Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Sugimoto, Hideki' 'Miyake, Hiroyuki' 'Tsukube, Hiroshi' _publ_contact_author_name 'Dr Hideki Sugimoto' _publ_contact_author_address ; Department of Chemistry Osaka City University Graduate School of Science Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email ' sugimoto@sci.osaka-cu.ac.jp' _publ_contact_author_fax ' +81-6-6605-2522 ' _publ_contact_author_phone ' +81-6-6605-2548 ' _publ_requested_journal ' J. Chem. Soc. Dalton Trans.' _publ_requested_category ' Coordination Chemistry' _publ_requested_coeditor_name ? #--------------------------------------------------------------------------- #-- # TITLE AND AUTHOR LIST _publ_section_title ; Receptor Versatility of Tris(2-pyridiniummethyl)amine in Anion Binding through Hydrogen Bonding ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; data_tpaP3F18 _database_code_CSD 184348 _audit_creation_date 'Thu Jul 11 21:01:16 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H21 F12 N4 O6 P S2 ' _chemical_formula_moiety 'C20 H21 F12 N4 O6 P S2 ' _chemical_formula_weight 736.48 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.3822(9) _cell_length_b 12.2476(8) _cell_length_c 20.431(1) _cell_angle_alpha 90 _cell_angle_beta 98.580(3) _cell_angle_gamma 90 _cell_volume 3063.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 27999 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.934 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 18645 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7006 _reflns_number_gt 5409 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2656 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5409 _refine_ls_number_parameters 407 _refine_ls_goodness_of_fit_ref 1.880 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0030 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0096 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 1.14 _refine_diff_density_min -0.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.70747(7) 0.01482(7) 0.26966(5) 0.0650(3) Uani 1.00 d . . . S(2) S 0.7402(1) -0.50045(8) -0.15545(6) 0.0820(3) Uani 1.00 d . . . P(1) P 0.72917(7) -0.08643(7) 0.01040(4) 0.0617(3) Uani 1.00 d . . . F(1) F 0.8260(3) 0.0462(3) 0.3841(2) 0.119(1) Uani 1.00 d . . . F(2) F 0.7253(2) 0.1803(2) 0.3496(2) 0.0955(8) Uani 1.00 d . . . F(3) F 0.6521(3) 0.0393(3) 0.3864(2) 0.115(1) Uani 1.00 d . . . F(4) F 0.6454(5) -0.3193(3) -0.1329(3) 0.195(3) Uani 1.00 d . . . F(5) F 0.6563(6) -0.4350(4) -0.0543(3) 0.189(2) Uani 1.00 d . . . F(6) F 0.5385(4) -0.4605(4) -0.1459(4) 0.185(2) Uani 1.00 d . . . F(7) F 0.7386(3) -0.0635(2) 0.0879(1) 0.0999(8) Uani 1.00 d . . . F(8) F 0.8547(2) -0.1161(3) 0.0205(2) 0.118(1) Uani 1.00 d . . . F(9) F 0.6937(3) -0.2093(2) 0.0214(1) 0.0994(8) Uani 1.00 d . . . F(10) F 0.7220(3) -0.1055(2) -0.0674(1) 0.0930(7) Uani 1.00 d . . . F(11) F 0.6050(2) -0.0530(3) 0.0010(2) 0.1120(10) Uani 1.00 d . . . F(12) F 0.7584(3) 0.0386(2) -0.0018(2) 0.1038(9) Uani 1.00 d . . . O(1) O 0.7934(2) 0.0645(2) 0.2384(1) 0.0705(6) Uani 1.00 d . . . O(2) O 0.6011(3) 0.0534(3) 0.2424(2) 0.0987(10) Uani 1.00 d . . . O(3) O 0.7222(3) -0.1009(2) 0.2793(2) 0.101(1) Uani 1.00 d . . . O(4) O 0.8405(4) -0.4545(5) -0.1279(3) 0.170(2) Uani 1.00 d . . . O(5) O 0.7147(4) -0.4740(3) -0.2240(2) 0.111(1) Uani 1.00 d . . . O(6) O 0.7176(3) -0.6103(3) -0.1384(2) 0.105(1) Uani 1.00 d . . . N(1) N 0.9760(2) 0.1753(2) 0.1570(1) 0.0486(5) Uani 1.00 d . . . N(2) N 0.7456(2) 0.2040(2) 0.1247(1) 0.0602(6) Uani 1.00 d . . . N(3) N 0.9543(2) -0.0518(2) 0.1837(2) 