Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 X-Sun-Content-Length: 40308 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 771 data_[2a](PF6)2_(CH3CN) _database_code_CSD 157684 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kazushi, Shiren' 'Ooyama, Dai' 'Tanaka, Koji' 'Tomon, Takashi' 'Wada, Tohru' _publ_contact_author_name 'Prof Takashi Tomon' _publ_contact_author_address ; Department of Structural Molecular Science Graduate University for Advanced Studies 38 Nishigonaka Myodaiji Okazaki Aichi 444-8585 JAPAN ; #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jan 18 20:53:59 2001' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_formula_weight 932.65 _chemical_formula_sum 'C33 H31 F12 N7 O P2 Ru ' #------------------------------------------------------------------------------ _cell_length_a 12.495(2) _cell_length_b 19.134(4) _cell_length_c 15.602(3) _cell_angle_alpha 89 _cell_angle_beta 90 _cell_angle_gamma 89 _cell_volume 3729(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.3 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.37 _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1872.00 _exptl_absorpt_coefficient_mu 6.06 _exptl_absorpt_correction_type psi-scan(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.935 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.46 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -2 -2 1 0 -2 -1 0 _diffrn_reflns_number 4889 _reflns_number_total 4778 _reflns_number_observed 2566 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.091 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05633 _diffrn_orient_matrix_UB_12 -0.03403 _diffrn_orient_matrix_UB_13 0.01819 _diffrn_orient_matrix_UB_21 -0.02337 _diffrn_orient_matrix_UB_22 0.03290 _diffrn_orient_matrix_UB_23 0.04615 _diffrn_orient_matrix_UB_31 -0.05182 _diffrn_orient_matrix_UB_32 0.02216 _diffrn_orient_matrix_UB_33 -0.04059 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 132 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 124 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 28 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 48 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru1 0.70518(5) 0.06224(3) 0.2672(2) 0.0386(1) Uani d . 1.00 . P1 0.7069(3) 0.2461(2) -0.0773(3) 0.078(1) Uani d . 1.00 . P2 0.9281 -0.1657 0.0110 0.0681 Uiso d . 1.00 . F1 0.726(1) 0.3237(7) -0.082(2) 0.216(8) Uani d . 1.00 . F2 0.5863(9) 0.2564(10) -0.0672(10) 0.177(6) Uani d . 1.00 . F3 0.724(1) 0.243(1) 0.0218(8) 0.184(6) Uani d . 1.00 . F4 0.8325(8) 0.2383(7) -0.0866(9) 0.131(4) Uani d . 1.00 . F5 0.684(1) 0.244(1) -0.1747(8) 0.194(6) Uani d . 1.00 . F6 0.686(2) 0.1658(8) -0.069(2) 0.257(10) Uani d . 1.00 . F7 0.9480 -0.1486 -0.0865 0.1377 Uiso d . 1.00 . F8 0.9084 -0.1832 0.1073 0.1274 Uiso d . 1.00 . F9 0.8161 -0.1377 0.0042 0.1100 Uiso d . 0.40 . F10 0.8597 -0.0979 0.0005 0.1057 Uiso d . 0.40 . F11 0.9225 -0.0889 0.0535 0.1152 Uiso d . 0.40 . F12 1.0130 -0.1044 0.0383 0.1163 Uiso d . 0.50 . F13 1.0407 -0.1381 0.0074 0.1131 Uiso d . 0.40 . F14 1.0337 -0.2128 0.0261 0.1319 Uiso d . 