Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sven Rau' _publ_contact_author_address ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; _publ_contact_author_phone +49-3641-948113 _publ_contact_author_fax +49-3641-948102 _publ_contact_author_email Sven.Rau@uni-jena.de # 2. TITLE AND AUTHOR LIST _publ_section_title ; Derivatives of dipyrido[3,2-a:2,3-c]phenazine and its ruthenium complexes, influence of arylic substitution on photophysical properties ; loop_ _publ_author_name _publ_author_address S.Rau ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; W.Henry ; National Centre for Sensor Research Dublin City University School of Chemical Sciences Glas Nevin Dublin 9 Ireland ; J.G.Voss ; National Centre for Sensor Research Dublin City University School of Chemical Sciences Glas Nevin Dublin 9 Ireland ; B.Schafer ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; H.Gorls ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; J.Popp ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Physikalische Chemie Helmholtzweg 4 D-07743 Jena Germany ; M.Presselt ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Physikalische Chemie Helmholtzweg 4 07743 Jena Germany ; ; M.Schmitt ; ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Physikalische Chemie Helmholtzweg 4 07743 Jena Germany ; data_FO2409_1 _database_code_depnum_ccdc_archive 'CCDC 290998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H26 N4 * C7 H7' _chemical_formula_weight 677.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.3762(6) _cell_length_b 12.7563(7) _cell_length_c 13.6865(5) _cell_angle_alpha 97.221(3) _cell_angle_beta 102.933(3) _cell_angle_gamma 110.078(2) _cell_volume 1773.1(1) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 710 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12620 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8025 _reflns_number_gt 4464 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _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^)+(0.1459P)^2^+1.0671P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8025 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2938 _refine_ls_wR_factor_gt 0.2433 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.1669(3) 0.4157(3) 0.1611(2) 0.0665(9) Uani 1 1 d . . . N2 N 0.4160(3) 0.5700(3) 0.1993(2) 0.0625(8) Uani 1 1 d . . . N3 N 0.3159(2) 0.2182(2) 0.40831(18) 0.0445(6) Uani 1 1 d . . . N4 N 0.5705(2) 0.3903(2) 0.46051(18) 0.0439(6) Uani 1 1 d . . . C1 C 0.2631(3) 0.4036(3) 0.2321(2) 0.0527(8) Uani 1 1 d . . . C2 C 0.0471(5) 0.3376(4) 0.1407(3) 0.0792(12) Uani 1 1 d . . . H2A H -0.0205 0.3459 0.0912 0.095 Uiso 1 1 calc R . . C3 C 0.0132(4) 0.2441(4) 0.1867(3) 0.0764(12) Uani 1 1 d . . . H3A H -0.0743 0.1900 0.1683 0.092 Uiso 1 1 calc R . . C4 C 0.1100(4) 0.2329(3) 0.2591(3) 0.0634(10) Uani 1 1 d . . . H4A H 0.0904 0.1707 0.2925 0.076 Uiso 1 1 calc R . . C5 C 0.2376(3) 0.3132(3) 0.2837(2) 0.0503(8) Uani 1 1 d . . . C6 C 0.3435(3) 0.3057(3) 0.3623(2) 0.0433(7) Uani 1 1 d . . . C7 C 0.4719(3) 0.3915(3) 0.3882(2) 0.0427(7) Uani 1 1 d . . . C8 C 0.4969(3) 0.4842(3) 0.3324(2) 0.0467(7) Uani 1 1 d . . . C9 C 0.6212(4) 0.5687(3) 0.3552(3) 0.0567(8) Uani 1 1 d . . . H9A H 0.6911 0.5685 0.4081 0.068 Uiso 1 1 calc R . . C10 C 0.6412(4) 0.6527(3) 0.2998(3) 0.0663(10) Uani 1 1 d . . . H10A H 0.7246 0.7124 0.3139 0.080 Uiso 1 1 calc R . . C11 C 0.5348(4) 0.6474(4) 0.2219(3) 0.0687(11) Uani 1 1 d . . . H11A H 0.5497 0.7043 0.1824 0.082 Uiso 1 1 calc R . . C12 C 0.3959(4) 0.4885(3) 0.2551(2) 0.0517(8) Uani 1 1 d . . . C13 C 0.4163(3) 0.2159(3) 0.4821(2) 0.0419(7) Uani 1 1 d . . . C14 C 0.5428(3) 0.3022(2) 0.5096(2) 0.0402(6) Uani 1 1 d . . . C15 C 0.6437(3) 0.2949(2) 0.5870(2) 0.0420(7) Uani 1 1 d . . . H15A H 0.7295 0.3518 0.6041 0.050 Uiso 1 1 calc R . . C16 C 0.6198(3) 0.2069(2) 0.6381(2) 0.0414(7) Uani 1 1 d . . . C17 C 0.4898(3) 0.1214(2) 0.6129(2) 0.0413(7) Uani 1 1 d . . . C18 C 0.3924(3) 0.1261(3) 0.5361(2) 0.0433(7) Uani 1 1 d . . . H18A H 0.3072 0.0683 0.5186 0.052 Uiso 1 1 calc R . . C19 C 0.4540(3) 0.0305(2) 0.6716(2) 0.0419(7) Uani 1 1 d . . . C20 C 0.4863(3) 0.0578(3) 0.7783(2) 0.0482(7) Uani 1 1 d . . . H20A H 0.5354 0.1350 0.8143 0.058 Uiso 1 1 calc R . . C21 C 0.4480(3) -0.0256(3) 0.8325(2) 0.0482(8) Uani 1 1 d . . . H21A H 0.4703 -0.0045 0.9053 0.058 Uiso 1 1 calc R . . C22 C 0.3771(3) -0.1405(2) 0.7830(2) 0.0400(6) Uani 1 1 d . . . C23 C 0.3450(3) -0.1675(3) 0.6758(2) 0.0449(7) Uani 1 1 d . . . H23A H 0.2969 -0.2448 0.6396 0.054 Uiso 1 1 calc R . . C24 C 0.3825(3) -0.0832(3) 0.6218(2) 0.0448(7) Uani 1 1 d . . . H24A H 0.3586 -0.1036 0.5489 0.054 Uiso 1 1 calc R . . C25 C 0.3420(3) -0.2293(3) 0.8429(2) 0.0432(7) Uani 1 1 d . . . C26 C 0.3167(3) -0.2052(3) 0.9365(2) 0.0529(8) Uani 1 1 d . . . H26A H 0.3179 -0.1316 0.9608 0.063 Uiso 1 1 calc R . . C27 C 0.2898(3) -0.2873(4) 0.9946(2) 0.0656(11) Uani 1 1 d . . . H27A H 0.2726 -0.2693 1.0580 0.079 Uiso 1 1 calc R . . C28 C 0.2878(4) -0.3940(4) 0.9616(3) 0.0711(11) Uani 1 1 d . . . H28A H 0.2709 -0.4496 1.0023 0.085 Uiso 1 1 calc R . . C29 C 