48A C49A C50A C51A 0.0 . . . . ? C49A C50A C51A C52A 0.0 . . . . ? C50A C51A C52A C53A 0.0 . . . . ? C51A C52A C53A C48A 0.0 . . . . ? C49A C48A C53A C52A 0.0 . . . . ? C54A C48A C53A C52A -178.6(10) . . . . ? C53B C48B C49B C50B 0.0 . . . . ? C54B C48B C49B C50B -170.4 . . . . ? C48B C49B C50B C51B 0.0 . . . . ? C49B C50B C51B C52B 0.0 . . . . ? C50B C51B C52B C53B 0.0 . . . . ? C51B C52B C53B C48B 0.0 . . . . ? C49B C48B C53B C52B 0.0 . . . . ? C54B C48B C53B C52B 166.5 . . . . ? C10 C9 N1 C1 0.7(5) . . . . ? C14 C9 N1 C1 -179.5(3) . . . . ? C10 C9 N1 Ru1 -179.3(2) . . . . ? C14 C9 N1 Ru1 0.4(3) . . . . ? C2 C1 N1 C9 -0.9(5) . . . . ? C2 C1 N1 Ru1 179.1(3) . . . . ? C10 C11 N2 C4 0.5(5) . . . . ? C12 C11 N2 C4 -178.7(3) . . . . ? C3 C4 N2 C11 0.8(5) . . . . ? C13 C12 N3 C5 -0.2(5) . . . . ? C11 C12 N3 C5 179.8(3) . . . . ? C6 C5 N3 C12 1.5(6) . . . . ? C13 C14 N4 C8 -0.8(4) . . . . ? C9 C14 N4 C8 178.9(3) . . . . ? C13 C14 N4 Ru1 176.7(2) . . . . ? C9 C14 N4 Ru1 -3.6(3) . . . . ? C7 C8 N4 C14 0.9(5) . . . . ? C7 C8 N4 Ru1 -176.1(3) . . . . ? C18 C17 N5 C21 -4.3(5) . . . . ? C18 C17 N5 Ru1 166.9(3) . . . . ? C20 C21 N5 C17 4.3(5) . . . . ? C22 C21 N5 C17 -178.2(3) . . . . ? C20 C21 N5 Ru1 -167.9(3) . . . . ? C22 C21 N5 Ru1 9.6(4) . . . . ? C23 C22 N6 C26 2.1(5) . . . . ? C21 C22 N6 C26 -177.6(3) . . . . ? C23 C22 N6 Ru1 179.9(3) . . . . ? C21 C22 N6 Ru1 0.2(4) . . . . ? C25 C26 N6 C22 -1.5(5) . . . . ? C25 C26 N6 Ru1 -179.1(3) . . . . ? C32 C33 N7 C29 -2.4(4) . . . . ? C34 C33 N7 C29 176.0(2) . . . . ? C32 C33 N7 Ru1 175.0(2) . . . . ? C34 C33 N7 Ru1 -6.6(3) . . . . ? C30 C29 N7 C33 1.4(4) . . . . ? C30 C29 N7 Ru1 -175.8(2) . . . . ? C37 C38 N8 C34 -2.8(5) . . . . ? C37 C38 N8 Ru1 175.1(3) . . . . ? C35 C34 N8 C38 3.7(4) . . . . ? C33 C34 N8 C38 -175.5(3) . . . . ? C35 C34 N8 Ru1 -174.5(2) . . . . ? C33 C34 N8 Ru1 6.3(3) . . . . ? F12A F11A P2 F10B -172.5(7) . . . . ? F12A F11A P2 F12B -12.9(8) . . . . ? F12A F11A P2 F9B -10.5(13) . . . . ? F12A F11A P2 F11B 172(2) . . . . ? F12A F11A P2 F8 -96.2(5) . . . . ? F12A F11A P2 F7 82.5(5) . . . . ? F12A F11A P2 F10A 165.9(6) . . . . ? F12A F11A P2 F9A 172(3) . . . . ? F9B F12B P2 F11A 177.4(12) . . . . ? F9B F12B P2 F10B -21.7(16) . . . . ? F9B F12B P2 F11B -178.6(11) . . . . ? F9B F12B P2 F8 -98.6(13) . . . . ? F9B F12B P2 F7 83.3(13) . . . . ? F9B F12B P2 F10A 2(3) . . . . ? F9B F12B P2 F12A 163.5(16) . . . . ? F9B F12B P2 F9A -3.7(13) . . . . ? F12B F9B P2 F11A -4.0(19) . . . . ? F12B F9B P2 F10B 161.8(14) . . . . ? F12B F9B P2 F11B 7(6) . . . . ? F12B F9B P2 F8 80.0(13) . . . . ? F12B F9B P2 F7 -98.0(13) . . . . ? F12B F9B P2 F10A -179.4(11) . . . . ? F12B F9B P2 F12A -12.8(12) . . . . ? F12B F9B P2 F9A 175.2(16) . . . . ? F11A F12A P2 F10B 129(6) . . . . ? F11A F12A P2 F12B 164.0(10) . . . . ? F11A F12A P2 F9B 173.3(8) . . . . ? F11A F12A P2 F11B -4.1(11) . . . . ? F11A F12A P2 F8 83.0(7) . . . . ? F11A F12A P2 F7 -96.4(7) . . . . ? F11A F12A P2 F10A -24.3(10) . . . . ? F11A F12A P2 F9A -177.9(9) . . . . ? C9 N1 Ru1 N4 -1.8(2) . . . . ? C1 N1 Ru1 N4 178.2(3) . . . . ? C9 N1 Ru1 N8 -100.9(2) . . . . ? C1 N1 Ru1 N8 79.1(3) . . . . ? C9 N1 Ru1 N5 87.8(2) . . . . ? C1 N1 Ru1 N5 -92.2(3) . . . . ? C9 N1 Ru1 N7 -178.8(2) . . . . ? C1 N1 Ru1 N7 1.2(3) . . . . ? C9 N1 Ru1 N6 42.0(10) . . . . ? C1 N1 Ru1 N6 -138.1(8) . . . . ? C14 N4 Ru1 N1 2.9(2) . . . . ? C8 N4 Ru1 N1 180.0(3) . . . . ? C14 N4 Ru1 N8 91.7(2) . . . . ? C8 N4 Ru1 N8 -91.3(3) . . . . ? C14 N4 Ru1 N5 -94.3(2) . . . . ? C8 N4 Ru1 N5 82.8(3) . . . . ? C14 N4 Ru1 N7 40.5(12) . . . . ? C8 N4 Ru1 N7 -142.5(10) . . . . ? C14 N4 Ru1 N6 -172.9(2) . . . . ? C8 N4 Ru1 N6 4.2(3) . . . . ? C38 N8 Ru1 N1 77.4(3) . . . . ? C34 N8 Ru1 N1 -104.6(2) . . . . ? C38 N8 Ru1 N4 -1.7(3) . . . . ? C34 N8 Ru1 N4 176.3(2) . . . . ? C38 N8 Ru1 N5 -150.8(4) . . . . ? C34 N8 Ru1 N5 27.2(6) . . . . ? C38 N8 Ru1 N7 174.5(3) . . . . ? C34 N8 Ru1 N7 -7.5(2) . . . . ? C38 N8 Ru1 N6 -98.9(3) . . . . ? C34 N8 Ru1 N6 79.1(2) . . . . ? C17 N5 Ru1 N1 5.7(3) . . . . ? C21 N5 Ru1 N1 177.1(2) . . . . ? C17 N5 Ru1 N4 84.9(3) . . . . ? C21 N5 Ru1 N4 -103.7(2) . . . . ? C17 N5 Ru1 N8 -125.5(5) . . . . ? C21 N5 Ru1 N8 45.8(6) . . . . ? C17 N5 Ru1 N7 -91.6(3) . . . . ? C21 N5 Ru1 N7 79.7(2) . . . . ? C17 N5 Ru1 N6 -178.7(3) . . . . ? C21 N5 Ru1 N6 -7.3(2) . . . . ? C33 N7 Ru1 N1 96.6(2) . . . . ? C29 N7 Ru1 N1 -86.2(2) . . . . ? C33 N7 Ru1 N4 59.5(12) . . . . ? C29 N7 Ru1 N4 -123.3(11) . . . . ? C33 N7 Ru1 N8 7.62(19) . . . . ? C29 N7 Ru1 N8 -175.2(3) . . . . ? C33 N7 Ru1 N5 -165.8(2) . . . . ? C29 N7 Ru1 N5 11.4(2) . . . . ? C33 N7 Ru1 N6 -87.3(2) . . . . ? C29 N7 Ru1 N6 89.8(2) . . . . ? C22 N6 Ru1 N1 50.3(10) . . . . ? C26 N6 Ru1 N1 -132.1(8) . . . . ? C22 N6 Ru1 N4 93.4(2) . . . . ? C26 N6 Ru1 N4 -89.0(3) . . . . ? C22 N6 Ru1 N8 -167.0(2) . . . . ? C26 N6 Ru1 N8 10.5(3) . . . . ? C22 N6 Ru1 N5 3.7(2) . . . . ? C26 N6 Ru1 N5 -178.7(3) . . . . ? C22 N6 Ru1 N7 -89.3(2) . . . . ? C26 N6 Ru1 N7 88.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.703 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.062 #====================================================================== data_brie8i _database_code_depnum_ccdc_archive 'CCDC 844738' #TrackingRef '- brie8i.