0.50 . F15 0.9602 -0.2457 -0.0071 0.1125 Uiso d . 0.40 . F16 0.8737 -0.2344 -0.0200 0.1058 Uiso d . 0.50 . F17 0.8086 -0.1950 0.0081 0.1183 Uiso d . 0.50 . O1 1.0030(7) -0.0770(4) 0.3585(6) 0.065(2) Uani d . 1.00 . N1 0.8272(7) 0.0653(5) 0.1818(6) 0.047(2) Uani d . 1.00 . N2 0.9216(8) 0.0230(5) 0.2984(7) 0.048(2) Uani d . 1.00 . N3 0.7356(7) 0.1669(4) 0.2873(6) 0.048(2) Uani d . 1.00 . N4 0.5855(7) 0.1127(5) 0.1892(6) 0.049(2) Uani d . 1.00 . N5 0.5844(7) 0.0528(5) 0.3582(6) 0.049(2) Uani d . 1.00 . N6 0.6524(7) -0.0378(4) 0.2455(5) 0.044(2) Uani d . 1.00 . N7 0.663(1) 0.0488(9) 0.631(2) 0.143(7) Uani d . 1.00 . C1 0.8117(10) -0.0013(7) 0.4291(8) 0.060(3) Uani d . 1.00 . C2 0.8196(8) 0.0252(5) 0.3367(8) 0.043(2) Uani d . 1.00 . C3 0.991(1) -0.1205(6) 0.2870(10) 0.074(4) Uani d . 1.00 . C4 1.0150(9) -0.0058(7) 0.3402(10) 0.064(3) Uani d . 1.00 . C5 1.114(1) 0.0074(8) 0.290(1) 0.078(5) Uani d . 1.00 . C6 1.119(1) 0.0352(9) 0.215(1) 0.075(4) Uani d . 1.00 . C7 1.010(1) 0.0840(7) 0.087(1) 0.076(4) Uani d . 1.00 . C8 0.917(1) 0.1036(7) 0.0532(8) 0.072(4) Uani d . 1.00 . C9 0.823(1) 0.0913(7) 0.1007(8) 0.066(3) Uani d . 1.00 . C10 1.0184(9) 0.0551(6) 0.169(1) 0.063(3) Uani d . 1.00 . C11 0.924(1) 0.0479(5) 0.2144(8) 0.047(2) Uani d . 1.00 . C12 0.8173(10) 0.1930(7) 0.3351(9) 0.060(3) Uani d . 1.00 . C13 0.844(1) 0.2653(7) 0.341(1) 0.076(4) Uani d . 1.00 . C14 0.780(1) 0.3100(6) 0.295(1) 0.085(5) Uani d . 1.00 . C15 0.697(1) 0.2845(6) 0.246(1) 0.083(5) Uani d . 1.00 . C16 0.6768(8) 0.2142(5) 0.2420(7) 0.047(2) Uani d . 1.00 . C17 0.5920(9) 0.1842(6) 0.1882(8) 0.054(3) Uani d . 1.00 . C18 0.524(1) 0.2249(8) 0.1400(10) 0.078(4) Uani d . 1.00 . C19 0.437(1) 0.1882(9) 0.094(1) 0.090(5) Uani d . 1.00 . C20 0.438(1) 0.1206(8) 0.095(1) 0.074(4) Uani d . 1.00 . C21 0.509(1) 0.0821(7) 0.1424(10) 0.062(4) Uani d . 1.00 . C22 0.553(1) 0.1014(7) 0.4141(9) 0.059(4) Uani d . 1.00 . C23 0.465(1) 0.0952(8) 0.4635(9) 0.066(4) Uani d . 1.00 . C24 0.408(1) 0.0326(9) 0.461(1) 0.091(5) Uani d . 1.00 . C25 0.439(1) -0.0169(8) 0.406(1) 0.076(4) Uani d . 1.00 . C26 0.5267(9) -0.0070(7) 0.3549(9) 0.057(3) Uani d . 1.00 . C27 0.5686(9) -0.0600(6) 0.2944(8) 0.054(3) Uani d . 1.00 . C28 0.527(1) -0.1279(6) 0.286(1) 0.071(4) Uani d . 1.00 . C29 0.575(1) -0.1725(6) 0.229(1) 0.078(4) Uani d . 1.00 . C30 0.651(1) -0.1491(6) 0.1764(9) 0.063(3) Uani d . 1.00 . C31 0.6931(8) -0.0829(5) 0.1896(8) 0.050(3) Uani d . 1.00 . C32 0.695(1) 0.1024(10) 0.634(1) 0.098(6) Uani d . 1.00 . C33 0.744(2) 0.169(1) 0.641(2) 0.117(7) Uani d . 1.00 . H1 0.8332 -0.0489 0.4321 0.0740 Uiso calc . 1.00 . H2 0.7396 0.0026 0.4487 0.0740 Uiso calc . 1.00 . H3 0.8567 0.0259 0.4653 0.0740 Uiso calc . 1.00 . H4 1.0514 -0.1165 0.2496 0.0935 Uiso calc . 1.00 . H5 0.9829 -0.1678 0.3037 0.0935 Uiso calc . 1.00 . H6 0.9283 -0.1069 0.2548 0.0935 Uiso calc . 1.00 . H7 1.0233 0.0182 0.3930 0.0778 Uiso calc . 1.00 . H8 1.1796 -0.0065 0.3160 0.0928 Uiso calc . 1.00 . H9 1.1865 0.0424 0.1880 0.0891 Uiso calc . 1.00 . H10 1.0745 0.0900 0.0550 0.0913 Uiso calc . 1.00 . H11 0.9147 0.1247 -0.0021 0.0842 Uiso calc . 