0.3105(4) -0.4191(3) 0.8696(3) 0.0731(11) Uani 1 1 d . . . H29A H 0.3081 -0.4932 0.8457 0.088 Uiso 1 1 calc R . . C30 C 0.3371(4) -0.3382(3) 0.8104(3) 0.0599(9) Uani 1 1 d . . . H30A H 0.3522 -0.3579 0.7463 0.072 Uiso 1 1 calc R . . C31 C 0.7339(3) 0.1993(3) 0.7115(2) 0.0421(7) Uani 1 1 d . . . C32 C 0.8302(3) 0.2966(3) 0.7806(2) 0.0456(7) Uani 1 1 d . . . H32A H 0.8190 0.3673 0.7855 0.055 Uiso 1 1 calc R . . C33 C 0.9420(3) 0.2917(3) 0.8421(2) 0.0486(7) Uani 1 1 d . . . H33A H 1.0066 0.3594 0.8880 0.058 Uiso 1 1 calc R . . C34 C 0.9614(3) 0.1888(3) 0.8379(2) 0.0502(8) Uani 1 1 d . . . C35 C 0.8623(3) 0.0911(3) 0.7701(3) 0.0519(8) Uani 1 1 d . . . H35A H 0.8720 0.0198 0.7660 0.062 Uiso 1 1 calc R . . C36 C 0.7512(3) 0.0964(3) 0.7091(2) 0.0488(7) Uani 1 1 d . . . H36A H 0.6852 0.0284 0.6646 0.059 Uiso 1 1 calc R . . C37 C 1.0838(3) 0.1838(3) 0.9010(3) 0.0595(9) Uani 1 1 d . . . C38 C 1.1985(4) 0.2774(4) 0.9372(3) 0.0750(11) Uani 1 1 d . . . H38A H 1.2008 0.3483 0.9211 0.090 Uiso 1 1 calc R . . C39 C 1.3116(4) 0.2723(5) 0.9966(4) 0.0946(16) Uani 1 1 d . . . H39A H 1.3898 0.3391 1.0199 0.114 Uiso 1 1 calc R . . C40 C 1.3117(5) 0.1746(5) 1.0215(5) 0.1082(19) Uani 1 1 d . . . H40A H 1.3903 0.1712 1.0602 0.130 Uiso 1 1 calc R . . C41 C 1.1989(6) 0.0798(5) 0.9911(5) 0.130(3) Uani 1 1 d . . . H41A H 1.1984 0.0108 1.0108 0.156 Uiso 1 1 calc R . . C42 C 1.0840(5) 0.0830(4) 0.9314(4) 0.1046(18) Uani 1 1 d . . . H42A H 1.0055 0.0166 0.9113 0.126 Uiso 1 1 calc R . . C1TA C 0.0551(8) -0.0847(7) 0.5211(7) 0.151(3) Uiso 1 1 d . . . C2TA C 0.0679(7) 0.0134(6) 0.5980(5) 0.122(2) Uiso 1 1 d . . . C3TA C 0.0148(8) 0.0921(7) 0.5745(6) 0.137(2) Uiso 1 1 d . . . C4TA C 0.1411(10) 0.0205(8) 0.6888(7) 0.086(3) Uiso 0.50 1 d P . . C1T C -0.0109(11) 0.5399(10) 0.4586(8) 0.094(3) Uiso 0.50 1 d P . . C2T C 0.0119(6) 0.4398(6) 0.4321(5) 0.1160(19) Uiso 1 1 d . . . C3T C 0.0302(14) 0.3793(12) 0.4928(11) 0.124(4) Uiso 0.50 1 d P . . C4T C 0.0264(8) 0.3942(7) 0.6031(6) 0.149(3) Uiso 1 1 d . . . C5T C 0.0094(12) 0.5005(11) 0.6299(9) 0.108(3) Uiso 0.50 1 d P . . 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 N1 0.077(2) 0.066(2) 0.0630(18) 0.0237(15) 0.0065(16) 0.0399(18) N2 0.078(2) 0.0639(19) 0.0698(19) 0.0382(16) 0.0327(16) 0.0408(17) N3 0.0464(14) 0.0425(14) 0.0447(13) 0.0134(11) 0.0104(11) 0.0173(11) N4 0.0478(14) 0.0393(14) 0.0468(13) 0.0148(11) 0.0149(11) 0.0167(11) C1 0.064(2) 0.055(2) 0.0466(17) 0.0154(15) 0.0104(15) 0.0340(17) C2 0.075(3) 0.079(3) 0.076(3) 0.023(2) -0.008(2) 0.037(2) C3 0.065(2) 0.067(2) 0.081(3) 0.017(2) -0.010(2) 0.025(2) C4 0.062(2) 0.055(2) 0.067(2) 0.0162(17) 0.0004(17) 0.0250(18) C5 0.0548(19) 0.0503(19) 0.0471(16) 0.0117(14) 0.0080(14) 0.0258(16) C6 0.0490(17) 0.0411(16) 0.0422(15) 0.0131(12) 0.0116(13) 0.0200(14) C7 0.0522(17) 0.0412(16) 0.0433(15) 0.0131(13) 0.0178(13) 0.0243(14) C8 0.0579(19) 0.0456(17) 0.0493(17) 0.0181(14) 0.0220(15) 0.0280(15) C9 0.067(2) 0.054(2) 0.064(2) 0.0264(16) 0.0284(17) 0.0294(18) C10 0.072(2) 0.055(2) 0.087(3) 0.035(2) 0.036(2) 0.0281(19) C11 0.093(3) 0.069(3) 0.081(3) 0.047(2) 0.047(2) 0.050(2) C12 0.070(2) 0.0529(19) 0.0500(17) 0.0212(15) 0.0257(16) 0.0364(17) C13 0.0456(16) 0.0425(16) 0.0367(14) 0.0093(12) 0.0088(12) 0.0176(13) C14 0.0427(15) 0.0369(15) 0.0411(14) 0.0101(12) 0.0128(12) 0.0144(12) C15 0.0404(15) 0.0374(15) 0.0428(15) 0.0081(12) 0.0094(12) 0.0102(12) C16 0.0453(16) 0.0386(16) 0.0373(14) 0.0077(12) 0.0094(12) 0.0144(13) C17 0.0469(16) 0.0362(15) 0.0364(14) 0.0090(12) 0.0086(12) 0.0124(13) C18 0.0426(15) 0.0391(16) 0.0427(15) 0.0123(12) 0.0105(13) 0.0089(13) C19 0.0423(15) 0.0392(16) 0.0405(15) 0.0132(12) 0.0091(12) 0.0115(13) C20 0.0513(17) 0.0417(17) 0.0401(15) 0.0086(13) 0.0042(13) 0.0098(14) C21 0.0499(17) 0.0526(19) 0.0345(14) 0.0109(13) 0.0071(13) 0.0131(15) C22 0.0370(14) 0.0443(16) 0.0375(14) 0.0121(12) 0.0072(12) 0.0153(13) C23 0.0493(17) 0.0407(16) 0.0403(15) 0.0087(12) 0.0104(13) 0.0137(13) C24 0.0498(17) 0.0445(17) 0.0358(14) 0.0103(12) 0.0103(12) 0.0137(14) C25 0.0369(14) 0.0502(18) 0.0387(15) 0.0155(13) 0.0072(12) 0.0126(13) C26 0.0457(17) 0.059(2) 0.0404(16) 0.0090(14) 0.0095(13) 0.0061(15) C27 0.055(2) 0.083(3) 0.0359(16) 0.0154(17) 0.0112(14) -0.0012(19) C28 0.072(3) 0.067(3) 0.056(2) 0.0309(19) 0.0073(18) 0.006(2) C29 0.097(3) 0.059(2) 0.074(2) 0.034(2) 0.030(2) 0.034(2) C30 0.076(2) 0.058(2) 0.0582(19) 0.0273(17) 0.0297(18) 0.0296(19) C31 0.0441(16) 0.0426(16) 0.0378(14) 0.0115(12) 0.0099(12) 0.0148(13) C32 0.0495(17) 0.0408(16) 0.0460(16) 0.0129(13) 0.0120(13) 0.0166(14) C33 0.0449(16) 0.0431(17) 0.0489(17) 0.0062(14) 0.0064(13) 0.0121(14) C34 0.0462(17) 0.055(2) 0.0496(17) 0.0123(15) 0.0114(14) 0.0214(15) C35 0.0524(18) 0.0433(18) 0.0599(19) 0.0103(15) 0.0129(15) 0.0205(15) C36 0.0480(17) 0.0417(17) 0.0491(17) 0.0069(13) 0.0056(14) 0.0142(14) C37 0.0482(18) 0.062(2) 0.065(2) 0.0088(17) 0.0077(16) 0.0251(17) C38 0.051(2) 0.078(3) 0.084(3) 0.008(2) 0.0048(19) 0.023(2) C39 0.052(2) 0.114(4) 0.097(3) -0.005(3) -0.004(2) 0.033(3) C40 0.063(3) 0.117(4) 0.128(4) -0.007(4) -0.015(3) 0.052(3) C41 0.094(4) 0.097(4) 