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(4,4'-Ditertbutyl-2,2'-bipyridyl)(1,6,7,12-tetraazaperylene)-ruthenium(ii) bis(hexafluorophosphate) ; _chemical_name_common ; bis(4,4'-Ditertbutyl-2,2'-bipyridyl)(1,6,7,12- tetraazaperylene)-ruthenium(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C52 H56 N8 2+ , F12 P2 2- , C9 H18 O3 , H1 O0.5' _chemical_formula_sum 'C61 H75 F12 N8 O3.50 P2 Ru' _chemical_formula_weight 1367.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6866(10) _cell_length_b 16.5502(16) _cell_length_c 18.6083(17) _cell_angle_alpha 67.838(7) _cell_angle_beta 81.554(7) _cell_angle_gamma 75.338(7) _cell_volume 3219.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 15631 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 26.83 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.140 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method ? _exptl_crystal_F_000 1414 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.9333 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was embedded in perfluoropolyalkylether oil. ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 210(2) _diffrn_measurement_method 'rotation method, delta omega = 1.0 deg' _diffrn_measurement_details ; 180 frames, detector distance = 120 mm ; _diffrn_reflns_number 20910 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10650 _reflns_number_gt 6877 _reflns_threshold_expression >2sigma(I) _publ_section_exptl_refinement ; The hydrogen atoms of water molecule were found from the difference Fourier map. All the other hydrogen atoms were calculated in idealized positions and allowed to ride on their corresponding carbon atoms. ; _computing_data_collection 'X-AREA (Stoe, 2006)' _computing_cell_refinement 'X-AREA (Stoe, 2002)' _computing_data_reduction 'X-RED32 (Stoe, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10650 _refine_ls_number_parameters 895 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3650(3) 0.8369(3) 0.6334(2) 0.0424(10) Uani 1 1 d . . . H1 H 0.4183 0.7875 0.6631 0.051 Uiso 1 1 calc R . . C2 C 0.4023(4) 0.8870(3) 0.5610(2) 0.0464(11) Uani 1 1 d . . . H2 H 0.4791 0.8700 0.5420 0.056 Uiso 1 1 calc R . . C3 C 0.3548(4) 1.0217(3) 0.4392(2) 0.0549(12) Uani 1 1 d . . . H3 H 0.4299 1.0106 0.4155 0.066 Uiso 1 1 calc R . . C4 C 0.2701(5) 1.0937(3) 0.4020(3) 0.0619(13) Uani 1 1 d . . . H4 H 0.2907 1.1304 0.3524 0.074 Uiso 1 1 calc R . . C5 C -0.1806(5) 1.1697(3) 0.5296(3) 0.0629(13) Uani 1 1 d . . . H5 H -0.2347 1.2197 0.5015 0.075 Uiso 1 1 calc R . . C6 C -0.2188(4) 1.1177(3) 0.6006(3) 0.0576(12) Uani 1 1 d . . . H6 H -0.2963 1.1319 0.6199 0.069 Uiso 1 1 calc R . . C7 C -0.1635(4) 0.9799(3) 0.7188(2) 0.0518(11) Uani 1 1 d . . . H7 H -0.2388 0.9886 0.7429 0.062 Uiso 1 1 calc R . . C8 C -0.0785(4) 0.9083(3) 0.7547(2) 0.0455(10) Uani 1 1 d . . . H8 H -0.0978 0.8691 0.8035 0.055 Uiso 1 1 calc R . . C9 C 0.1779(3) 0.9296(2) 0.6206(2) 0.0346(9) Uani 1 1 d . . . C10 C 0.2109(3) 0.9863(3) 0.5457(2) 0.0393(9) Uani 1 1 d . . . C11 C 0.1299(4) 1.0628(3) 0.5022(2) 0.0448(10) Uani 1 1 d . . . C12 C 0.0078(4) 1.0838(3) 0.5362(2) 0.0449(10) Uani 1 1 d . . . C13 C -0.0225(3) 1.0247(2) 0.6117(2) 0.0393(9) Uani 1 1 d . . . C14 C 0.0594(3) 0.9489(2) 0.6528(2) 0.0357(9) Uani 1 1 d . . . C15 C 0.3262(4) 0.9643(3) 0.5143(2) 0.0428(10) Uani 1 1 d . . . C16 C -0.1378(4) 1.0417(3) 0.6445(2) 0.0456(10) Uani 1 1 d . . . C17 C 0.2691(4) 0.9187(2) 0.8082(2) 0.0436(10) Uani 1 1 d . . . H17 H 0.3004 0.9354 0.7571 0.052 Uiso 1 1 calc R . . C18 C 0.2891(4) 0.9601(3) 0.8552(2) 0.0469(10) Uani 1 1 d . . . H18 H 0.3325 1.0046 0.8351 0.056 Uiso 1 1 calc R . . C19 C 0.2459(4) 0.9368(2) 0.9320(2) 0.0407(10) Uani 1 1 d . . . C20 C 0.1790(3) 0.8706(2) 0.9577(2) 0.0375(9) Uani 1 1 d . . . H20 H 0.1467 0.8534 1.0086 0.045 Uiso 1 1 calc R . . C21 C 0.1603(3) 0.8308(2) 0.90870(19) 0.0331(8) Uani 1 1 d . . . C22 C 0.0900(3) 0.7610(2) 0.9310(2) 0.0341(9) Uani 1 1 d . . . C23 C 0.0316(3) 0.7289(2) 1.0025(2) 0.0361(9) Uani 1 1 d . . . H23 H 0.0376 0.7502 1.0412 0.043 Uiso 1 1 calc R . . C24 C -0.0360(3) 0.6655(2) 1.0179(2) 0.0373(9) Uani 1 1 d . . . C25 C -0.0404(4) 0.6364(3) 0.9577(2) 0.0451(10) Uani 1 1 d . . . H25 H -0.0841 0.5938 0.9650 0.054 Uiso 1 1 calc R . . C26 C 0.0194(3) 0.6699(2) 0.8872(2) 0.0404(9) Uani 1 1 d . . . H26 H 0.0148 0.6491 0.8480 0.048 Uiso 1 1 calc R . . C27 C 0.2661(4) 0.9812(3) 0.9862(2) 0.0486(11) Uani 1 1 d . . . C28 C 0.3456(4) 1.0483(3) 0.9463(3) 0.0674(14) Uani 1 1 d . . . H28A H 0.3089 1.0940 0.9013 0.101 Uiso 1 1 calc R . . H28B H 0.4210 1.0180 0.9308 0.101 Uiso 1 1 calc R . . H28C H 0.3568 1.0749 0.9818 0.101 Uiso 1 1 calc R . . C29 C 0.1469(4) 1.0311(3) 1.0106(3) 0.0626(13) Uani 1 1 d . . . H29A H 0.0964 0.9898 1.0366 0.094 Uiso 1 1 calc R . . H29B H 0.1102 1.0764 0.9654 0.094 Uiso 1 1 calc R . . H29C H 0.1595 1.0586 1.0451 0.094 Uiso 1 1 calc R . . C30 C 0.3251(4) 0.9096(3) 1.0584(3) 0.0671(13) Uani 1 1 d . . . H30A H 0.3995 0.8779 1.0431 0.101 Uiso 1 1 calc R . . H30B H 0.2744 0.8686 1.0851 0.101 Uiso 1 1 calc R . . H30C H 0.3384 0.9375 1.0924 0.101 Uiso 1 1 calc R . . C31 C -0.1003(4) 0.6292(3) 1.0978(2) 0.0453(10) Uani 1 1 d . . . C32 C -0.1901(4) 0.5777(3) 1.0945(3) 0.0700(14) Uani 1 1 d . . . H32A H -0.1500 0.5289 1.0778 0.105 Uiso 1 1 calc R . . H32B H -0.2486 0.6170 1.0584 0.105 Uiso 1 1 calc R . . H32C H -0.2281 0.5549 