1.00 . H12 0.7561 0.1005 0.0753 0.0791 Uiso calc . 1.00 . H13 0.8596 0.1605 0.3663 0.0717 Uiso calc . 1.00 . H14 0.9020 0.2817 0.3743 0.0935 Uiso calc . 1.00 . H15 0.7921 0.3593 0.2973 0.1049 Uiso calc . 1.00 . H16 0.6526 0.3162 0.2149 0.0997 Uiso calc . 1.00 . H17 0.5316 0.2744 0.1367 0.0957 Uiso calc . 1.00 . H18 0.3804 0.2119 0.0656 0.1096 Uiso calc . 1.00 . H19 0.3890 0.0954 0.0583 0.0916 Uiso calc . 1.00 . H20 0.5030 0.0321 0.1425 0.0737 Uiso calc . 1.00 . H21 0.5949 0.1421 0.4194 0.0715 Uiso calc . 1.00 . H22 0.4424 0.1314 0.4987 0.0803 Uiso calc . 1.00 . H23 0.3471 0.0245 0.4954 0.1094 Uiso calc . 1.00 . H24 0.4016 -0.0593 0.4030 0.0921 Uiso calc . 1.00 . H25 0.4658 -0.1415 0.3192 0.0845 Uiso calc . 1.00 . H26 0.5528 -0.2200 0.2261 0.0929 Uiso calc . 1.00 . H27 0.6765 -0.1773 0.1306 0.0764 Uiso calc . 1.00 . H28 0.7537 -0.0688 0.1568 0.0598 Uiso calc . 1.00 . H29 0.7101 0.2000 0.6022 0.1415 Uiso calc . 1.00 . H30 0.8178 0.1647 0.6262 0.1415 Uiso calc . 1.00 . H31 0.7370 0.1849 0.6975 0.1415 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0428(3) 0.0369(3) 0.0363(3) 0.0045(3) -0.0007(5) 0.0064(5) P(1) 0.071(2) 0.089(2) 0.075(2) -0.023(2) -0.025(2) 0.012(2) F(1) 0.18(1) 0.081(4) 0.39(3) 0.006(8) -0.11(2) 0.00(1) F(2) 0.067(3) 0.31(2) 0.16(1) -0.031(8) -0.005(7) 0.07(1) F(3) 0.143(10) 0.33(2) 0.081(3) -0.10(1) -0.046(7) 0.05(1) F(4) 0.078(3) 0.16(1) 0.15(1) 0.011(7) -0.001(7) -0.006(9) F(5) 0.21(1) 0.30(2) 0.073(4) -0.09(1) -0.031(8) -0.01(1) F(6) 0.28(2) 0.095(6) 0.40(3) -0.09(1) -0.18(2) 0.08(1) O(1) 0.076(5) 0.060(4) 0.060(5) 0.024(4) -0.017(4) 0.001(4) N(1) 0.051(3) 0.053(5) 0.037(4) -0.006(4) 0.007(2) -0.010(4) N(2) 0.041(4) 0.053(6) 0.050(5) 0.001(4) -0.001(3) 0.001(4) N(3) 0.053(5) 0.039(2) 0.052(7) 0.001(3) 0.007(3) 0.002(3) N(4) 0.042(4) 0.061(4) 0.044(5) 0.020(3) 0.001(3) 0.007(4) N(5) 0.048(4) 0.058(5) 0.042(4) 0.012(3) 0.007(3) 0.018(4) N(6) 0.051(4) 0.037(2) 0.045(5) 0.006(3) -0.004(3) 0.009(3) N(7) 0.09(1) 0.10(1) 0.24(2) -0.029(9) 0.01(1) 0.02(1) C(1) 0.071(8) 0.062(7) 0.049(5) 0.017(6) -0.010(6) 0.002(5) C(2) 0.040(4) 0.036(5) 0.053(5) 0.010(4) -0.005(3) 0.005(4) C(3) 0.083(8) 0.053(6) 0.09(1) 0.006(6) -0.015(8) -0.024(7) C(4) 0.043(5) 0.055(4) 0.094(10) 0.017(5) -0.023(5) -0.017(6) C(5) 0.052(6) 0.08(1) 0.10(1) 0.028(7) 0.001(6) -0.022(7) C(6) 0.045(6) 0.079(10) 0.10(1) -0.006(6) 0.019(6) -0.022(8) C(7) 0.089(8) 0.058(7) 0.081(7) -0.004(7) 0.045(6) -0.022(6) C(8) 0.110(8) 0.059(8) 0.046(7) 0.001(7) 0.025(6) -0.004(6) C(9) 0.101(9) 0.054(6) 0.044(5) 0.011(7) 0.010(6) 0.008(5) C(10) 0.051(5) 0.039(6) 0.099(8) -0.002(5) 0.028(5) 0.006(6) C(11) 0.055(4) 0.034(6) 0.051(5) 0.017(4) 0.013(4) -0.002(4) C(12) 0.058(7) 0.057(5) 0.064(7) -0.003(5) -0.005(5) -0.007(6) C(13) 0.082(9) 0.058(6) 0.089(10) -0.007(6) -0.011(8) -0.014(6) C(14) 0.11(1) 0.036(5) 0.11(1) -0.009(6) -0.021(8) -0.001(6) C(15) 0.090(9) 0.040(4) 0.12(2) 0.018(5) -0.020(8) 0.002(7) C(16) 0.042(5) 0.043(4) 0.057(6) 0.004(3) 0.015(3) 0.005(4) C(17) 0.048(6) 0.064(4) 0.052(6) -0.001(4) 0.008(4) 0.010(5) C(18) 0.081(9) 0.085(9) 