0.178(6) 0.018(4) -0.028(4) 0.058(3) C42 0.081(3) 0.080(3) 0.133(4) 0.018(3) -0.020(3) 0.040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.324(5) . ? N1 C1 1.357(4) . ? N2 C11 1.311(5) . ? N2 C12 1.352(4) . ? N3 C6 1.328(4) . ? N3 C13 1.357(4) . ? N4 C7 1.325(4) . ? N4 C14 1.362(4) . ? C1 C5 1.406(4) . ? C1 C12 1.460(5) . ? C2 C3 1.397(6) . ? C3 C4 1.367(5) . ? C4 C5 1.395(5) . ? C5 C6 1.465(4) . ? C6 C7 1.425(4) . ? C7 C8 1.468(4) . ? C8 C9 1.389(5) . ? C8 C12 1.399(4) . ? C9 C10 1.374(5) . ? C10 C11 1.398(6) . ? C13 C14 1.410(4) . ? C13 C18 1.421(4) . ? C14 C15 1.416(4) . ? C15 C16 1.377(4) . ? C16 C17 1.437(4) . ? C16 C31 1.494(4) . ? C17 C18 1.370(4) . ? C17 C19 1.488(4) . ? C19 C24 1.387(4) . ? C19 C20 1.390(4) . ? C20 C21 1.377(4) . ? C21 C22 1.397(4) . ? C22 C23 1.396(4) . ? C22 C25 1.478(4) . ? C23 C24 1.383(4) . ? C25 C30 1.383(5) . ? C25 C26 1.395(4) . ? C26 C27 1.385(5) . ? C27 C28 1.370(6) . ? C28 C29 1.363(6) . ? C29 C30 1.386(5) . ? C31 C36 1.391(4) . ? C31 C32 1.393(4) . ? C32 C33 1.385(4) . ? C33 C34 1.399(4) . ? C34 C35 1.400(5) . ? C34 C37 1.492(4) . ? C35 C36 1.378(4) . ? C37 C38 1.365(5) . ? C37 C42 1.401(6) . ? C38 C39 1.388(6) . ? C39 C40 1.333(7) . ? C40 C41 1.361(8) . ? C41 C42 1.395(6) . ? C1TA C3TA 1.343(9) 2_556 ? C1TA C2TA 1.473(10) . ? C2TA C4TA 1.304(10) . ? C2TA C3TA 1.374(9) . ? C3TA C1TA 1.343(9) 2_556 ? C1T C3T 1.265(16) 2_566 ? C1T C5T 1.262(15) 2_566 ? C1T C4T 1.290(12) 2_566 ? C1T C2T 1.408(12) . ? C1T C2T 1.488(12) 2_566 ? C1T C1T 1.65(2) 2_566 ? C2T C3T 1.234(14) . ? C2T C5T 1.248(12) 2_566 ? C2T C1T 1.488(12) 2_566 ? C3T C1T 1.265(16) 2_566 ? C3T C4T 1.509(15) . ? C4T C1T 1.290(12) 2_566 ? C4T C5T 1.449(14) . ? C5T C2T 1.248(12) 2_566 ? C5T C1T 1.262(15) 2_566 ? 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 N1 C1 117.4(3) . . ? C11 N2 C12 117.2(3) . . ? C6 N3 C13 116.3(3) . . ? C7 N4 C14 116.4(3) . . ? N1 C1 C5 121.9(3) . . ? N1 C1 C12 118.1(3) . . ? C5 C1 C12 120.0(3) . . ? N1 C2 C3 124.7(3) . . ? C4 C3 C2 117.8(4) . . ? C3 C4 C5 119.6(3) . . ? C4 C5 C1 118.6(3) . . ? C4 C5 C6 121.3(3) . . ? C1 C5 C6 120.1(3) . . ? N3 C6 C7 121.8(3) . . ? N3 C6 C5 118.3(3) . . ? C7 C6 C5 119.9(3) . . ? N4 C7 C6 122.3(3) . . ? N4 C7 C8 118.5(3) . . ? C6 C7 C8 119.2(3) . . ? C9 C8 C12 118.9(3) . . ? C9 C8 C7 120.6(3) . . ? C12 C8 C7 120.4(3) . . ? C10 C9 C8 118.9(3) . . ? C9 C10 C11 117.8(4) . . ? N2 C11 C10 124.9(3) . . ? N2 C12 C8 122.2(3) . . ? N2 C12 C1 117.5(3) . . ? C8 C12 C1 120.3(3) . . ? N3 C13 C14 122.0(3) . . ? N3 C13 C18 119.1(3) . . ? C14 C13 C18 118.9(3) . . ? N4 C14 C13 121.2(3) . . ? N4 C14 C15 119.4(3) . . ? C13 C14 C15 119.4(3) . . ? C16 C15 C14 121.2(3) . . ? C15 C16 C17 119.4(3) . . ? C15 C16 C31 117.7(3) . . ? C17 C16 C31 122.6(2) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 C19 117.8(3) . . ? C16 C17 C19 122.3(2) . . ? C17 C18 C13 121.3(3) . . ? C24 C19 C20 117.8(3) . . ? C24 C19 C17 121.3(2) . . ? C20 C19 C17 120.9(3) . . ? C21 C20 C19 120.9(3) . . ? C20 C21 C22 121.6(3) . . ? C23 C22 C21 117.3(3) . . ? C23 C22 C25 122.0(3) . . ? C21 C22 C25 120.7(2) . . ? C24 C23 C22 120.8(3) . . ? C23 C24 C19 121.6(3) . . ? C30 C25 C26 117.3(3) . . ? C30 C25 C22 121.6(3) . . ? C26 C25 C22 121.1(3) . . ? C27 C26 C25 120.8(4) . . ? C28 C27 C26 120.8(3) . . ? C29 C28 C27 118.9(3) . . ? C28 C29 C30 121.0(4) . . ? C25 C30 C29 121.1(3) . . ? C36 C31 C32 117.9(3) . . ? C36 C31 C16 121.1(3) . . ? C32 C31 C16 120.9(3) . . ? C33 C32 C31 121.0(3) . . ? C32 C33 C34 121.2(3) . . ? C33 C34 C35 117.2(3) . . ? C33 C34 C37 121.5(3) . . ? C35 C34 C37 121.3(3) . . ? C36 C35 C34 121.4(3) . . ? C35 C36 C31 121.2(3) . . ? C38 C37 C42 116.6(4) . . ? C38 C37 C34 122.4(3) . . ? C42 C37 C34 120.9(4) . . ? C37 C38 C39 122.1(4) . . ? C40 C39 C38 120.6(5) . . ? C39 C40 C41 119.8(4) . . ? C40 C41 C42 120.5(5) . . ? C41 C42 C37 120.3(5) . . ? C3TA C1TA C2TA 114.4(7) 2_556 . ? C4TA C2TA C3TA 124.1(8) . . ? C4TA C2TA C1TA 112.6(8) . . ? C3TA C2TA C1TA 123.2(7) . . ? C1TA C3TA C2TA 122.4(8) 2_556 . ? C3T C1T C5T 141.4(13) 2_566 2_566 ? C3T C1T C4T 72.4(10) 2_566 2_566 ? C5T C1T C4T 69.2(8) 2_566 2_566 ? C3T C1T C2T 163.1(12) 2_566 . ? C5T C1T C2T 55.4(8) 2_566 . ? C4T C1T C2T 124.5(10) 2_566 . ? C3T C1T C2T 52.5(8) 2_566 2_566 ? C5T C1T C2T 165.8(11) 2_566 2_566 ? C4T C1T C2T 124.9(10) 2_566 2_566 ? C2T C1T C2T 110.6(8) . 2_566 ? C3T C1T C1T 105.5(12) 2_566 2_566 ? C5T C1T C1T 113.0(13) 2_566 2_566 ? C4T C1T C1T 177.7(13) 2_566 2_566 ? C2T C1T C1T 57.6(7) . 2_566 ? C2T C1T C1T 53.0(7) 2_566 2_566 ? C3T C2T C5T 178.6(11) . 2_566 ? C3T C2T C1T 123.8(10) . . ? C5T C2T C1T 56.3(7) 2_566 . ? C3T C2T C1T 54.4(8) . 2_566 ? C5T C2T C1T 125.7(9) 2_566 2_566 ? C1T C2T C1T 69.4(8) . 2_566 ? C2T C3T C1T 73.1(10) . 2_566 ? C2T C3T C4T 127.6(12) . . ? C1T C3T C4T 54.5(8) 2_566 . ? C1T C4T C5T 54.5(7) 2_566 . ? C1T C4T C3T 53.0(7) 2_566 . ? C5T C4T C3T 107.5(9) . . ? C2T C5T C1T 68.3(8) 2_566 2_566 ? C2T C5T C4T 124.5(11) 2_566 . ? C1T C5T C4T 56.3(8) 2_566 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.779 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.064 data_FO1978_1 _database_code_depnum_ccdc_archive 'CCDC 290999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H62 Br2 F12 N10 P2 Ru' _chemical_formula_weight 1450.