1.1451 0.105 Uiso 1 1 calc R . . C33 C -0.1652(5) 0.7064(3) 1.1238(3) 0.0801(17) Uani 1 1 d . . . H33A H -0.2227 0.7458 1.0870 0.120 Uiso 1 1 calc R . . H33B H -0.1094 0.7385 1.1269 0.120 Uiso 1 1 calc R . . H33C H -0.2046 0.6836 1.1740 0.120 Uiso 1 1 calc R . . C34 C -0.0082(4) 0.5642(3) 1.1551(2) 0.0751(15) Uani 1 1 d . . . H34A H 0.0489 0.5951 1.1586 0.113 Uiso 1 1 calc R . . H34B H 0.0311 0.5161 1.1373 0.113 Uiso 1 1 calc R . . H34C H -0.0469 0.5406 1.2054 0.113 Uiso 1 1 calc R . . C35 C 0.4007(4) 0.6775(3) 0.8496(2) 0.0434(10) Uani 1 1 d . . . H35 H 0.3939 0.7239 0.8676 0.052 Uiso 1 1 calc R . . C36 C 0.4938(4) 0.6051(3) 0.8719(2) 0.0480(10) Uani 1 1 d . . . H36 H 0.5488 0.6044 0.9037 0.058 Uiso 1 1 calc R . . C37 C 0.5077(4) 0.5330(3) 0.8482(2) 0.0431(10) Uani 1 1 d . . . C38 C 0.4240(4) 0.5410(3) 0.7983(2) 0.0395(10) Uani 1 1 d . . . H38 H 0.4298 0.4953 0.7796 0.047 Uiso 1 1 calc R . . C39 C 0.3323(3) 0.6156(2) 0.77617(19) 0.0332(9) Uani 1 1 d . . . C40 C 0.2410(3) 0.6285(2) 0.72359(19) 0.0348(9) Uani 1 1 d . . . C41 C 0.2454(4) 0.5743(2) 0.6817(2) 0.0414(10) Uani 1 1 d . . . H41 H 0.3078 0.5251 0.6873 0.050 Uiso 1 1 calc R . . C42 C 0.1578(4) 0.5923(3) 0.6312(2) 0.0431(10) Uani 1 1 d . . . C43 C 0.0632(4) 0.6635(3) 0.6296(2) 0.0484(11) Uani 1 1 d . . . H43 H -0.0008 0.6753 0.6000 0.058 Uiso 1 1 calc R . . C44 C 0.0635(4) 0.7168(3) 0.6717(2) 0.0410(10) Uani 1 1 d . . . H44 H 0.0001 0.7650 0.6683 0.049 Uiso 1 1 calc R . . C45 C 0.6059(4) 0.4489(3) 0.8743(2) 0.0540(11) Uani 1 1 d . . . C46 C 0.6861(4) 0.4540(3) 0.9303(3) 0.0699(13) Uani 1 1 d . . . H46A H 0.6396 0.4602 0.9757 0.105 Uiso 1 1 calc R . . H46B H 0.7220 0.5046 0.9049 0.105 Uiso 1 1 calc R . . H46C H 0.7468 0.4003 0.9453 0.105 Uiso 1 1 calc R . . C47 C 0.5492(5) 0.3676(3) 0.9171(3) 0.0750(15) Uani 1 1 d . . . H47A H 0.5003 0.3622 0.8827 0.113 Uiso 1 1 calc R . . H47B H 0.5016 0.3755 0.9616 0.113 Uiso 1 1 calc R . . H47C H 0.6103 0.3144 0.9337 0.113 Uiso 1 1 calc R . . C48 C 0.6825(5) 0.4377(4) 0.8032(3) 0.0812(16) Uani 1 1 d . . . H48A H 0.7170 0.4889 0.7770 0.122 Uiso 1 1 calc R . . H48B H 0.6344 0.4322 0.7685 0.122 Uiso 1 1 calc R . . H48C H 0.7444 0.3850 0.8196 0.122 Uiso 1 1 calc R . . C49 C 0.1673(5) 0.5363(3) 0.5807(2) 0.0600(13) Uani 1 1 d . . . C50 C 0.1317(8) 0.4513(4) 0.6272(3) 0.139(3) Uani 1 1 d . . . H50A H 0.0512 0.4634 0.6472 0.209 Uiso 1 1 calc R . . H50B H 0.1826 0.4187 0.6695 0.209 Uiso 1 1 calc R . . H50C H 0.1381 0.4165 0.5950 0.209 Uiso 1 1 calc R . . C51 C 0.2948(6) 0.5191(6) 0.5473(4) 0.152(4) Uani 1 1 d . . . H51A H 0.3472 0.4882 0.5891 0.228 Uiso 1 1 calc R . . H51B H 0.3156 0.5750 0.5160 0.228 Uiso 1 1 calc R . . H51C H 0.3018 0.4833 0.5159 0.228 Uiso 1 1 calc R . . C52 C 0.0916(7) 0.5863(4) 0.5117(3) 0.120(3) Uani 1 1 d . . . H52A H 0.1174 0.6404 0.4807 0.180 Uiso 1 1 calc R . . H52B H 0.0103 0.6006 0.5295 0.180 Uiso 1 1 calc R . . H52C H 0.0990 0.5497 0.4810 0.180 Uiso 1 1 calc R . . C53 C 0.5032(6) 0.3126(4) 0.7195(3) 0.0859(17) Uani 1 1 d . . . C54 C 0.4937(8) 0.2255(5) 0.7750(4) 0.142(3) Uani 1 1 d . . . H54A H 0.5707 0.1921 0.7927 0.214 Uiso 1 1 calc R . . H54B H 0.4622 0.1944 0.7509 0.214 Uiso 1 1 calc R . . H54C H 0.4419 0.2321 0.8185 0.214 Uiso 1 1 calc R . . C55 C 0.5791(9) 0.3170(6) 0.6494(5) 0.190(5) Uani 1 1 d . . . H55A H 0.5511 0.2886 0.6210 0.285 Uiso 1 1 calc R . . H55B H 0.6587 0.2868 0.6633 0.285 Uiso 1 1 calc R . . H55C H 0.5774 0.3783 0.6177 0.285 Uiso 1 1 calc R . . C56 C 0.0483(5) 0.8015(3) 1.2159(3) 0.0660(13) Uani 1 1 d . . . C57 C -0.0030(6) 0.8915(4) 1.2161(3) 0.113(2) Uani 1 1 d . . . H57A H 0.0423 0.9053 1.2473 0.169 Uiso 1 1 calc R . . H57B H -0.0833 0.8948 1.2372 0.169 Uiso 1 1 calc R . . H57C H -0.0015 0.9337 1.1639 0.169 Uiso 1 1 calc R . . C58 C 0.0551(8) 0.7265(4) 1.2909(3) 0.145(3) Uani 1 1 d . . . H58C H 0.0906 0.6715 1.2824 0.217 Uiso 1 1 calc R . . H58B H -0.0233 0.7240 1.3146 0.217 Uiso 1 1 calc R . . H58A H 0.1022 0.7350 1.3245 0.217 Uiso 1 1 calc R . . C59 C 0.6495(10) 0.6402(6) 0.6212(4) 0.143(3) Uani 1 1 d . . . C60 C 0.5513(6) 0.6333(5) 0.5843(4) 0.112(2) Uani 1 1 d . . . H60A H 0.5468 0.5717 0.6006 0.168 Uiso 1 1 calc R . . H60B H 0.5647 0.6567 0.5288 0.168 Uiso 1 1 calc R . . H60C H 0.4783 0.6668 0.5993 0.168 Uiso 1 1 calc R . . C61 C 0.7638(7) 0.5949(10) 0.6058(5) 0.255(8) Uani 1 1 d . . . H61A H 0.7836 0.6167 0.5509 0.382 Uiso 1 1 calc R . . H61B H 0.7661 0.5320 0.6233 0.382 Uiso 1 1 calc R . . H61C H 0.8198 0.6049 0.6328 0.382 Uiso 1 1 calc R . . P1A P 0.6358(2) 0.81616(15) 0.8944(2) 0.0646(6) Uani 0.70 1 d P A 1 F1A F 0.5997(5) 0.9211(3) 0.8694(5) 0.124(2) Uani 0.70 1 d P A 1 F2A F 0.6732(11) 0.7101(7) 0.9183(5) 0.0737(19) Uani 0.70 1 d P A 1 F3A F 0.5950(6) 0.8045(4) 0.9810(4) 0.149(3) Uani 0.70 1 d P A 1 F4A F 0.5165(7) 0.8018(5) 0.9027(5) 0.118(3) Uani 0.70 1 d P A 1 F5A F 0.6862(13) 0.8257(8) 0.8083(5) 0.146(5) Uani 0.70 1 d P A 1 F6A F 0.7613(6) 0.8208(5) 0.9113(3) 0.0744(17) Uani 0.70 1 d P A 1 P1B P 0.6487(6) 0.7976(5) 0.8516(5) 0.0790(19) Uani 0.30 1 d P B 2 F1B F 0.6149(12) 0.9029(11) 0.8103(9) 0.106(4) Uani 0.30 1 d P B 2 F2B F 0.685(3) 0.6920(18) 0.8912(14) 0.120(8) Uani 0.30 1 d P B 2 F3B F 0.5735(17) 0.7815(14) 0.7958(9) 0.145(8) Uani 0.30 1 d P B 2 F4B F 0.5316(18) 0.8201(12) 0.8423(16) 0.140(11) Uani 0.30 1 d P B 2 F5B F 