0.068(8) 0.023(6) -0.016(6) 0.034(7) C(19) 0.077(9) 0.087(7) 0.11(1) 0.010(8) -0.018(8) 0.028(9) C(20) 0.055(7) 0.087(7) 0.08(1) -0.007(7) -0.027(7) 0.023(8) C(21) 0.054(7) 0.065(8) 0.066(8) -0.003(5) -0.009(5) -0.002(6) C(22) 0.066(7) 0.058(7) 0.053(7) 0.017(6) 0.010(5) 0.011(5) C(23) 0.072(8) 0.072(7) 0.053(7) 0.030(6) 0.019(6) 0.005(7) C(24) 0.10(1) 0.077(8) 0.10(1) 0.003(7) 0.051(9) 0.027(7) C(25) 0.058(7) 0.094(10) 0.076(9) -0.009(7) 0.022(6) 0.018(7) C(26) 0.051(6) 0.063(6) 0.056(7) 0.001(4) 0.002(4) 0.011(5) C(27) 0.047(5) 0.049(4) 0.067(7) -0.003(4) 0.001(4) 0.014(4) C(28) 0.070(7) 0.052(5) 0.09(1) -0.016(5) 0.007(7) 0.010(6) C(29) 0.086(9) 0.038(6) 0.11(1) -0.013(6) 0.010(7) 0.003(6) C(30) 0.079(8) 0.035(4) 0.075(8) 0.022(4) -0.005(6) -0.005(5) C(31) 0.049(6) 0.044(4) 0.055(6) 0.010(4) 0.004(5) -0.001(4) C(32) 0.061(9) 0.10(1) 0.13(2) -0.009(8) 0.017(9) 0.00(1) C(33) 0.11(1) 0.08(1) 0.16(2) 0.001(9) -0.02(1) 0.02(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00228|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2566 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0505 _refine_ls_wR_factor_obs 0.0715 _refine_ls_goodness_of_fit_obs 1.224 _refine_ls_shift/esd_max 0.0157 _refine_ls_shift/esd_mean 0.0032 _refine_diff_density_min -0.43 _refine_diff_density_max 0.79 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU1 N1 2.026(10) 1_555 1_555 yes RU1 N3 2.061(9) 1_555 1_555 yes RU1 N4 2.156(9) 1_555 1_555 yes RU1 N5 2.080(10) 1_555 1_555 yes RU1 N6 2.052(9) 1_555 1_555 yes RU1 C2 1.93(1) 1_555 1_555 yes P1 F1 1.51(1) 1_555 1_555 yes P1 F2 1.53(1) 1_555 1_555 yes P1 F3 1.56(1) 1_555 1_555 yes P1 F4 1.58(1) 1_555 1_555 yes P1 F5 1.55(1) 1_555 1_555 yes P1 F6 1.56(2) 1_555 1_555 yes P2 F7 1.575 1_555 1_555 yes P2 F8 1.559 1_555 1_555 yes P2 F9 1.5021(3) 1_555 1_555 yes P2 F10 1.5621(1) 1_555 1_555 yes P2 F11 1.614 1_555 1_555 yes P2 F12 1.6385(1) 1_555 1_555 yes P2 F13 1.5043(3) 1_555 1_555 yes P2 F14 1.6153(2) 1_555 1_555 yes P2 F15 1.606 1_555 1_555 yes P2 F16 1.5558(1) 1_555 1_555 yes P2 F17 1.5954(3) 1_555 1_555 yes F9 F10 0.9382(1) 1_555 1_555 yes F9 F17 1.101 1_555 1_555 yes F10 F11 1.1528(1) 1_555 1_555 yes F11 F12 1.1926(2) 1_555 1_555 yes F12 F13 0.878 1_555 1_555 yes F13 F14 1.461 1_555 1_555 yes F14 F15 1.2277(1) 1_555 1_555 yes F15 F16 1.1198(2) 1_555 1_555 yes F16 F17 1.1925(1) 1_555 1_555 yes O1 C3 1.40(2) 1_555 1_555 yes O1 C4 1.40(2) 1_555 1_555 yes N1 C9 1.36(2) 1_555 1_555 yes N1 C11 1.35(2) 1_555 1_555 yes N2 C2 1.41(1) 1_555 1_555 yes N2 C4 1.45(2) 1_555 1_555 yes N2 C11 1.40(2) 1_555 1_555 yes N3 C12 1.36(2) 1_555 1_555 yes N3 C16 1.36(1) 1_555 1_555 yes N4 C17 1.37(2) 1_555 1_555 yes N4 C21 1.34(2) 1_555 1_555 yes N5 C22 1.33(2) 1_555 1_555 yes N5 C26 1.35(2) 1_555 1_555 yes N6 C27 1.36(1) 1_555 1_555 yes N6 C31 1.33(1) 1_555 1_555 yes N7 C32 1.10(2) 1_555 1_555 yes C1 C2 1.53(2) 1_555 1_555 yes C4 C5 1.49(2) 1_555 1_555 yes C5 C6 1.30(3) 1_555 1_555 yes C6 C10 1.49(2) 1_555 1_555 yes C7 C8 1.34(2) 1_555 1_555 yes C7 C10 1.40(2) 1_555 1_555 yes C8 C9 1.40(2) 1_555 1_555 yes