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 12.7435(3) _cell_length_b 15.0747(3) _cell_length_c 16.6350(4) _cell_angle_alpha 91.617(1) _cell_angle_beta 97.359(1) _cell_angle_gamma 98.611(1) _cell_volume 3129.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9519 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22044 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14161 _reflns_number_gt 10601 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _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^)+(0.0904P)^2^+10.7115P] 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 14161 _refine_ls_number_parameters 760 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1922 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.74133(3) 0.59807(3) 0.72791(2) 0.02611(11) Uani 1 1 d . . . Br1 Br 0.22549(5) 1.04216(4) 0.32760(4) 0.05024(18) Uani 1 1 d . . . Br2 Br 0.18711(6) 1.11970(5) 0.50983(4) 0.0590(2) Uani 1 1 d . . . N1 N 0.6730(3) 0.6263(3) 0.6141(2) 0.0283(8) Uani 1 1 d . . . N2 N 0.6495(3) 0.6930(3) 0.7574(2) 0.0304(8) Uani 1 1 d . . . N3 N 0.4590(3) 0.8294(3) 0.4799(3) 0.0352(9) Uani 1 1 d . . . N4 N 0.4357(3) 0.9031(3) 0.6338(3) 0.0343(9) Uani 1 1 d . . . N5 N 0.6294(3) 0.4851(3) 0.7280(2) 0.0296(8) Uani 1 1 d . . . N6 N 0.8212(3) 0.5009(3) 0.6870(2) 0.0278(8) Uani 1 1 d . . . N7 N 0.8074(3) 0.5889(3) 0.8460(3) 0.0335(9) Uani 1 1 d . . . N8 N 0.8693(3) 0.7004(3) 0.7397(3) 0.0315(9) Uani 1 1 d . . . C1 C 0.6818(4) 0.5862(4) 0.5420(3) 0.0344(11) Uani 1 1 d . . . H1A H 0.7226 0.5384 0.5412 0.041 Uiso 1 1 calc R . . C2 C 0.6329(4) 0.6129(4) 0.4691(3) 0.0392(12) Uani 1 1 d . . . H2A H 0.6402 0.5834 0.4194 0.047 Uiso 1 1 calc R . . C3 C 0.5736(4) 0.6822(4) 0.4693(3) 0.0379(12) Uani 1 1 d . . . H3A H 0.5399 0.7010 0.4197 0.045 Uiso 1 1 calc R . . C4 C 0.5638(4) 0.7245(3) 0.5429(3) 0.0311(10) Uani 1 1 d . . . C5 C 0.6127(4) 0.6928(3) 0.6136(3) 0.0287(9) Uani 1 1 d . . . C6 C 0.6011(4) 0.7307(3) 0.6924(3) 0.0285(9) Uani 1 1 d . . . C7 C 0.5421(4) 0.8009(3) 0.7002(3) 0.0310(10) Uani 1 1 d . . . C8 C 0.5347(4) 0.8352(4) 0.7777(3) 0.0371(11) Uani 1 1 d . . . H8A H 0.4963 0.8836 0.7847 0.044 Uiso 1 1 calc R . . C9 C 0.5840(5) 0.7976(4) 0.8436(3) 0.0420(12) Uani 1 1 d . . . H9A H 0.5799 0.8197 0.8969 0.050 Uiso 1 1 calc R . . C10 C 0.6402(4) 0.7268(4) 0.8320(3) 0.0367(11) Uani 1 1 d . . . H10A H 0.6732 0.7012 0.8783 0.044 Uiso 1 1 calc R . . C11 C 0.5018(4) 0.7980(3) 0.5485(3) 0.0325(10) Uani 1 1 d . . . C12 C 0.4917(4) 0.8362(3) 0.6266(3) 0.0302(10) Uani 1 1 d . . . C13 C 0.4023(4) 0.8971(3) 0.4881(3) 0.0351(11) Uani 1 1 d . . . C14 C 0.3535(4) 0.9327(4) 0.4163(3) 0.0389(12) Uani 1 1 d . . . H14A H 0.3645 0.9110 0.3644 0.047 Uiso 1 1 calc R . . C15 C 0.2912(4) 0.9977(4) 0.4225(4) 0.0402(12) Uani 1 1 d . . . C16 C 0.2774(4) 1.0320(4) 0.5006(4) 0.0398(12) Uani 1 1 d . . . C17 C 0.3247(4) 1.0010(4) 0.5691(4) 0.0407(12) Uani 1 1 d . . . H17A H 0.3145 1.0247 0.6206 0.049 Uiso 1 1 calc R . . C18 C 0.3896(4) 0.9331(3) 0.5642(3) 0.0352(11) Uani 1 1 d . . . C19 C 0.5322(4) 0.4825(4) 0.7523(3) 0.0330(10) Uani 1 1 d . . . H19A H 0.5065 0.5374 0.7614 0.040 Uiso 1 1 calc R . . C20 C 0.4693(4) 0.4035(4) 0.7644(3) 0.0359(11) Uani 1 1 d . . . H20A H 0.4013 0.4049 0.7817 0.043 Uiso 1 1 calc R . . C21 C 0.5029(4) 0.3210(4) 0.7520(3) 0.0354(11) Uani 1 1 d . . . C22 C 0.6019(4) 0.3247(3) 0.7231(3) 0.0323(10) Uani 1 1 d . . . H22A H 0.6280 0.2704 0.7120 0.039 Uiso 1 1 calc R . . C23 C 0.6621(4) 0.4060(3) 0.7103(3) 0.0289(10) Uani 1 1 d . . . C24 C 0.7682(4) 0.4157(3) 0.6808(3) 0.0277(9) Uani 1 1 d . . . C25 C 0.8103(4) 0.3458(3) 0.6471(3) 0.0314(10) Uani 1 1 d . . . H25A H 0.7706 0.2869 0.6429 0.038 Uiso 1 1 calc R . . C26 C 0.9104(4) 0.3607(3) 0.6192(3) 0.0308(10) Uani 1 1 d . A . C27 C 0.9652(4) 0.4477(3) 0.6289(3) 0.0327(10) Uani 1 1 d . . . H27A H 1.0343 0.4612 0.6126 0.039 Uiso 1 1 calc R . . C28 C 0.9185(4) 0.5155(3) 0.6628(3) 0.0305(10) Uani 1 1 d . . . H28A H 0.9575 0.5747 0.6689 0.037 Uiso 1 1 calc R . . C29 C 0.4357(5) 0.2343(4) 0.7713(3) 0.0420(12) Uani 1 1 d . . . C30 C 0.3200(5) 0.2305(5) 0.7290(5) 0.0591(17) Uani 1 1 d . . . H30A H 0.3198 0.2303 0.6701 0.089 Uiso 1 1 calc R . . H30B H 0.2909 0.2832 0.7470 0.089 Uiso 1 1 calc R . . H30C H 0.2757 0.1758 0.7432 0.089 Uiso 1 1 calc R . . C31 C 0.4358(7) 0.2347(5) 0.8637(4) 0.0610(18) Uani 1 1 d . . . H31A H 0.5092 0.2369 0.8906 0.091 Uiso 1 1 calc R . . H31B H 0.3913 0.1800 0.8778 0.091 Uiso 1 1 calc R . . H31C H 0.4068 0.2875 0.8816 0.091 Uiso 1 1 calc R . . C32 C 0.4778(5) 0.1510(4) 0.7427(4) 0.0512(15) Uani 1 1 d . . . H32A H 0.5513 0.1517 0.7689 0.077 Uiso 1 1 calc R . . H32B H 0.4770 0.1507 0.6837 0.077 Uiso 1 1 calc R . . H32C H 0.4323 0.0970 0.7570 0.077 Uiso 1 1 calc R . . C33 C 0.9593(4) 0.2845(4) 0.5820(4) 0.0400(12) Uani 1 1 d . . . C34 C 1.0505(12) 0.2672(10) 0.6445(8) 0.052(3) Uani 0.50 1 d P A 1 H34A H 1.1133 0.3127 0.6417 0.078 Uiso 0.50 1 