0.7594(17) 0.7901(15) 0.7923(14) 0.112(7) Uani 0.30 1 d P B 2 F6B F 0.7285(16) 0.8051(15) 0.9090(15) 0.148(10) Uani 0.30 1 d P B 2 F7 F 0.3375(3) 1.1638(3) 0.53186(19) 0.1206(13) Uani 1 1 d . . . F8 F 0.2950(5) 1.1577(4) 0.7043(2) 0.162(2) Uani 1 1 d . . . F9A F 0.1887(11) 1.1538(12) 0.6200(9) 0.175(6) Uani 0.70 1 d P C 1 F10A F 0.2900(15) 1.2620(6) 0.5962(7) 0.163(6) Uani 0.70 1 d P C 1 F11A F 0.4539(6) 1.1662(7) 0.6123(4) 0.140(2) Uani 0.80 1 d P C 1 F12A F 0.3615(8) 1.0559(3) 0.6401(4) 0.134(2) Uani 0.80 1 d P C 1 F9B F 0.223(3) 1.1064(17) 0.6389(15) 0.144(15) Uani 0.30 1 d P C 2 F10B F 0.205(3) 1.2461(16) 0.5831(15) 0.160(11) Uani 0.30 1 d P C 2 F11B F 0.377(3) 1.238(2) 0.598(2) 0.119(10) Uani 0.20 1 d P C 2 F12B F 0.413(3) 1.0928(18) 0.6688(12) 0.129(7) Uani 0.20 1 d P C 2 N1 N 0.2515(3) 0.8568(2) 0.66410(17) 0.0352(8) Uani 1 1 d . . . N2 N 0.1586(3) 1.1161(2) 0.43134(19) 0.0576(10) Uani 1 1 d . . . N3 N -0.0701(4) 1.1541(2) 0.4965(2) 0.0573(10) Uani 1 1 d . . . N4 N 0.0342(3) 0.8907(2) 0.72293(16) 0.0365(8) Uani 1 1 d . . . N5 N 0.2056(3) 0.85472(18) 0.83348(16) 0.0337(7) Uani 1 1 d . . . N6 N 0.0841(3) 0.73147(19) 0.87260(16) 0.0342(7) Uani 1 1 d . . . N7 N 0.3194(3) 0.68377(19) 0.80286(16) 0.0337(7) Uani 1 1 d . . . N8 N 0.1510(3) 0.7019(2) 0.71689(16) 0.0346(7) Uani 1 1 d . . . O1 O 0.4468(5) 0.3800(3) 0.7266(3) 0.1348(19) Uani 1 1 d . . . O2 O 0.0831(4) 0.7888(3) 1.1553(2) 0.0939(12) Uani 1 1 d . . . O3 O 0.6197(7) 0.6853(4) 0.6687(3) 0.182(3) Uani 1 1 d . . . O4 O 0.7989(8) 0.6661(6) 0.7708(5) 0.088(3) Uani 0.50 1 d P . . H400 H 0.774(13) 0.694(10) 0.788(8) 0.106 Uiso 0.50 1 d P . . H401 H 0.7589 0.6384 0.7993 0.106 Uiso 0.50 1 d P . . P2 P 0.31743(17) 1.16181(11) 0.61802(8) 0.0833(5) Uani 1 1 d . C . Ru1 Ru 0.17364(3) 0.78699(2) 0.768625(18) 0.03208(9) 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 0.033(2) 0.046(2) 0.049(2) -0.0209(19) 0.002(2) -0.006(2) C2 0.040(3) 0.056(3) 0.048(2) -0.022(2) 0.011(2) -0.020(2) C3 0.054(3) 0.075(3) 0.040(2) -0.017(2) 0.010(2) -0.032(3) C4 0.061(4) 0.078(3) 0.041(2) -0.004(2) -0.003(2) -0.031(3) C5 0.055(4) 0.043(3) 0.076(3) -0.007(2) -0.020(3) 0.003(2) C6 0.045(3) 0.051(3) 0.071(3) -0.018(2) -0.010(2) -0.002(2) C7 0.037(3) 0.053(3) 0.059(3) -0.018(2) 0.001(2) -0.004(2) C8 0.034(3) 0.049(2) 0.045(2) -0.013(2) 0.006(2) -0.005(2) C9 0.033(2) 0.038(2) 0.036(2) -0.0154(18) 0.0009(18) -0.011(2) C10 0.037(3) 0.043(2) 0.037(2) -0.0103(18) -0.0009(19) -0.014(2) C11 0.045(3) 0.047(2) 0.042(2) -0.012(2) -0.003(2) -0.016(2) C12 0.044(3) 0.041(2) 0.046(2) -0.0068(19) -0.013(2) -0.010(2) C13 0.034(3) 0.038(2) 0.043(2) -0.0108(18) -0.0075(19) -0.005(2) C14 0.036(2) 0.036(2) 0.036(2) -0.0133(17) 0.0025(18) -0.011(2) C15 0.041(3) 0.051(2) 0.040(2) -0.017(2) 0.002(2) -0.018(2) C16 0.040(3) 0.040(2) 0.052(2) -0.013(2) -0.010(2) -0.002(2) C17 0.045(3) 0.042(2) 0.045(2) -0.0134(19) 0.0047(19) -0.019(2) C18 0.052(3) 0.040(2) 0.053(2) -0.0139(19) -0.004(2) -0.021(2) C19 0.040(3) 0.035(2) 0.049(2) -0.0160(18) -0.009(2) -0.008(2) C20 0.036(2) 0.038(2) 0.039(2) -0.0130(17) -0.0022(18) -0.0094(19) C21 0.030(2) 0.0301(19) 0.038(2) -0.0111(16) -0.0035(17) -0.0056(18) C22 0.031(2) 0.0302(19) 0.040(2) -0.0112(16) -0.0027(17) -0.0060(18) C23 0.037(2) 0.036(2) 0.0332(19) -0.0112(16) 0.0002(17) -0.0072(19) C24 0.033(2) 0.036(2) 0.036(2) -0.0055(17) -0.0001(18) -0.0077(19) C25 0.045(3) 0.041(2) 0.052(2) -0.0133(19) 0.004(2) -0.022(2) C26 0.044(3) 0.037(2) 0.045(2) -0.0179(18) -0.0009(19) -0.013(2) C27 0.049(3) 0.048(2) 0.059(3) -0.025(2) -0.008(2) -0.016(2) C28 0.074(4) 0.068(3) 0.086(3) -0.042(3) -0.003(3) -0.038(3) C29 0.068(4) 0.063(3) 0.073(3) -0.041(3) -0.006(3) -0.016(3) C30 0.074(4) 0.070(3) 0.068(3) -0.029(3) -0.020(3) -0.020(3) C31 0.043(3) 0.045(2) 0.042(2) -0.0096(19) 0.007(2) -0.014(2) C32 0.064(4) 0.082(3) 0.063(3) -0.014(3) 0.009(3) -0.038(3) C33 0.099(4) 0.065(3) 0.070(3) -0.025(3) 0.037(3) -0.031(3) C34 0.064(4) 0.088(4) 0.044(3) 0.005(3) 0.000(2) -0.013(3) C35 0.040(3) 0.047(2) 0.050(2) -0.024(2) -0.012(2) -0.006(2) C36 0.038(3) 0.059(3) 0.050(2) -0.023(2) -0.014(2) -0.003(2) C37 0.036(3) 0.047(2) 0.040(2) -0.0120(19) -0.0011(19) -0.005(2) C38 0.041(3) 0.040(2) 0.037(2) -0.0148(18) -0.0009(19) -0.008(2) C39 0.032(2) 0.035(2) 0.0314(19) -0.0111(16) -0.0025(17) -0.0075(19) C40 0.040(3) 0.036(2) 0.0319(19) -0.0130(16) -0.0006(17) -0.013(2) C41 0.050(3) 0.039(2) 0.038(2) -0.0139(17) -0.0051(19) -0.011(2) C42 0.055(3) 0.044(2) 0.035(2) -0.0130(18) -0.002(2) -0.020(2) C43 0.057(3) 0.057(3) 0.040(2) -0.013(2) -0.014(2) -0.026(3) C44 0.038(3) 0.043(2) 0.039(2) -0.0084(18) -0.0088(19) -0.010(2) C45 0.041(3) 0.053(3) 0.057(3) -0.016(2) -0.008(2) 0.008(2) C46 0.049(3) 0.075(3) 0.072(3) -0.019(3) -0.022(3) 0.010(3) C47 0.070(4) 0.053(3) 0.088(4) -0.017(3) -0.013(3) 0.004(3) C48 0.061(4) 0.093(4) 0.073(3) -0.034(3) -0.005(3) 0.019(3) C49 0.081(4) 0.065(3) 0.050(3) -0.031(2) -0.009(2) -0.024(3) C50 0.289(11) 0.078(4) 0.088(4) -0.046(4) 0.013(5) -0.092(6) C51 0.115(6) 0.280(10) 0.147(6) -0.177(8) 0.034(5) -0.059(7) C52 0.189(8) 0.110(5) 0.083(4) -0.055(4) -0.056(5) -0.010(5) C53 0.102(5) 0.070(4) 0.094(4) -0.046(3) -0.009(4) -0.004(4) C54 0.185(9) 0.104(6) 0.131(6) -0.016(5) -0.044(6) -0.039(6) C55 0.214(10) 0.162(8) 0.216(10) -0.118(8) 0.123(9) -0.079(8) C56 