C10 C11 1.38(2) 1_555 1_555 yes C12 C13 1.43(2) 1_555 1_555 yes C13 C14 1.37(2) 1_555 1_555 yes C14 C15 1.37(2) 1_555 1_555 yes C15 C16 1.37(2) 1_555 1_555 yes C16 C17 1.47(2) 1_555 1_555 yes C17 C18 1.38(2) 1_555 1_555 yes C18 C19 1.48(2) 1_555 1_555 yes C19 C20 1.29(2) 1_555 1_555 yes C20 C21 1.37(2) 1_555 1_555 yes C22 C23 1.35(2) 1_555 1_555 yes C23 C24 1.39(2) 1_555 1_555 yes C24 C25 1.33(2) 1_555 1_555 yes C25 C26 1.36(2) 1_555 1_555 yes C26 C27 1.48(2) 1_555 1_555 yes C27 C28 1.41(2) 1_555 1_555 yes C28 C29 1.37(2) 1_555 1_555 yes C29 C30 1.34(2) 1_555 1_555 yes C30 C31 1.39(2) 1_555 1_555 yes C32 C33 1.42(3) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU1 N3 86.2(4) 1_555 1_555 1_555 yes N1 RU1 N4 97.9(4) 1_555 1_555 1_555 yes N1 RU1 N5 176.1(4) 1_555 1_555 1_555 yes N1 RU1 N6 99.2(4) 1_555 1_555 1_555 yes N1 RU1 C2 79.8(5) 1_555 1_555 1_555 yes N3 RU1 N4 77.2(4) 1_555 1_555 1_555 yes N3 RU1 N5 96.6(4) 1_555 1_555 1_555 yes N3 RU1 N6 171.8(4) 1_555 1_555 1_555 yes N3 RU1 C2 97.8(4) 1_555 1_555 1_555 yes N4 RU1 N5 85.5(4) 1_555 1_555 1_555 yes N4 RU1 N6 95.8(4) 1_555 1_555 1_555 yes N4 RU1 C2 174.7(4) 1_555 1_555 1_555 yes N5 RU1 N6 78.4(4) 1_555 1_555 1_555 yes N5 RU1 C2 97.0(5) 1_555 1_555 1_555 yes N6 RU1 C2 89.3(4) 1_555 1_555 1_555 yes F1 P1 F2 91(1) 1_555 1_555 1_555 yes F1 P1 F3 93(1) 1_555 1_555 1_555 yes F1 P1 F4 86.1(9) 1_555 1_555 1_555 yes F1 P1 F5 90(1) 1_555 1_555 1_555 yes F1 P1 F6 177(1) 1_555 1_555 1_555 yes F2 P1 F3 91.9(9) 1_555 1_555 1_555 yes F2 P1 F4 177(1) 1_555 1_555 1_555 yes F2 P1 F5 85.4(9) 1_555 1_555 1_555 yes F2 P1 F6 87(1) 1_555 1_555 1_555 yes F3 P1 F4 87.4(9) 1_555 1_555 1_555 yes F3 P1 F5 175.6(9) 1_555 1_555 1_555 yes F3 P1 F6 85(1) 1_555 1_555 1_555 yes F4 P1 F5 95.3(10) 1_555 1_555 1_555 yes F4 P1 F6 94(1) 1_555 1_555 1_555 yes F5 P1 F6 91(1) 1_555 1_555 1_555 yes F7 P2 F8 179.6 1_555 1_555 1_555 yes F7 P2 F9 90.336(3) 1_555 1_555 1_555 yes F7 P2 F10 79.235(3) 1_555 1_555 1_555 yes F7 P2 F11 102.3815(1) 1_555 1_555 1_555 yes F7 P2 F12 90.021(2) 1_555 1_555 1_555 yes F7 P2 F13 75.1113(7) 1_555 1_555 1_555 yes F7 P2 F14 97.347(4) 1_555 1_555 1_555 yes F7 P2 F15 89.3314(9) 1_555 1_555 1_555 yes F7 P2 F16 86.825(2) 1_555 1_555 1_555 yes F7 P2 F17 101.162(1) 1_555 1_555 1_555 yes F8 P2 F9 89.815(3) 1_555 1_555 1_555 yes F8 P2 F10 101.079(3) 1_555 1_555 1_555 yes F8 P2 F11 77.9875(1) 1_555 1_555 1_555 yes F8 P2 F12 90.238(2) 1_555 1_555 1_555 yes F8 P2 F13 104.9885(7) 1_555 1_555 1_555 yes F8 P2 F14 82.436(4) 1_555 1_555 1_555 yes F8 P2 F15 90.3043(9) 1_555 1_555 1_555 yes F8 P2 F16 92.859(2) 1_555 1_555 1_555 yes F8 P2 F17 78.735(1) 1_555 1_555 1_555 yes F9 P2 F10 35.590(1) 1_555 1_555 1_555 yes F9 P2 F11 70.346(3) 1_555 1_555 1_555 yes F9 P2 F12 111.474(9) 1_555 1_555 1_555 yes F9 P2 F13 138.077(7) 1_555 1_555 1_555 yes F9 P2 F14 165.975(2) 1_555 1_555 1_555 yes F9 P2 F15 124.0401(7) 1_555 1_555 1_555 yes F9 P2 F16 82.669(8) 1_555 1_555 1_555 yes F9 P2 F17 41.505(7) 1_555 1_555 1_555 yes F10 P2 F11 42.523(3) 1_555 1_555 1_555 yes F10 P2 F12 77.689(10) 1_555 1_555 1_555 yes F10 