calc PR A 1 H34B H 1.0683 0.2074 0.6333 0.078 Uiso 0.50 1 calc PR A 1 H34C H 1.0288 0.2702 0.6988 0.078 Uiso 0.50 1 calc PR A 1 C35 C 0.8831(12) 0.2037(9) 0.5601(11) 0.051(3) Uani 0.50 1 d P A 1 H35A H 0.8372 0.2121 0.5098 0.077 Uiso 0.50 1 calc PR A 1 H35B H 0.8389 0.1910 0.6037 0.077 Uiso 0.50 1 calc PR A 1 H35C H 0.9216 0.1533 0.5519 0.077 Uiso 0.50 1 calc PR A 1 C36 C 1.0043(12) 0.3188(11) 0.5037(9) 0.047(3) Uani 0.50 1 d P A 1 H36A H 0.9613 0.3621 0.4791 0.071 Uiso 0.50 1 calc PR A 1 H36B H 1.0012 0.2679 0.4650 0.071 Uiso 0.50 1 calc PR A 1 H36C H 1.0788 0.3478 0.5177 0.071 Uiso 0.50 1 calc PR A 1 C34A C 0.9813(19) 0.2139(12) 0.6497(12) 0.082(5) Uani 0.50 1 d P A 2 H34D H 1.0337 0.2434 0.6943 0.123 Uiso 0.50 1 calc PR A 2 H34E H 1.0095 0.1637 0.6257 0.123 Uiso 0.50 1 calc PR A 2 H34F H 0.9143 0.1912 0.6704 0.123 Uiso 0.50 1 calc PR A 2 C35A C 0.8767(16) 0.2318(14) 0.5162(12) 0.078(6) Uani 0.50 1 d P A 2 H35D H 0.8584 0.2715 0.4727 0.116 Uiso 0.50 1 calc PR A 2 H35E H 0.8120 0.2084 0.5397 0.116 Uiso 0.50 1 calc PR A 2 H35F H 0.9068 0.1817 0.4940 0.116 Uiso 0.50 1 calc PR A 2 C36A C 1.0582(18) 0.3181(13) 0.5456(18) 0.100(9) Uani 0.50 1 d P A 2 H36D H 1.0412 0.3595 0.5032 0.150 Uiso 0.50 1 calc PR A 2 H36E H 1.0853 0.2672 0.5220 0.150 Uiso 0.50 1 calc PR A 2 H36F H 1.1128 0.3496 0.5878 0.150 Uiso 0.50 1 calc PR A 2 C37 C 0.7684(5) 0.5293(4) 0.8981(3) 0.0413(12) Uani 1 1 d . . . H37A H 0.7130 0.4816 0.8776 0.050 Uiso 1 1 calc R . . C38 C 0.8062(5) 0.5352(5) 0.9799(4) 0.0508(15) Uani 1 1 d . . . H38A H 0.7767 0.4918 1.0145 0.061 Uiso 1 1 calc R . . C39 C 0.8864(5) 0.6032(6) 1.0119(4) 0.0581(19) Uani 1 1 d . B . C40 C 0.9282(5) 0.6617(6) 0.9579(4) 0.0580(18) Uani 1 1 d . . . H40A H 0.9855 0.7083 0.9770 0.070 Uiso 1 1 calc R . . C41 C 0.8881(4) 0.6536(4) 0.8756(3) 0.0404(12) Uani 1 1 d . . . C42 C 0.9261(4) 0.7162(4) 0.8134(3) 0.0393(12) Uani 1 1 d . . . C43 C 1.0124(5) 0.7846(5) 0.8304(4) 0.0526(15) Uani 1 1 d . . . H43A H 1.0504 0.7936 0.8837 0.063 Uiso 1 1 calc R . . C44 C 1.0435(5) 0.8399(4) 0.7698(4) 0.0503(15) Uani 1 1 d . C . C45 C 0.9850(5) 0.8226(4) 0.6936(4) 0.0464(14) Uani 1 1 d . . . H45A H 1.0037 0.8586 0.6501 0.056 Uiso 1 1 calc R . . C46 C 0.8991(4) 0.7532(3) 0.6803(4) 0.0376(11) Uani 1 1 d . . . H46A H 0.8602 0.7426 0.6274 0.045 Uiso 1 1 calc R . . C47 C 0.9230(5) 0.6098(7) 1.1023(4) 0.089(3) Uani 1 1 d D . . C48 C 0.8328(10) 0.6282(12) 1.1481(9) 0.066(4) Uiso 0.50 1 d PD B 1 H48A H 0.8134 0.6870 1.1344 0.099 Uiso 0.50 1 calc PR B 1 H48B H 0.8560 0.6280 1.2065 0.099 Uiso 0.50 1 calc PR B 1 H48C H 0.7705 0.5816 1.1329 0.099 Uiso 0.50 1 calc PR B 1 C49 C 0.9408(18) 0.5174(9) 1.1314(13) 0.096(6) Uiso 0.50 1 d PD B 1 H49A H 0.9379 0.4759 1.0844 0.144 Uiso 0.50 1 calc PR B 1 H49B H 0.8849 0.4946 1.1642 0.144 Uiso 0.50 1 calc PR B 1 H49C H 1.0112 0.5223 1.1643 0.144 Uiso 0.50 1 calc PR B 1 C50 C 1.0305(9) 0.6676(11) 1.1286(10) 0.070(4) Uiso 0.50 1 d PD B 1 H50A H 1.0274 0.7291 1.1121 0.105 Uiso 0.50 1 calc PR B 1 H50B H 1.0859 0.6433 1.1030 0.105 Uiso 0.50 1 calc PR B 1 H50C H 1.0477 0.6677 1.1877 0.105 Uiso 0.50 1 calc PR B 1 C48A C 0.912(3) 0.7068(11) 1.122(2) 0.161(12) Uiso 0.50 1 d PD B 2 H48D H 0.8987 0.7379 1.0720 0.241 Uiso 0.50 1 calc PR B 2 H48E H 0.9776 0.7370 1.1548 0.241 Uiso 0.50 1 calc PR B 2 H48F H 0.8513 0.7079 1.1534 0.241 Uiso 0.50 1 calc PR B 2 C49A C 0.8445(13) 0.5799(14) 1.1606(10) 0.081(5) Uiso 0.50 1 d PD B 2 H49D H 0.7997 0.6264 1.1671 0.121 Uiso 0.50 1 calc PR B 2 H49E H 0.8838 0.5700 1.2134 0.121 Uiso 0.50 1 calc PR B 2 H49F H 0.7990 0.5238 1.1391 0.121 Uiso 0.50 1 calc PR B 2 C50A C 1.0430(6) 0.6217(11) 1.1249(9) 0.057(3) Uiso 0.50 1 d PD B 2 H50D H 1.0743 0.6830 1.1143 0.085 Uiso 0.50 1 calc PR B 2 H50E H 1.0727 0.5787 1.0925 0.085 Uiso 0.50 1 calc PR B 2 H50F H 1.0600 0.6112 1.1827 0.085 Uiso 0.50 1 calc PR B 2 C51 C 1.1374(5) 0.9171(5) 0.7853(4) 0.075(2) Uani 1 1 d D . . C52 C 1.1180(16) 0.9929(10) 0.7295(11) 0.077(5) Uiso 0.50 1 d PD C 1 H52A H 1.1784 1.0421 0.7403 0.115 Uiso 0.50 1 calc PR C 1 H52B H 1.0519 1.0148 0.7395 0.115 Uiso 0.50 1 calc PR C 1 H52C H 1.1111 0.9707 0.6729 0.115 Uiso 0.50 1 calc PR C 1 C53 C 1.2260(13) 0.8869(14) 0.7431(13) 0.063(5) Uiso 0.50 1 d PD C 1 H53A H 1.2888 0.9340 0.7506 0.094 Uiso 0.50 1 calc PR C 1 H53B H 1.2008 0.8755 0.6850 0.094 Uiso 0.50 1 calc PR C 1 H53C H 1.2453 0.8316 0.7664 0.094 Uiso 0.50 1 calc PR C 1 C54 C 1.1859(13) 0.9258(12) 0.8742(5) 0.067(4) Uiso 0.50 1 d PD C 1 H54A H 1.2452 0.9761 0.8824 0.100 Uiso 0.50 1 calc PR C 1 H54B H 1.2126 0.8701 0.8895 0.100 Uiso 0.50 1 calc PR C 1 H54C H 1.1310 0.9368 0.9079 0.100 Uiso 0.50 1 calc PR C 1 C52A C 1.2408(18) 0.888(3) 0.766(2) 0.135(15) Uiso 0.50 1 d PD C 2 H52D H 1.2991 0.9392 0.7759 0.202 Uiso 0.50 1 calc PR C 2 H52E H 1.2322 0.8678 0.7083 0.202 Uiso 0.50 1 calc PR C 2 H52F H 1.2579 0.8391 0.7997 0.202 Uiso 0.50 1 calc PR C 2 C53A C 1.0989(17) 1.0056(9) 0.7654(14) 0.086(6) Uiso 0.50 1 d PD C 2 H53D H 1.1595 1.0547 0.7756 0.130 Uiso 0.50 1 calc PR C 2 H53E H 1.0444 1.0159 0.7996 0.130 Uiso 0.50 1 calc PR C 2 H53F H 1.0681 1.0033 0.7081 0.130 