0.072(4) 0.074(3) 0.058(3) -0.025(3) -0.002(3) -0.025(3) C57 0.153(7) 0.084(4) 0.090(4) -0.036(4) 0.026(4) -0.015(4) C58 0.202(9) 0.106(5) 0.075(4) -0.005(4) 0.028(5) -0.009(6) C59 0.216(11) 0.152(7) 0.060(4) -0.016(4) 0.006(6) -0.081(8) C60 0.117(6) 0.124(6) 0.113(5) -0.057(5) 0.013(5) -0.044(5) C61 0.074(6) 0.54(2) 0.130(7) -0.158(12) 0.020(6) 0.014(10) P1A 0.0541(17) 0.0591(13) 0.0876(18) -0.0296(13) -0.0102(14) -0.0153(12) F1A 0.105(5) 0.064(3) 0.219(7) -0.057(4) -0.057(5) -0.005(3) F2A 0.085(4) 0.063(4) 0.075(4) -0.023(3) -0.008(3) -0.020(3) F3A 0.162(5) 0.160(5) 0.178(6) -0.118(5) 0.113(5) -0.102(5) F4A 0.098(5) 0.101(5) 0.146(6) -0.031(5) -0.002(5) -0.030(4) F5A 0.286(17) 0.121(10) 0.062(5) -0.029(5) -0.013(9) -0.100(11) F6A 0.052(4) 0.102(4) 0.086(3) -0.043(3) 0.002(3) -0.035(3) P1B 0.074(5) 0.095(5) 0.062(4) -0.008(4) 0.004(4) -0.044(4) F1B 0.093(10) 0.073(9) 0.131(12) 0.004(8) -0.016(9) -0.039(8) F2B 0.122(17) 0.098(16) 0.13(2) 0.007(11) -0.034(15) -0.059(14) F3B 0.150(16) 0.171(18) 0.104(12) 0.033(10) -0.069(10) -0.109(15) F4B 0.100(17) 0.088(11) 0.23(3) 0.009(15) -0.12(2) -0.050(11) F5B 0.118(14) 0.123(17) 0.113(15) -0.034(10) -0.004(10) -0.073(12) F6B 0.069(12) 0.093(12) 0.29(2) -0.039(11) -0.115(13) -0.021(10) F7 0.128(3) 0.157(3) 0.080(2) -0.060(2) 0.038(2) -0.035(3) F8 0.223(5) 0.229(5) 0.083(3) -0.076(3) 0.043(3) -0.128(5) F9A 0.077(5) 0.326(18) 0.178(11) -0.176(14) 0.036(6) -0.030(10) F10A 0.243(17) 0.069(4) 0.142(7) -0.045(4) 0.052(12) 0.004(10) F11A 0.106(5) 0.188(7) 0.172(6) -0.101(6) 0.028(4) -0.077(5) F12A 0.170(7) 0.088(4) 0.138(5) -0.030(3) 0.019(5) -0.049(4) F9B 0.22(4) 0.158(19) 0.130(15) -0.105(15) 0.12(2) -0.17(3) F10B 0.20(3) 0.085(15) 0.169(16) -0.036(12) -0.064(17) 0.026(15) F11B 0.11(3) 0.09(2) 0.15(2) -0.05(2) 0.06(2) -0.06(2) F12B 0.14(2) 0.091(15) 0.100(15) 0.006(13) -0.039(15) 0.024(16) N1 0.030(2) 0.0382(18) 0.0396(18) -0.0171(15) -0.0007(16) -0.0063(17) N2 0.060(3) 0.063(2) 0.0397(19) 0.0021(17) -0.0066(19) -0.025(2) N3 0.052(3) 0.046(2) 0.062(2) -0.0043(18) -0.018(2) -0.006(2) N4 0.033(2) 0.0390(18) 0.0348(17) -0.0116(15) -0.0017(15) -0.0051(16) N5 0.035(2) 0.0295(16) 0.0341(16) -0.0086(13) -0.0005(14) -0.0067(15) N6 0.035(2) 0.0315(17) 0.0354(17) -0.0101(14) -0.0016(14) -0.0096(16) N7 0.034(2) 0.0373(17) 0.0326(16) -0.0121(14) -0.0020(14) -0.0125(16) N8 0.035(2) 0.0378(18) 0.0297(16) -0.0093(14) -0.0035(15) -0.0090(17) O1 0.187(5) 0.095(3) 0.131(4) -0.075(3) -0.048(4) 0.029(3) O2 0.126(4) 0.102(3) 0.071(2) -0.049(2) 0.019(2) -0.041(3) O3 0.296(9) 0.135(5) 0.111(4) -0.038(4) -0.033(5) -0.040(5) O4 0.079(6) 0.092(6) 0.093(6) -0.045(4) 0.021(4) -0.014(5) P2 0.1096(15) 0.0776(11) 0.0663(9) -0.0282(8) 0.0254(10) -0.0394(11) Ru1 0.03207(19) 0.03229(16) 0.03220(16) -0.01107(12) -0.00050(13) -0.00890(14) _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 1.364(5) . ? C1 N1 1.376(5) . ? C1 H1 0.9300 . ? C2 C15 1.412(6) . ? C2 H2 0.9300 . ? C3 C4 1.364(6) . ? C3 C15 1.410(5) . ? C3 H3 0.9300 . ? C4 N2 1.354(6) . ? C4 H4 0.9300 . ? C5 N3 1.353(6) . ? C5 C6 1.360(6) . ? C5 H5 0.9300 . ? C6 C16 1.413(6) . ? C6 H6 0.9300 . ? C7 C8 1.356(6) . ? C7 C16 1.419(5) . ? C7 H7 0.9300 . ? C8 N4 1.370(5) . ? C8 H8 0.9300 . ? C9 N1 1.338(5) . ? C9 C10 1.418(5) . ? C9 C14 1.433(5) . ? C10 C15 1.404(5) . ? C10 C11 1.414(5) . ? C11 N2 1.331(5) . ? C11 C12 1.486(6) . ? C12 N3 1.319(5) . ? C12 C13 1.432(5) . ? C13 C14 1.400(5) . ? C13 C16 1.401(5) . ? C14 N4 1.342(4) . ? C17 N5 1.346(4) . ? C17 C18 1.373(5) . ? C17 H17 0.9300 . ? C18 C19 1.385(5) . ? C18 H18 0.9300 . ? C19 C20 1.403(5) . ? C19 C27 1.526(5) . ? C20 C21 1.378(5) . ? C20 H20 0.9300 . ? C21 N5 1.366(4) . ? C21 C22 1.483(4) . ? C22 N6 1.364(4) . ? C22 C23 1.379(4) . ? C23 C24 1.392(5) . ? C23 H23 0.9300 . ? C24 C25 1.387(5) . ? C24 C31 1.537(5) . ? C25 C26 1.377(5) . ? C25 H25 0.9300 . ? C26 N6 1.343(4) . ? C26 H26 0.9300 . ? C27 C29 1.530(6) . ? C27 C30 1.531(6) . ? C27 C28 1.532(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.520(6) . ? C31 C34 1.530(6) . ? C31 C32 1.530(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N7 1.340(5) . ? C35 C36 1.375(5) . ? C35 H35 0.9300 . ? C36 C37 1.387(5) . ? C36 H36 0.9300 . ? C37 C38 1.393(5) . ? C37 C45 1.528(6) . ? C38 C39 1.385(5) . ? C38 H38 0.9300 . ? C39 N7 1.362(4) . ? C39 C40 1.475(5) . ? C40 N8 1.369(5) . ? C40 C41 1.381(5) . ? C41 C42 1.392(5) . ? C41 H41 0.9300 . ? C42 C43 1.391(6) . ? C42 C49 1.527(5) . ? C43 C44 1.385(5) . ? C43 H43 0.9300 . ? C44 N8 1.336(5) . ? C44 H44 0.9300 . ? C45 C48 1.529(6) . ? C45 C46 1.537(6) . ? C45 C47 1.541(6) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.473(6) . ? C49 C52 1.509(7) . ? C49 C51 1.528(7) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O1 1.188(6) . ? C53 C54 1.442(8) . ? C53 C55 1.454(8) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 O2 1.218(5) . ? C56 C57 1.460(7) . ? C56 C58 1.473(7) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58C 0.9600 . ? C58 H58B 0.9600 . ? C58 H58A 0.9600 . ? C59 O3 1.317(9) . ? C59 C61 1.404(12) . ? C59 C60 1.470(10) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? P1A F4A 1.450(8) . ? P1A F3A 1.564(6) . ? P1A F6A 1.571(6) . ? P1A F1A 1.578(5) . ? P1A F5A 1.588(9) . ? P1A F2A 1.597(11) . ? P1B F4B 1.344(18) . ? P1B F6B 1.573(19) . ? P1B F5B 1.58(2) . ? P1B F1B 1.585(16) . ? P1B F3B 1.588(18) . ? P1B F2B 1.59(3) . ? F1B F4B 1.75(2) . ? F3B F4B 1.24(3) . ? F7 P2 1.575(3) . ? F8 P2 1.565(4) . ? F8 F12B 1.74(2) . ? F9A P2 1.537(11) . ? F10A P2 1.510(9) . ? F11A P2 1.601(6) . ? F12A P2 1.603(6) . ? F9B P2 1.528(16) . ? F10B P2 1.65(3) . ? F11B P2 1.50(2) . ? F12B P2 1.52(2) . ? N1 Ru1 2.065(3) . ? N4 Ru1 2.053(3) . ? N5 Ru1 2.054(3) . ? N6 Ru1 2.057(3) . ? N7 Ru1 2.061(3) . ? N8 Ru1 2.065(3) . ? O4 H400 0.65(13) . ? O4 H401 0.7499 . ? 