P2 F13 102.518(9) 1_555 1_555 1_555 yes F10 P2 F14 157.8 1_555 1_555 1_555 yes F10 P2 F15 155.362(2) 1_555 1_555 1_555 yes F10 P2 F16 115.446(8) 1_555 1_555 1_555 yes F10 P2 F17 77.070(9) 1_555 1_555 1_555 yes F11 P2 F12 43.014(6) 1_555 1_555 1_555 yes F11 P2 F13 74.716(4) 1_555 1_555 1_555 yes F11 P2 F14 118.911(3) 1_555 1_555 1_555 yes F11 P2 F15 161.854(1) 1_555 1_555 1_555 yes F11 P2 F16 151.345(5) 1_555 1_555 1_555 yes F11 P2 F17 106.895(4) 1_555 1_555 1_555 yes F12 P2 F13 32.075(2) 1_555 1_555 1_555 yes F12 P2 F14 80.368(10) 1_555 1_555 1_555 yes F12 P2 F15 124.485(8) 1_555 1_555 1_555 yes F12 P2 F16 165.546(1) 1_555 1_555 1_555 yes F12 P2 F17 149.848(2) 1_555 1_555 1_555 yes F13 P2 F14 55.734(9) 1_555 1_555 1_555 yes F13 P2 F15 95.390(6) 1_555 1_555 1_555 yes F13 P2 F16 133.890(1) 1_555 1_555 1_555 yes F13 P2 F17 176.2351(6) 1_555 1_555 1_555 yes F14 P2 F15 44.804(2) 1_555 1_555 1_555 yes F14 P2 F16 86.047(9) 1_555 1_555 1_555 yes F14 P2 F17 124.951(9) 1_555 1_555 1_555 yes F15 P2 F16 41.448(7) 1_555 1_555 1_555 yes F15 P2 F17 83.947(6) 1_555 1_555 1_555 yes F16 P2 F17 44.4519(9) 1_555 1_555 1_555 yes P2 F9 F10 75.699(9) 1_555 1_555 1_555 yes P2 F9 F17 73.795(5) 1_555 1_555 1_555 yes F10 F9 F17 149.384(4) 1_555 1_555 1_555 yes P2 F10 F9 68.71(1) 1_555 1_555 1_555 yes P2 F10 F11 71.143(6) 1_555 1_555 1_555 yes F9 F10 F11 118.177(5) 1_555 1_555 1_555 yes P2 F11 F10 66.334(3) 1_555 1_555 1_555 yes P2 F11 F12 69.588(3) 1_555 1_555 1_555 yes F10 F11 F12 117.794(8) 1_555 1_555 1_555 yes P2 F12 F11 67.399(9) 1_555 1_555 1_555 yes P2 F12 F13 65.514(9) 1_555 1_555 1_555 yes F11 F12 F13 131.7851(7) 1_555 1_555 1_555 yes P2 F13 F12 82.411(7) 1_555 1_555 1_555 yes P2 F13 F14 65.982(3) 1_555 1_555 1_555 yes F12 F13 F14 125.827(2) 1_555 1_555 1_555 yes P2 F14 F13 58.284(6) 1_555 1_555 1_555 yes P2 F14 F15 67.196(9) 1_555 1_555 1_555 yes F13 F14 F15 117.428(2) 1_555 1_555 1_555 yes P2 F15 F14 68.000(7) 1_555 1_555 1_555 yes P2 F15 F16 66.875(1) 1_555 1_555 1_555 yes F14 F15 F16 134.349(6) 1_555 1_555 1_555 yes P2 F16 F15 71.677(6) 1_555 1_555 1_555 yes P2 F16 F17 69.536(10) 1_555 1_555 1_555 yes F15 F16 F17 135.590(5) 1_555 1_555 1_555 yes P2 F17 F9 64.700(3) 1_555 1_555 1_555 yes P2 F17 F16 66.012(9) 1_555 1_555 1_555 yes F9 F17 F16 123.412(5) 1_555 1_555 1_555 yes C3 O1 C4 115(1) 1_555 1_555 1_555 yes RU1 N1 C9 126.6(10) 1_555 1_555 1_555 yes RU1 N1 C11 114.8(8) 1_555 1_555 1_555 yes C9 N1 C11 117(1) 1_555 1_555 1_555 yes C2 N2 C4 123(1) 1_555 1_555 1_555 yes C2 N2 C11 114(1) 1_555 1_555 1_555 yes C4 N2 C11 122(1) 1_555 1_555 1_555 yes RU1 N3 C12 125.3(8) 1_555 1_555 1_555 yes RU1 N3 C16 117.9(8) 1_555 1_555 1_555 yes C12 N3 C16 116.4(10) 1_555 1_555 1_555 yes RU1 N4 C17 114.4(8) 1_555 1_555 1_555 yes RU1 N4 C21 127.5(9) 1_555 1_555 1_555 yes C17 N4 C21 118(1) 1_555 1_555 1_555 yes RU1 N5 C22 126.8(9) 1_555 1_555 1_555 yes RU1 N5 C26 115.7(9) 1_555 1_555 1_555 yes C22 N5 C26 117(1) 1_555 1_555 1_555 yes RU1 N6 C27 116.5(8) 1_555 1_555 1_555 yes RU1 N6 C31 126.3(8) 1_555 1_555 1_555 yes C27 N6 C31 117(1) 1_555 1_555 1_555 yes