Uiso 0.50 1 calc PR C 2 C54A C 1.146(2) 0.9617(17) 0.8694(8) 0.114(8) Uiso 0.50 1 d PD C 2 H54D H 1.2065 1.0112 0.8767 0.171 Uiso 0.50 1 calc PR C 2 H54E H 1.1579 0.9176 0.9104 0.171 Uiso 0.50 1 calc PR C 2 H54F H 1.0798 0.9853 0.8754 0.171 Uiso 0.50 1 calc PR C 2 P2 P 0.5000 0.0000 0.0000 0.0533(6) Uani 1 2 d S . . F21 F 0.3950(4) 0.0467(3) -0.0028(3) 0.0777(13) Uani 1 1 d . . . F22 F 0.5109(5) -0.0008(4) 0.0955(3) 0.1004(18) Uani 1 1 d . . . F23 F 0.5707(5) 0.0953(3) 0.0069(4) 0.1052(19) Uani 1 1 d . . . P3 P 0.5000 0.5000 0.0000 0.0466(5) Uani 1 2 d S . . F31 F 0.5933(4) 0.5156(4) 0.0739(2) 0.0769(13) Uani 1 1 d . . . F32 F 0.4411(4) 0.4183(3) 0.0441(3) 0.0750(13) Uani 1 1 d . . . F33 F 0.4364(3) 0.5678(3) 0.0435(2) 0.0562(9) Uani 1 1 d . . . P1 P 0.72491(13) 0.39793(11) 0.35612(12) 0.0501(4) Uani 1 1 d . . . F11 F 0.7360(4) 0.4969(3) 0.3234(3) 0.0718(12) Uani 1 1 d . . . F12 F 0.6195(3) 0.4157(3) 0.3935(3) 0.0765(13) Uani 1 1 d . . . F13 F 0.7965(4) 0.4383(3) 0.4379(3) 0.0755(12) Uani 1 1 d . . . F14 F 0.8285(3) 0.3808(3) 0.3196(3) 0.0816(14) Uani 1 1 d . . . F15 F 0.6502(4) 0.3612(5) 0.2741(4) 0.110(2) Uani 1 1 d . . . F16 F 0.7125(4) 0.3004(3) 0.3895(5) 0.110(2) Uani 1 1 d . . . N1AN N 0.2251(7) 0.8266(6) 0.2330(6) 0.099(2) Uiso 1 1 d . . . C1AN C 0.2255(15) 0.9201(13) 0.1064(12) 0.162(6) Uiso 1 1 d . . . H1A1 H 0.1782 0.9651 0.1103 0.243 Uiso 1 1 calc . . . H1A2 H 0.2011 0.8820 0.0568 0.243 Uiso 1 1 calc . . . H1A3 H 0.2988 0.9503 0.1048 0.243 Uiso 1 1 calc . . . C2AN C 0.2232(8) 0.8647(7) 0.1767(7) 0.091(3) Uiso 1 1 d . . . N2AN N 0.8006(11) 0.2675(9) 0.0114(8) 0.147(4) Uiso 1 1 d . . . C3AN C 0.6545(10) 0.3000(8) 0.0919(8) 0.107(3) Uiso 1 1 d . . . H3A1 H 0.5930 0.3145 0.0558 0.161 Uiso 1 1 calc . . . H3A2 H 0.6794 0.3491 0.1330 0.161 Uiso 1 1 calc . . . H3A3 H 0.6331 0.2444 0.1187 0.161 Uiso 1 1 calc . . . C4AN C 0.7355(9) 0.2890(8) 0.0476(7) 0.097(3) Uiso 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 Ru 0.02717(19) 0.02755(19) 0.02488(19) 0.00333(14) 0.00391(13) 0.00752(14) Br1 0.0498(3) 0.0492(3) 0.0554(4) 0.0183(3) 0.0015(3) 0.0212(3) Br2 0.0711(4) 0.0496(4) 0.0637(4) 0.0035(3) 0.0033(3) 0.0378(3) N1 0.0285(19) 0.031(2) 0.027(2) 0.0041(16) 0.0045(15) 0.0083(16) N2 0.030(2) 0.034(2) 0.028(2) 0.0005(17) 0.0047(16) 0.0061(16) N3 0.033(2) 0.040(2) 0.035(2) 0.0061(19) 0.0053(17) 0.0109(18) N4 0.034(2) 0.031(2) 0.038(2) 0.0022(18) 0.0034(18) 0.0069(17) N5 0.030(2) 0.033(2) 0.027(2) 0.0030(16) 0.0047(16) 0.0079(16) N6 0.030(2) 0.0269(19) 0.028(2) 0.0071(16) 0.0038(16) 0.0067(15) N7 0.037(2) 0.037(2) 0.028(2) 0.0022(18) 0.0050(17) 0.0114(18) N8 0.030(2) 0.030(2) 0.034(2) 0.0006(17) 0.0028(17) 0.0061(16) C1 0.040(3) 0.037(3) 0.030(2) -0.002(2) 0.006(2) 0.015(2) C2 0.046(3) 0.049(3) 0.026(2) 0.000(2) 0.005(2) 0.018(2) C3 0.040(3) 0.049(3) 0.028(2) 0.005(2) 0.002(2) 0.018(2) C4 0.029(2) 0.034(2) 0.032(2) 0.002(2) 0.0049(19) 0.0111(19) C5 0.027(2) 0.030(2) 0.029(2) 0.0021(19) 0.0040(18) 0.0040(18) C6 0.030(2) 0.028(2) 0.029(2) 0.0017(19) 0.0073(18) 0.0051(18) C7 0.034(2) 0.030(2) 0.031(2) 0.0019(19) 0.0064(19) 0.0087(19) C8 0.042(3) 0.038(3) 0.036(3) -0.001(2) 0.009(2) 0.017(2) C9 0.053(3) 0.046(3) 0.030(3) -0.004(2) 0.005(2) 0.017(3) C10 0.043(3) 0.040(3) 0.028(2) 0.000(2) 0.003(2) 0.013(2) C11 0.027(2) 0.032(2) 0.039(3) 0.008(2) 0.006(2) 0.0063(19) C12 0.028(2) 0.030(2) 0.034(3) 0.004(2) 0.0045(19) 0.0065(18) C13 0.032(2) 0.032(3) 0.043(3) 0.010(2) 0.004(2) 0.009(2) C14 0.042(3) 0.039(3) 0.039(3) 0.010(2) 0.004(2) 0.015(2) C15 0.034(3) 0.033(3) 0.055(3) 0.013(2) 0.004(2) 0.010(2) C16 0.038(3) 0.030(3) 0.054(3) 0.004(2) 0.004(2) 0.013(2) C17 0.041(3) 0.034(3) 0.048(3) 0.000(2) 0.002(2) 0.012(2) C18 0.033(3) 0.027(2) 0.046(3) 0.006(2) 0.003(2) 0.0074(19) C19 0.031(2) 0.038(3) 0.033(3) 0.003(2) 0.007(2) 0.010(2) C20 0.030(2) 0.046(3) 0.032(3) 0.002(2) 0.007(2) 0.003(2) C21 0.036(3) 0.040(3) 0.029(2) 0.005(2) 0.006(2) 0.002(2) C22 0.033(2) 0.033(2) 0.031(2) 0.001(2) 0.0036(19) 0.0045(19) C23 0.027(2) 0.036(2) 0.025(2) 0.0048(19) 0.0024(17) 0.0071(18) C24 0.026(2) 0.032(2) 0.025(2) 0.0025(19) 0.0025(17) 0.0067(18) C25 0.033(2) 0.028(2) 0.034(3) 0.005(2) 0.006(2) 0.0056(19) C26 0.033(2) 0.032(2) 0.030(2) 0.001(2) 0.0048(19) 0.0098(19) C27 0.029(2) 0.032(2) 0.038(3) 0.004(2) 0.006(2) 0.0060(19) C28 0.028(2) 0.031(2) 0.033(2) 0.006(2) 0.0051(19) 0.0044(18) C29 0.042(3) 0.043(3) 0.040(3) 0.004(2) 0.012(2) -0.003(2) C30 0.048(4) 0.059(4) 0.067(4) -0.001(3) 0.015(3) -0.010(3) C31 0.085(5) 0.049(4) 0.051(4) 0.013(3) 0.030(4) -0.002(3) C32 0.055(4) 0.037(3) 0.060(4) 0.001(3) 0.020(3) -0.006(3) C33 0.036(3) 0.039(3) 0.049(3) -0.002(2) 0.011(2) 0.013(2) C34 0.066(9) 0.054(8) 0.044(7) -0.008(6) 0.000(6) 0.043(7) C35 0.045(7) 0.037(7) 0.071(10) -0.019(7) 0.010(7) 0.007(5) C36 0.043(8) 0.052(8) 0.052(8) -0.010(6) 0.026(6) 0.008(7) C34A 0.115(16) 0.059(10) 0.088(12) 0.011(9) 0.019(11) 0.058(11) C35A 0.088(12) 0.074(13) 0.066(11) -0.044(10) -0.027(10) 0.039(10) C36A 0.080(14) 0.055(10) 0.18(3) -0.029(14) 0.089(16) 0.006(10) C37 0.043(3) 0.050(3) 0.034(3) 0.008(2) 0.008(2) 0.012(2) C38 