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 122.4(4) . . ? C2 C1 H1 118.8 . . ? N1 C1 H1 118.8 . . ? C1 C2 C15 121.2(4) . . ? C1 C2 H2 119.4 . . ? C15 C2 H2 119.4 . . ? C4 C3 C15 118.7(4) . . ? C4 C3 H3 120.6 . . ? C15 C3 H3 120.6 . . ? N2 C4 C3 125.4(4) . . ? N2 C4 H4 117.3 . . ? C3 C4 H4 117.3 . . ? N3 C5 C6 125.1(4) . . ? N3 C5 H5 117.5 . . ? C6 C5 H5 117.5 . . ? C5 C6 C16 118.4(4) . . ? C5 C6 H6 120.8 . . ? C16 C6 H6 120.8 . . ? C8 C7 C16 120.1(4) . . ? C8 C7 H7 119.9 . . ? C16 C7 H7 119.9 . . ? C7 C8 N4 123.5(4) . . ? C7 C8 H8 118.3 . . ? N4 C8 H8 118.3 . . ? N1 C9 C10 123.6(3) . . ? N1 C9 C14 116.7(3) . . ? C10 C9 C14 119.6(4) . . ? C15 C10 C11 120.0(3) . . ? C15 C10 C9 118.6(4) . . ? C11 C10 C9 121.4(3) . . ? N2 C11 C10 122.4(4) . . ? N2 C11 C12 118.7(4) . . ? C10 C11 C12 118.9(3) . . ? N3 C12 C13 121.7(4) . . ? N3 C12 C11 120.3(4) . . ? C13 C12 C11 118.0(4) . . ? C14 C13 C16 119.1(3) . . ? C14 C13 C12 121.5(3) . . ? C16 C13 C12 119.3(4) . . ? N4 C14 C13 123.6(3) . . ? N4 C14 C9 116.1(3) . . ? C13 C14 C9 120.4(3) . . ? C10 C15 C3 116.7(4) . . ? C10 C15 C2 116.9(3) . . ? C3 C15 C2 126.4(4) . . ? C13 C16 C6 117.5(4) . . ? C13 C16 C7 116.9(4) . . ? C6 C16 C7 125.6(4) . . ? N5 C17 C18 122.3(3) . . ? N5 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 116.2(3) . . ? C18 C19 C27 122.8(3) . . ? C20 C19 C27 121.0(3) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? N5 C21 C20 121.2(3) . . ? N5 C21 C22 114.4(3) . . ? C20 C21 C22 124.4(3) . . ? N6 C22 C23 121.4(3) . . ? N6 C22 C21 113.8(3) . . ? C23 C22 C21 124.8(3) . . ? C22 C23 C24 121.2(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 116.3(3) . . ? C25 C24 C31 122.4(3) . . ? C23 C24 C31 121.3(3) . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? N6 C26 C25 122.8(3) . . ? N6 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C19 C27 C29 109.4(3) . . ? C19 C27 C30 109.3(3) . . ? C29 C27 C30 109.4(4) . . ? C19 C27 C28 111.5(3) . . ? C29 C27 C28 108.4(3) . . ? C30 C27 C28 108.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C34 111.3(4) . . ? C33 C31 C32 108.8(4) . . ? C34 C31 C32 107.8(4) . . ? C33 C31 C24 109.6(3) . . ? C34 C31 C24 108.3(3) . . ? C32 C31 C24 111.0(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N7 C35 C36 122.5(3) . . ? N7 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C37 121.5(4) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 115.4(4) . . ? C36 C37 C45 123.7(4) . . ? C38 C37 C45 120.8(4) . . ? C39 C38 C37 121.4(3) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? N7 C39 C38 121.4(3) . . ? N7 C39 C40 114.4(3) . . ? C38 C39 C40 124.2(3) . . ? N8 C40 C41 121.5(3) . . ? N8 C40 C39 114.3(3) . . ? C41 C40 C39 124.2(4) . . ? C40 C41 C42 121.0(4) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C43 C42 C41 116.4(3) . . ? C43 C42 C49 122.7(4) . . ? C41 C42 C49 120.9(4) . . ? C44 C43 C42 120.5(4) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? N8 C44 C43 122.7(4) . . ? N8 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C37 C45 C48 109.4(4) . . ? C37 C45 C46 111.8(4) . . ? C48 C45 C46 108.3(4) . . ? C37 C45 C47 108.9(3) . . ? C48 C45 C47 110.4(4) . . ? C46 C45 C47 108.0(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C52 110.0(5) . . ? C50 C49 C42 110.0(4) . . ? C52 C49 C42 111.1(4) . . ? C50 C49 C51 110.7(6) . . ? C52 C49 C51 106.0(5) . . ? C42 C49 C51 108.9(4) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O1 C53 C54 122.8(6) . . ? O1 C53 C55 119.1(6) . . ? C54 C53 C55 118.0(6) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O2 C56 C57 120.8(5) . . ? O2 C56 C58 121.1(5) . . ? C57 C56 C58 118.1(5) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58C 109.5 . . ? C56 C58 H58B 109.5 . . ? H58C C58 H58B 109.5 . . ? C56 C58 H58A 109.5 . . ? H58C C58 H58A 109.5 . . ? H58B C58 H58A 109.5 . . ? O3 C59 C61 126.6(10) . . ? O3 C59 C60 115.9(9) . . ? C61 C59 C60 117.4(8) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? F4A P1A F3A 75.7(4) . . ? F4A P1A F6A 163.7(5) . . ? F3A P1A F6A 88.6(3) . . ? F4A P1A F1A 96.4(4) . . ? F3A P1A F1A 91.2(4) . . ? F6A P1A F1A 88.2(4) . . ? F4A P1A F5A 107.8(6) . . ? F3A P1A F5A 176.1(6) . . ? F6A P1A F5A 87.8(5) . . ? F1A P1A F5A 90.1(5) . . ? F4A P1A F2A 83.9(5) . . ? F3A P1A F2A 89.8(4) . . ? F6A P1A F2A 91.7(5) . . ? F1A P1A F2A 179.0(5) . . ? F5A P1A F2A 88.9(5) . . ? F4B P1B F6B 134.0(18) . . ? F4B P1B F5B 131.8(17) . . ? F6B P1B F5B 90.5(12) . . ? F4B P1B F1B 72.9(9) . . ? F6B P1B F1B 91.8(11) . . ? F5B P1B F1B 91.5(10) . . ? F4B P1B F3B 49.1(12) . . ? F6B P1B F3B 175.2(13) . . ? F5B P1B F3B 88.0(12) . . ? F1B P1B F3B 92.8(11) . . ? F4B P1B F2B 108.1(13) . . ? F6B P1B F2B 88.4(13) . . ? F5B P1B F2B 86.9(13) . . ? F1B P1B F2B 178.4(14) . . ? F3B P1B F2B 87.0(12) . . ? P1B F1B F4B 47.2(7) . . ? F4B F3B P1B 55.1(10) . . ? F3B