C2 C1 H1 110(1) 1_555 1_555 1_555 no C2 C1 H2 109(1) 1_555 1_555 1_555 no C2 C1 H3 109(1) 1_555 1_555 1_555 no H1 C1 H2 109(1) 1_555 1_555 1_555 no H1 C1 H3 109(1) 1_555 1_555 1_555 no H2 C1 H3 108(1) 1_555 1_555 1_555 no RU1 C2 N2 116.3(8) 1_555 1_555 1_555 yes RU1 C2 C1 127.1(9) 1_555 1_555 1_555 yes N2 C2 C1 116.7(10) 1_555 1_555 1_555 yes O1 C3 H4 110(1) 1_555 1_555 1_555 no O1 C3 H5 111(1) 1_555 1_555 1_555 no O1 C3 H6 110(1) 1_555 1_555 1_555 no H4 C3 H5 108(1) 1_555 1_555 1_555 no H4 C3 H6 107(1) 1_555 1_555 1_555 no H5 C3 H6 108(1) 1_555 1_555 1_555 no O1 C4 N2 112(1) 1_555 1_555 1_555 yes O1 C4 C5 111(1) 1_555 1_555 1_555 yes O1 C4 H7 107(1) 1_555 1_555 1_555 no N2 C4 C5 111(1) 1_555 1_555 1_555 yes N2 C4 H7 107(1) 1_555 1_555 1_555 no C5 C4 H7 106(1) 1_555 1_555 1_555 no C4 C5 C6 125(1) 1_555 1_555 1_555 yes C4 C5 H8 116(1) 1_555 1_555 1_555 no C6 C5 H8 117(1) 1_555 1_555 1_555 no C5 C6 C10 119(1) 1_555 1_555 1_555 yes C5 C6 H9 119(1) 1_555 1_555 1_555 no C10 C6 H9 120(1) 1_555 1_555 1_555 no C8 C7 C10 122(1) 1_555 1_555 1_555 yes C8 C7 H10 119(1) 1_555 1_555 1_555 no C10 C7 H10 118(1) 1_555 1_555 1_555 no C7 C8 C9 117(1) 1_555 1_555 1_555 yes C7 C8 H11 120(1) 1_555 1_555 1_555 no C9 C8 H11 121(1) 1_555 1_555 1_555 no N1 C9 C8 121(1) 1_555 1_555 1_555 yes N1 C9 H12 119(1) 1_555 1_555 1_555 no C8 C9 H12 119(1) 1_555 1_555 1_555 no C6 C10 C7 126(1) 1_555 1_555 1_555 yes C6 C10 C11 117(1) 1_555 1_555 1_555 yes C7 C10 C11 116(1) 1_555 1_555 1_555 yes N1 C11 N2 114(1) 1_555 1_555 1_555 yes N1 C11 C10 123(1) 1_555 1_555 1_555 yes N2 C11 C10 122(1) 1_555 1_555 1_555 yes N3 C12 C13 124(1) 1_555 1_555 1_555 yes N3 C12 H13 117(1) 1_555 1_555 1_555 no C13 C12 H13 118(1) 1_555 1_555 1_555 no C12 C13 C14 116(1) 1_555 1_555 1_555 yes C12 C13 H14 122(1) 1_555 1_555 1_555 no C14 C13 H14 121(1) 1_555 1_555 1_555 no C13 C14 C15 120(1) 1_555 1_555 1_555 yes C13 C14 H15 120(1) 1_555 1_555 1_555 no C15 C14 H15 119(1) 1_555 1_555 1_555 no C14 C15 C16 120(1) 1_555 1_555 1_555 yes C14 C15 H16 119(1) 1_555 1_555 1_555 no C16 C15 H16 119(1) 1_555 1_555 1_555 no N3 C16 C15 121(1) 1_555 1_555 1_555 yes N3 C16 C17 115(1) 1_555 1_555 1_555 yes C15 C16 C17 122(1) 1_555 1_555 1_555 yes N4 C17 C16 115(1) 1_555 1_555 1_555 yes N4 C17 C18 122(1) 1_555 1_555 1_555 yes C16 C17 C18 122(1) 1_555 1_555 1_555 yes C17 C18 C19 116(1) 1_555 1_555 1_555 yes C17 C18 H17 122(1) 1_555 1_555 1_555 no C19 C18 H17 121(1) 1_555 1_555 1_555 no C18 C19 C20 117(1) 1_555 1_555 1_555 yes C18 C19 H18 123(1) 1_555 1_555 1_555 no C20 C19 H18 119(1) 1_555 1_555 1_555 no C19 C20 C21 123(1) 1_555 1_555 1_555 yes C19 C20 H19 119(1) 1_555 1_555 1_555 no C21 C20 H19 117(1) 1_555 1_555 1_555 no N4 C21 C20 121(1) 1_555 1_555 1_555 yes N4 C21 H20 119(1) 1_555 1_555 1_555 no C20 C21 H20 119(1) 1_555 1_555 1_555 no N5 C22 C23 123(1) 1_555 1_555 1_555 yes N5 C22 H21 118(1) 1_555 1_555 1_555 no C23 C22 H21 118(1) 1_555 1_555 1_555 no C22 C23 C24 118(1) 1_555 1_555 1_555 yes C22 C23 H22 121(1) 1_555 1_555 1_555 no C24 C23 H22 120(1) 1_555 1_555 1_555 no C23 C24 C25 118(1) 1_555 