0.046(3) 0.076(4) 0.034(3) 0.018(3) 0.005(2) 0.018(3) C39 0.032(3) 0.110(6) 0.033(3) 0.011(3) 0.002(2) 0.013(3) C40 0.039(3) 0.094(5) 0.036(3) -0.007(3) 0.002(2) -0.001(3) C41 0.036(3) 0.053(3) 0.031(3) -0.001(2) 0.002(2) 0.007(2) C42 0.034(3) 0.045(3) 0.040(3) -0.002(2) 0.008(2) 0.005(2) C43 0.039(3) 0.061(4) 0.051(4) -0.009(3) 0.007(3) -0.009(3) C44 0.041(3) 0.045(3) 0.064(4) -0.005(3) 0.011(3) -0.001(2) C45 0.041(3) 0.033(3) 0.069(4) 0.011(3) 0.015(3) 0.007(2) C46 0.040(3) 0.029(2) 0.046(3) 0.005(2) 0.006(2) 0.010(2) C47 0.050(4) 0.184(11) 0.030(3) 0.002(5) 0.002(3) 0.016(5) C51 0.059(4) 0.072(5) 0.081(5) 0.000(4) 0.007(4) -0.024(4) P2 0.0647(15) 0.0407(12) 0.0546(14) -0.0053(10) 0.0047(11) 0.0126(10) F21 0.072(3) 0.078(3) 0.086(3) -0.009(2) 0.004(2) 0.031(2) F22 0.137(5) 0.116(4) 0.057(3) -0.007(3) 0.009(3) 0.053(4) F23 0.090(4) 0.059(3) 0.159(6) 0.008(3) 0.003(4) -0.003(3) P3 0.0517(12) 0.0544(13) 0.0360(11) 0.0034(9) 0.0137(9) 0.0088(10) F31 0.065(3) 0.120(4) 0.048(2) -0.020(2) 0.0011(19) 0.031(3) F32 0.086(3) 0.062(3) 0.090(3) 0.021(2) 0.052(3) 0.016(2) F33 0.064(2) 0.061(2) 0.048(2) -0.0023(17) 0.0214(17) 0.0133(18) P1 0.0391(8) 0.0429(8) 0.0650(10) -0.0091(7) 0.0051(7) 0.0000(6) F11 0.072(3) 0.069(3) 0.081(3) 0.021(2) 0.021(2) 0.018(2) F12 0.055(2) 0.067(3) 0.107(4) -0.012(2) 0.030(2) -0.004(2) F13 0.069(3) 0.085(3) 0.064(3) -0.003(2) -0.006(2) 0.000(2) F14 0.054(2) 0.067(3) 0.125(4) -0.025(3) 0.027(3) 0.009(2) F15 0.068(3) 0.141(5) 0.106(4) -0.062(4) -0.010(3) 0.003(3) F16 0.076(3) 0.045(2) 0.213(7) 0.022(3) 0.038(4) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N6 2.052(4) . ? Ru N5 2.051(4) . ? Ru N7 2.053(4) . ? Ru N8 2.056(4) . ? Ru N1 2.063(4) . ? Ru N2 2.065(4) . ? Br1 C15 1.880(5) . ? Br2 C16 1.894(5) . ? N1 C5 1.352(6) . ? N1 C1 1.353(6) . ? N2 C6 1.357(6) . ? N2 C10 1.355(7) . ? N3 C11 1.331(7) . ? N3 C13 1.348(7) . ? N4 C12 1.330(6) . ? N4 C18 1.352(7) . ? N5 C19 1.347(6) . ? N5 C23 1.358(6) . ? N6 C28 1.342(6) . ? N6 C24 1.353(6) . ? N7 C41 1.340(7) . ? N7 C37 1.351(7) . ? N8 C42 1.338(7) . ? N8 C46 1.343(7) . ? C1 C2 1.389(7) . ? C2 C3 1.378(7) . ? C3 C4 1.393(7) . ? C4 C5 1.390(7) . ? C4 C11 1.462(7) . ? C5 C6 1.448(7) . ? C6 C7 1.399(7) . ? C7 C8 1.396(7) . ? C7 C12 1.460(7) . ? C8 C9 1.372(8) . ? C9 C10 1.392(8) . ? C11 C12 1.435(7) . ? C13 C18 1.400(8) . ? C13 C14 1.432(7) . ? C14 C15 1.359(7) . ? C15 C16 1.425(9) . ? C16 C17 1.349(8) . ? C17 C18 1.417(7) . ? C19 C20 1.368(7) . ? C20 C21 1.393(8) . ? C21 C22 1.400(7) . ? C21 C29 1.518(7) . ? C22 C23 1.383(7) . ? C23 C24 1.485(6) . ? C24 C25 1.388(7) . ? C25 C26 1.402(7) . ? C26 C27 1.386(7) . ? C26 C33 1.536(7) . ? C27 C28 1.396(7) . ? C29 C32 1.525(9) . ? C29 C30 1.542(9) . ? C29 C31 1.536(8) . ? C33 C35 1.445(15) . ? C33 C36A 1.495(18) . ? C33 C34 1.516(13) . ? C33 C35A 1.531(17) . ? C33 C36 1.561(16) . ? C33 C34A 1.599(17) . ? C37 C38 1.381(8) . ? C38 C39 1.377(10) . ? C39 C40 1.377(10) . ? C39 C47 1.512(9) . ? C40 C41 1.393(8) . ? C41 C42 1.497(8) . ? C42 C43 1.385(8) . ? C43 C44 1.386(9) . ? C44 C45 1.382(9) . ? C44 C51 1.529(9) . ? C45 C46 1.386(8) . ? C47 C50A 1.509(4) . ? C47 C49A 1.512(4) . ? C47 C48 1.512(4) . ? C47 C50 1.515(4) . ? C47 C48A 1.524(4) . ? C47 C49 1.527(4) . ? C51 C53A 1.519(3) . ? C51 C54A 1.520(3) . ? C51 C52A 1.520(3) . ? C51 C52 1.521(3) . ? C51 C53 1.521(3) . ? C51 C54 1.522(3) . ? C53A C54A 1.93(3) . ? P2 F23 1.570(5) 2_655 ? P2 F23 1.570(5) . ? P2 F22 1.577(5) . ? P2 F22 1.577(5) 2_655 ? P2 F21 1.598(4) 2_655 ? P2 F21 1.598(4) . ? P3 F31 1.583(4) 2_665 ? P3 F31 1.583(4) . ? P3 F32 1.592(4) 2_665 ? P3 F32 1.592(4) . ? P3 F33 1.606(4) 2_665 ? P3 F33 1.606(4) . ? P1 F14 1.574(4) . ? P1 F16 1.579(5) . ? P1 F13 1.588(5) . ? P1 F15 1.594(5) . ? P1 F11 1.596(5) . ? P1 F12 1.605(4) . ? N1AN C2AN 1.111(12) . ? C1AN C2AN 1.456(19) . ? N2AN C4AN 1.164(15) . ? C3AN C4AN 1.371(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ru N5 78.61(16) . . ? N6 Ru N7 92.41(16) . . ? N5 Ru N7 94.41(17) . . ? N6 Ru N8 96.20(16) . . ? N5 Ru N8 170.86(16) . . ? N7 Ru N8 78.17(17) . . ? N6 Ru N1 95.07(15) . . ? N5 Ru N1 90.71(16) . . ? N7 Ru N1 171.65(17) . . ? N8 Ru N1 97.29(16) . . ? N6 Ru N2 173.69(16) . . ? N5 Ru N2 98.77(16) . . ? N7 Ru N2 93.52(16) . . ? N8 Ru N2 87.13(16) . . ? N1 Ru N2 79.16(16) . . ? C5 N1 C1 117.8(4) . . ? C5 N1 Ru 114.5(3) . . ? C1 N1 Ru 127.7(3) . . ? C6 N2 C10 117.3(4) . . ? C6 N2 Ru 114.2(3) . . ? C10 N2 Ru 128.2(3) . . ? C11 N3 C13 116.1(5) . . ? C12 N4 C18 116.7(5) . . ? C19 N5 C23 118.1(4) . . ? C19 N5 Ru 125.5(3) . . ? C23 N5 Ru 116.0(3) . . ? C28 N6 C24 117.9(4) . . ? C28 N6 Ru 125.6(3) . . ? C24 N6 Ru 116.4(3) . . ? C41 N7 C37 117.8(5) . . ? C41 N7 Ru 116.6(3) . . ? C37 N7 Ru 125.1(4) . . ? C42 N8 C46 117.8(5) . . ? C42 N8 Ru 116.6(3) . . ? C46 N8 Ru 125.6(4) . . ? N1 C1 C2 121.9(5) . . ? C3 C2 C1 119.8(5) . . ? C2 C3 C4 119.2(5) . . ? C5 C4 C3 118.0(4) . . ? C5 C4 C11 119.3(5) . . ? C3 C4 C11 122.7(4) . . ? N1 C5 C4 123.3(4) . . ? N1 C5 C6 115.9(4) . . ? C4 C5 C6 120.8(4) . . ? N2 C6 C7 122.7(4) . . ? N2 C6 C5 115.8(4) . . ? C7 C6 C5 121.5(4) . . ? C8 