F4B P1B 75.8(19) . . ? F3B F4B F1B 99(2) . . ? P1B F4B F1B 59.9(8) . . ? P2 F8 F12B 54.4(7) . . ? P2 F12B F8 57.1(8) . . ? C9 N1 C1 117.3(3) . . ? C9 N1 Ru1 113.7(2) . . ? C1 N1 Ru1 129.0(3) . . ? C11 N2 C4 116.8(4) . . ? C12 N3 C5 118.0(4) . . ? C14 N4 C8 116.8(3) . . ? C14 N4 Ru1 114.3(2) . . ? C8 N4 Ru1 128.8(3) . . ? C17 N5 C21 118.2(3) . . ? C17 N5 Ru1 125.3(2) . . ? C21 N5 Ru1 116.5(2) . . ? C26 N6 C22 117.7(3) . . ? C26 N6 Ru1 125.5(2) . . ? C22 N6 Ru1 116.9(2) . . ? C35 N7 C39 117.6(3) . . ? C35 N7 Ru1 125.8(3) . . ? C39 N7 Ru1 116.6(2) . . ? C44 N8 C40 117.8(3) . . ? C44 N8 Ru1 125.9(3) . . ? C40 N8 Ru1 116.0(2) . . ? H400 O4 H401 82.7 . . ? F11B P2 F10A 38.6(12) . . ? F11B P2 F12B 95.4(18) . . ? F10A P2 F12B 128.4(14) . . ? F11B P2 F9B 162.2(17) . . ? F10A P2 F9B 123.7(13) . . ? F12B P2 F9B 98.6(17) . . ? F11B P2 F9A 134.5(15) . . ? F10A P2 F9A 96.0(8) . . ? F12B P2 F9A 125.8(13) . . ? F9B P2 F9A 28.5(13) . . ? F11B P2 F8 90.3(13) . . ? F10A P2 F8 85.9(5) . . ? F12B P2 F8 68.5(9) . . ? F9B P2 F8 84.8(9) . . ? F9A P2 F8 88.5(5) . . ? F11B P2 F7 91.5(13) . . ? F10A P2 F7 95.3(5) . . ? F12B P2 F7 111.5(9) . . ? F9B P2 F7 93.4(9) . . ? F9A P2 F7 90.0(5) . . ? F8 P2 F7 178.2(2) . . ? F11B P2 F11A 47.9(13) . . ? F10A P2 F11A 86.5(6) . . ? F12B P2 F11A 53.7(11) . . ? F9B P2 F11A 149.5(13) . . ? F9A P2 F11A 176.2(5) . . ? F8 P2 F11A 94.6(3) . . ? F7 P2 F11A 86.8(3) . . ? F11B P2 F12A 135.1(15) . . ? F10A P2 F12A 173.8(7) . . ? F12B P2 F12A 46.9(12) . . ? F9B P2 F12A 62.5(11) . . ? F9A P2 F12A 90.2(6) . . ? F8 P2 F12A 94.9(3) . . ? F7 P2 F12A 84.0(3) . . ? F11A P2 F12A 87.3(4) . . ? F11B P2 F10B 80.2(15) . . ? F10A P2 F10B 43.0(8) . . ? F12B P2 F10B 164.4(13) . . ? F9B P2 F10B 83.3(14) . . ? F9A P2 F10B 54.8(10) . . ? F8 P2 F10B 96.4(9) . . ? F7 P2 F10B 83.7(9) . . ? F11A P2 F10B 126.9(11) . . ? F12A P2 F10B 142.7(10) . . ? N4 Ru1 N5 88.97(12) . . ? N4 Ru1 N6 95.14(12) . . ? N5 Ru1 N6 78.37(11) . . ? N4 Ru1 N7 174.07(12) . . ? N5 Ru1 N7 94.88(12) . . ? N6 Ru1 N7 90.06(12) . . ? N4 Ru1 N8 98.27(12) . . ? N5 Ru1 N8 171.52(12) . . ? N6 Ru1 N8 96.49(11) . . ? N7 Ru1 N8 78.27(12) . . ? N4 Ru1 N1 79.19(13) . . ? N5 Ru1 N1 97.93(11) . . ? N6 Ru1 N1 173.36(13) . . ? N7 Ru1 N1 95.79(12) . . ? N8 Ru1 N1 87.81(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C15 1.9(6) . . . . ? C15 C3 C4 N2 0.4(7) . . . . ? N3 C5 C6 C16 0.5(7) . . . . ? C16 C7 C8 N4 -0.3(6) . . . . ? N1 C9 C10 C15 1.4(5) . . . . ? C14 C9 C10 C15 -177.8(3) . . . . ? N1 C9 C10 C11 -179.6(3) . . . . ? C14 C9 C10 C11 1.1(5) . . . . ? C15 C10 C11 N2 0.0(6) . . . . ? C9 C10 C11 N2 -179.0(3) . . . . ? C15 C10 C11 C12 178.9(3) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? N2 C11 C12 N3 -0.2(5) . . . . ? C10 C11 C12 N3 -179.2(3) . . . . ? N2 C11 C12 C13 178.7(3) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? N3 C12 C13 C14 178.3(3) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? N3 C12 C13 C16 0.2(6) . . . . ? C11 C12 C13 C16 -178.6(3) . . . . ? C16 C13 C14 N4 -0.4(5) . . . . ? C12 C13 C14 N4 -178.5(3) . . . . ? C16 C13 C14 C9 179.8(3) . . . . ? C12 C13 C14 C9 1.7(5) . . . . ? N1 C9 C14 N4 -1.1(5) . . . . ? C10 C9 C14 N4 178.2(3) . . . . ? N1 C9 C14 C13 178.7(3) . . . . ? C10 C9 C14 C13 -2.0(5) . . . . ? C11 C10 C15 C3 0.1(5) . . . . ? C9 C10 C15 C3 179.0(3) . . . . ? C11 C10 C15 C2 180.0(3) . . . . ? C9 C10 C15 C2 -1.0(5) . . . . ? C4 C3 C15 C10 -0.2(5) . . . . ? C4 C3 C15 C2 179.8(4) . . . . ? C1 C2 C15 C10 -0.6(5) . . . . ? C1 C2 C15 C3 179.4(4) . . . . ? C14 C13 C16 C6 -178.6(3) . . . . ? C12 C13 C16 C6 -0.4(5) . . . . ? C14 C13 C16 C7 0.5(5) . . . . ? C12 C13 C16 C7 178.7(3) . . . . ? C5 C6 C16 C13 0.1(6) . . . . ? C5 C6 C16 C7 -178.9(4) . . . . ? C8 C7 C16 C13 -0.2(6) . . . . ? C8 C7 C16 C6 178.8(4) . . . . ? N5 C17 C18 C19 1.0(6) . . . . ? C17 C18 C19 C20 -1.4(6) . . . . ? C17 C18 C19 C27 -179.9(4) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C27 C19 C20 C21 179.7(4) . . . . ? C19 C20 C21 N5 -0.4(6) . . . . ? C19 C20 C21 C22 -179.5(4) . . . . ? N5 C21 C22 N6 0.9(5) . . . . ? C20 C21 C22 N6 -179.9(3) . . . . ? N5 C21 C22 C23 -177.1(3) . . . . ? C20 C21 C22 C23 2.0(6) . . . . ? N6 C22 C23 C24 -0.3(6) . . . . ? C21 C22 C23 C24 177.7(4) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C22 C23 C24 C31 179.5(4) . . . . ? C23 C24 C25 C26 -0.3(6) . . . . ? C31 C24 C25 C26 -179.4(4) . . . . ? C24 C25 C26 N6 0.0(6) . . . . ? C18 C19 C27 C29 116.0(4) . . . . ? C20 C19 C27 C29 -62.4(5) . . . . ? C18 C19 C27 C30 -124.2(4) . . . . ? C20 C19 C27 C30 57.4(5) . . . . ? C18 C19 C27 C28 -3.9(6) . . . . ? C20 C19 C27 C28 177.7(4) . . . . ? C25 C24 C31 C33 -134.3(4) . . . . ? C23 C24 C31 C33 46.7(5) . . . . ? C25 C24 C31 C34 104.2(5) . . . . ? C23 C24 C31 C34 -74.9(5) . . . . ? C25 C24 C31 C32 -14.0(6) . . . . ? C23 C24 C31 C32 166.9(4) . . . . ? N7 C35 C36 C37 -1.2(6) . . . . ? C35 C36 C37 C38 2.3(5) . . . . ? C35 C36 C37 C45 -177.0(4) . . . . ? C36 C37 C38 C39 -1.4(5) . . . . ? C45 C37 C38 C39 178.0(3) . . . . ? C37 C38 C39 N7 -0.8(5) . . . . ? C37 C38 C39 C40 179.8(3) . . . . ? N7 C39 C40 N8 -6.8(4) . . . . ? C38 C39 C40 N8 172.6(3) . . . . ? N7 C39 C40 C41 171.0(3) . . . . ? C38 C39 C40 C41 -9.6(5) . . . . ? N8 C40 C41 C42 -0.2(5) . . . . ? C39 C40 C41 C42 -177.9(3) . . . . ? C40 C41 C42 C43 -4.1(5) . . . . ? C40 