1_555 1_555 yes C23 C24 H23 122(1) 1_555 1_555 1_555 no C25 C24 H23 119(1) 1_555 1_555 1_555 no C24 C25 C26 120(1) 1_555 1_555 1_555 yes C24 C25 H24 119(1) 1_555 1_555 1_555 no C26 C25 H24 119(1) 1_555 1_555 1_555 no N5 C26 C25 121(1) 1_555 1_555 1_555 yes N5 C26 C27 114(1) 1_555 1_555 1_555 yes C25 C26 C27 123(1) 1_555 1_555 1_555 yes N6 C27 C26 114(1) 1_555 1_555 1_555 yes N6 C27 C28 121(1) 1_555 1_555 1_555 yes C26 C27 C28 124(1) 1_555 1_555 1_555 yes C27 C28 C29 118(1) 1_555 1_555 1_555 yes C27 C28 H25 119(1) 1_555 1_555 1_555 no C29 C28 H25 121(1) 1_555 1_555 1_555 no C28 C29 C30 120(1) 1_555 1_555 1_555 yes C28 C29 H26 119(1) 1_555 1_555 1_555 no C30 C29 H26 120(1) 1_555 1_555 1_555 no C29 C30 C31 119(1) 1_555 1_555 1_555 yes C29 C30 H27 120(1) 1_555 1_555 1_555 no C31 C30 H27 120(1) 1_555 1_555 1_555 no N6 C31 C30 123(1) 1_555 1_555 1_555 yes N6 C31 H28 118(1) 1_555 1_555 1_555 no C30 C31 H28 118(1) 1_555 1_555 1_555 no N7 C32 C33 175(2) 1_555 1_555 1_555 yes C32 C33 H29 107(2) 1_555 1_555 1_555 no C32 C33 H30 108(2) 1_555 1_555 1_555 no C32 C33 H31 108(2) 1_555 1_555 1_555 no H29 C33 H30 109(2) 1_555 1_555 1_555 no H29 C33 H31 111(2) 1_555 1_555 1_555 no H30 C33 H31 110(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F1 C1 3.38(2) 1_555 3_654 ? F1 C3 3.56(3) 1_555 3_654 ? F1 O1 3.56(2) 1_555 3_654 ? F2 F4 3.19(2) 1_555 4_455 ? F2 C18 3.38(2) 1_555 1_555 ? F2 C19 3.40(2) 1_555 1_555 ? F2 C3 3.41(2) 1_555 3_654 ? F2 O1 3.57(2) 1_555 3_654 ? F3 C18 3.12(2) 1_555 1_555 ? F3 C19 3.18(2) 1_555 4_555 ? F3 C17 3.28(2) 1_555 1_555 ? F3 C9 3.40(2) 1_555 1_555 ? F3 C16 3.53(2) 1_555 1_555 ? F4 C19 3.41(2) 1_555 4_555 ? F4 C8 3.54(2) 1_555 1_555 ? F4 C29 3.55(2) 1_555 3_654 ? F5 C33 3.30(3) 1_555 1_554 ? F5 C3 3.43(3) 1_555 3_654 ? F5 C28 3.50(2) 1_555 2_654 ? F6 C25 3.27(2) 1_555 2_654 ? F6 C9 3.47(3) 1_555 1_555 ? F6 C28 3.56(2) 1_555 2_654 ? F7 C4 3.20(1) 1_555 2_754 ? F7 C12 3.29(1) 1_555 2_754 ? F7 C5 3.41(1) 1_555 2_754 ? F7 N2 3.41(1) 1_555 2_754 ? F7 C15 3.42(2) 1_555 3_644 ? F7 C14 3.48(2) 1_555 3_644 ? F8 C3 3.22(2) 1_555 1_555 ? F8 C33 3.45(2) 1_555 3_644 ? F8 C30 3.45(2) 1_555 1_555 ? F8 C31 3.54(1) 1_555 1_555 ? F9 C30 3.39(2) 1_555 1_555 ? F9 C31 3.44(1) 1_555 1_555 ? F9 C24 3.52(2) 1_555 2_654 ? F10 C4 3.56(1) 1_555 2_754 ? F11 C10 3.51(2) 1_555 1_555 ? F11 C7 3.53(2) 1_555 1_555 ? F11 C31 3.57(1) 1_555 1_555 ? F12 C1 3.43(1) 1_555 2_754 ? F13 C12 3.39(1) 1_555 2_754 ? F13 C33 3.45(3) 1_555 2_754 ? F13 C1 3.47(1) 1_555 2_754 ? F14 C33 3.41(3) 1_555 2_754 ? F14 C13 3.43(2) 1_555 2_754 ? F14 C12 3.54(1) 1_555 2_754 ? F15 C22 3.18(1) 1_555 3_644 ? F15 C23 3.22(2) 1_555 3_644 ? F15 C13 3.43(2) 1_555 2_754 ? F16 C22 3.43(2) 1_555 3_644 ? F16 C33 3.45(2) 1_555 3_644 ? F16 C13 3.48(2) 1_555 3_644 ? F16 C14 3.57(2) 1_555 3_644 ? F16 C12 3.57(1) 1_555 3_644 ? F17 C13 3.32(2) 1_555 3_644 ? F17 C33 3.39(2) 1_555 3_644 ? F17 C30 3.40(2) 1_555 1_555 ? F17 C14 3.50(2) 1_555 3_644 ? O1 C8 3.24(2) 1_555 2_755 ? O1 C7 3.58(2) 1_555 2_755 ? N7 C21 3.30(2) 1_555 2_655 ? N7 C6 3.43(3) 1_555 2_755 ? N7 C20 3.52(3) 1_555 2_655 ?