C7 C6 118.9(4) . . ? C8 C7 C12 122.5(4) . . ? C6 C7 C12 118.6(4) . . ? C9 C8 C7 118.7(5) . . ? C8 C9 C10 119.8(5) . . ? N2 C10 C9 122.6(5) . . ? N3 C11 C12 121.9(5) . . ? N3 C11 C4 118.3(5) . . ? C12 C11 C4 119.8(4) . . ? N4 C12 C11 121.3(4) . . ? N4 C12 C7 118.7(5) . . ? C11 C12 C7 120.0(4) . . ? N3 C13 C18 122.3(5) . . ? N3 C13 C14 118.4(5) . . ? C18 C13 C14 119.2(5) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 119.9(5) . . ? C14 C15 Br1 119.3(5) . . ? C16 C15 Br1 120.8(4) . . ? C17 C16 C15 121.4(5) . . ? C17 C16 Br2 118.5(5) . . ? C15 C16 Br2 120.1(4) . . ? C16 C17 C18 119.8(5) . . ? N4 C18 C13 121.6(5) . . ? N4 C18 C17 118.6(5) . . ? C13 C18 C17 119.8(5) . . ? N5 C19 C20 122.3(5) . . ? C19 C20 C21 121.3(5) . . ? C20 C21 C22 115.7(5) . . ? C20 C21 C29 120.7(5) . . ? C22 C21 C29 123.6(5) . . ? C23 C22 C21 121.0(5) . . ? N5 C23 C22 121.3(4) . . ? N5 C23 C24 114.2(4) . . ? C22 C23 C24 124.4(4) . . ? N6 C24 C25 121.5(4) . . ? N6 C24 C23 114.0(4) . . ? C25 C24 C23 124.5(4) . . ? C24 C25 C26 121.1(4) . . ? C27 C26 C25 116.5(4) . . ? C27 C26 C33 121.2(4) . . ? C25 C26 C33 122.3(4) . . ? C26 C27 C28 119.9(4) . . ? N6 C28 C27 123.0(5) . . ? C21 C29 C32 112.6(5) . . ? C21 C29 C30 109.3(5) . . ? C32 C29 C30 108.0(5) . . ? C21 C29 C31 107.7(5) . . ? C32 C29 C31 109.7(5) . . ? C30 C29 C31 109.4(5) . . ? C35 C33 C36A 128.6(11) . . ? C35 C33 C34 111.4(10) . . ? C36A C33 C34 75.5(14) . . ? C35 C33 C35A 33.3(9) . . ? C36A C33 C35A 108.8(15) . . ? C34 C33 C35A 138.5(10) . . ? C35 C33 C26 113.5(7) . . ? C36A C33 C26 112.7(8) . . ? C34 C33 C26 106.1(6) . . ? C35A C33 C26 109.4(8) . . ? C35 C33 C36 108.2(10) . . ? C36A C33 C36 34.8(11) . . ? C34 C33 C36 109.7(9) . . ? C35A C33 C36 79.0(12) . . ? C26 C33 C36 107.9(7) . . ? C35 C33 C34A 72.6(11) . . ? C36A C33 C34A 111.6(14) . . ? C34 C33 C34A 41.8(9) . . ? C35A C33 C34A 105.0(13) . . ? C26 C33 C34A 109.0(7) . . ? C36 C33 C34A 138.8(10) . . ? N7 C37 C38 122.3(6) . . ? C37 C38 C39 120.6(6) . . ? C40 C39 C38 116.6(6) . . ? C40 C39 C47 124.2(7) . . ? C38 C39 C47 119.3(6) . . ? C39 C40 C41 121.2(6) . . ? N7 C41 C40 121.4(5) . . ? N7 C41 C42 114.0(5) . . ? C40 C41 C42 124.6(6) . . ? N8 C42 C43 122.7(5) . . ? N8 C42 C41 114.2(5) . . ? C43 C42 C41 123.2(5) . . ? C42 C43 C44 120.1(6) . . ? C45 C44 C43 116.8(6) . . ? C45 C44 C51 120.8(6) . . ? C43 C44 C51 122.4(6) . . ? C44 C45 C46 120.5(6) . . ? N8 C46 C45 122.2(5) . . ? C39 C47 C50A 114.2(7) . . ? C39 C47 C49A 120.0(9) . . ? C50A C47 C49A 123.5(10) . . ? C39 C47 C48 110.3(8) . . ? C50A C47 C48 132.9(10) . . ? C49A C47 C48 30.4(8) . . ? C39 C47 C50 115.2(9) . . ? C50A C47 C50 28.1(8) . . ? C49A C47 C50 123.0(11) . . ? C48 C47 C50 115.8(11) . . ? C39 C47 C48A 100.6(15) . . ? C50A C47 C48A 96.0(16) . . ? C49A C47 C48A 88.9(16) . . ? C48 C47 C48A 61.0(15) . . ? C50 C47 C48A 68.0(15) . . ? C39 C47 C49 109.6(11) . . ? C50A C47 C49 77.5(11) . . ? C49A C47 C49 70.9(12) . . ? C48 C47 C49 101.3(12) . . ? C50 C47 C49 103.2(12) . . ? C48A C47 C49 149.1(17) . . ? C53A C51 C54A 78.7(14) . . ? C53A C51 C52A 126.4(18) . . ? C54A C51 C52A 114.0(18) . . ? C53A C51 C52 26.8(10) . . ? C54A C51 C52 103.0(14) . . ? C52A C51 C52 105.5(17) . . ? C53A C51 C53 120.2(13) . . ? C54A C51 C53 128.2(15) . . ? C52A C51 C53 14.9(18) . . ? C52 C51 C53 95.9(12) . . ? C53A C51 C44 110.0(10) . . ? C54A C51 C44 111.9(11) . . ? C52A C51 C44 111.6(17) . . ? C52 C51 C44 110.3(9) . . ? C53 C51 C44 105.5(9) . . ? C53A C51 C54 106.7(12) . . ? C54A C51 C54 30.2(11) . . ? C52A C51 C54 88.0(15) . . ? C52 C51 C54 127.2(12) . . ? C53 C51 C54 102.9(12) . . ? C44 C51 C54 111.3(8) . . ? C51 C53A C54A 50.7(7) . . ? C51 C54A C53A 50.6(7) . . ? F23 P2 F23 179.999(1) 2_655 . ? F23 P2 F22 90.3(4) 2_655 . ? F23 P2 F22 89.7(4) . . ? F23 P2 F22 89.7(4) 2_655 2_655 ? F23 P2 F22 90.3(4) . 2_655 ? F22 P2 F22 180.0 . 2_655 ? F23 P2 F21 89.6(3) 2_655 2_655 ? F23 P2 F21 90.4(3) . 2_655 ? F22 P2 F21 89.0(3) . 2_655 ? F22 P2 F21 91.0(3) 2_655 2_655 ? F23 P2 F21 90.4(3) 2_655 . ? F23 P2 F21 89.6(3) . . ? F22 P2 F21 91.0(3) . . ? F22 P2 F21 89.0(3) 2_655 . ? F21 P2 F21 180.0 2_655 . ? F31 P3 F31 179.998(2) 2_665 . ? F31 P3 F32 89.8(3) 2_665 2_665 ? F31 P3 F32 90.2(3) . 2_665 ? F31 P3 F32 90.2(3) 2_665 . ? F31 P3 F32 89.8(3) . . ? F32 P3 F32 180.000(1) 2_665 . ? F31 P3 F33 90.2(2) 2_665 2_665 ? F31 P3 F33 89.8(2) . 2_665 ? F32 P3 F33 90.1(2) 2_665 2_665 ? F32 P3 F33 89.9(2) . 2_665 ? F31 P3 F33 89.8(2) 2_665 . ? F31 P3 F33 90.2(2) . . ? F32 P3 F33 89.9(2) 2_665 . ? F32 P3 F33 90.1(2) . . ? F33 P3 F33 179.998(1) 2_665 . ? F14 P1 F16 90.2(3) . . ? F14 P1 F13 90.0(3) . . ? F16 P1 F13 91.3(3) . . ? F14 P1 F15 91.8(3) . . ? F16 P1 F15 90.6(4) . . ? F13 P1 F15 177.4(3) . . ? F14 P1 F11 90.8(3) . . ? F16 P1 F11 179.0(3) . . ? F13 P1 F11 88.4(3) . . ? F15 P1 F11 89.7(3) . . ? F14 P1 F12 179.8(3) . . ? F16 P1 F12 89.9(3) . . ? F13 P1 F12 89.8(3) . . ? F15 P1 F12 88.4(3) . . ? F11 P1 F12 89.1(2) . . ? N1AN C2AN C1AN 175.9(14) . . ? N2AN C4AN C3AN 170.9(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.672 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.119