C41 C42 C49 175.6(3) . . . . ? C41 C42 C43 C44 5.1(5) . . . . ? C49 C42 C43 C44 -174.6(3) . . . . ? C42 C43 C44 N8 -1.8(6) . . . . ? C36 C37 C45 C48 -119.5(4) . . . . ? C38 C37 C45 C48 61.2(5) . . . . ? C36 C37 C45 C46 0.5(5) . . . . ? C38 C37 C45 C46 -178.8(4) . . . . ? C36 C37 C45 C47 119.8(4) . . . . ? C38 C37 C45 C47 -59.5(5) . . . . ? C43 C42 C49 C50 -101.1(6) . . . . ? C41 C42 C49 C50 79.2(6) . . . . ? C43 C42 C49 C52 21.0(6) . . . . ? C41 C42 C49 C52 -158.7(4) . . . . ? C43 C42 C49 C51 137.5(5) . . . . ? C41 C42 C49 C51 -42.3(6) . . . . ? F6B P1B F1B F4B -135.8(18) . . . . ? F5B P1B F1B F4B 133.6(17) . . . . ? F3B P1B F1B F4B 45.5(14) . . . . ? F2B P1B F1B F4B 128(49) . . . . ? F6B P1B F3B F4B 131(15) . . . . ? F5B P1B F3B F4B -155.9(17) . . . . ? F1B P1B F3B F4B -64.4(16) . . . . ? F2B P1B F3B F4B 117.2(17) . . . . ? P1B F3B F4B F1B 55.7(8) . . . . ? F6B P1B F4B F3B -175.0(15) . . . . ? F5B P1B F4B F3B 33(2) . . . . ? F1B P1B F4B F3B 109.5(18) . . . . ? F2B P1B F4B F3B -69.1(18) . . . . ? F6B P1B F4B F1B 75.5(18) . . . . ? F5B P1B F4B F1B -76.3(15) . . . . ? F3B P1B F4B F1B -109.5(18) . . . . ? F2B P1B F4B F1B -178.7(14) . . . . ? P1B F1B F4B F3B -67.7(16) . . . . ? C10 C9 N1 C1 -0.2(5) . . . . ? C14 C9 N1 C1 179.1(3) . . . . ? C10 C9 N1 Ru1 -178.1(3) . . . . ? C14 C9 N1 Ru1 1.2(4) . . . . ? C2 C1 N1 C9 -1.5(5) . . . . ? C2 C1 N1 Ru1 176.1(3) . . . . ? C10 C11 N2 C4 0.1(6) . . . . ? C12 C11 N2 C4 -178.8(4) . . . . ? C3 C4 N2 C11 -0.3(6) . . . . ? C13 C12 N3 C5 0.3(6) . . . . ? C11 C12 N3 C5 179.1(4) . . . . ? C6 C5 N3 C12 -0.7(7) . . . . ? C13 C14 N4 C8 -0.1(5) . . . . ? C9 C14 N4 C8 179.7(3) . . . . ? C13 C14 N4 Ru1 -179.3(3) . . . . ? C9 C14 N4 Ru1 0.5(4) . . . . ? C7 C8 N4 C14 0.5(5) . . . . ? C7 C8 N4 Ru1 179.5(3) . . . . ? C18 C17 N5 C21 -0.1(6) . . . . ? C18 C17 N5 Ru1 -178.6(3) . . . . ? C20 C21 N5 C17 -0.2(5) . . . . ? C22 C21 N5 C17 179.0(3) . . . . ? C20 C21 N5 Ru1 178.5(3) . . . . ? C22 C21 N5 Ru1 -2.3(4) . . . . ? C25 C26 N6 C22 0.2(6) . . . . ? C25 C26 N6 Ru1 -178.8(3) . . . . ? C23 C22 N6 C26 0.0(5) . . . . ? C21 C22 N6 C26 -178.2(3) . . . . ? C23 C22 N6 Ru1 179.0(3) . . . . ? C21 C22 N6 Ru1 0.8(4) . . . . ? C36 C35 N7 C39 -1.1(5) . . . . ? C36 C35 N7 Ru1 177.9(3) . . . . ? C38 C39 N7 C35 2.0(5) . . . . ? C40 C39 N7 C35 -178.5(3) . . . . ? C38 C39 N7 Ru1 -177.0(3) . . . . ? C40 C39 N7 Ru1 2.4(4) . . . . ? C43 C44 N8 C40 -2.7(5) . . . . ? C43 C44 N8 Ru1 170.1(3) . . . . ? C41 C40 N8 C44 3.7(5) . . . . ? C39 C40 N8 C44 -178.4(3) . . . . ? C41 C40 N8 Ru1 -169.8(2) . . . . ? C39 C40 N8 Ru1 8.1(3) . . . . ? F8 F12B P2 F11B 88.2(12) . . . . ? F8 F12B P2 F10A 65.9(12) . . . . ? F8 F12B P2 F9B -80.9(10) . . . . ? F8 F12B P2 F9A -71.5(12) . . . . ? F8 F12B P2 F7 -178.1(2) . . . . ? F8 F12B P2 F11A 113.3(12) . . . . ? F8 F12B P2 F12A -119.5(13) . . . . ? F8 F12B P2 F10B 15(6) . . . . ? F12B F8 P2 F11B -95.7(18) . . . . ? F12B F8 P2 F10A -134.1(15) . . . . ? F12B F8 P2 F9B 101.4(17) . . . . ? F12B F8 P2 F9A 129.8(14) . . . . ? F12B F8 P2 F7 92(10) . . . . ? F12B F8 P2 F11A -48.0(13) . . . . ? F12B F8 P2 F12A 39.7(13) . . . . ? F12B F8 P2 F10B -175.9(16) . . . . ? C14 N4 Ru1 N5 98.3(2) . . . . ? C8 N4 Ru1 N5 -80.7(3) . . . . ? C14 N4 Ru1 N6 176.6(2) . . . . ? C8 N4 Ru1 N6 -2.5(3) . . . . ? C14 N4 Ru1 N7 -32.3(13) . . . . ? C8 N4 Ru1 N7 148.7(11) . . . . ? C14 N4 Ru1 N8 -86.1(2) . . . . ? C8 N4 Ru1 N8 94.8(3) . . . . ? C14 N4 Ru1 N1 0.1(2) . . . . ? C8 N4 Ru1 N1 -179.0(3) . . . . ? C17 N5 Ru1 N4 -83.9(3) . . . . ? C21 N5 Ru1 N4 97.6(3) . . . . ? C17 N5 Ru1 N6 -179.3(3) . . . . ? C21 N5 Ru1 N6 2.1(3) . . . . ? C17 N5 Ru1 N7 91.6(3) . . . . ? C21 N5 Ru1 N7 -86.9(3) . . . . ? C17 N5 Ru1 N8 127.4(8) . . . . ? C21 N5 Ru1 N8 -51.2(10) . . . . ? C17 N5 Ru1 N1 -4.9(3) . . . . ? C21 N5 Ru1 N1 176.5(3) . . . . ? C26 N6 Ru1 N4 89.5(3) . . . . ? C22 N6 Ru1 N4 -89.5(3) . . . . ? C26 N6 Ru1 N5 177.4(3) . . . . ? C22 N6 Ru1 N5 -1.6(3) . . . . ? C26 N6 Ru1 N7 -87.7(3) . . . . ? C22 N6 Ru1 N7 93.4(3) . . . . ? C26 N6 Ru1 N8 -9.5(3) . . . . ? C22 N6 Ru1 N8 171.6(3) . . . . ? C26 N6 Ru1 N1 120.6(11) . . . . ? C22 N6 Ru1 N1 -58.3(12) . . . . ? C35 N7 Ru1 N4 127.7(11) . . . . ? C39 N7 Ru1 N4 -53.3(13) . . . . ? C35 N7 Ru1 N5 -2.6(3) . . . . ? C39 N7 Ru1 N5 176.4(2) . . . . ? C35 N7 Ru1 N6 -81.0(3) . . . . ? C39 N7 Ru1 N6 98.0(2) . . . . ? C35 N7 Ru1 N8 -177.6(3) . . . . ? C39 N7 Ru1 N8 1.4(2) . . . . ? C35 N7 Ru1 N1 95.9(3) . . . . ? C39 N7 Ru1 N1 -85.1(2) . . . . ? C44 N8 Ru1 N4 -3.1(3) . . . . ? C40 N8 Ru1 N4 169.8(2) . . . . ? C44 N8 Ru1 N5 145.3(8) . . . . ? C40 N8 Ru1 N5 -41.8(10) . . . . ? C44 N8 Ru1 N6 93.1(3) . . . . ? C40 N8 Ru1 N6 -94.0(2) . . . . ? C44 N8 Ru1 N7 -178.2(3) . . . . ? C40 N8 Ru1 N7 -5.3(2) . . . . ? C44 N8 Ru1 N1 -81.8(3) . . . . ? C40 N8 Ru1 N1 91.1(2) . . . . ? C9 N1 Ru1 N4 -0.7(2) . . . . ? C1 N1 Ru1 N4 -178.3(3) . . . . ? C9 N1 Ru1 N5 -88.1(2) . . . . ? C1 N1 Ru1 N5 94.2(3) . . . . ? C9 N1 Ru1 N6 -32.3(12) . . . . ? C1 N1 Ru1 N6 150.0(10) . . . . ? C9 N1 Ru1 N7 176.2(2) . . . . ? C1 N1 Ru1 N7 -1.5(3) . . . . ? C9 N1 Ru1 N8 98.2(2) . . . . ? C1 N1 Ru1 N8 -79.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.622 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.054 #====================================================================== # end of cif file