0.0588(6) Uani 1.00 d . . . N(4) N 0.9809(3) 0.2392(3) 0.2989(2) 0.0735(8) Uani 1.00 d . . . C(1) C 0.6381(3) 0.1932(3) 0.1034(2) 0.0710(8) Uani 1.00 d . . . C(2) C 0.5940(3) 0.2421(3) 0.0450(3) 0.083(1) Uani 1.00 d . . . C(3) C 0.6606(4) 0.2996(3) 0.0100(2) 0.083(1) Uani 1.00 d . . . C(4) C 0.7709(3) 0.3088(3) 0.0328(2) 0.0680(8) Uani 1.00 d . . . C(5) C 0.8140(3) 0.2610(2) 0.0921(2) 0.0541(6) Uani 1.00 d . . . C(6) C 0.9312(3) 0.2742(2) 0.1223(2) 0.0581(7) Uani 1.00 d . . . C(7) C 0.9581(3) -0.1541(3) 0.2096(2) 0.0767(10) Uani 1.00 d . . . C(8) C 1.0276(4) -0.2287(3) 0.1906(3) 0.086(1) Uani 1.00 d . . . C(9) C 1.0929(4) -0.1995(3) 0.1451(3) 0.085(1) Uani 1.00 d . . . C(10) C 1.0877(3) -0.0953(3) 0.1184(2) 0.0697(9) Uani 1.00 d . . . C(11) C 1.0151(2) -0.0205(2) 0.1388(2) 0.0551(6) Uani 1.00 d . . . C(12) C 0.9976(3) 0.0915(3) 0.1088(2) 0.0602(7) Uani 1.00 d . . . C(13) C 0.9691(3) 0.2991(3) 0.3547(2) 0.0722(9) Uani 1.00 d . . . C(14) C 1.0345(3) 0.3879(3) 0.3716(2) 0.0713(8) Uani 1.00 d . . . C(15) C 1.1087(3) 0.4166(3) 0.3322(2) 0.0722(9) Uani 1.00 d . . . C(16) C 1.1189(2) 0.3573(2) 0.2776(2) 0.0539(6) Uani 1.00 d . . . C(17) C 1.0571(2) 0.2671(2) 0.2600(2) 0.0516(6) Uani 1.00 d . . . C(18) C 1.0784(2) 0.2028(2) 0.2008(2) 0.0553(6) Uani 1.00 d . . . C(19) C 0.7298(3) 0.0721(3) 0.3524(2) 0.0732(9) Uani 1.00 d . . . C(20) C 0.6425(8) -0.4224(5) -0.1173(4) 0.126(2) Uani 1.00 d . . . H(1) H 0.7741 0.1702 0.1651 0.0716 Uiso 1.00 calc . . . H(2) H 0.9049 -0.0018 0.1982 0.0682 Uiso 1.00 calc . . . H(3) H 0.9370 0.1775 0.2880 0.0899 Uiso 1.00 calc . . . H(4) H 0.5940 0.1512 0.1274 0.0844 Uiso 1.00 calc . . . H(5) H 0.5174 0.2369 0.0299 0.0967 Uiso 1.00 calc . . . H(6) H 0.6306 0.3349 -0.0305 0.1005 Uiso 1.00 calc . . . H(7) H 0.8173 0.3469 0.0075 0.0812 Uiso 1.00 calc . . . H(8) H 0.9728 0.2905 0.0877 0.0677 Uiso 1.00 calc . . . H(9) H 0.9363 0.3331 0.1525 0.0677 Uiso 1.00 calc . . . H(10) H 0.9128 -0.1711 0.2412 0.0887 Uiso 1.00 calc . . . H(11) H 1.0285 -0.3017 0.2079 0.0994 Uiso 1.00 calc . . . H(12) H 1.1420 -0.2512 0.1319 0.1015 Uiso 1.00 calc . . . H(13) H 1.1332 -0.0749 0.0869 0.0820 Uiso 1.00 calc . . . H(14) H 1.0594 0.1116 0.0902 0.0706 Uiso 1.00 calc . . . H(15) H 0.9350 0.0882 0.0751 0.0706 Uiso 1.00 calc . . . H(16) H 0.9153 0.2777 0.3799 0.0851 Uiso 1.00 calc . . . H(17) H 1.0262 0.4295 0.4095 0.0867 Uiso 1.00 calc . . . H(18) H 1.1561 0.4771 0.3431 0.0858 Uiso 1.00 calc . . . H(19) H 1.1697 0.3803 0.2500 0.0594 Uiso 1.00 calc . . . H(20) H 1.1238 0.2442 0.1767 0.0656 Uiso 1.00 calc . . . H(21) H 1.1148 0.1368 0.2158 0.0656 Uiso 1.00 calc . . . 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 S(1) 0.0671(5) 0.0623(5) 0.0727(5) -0.0127(3) 0.0330(4) -0.0049(4) S(2) 0.0922(7) 0.0697(6) 0.0864(7) -0.0051(4) 0.0206(5) 0.0035(5) P(1) 0.0614(5) 0.0679(5) 0.0568(5) -0.0053(3) 0.0124(4) 0.0033(4) F(1) 0.110(2) 0.151(3) 0.088(2) 0.025(2) -0.004(2) 0.001(2) F(2) 0.107(2) 0.075(1) 0.106(2) -0.006(1) 0.018(1) -0.025(1) F(3) 0.143(3) 0.123(2) 0.096(2) -0.023(2) 0.074(2) -0.011(2) F(4) 0.319(7) 0.074(2) 0.209(5) 0.032(3) 0.095(5) -0.005(2) F(5) 0.313(8) 0.144(4) 0.132(4) 0.007(4) 0.109(4) -0.015(3) F(6) 0.116(3) 0.199(5) 0.256(7) 0.007(3) 0.075(4) 0.004(4) F(7) 0.121(2) 0.119(2) 0.063(1) -0.009(2) 0.026(1) -0.008(1) F(8) 0.069(1) 0.178(3) 0.107(2) 0.021(2) 0.013(1) -0.013(2) F(9) 0.133(2) 0.076(1) 0.088(2) -0.019(1) 0.013(2) 0.015(1) F(10) 0.132(2) 0.090(1) 0.058(1) -0.009(1) 0.013(1) -0.002(1) F(11) 0.073(2) 0.132(2) 0.132(3) 0.020(1) 0.020(2) 0.033(2) F(12) 0.136(2) 0.077(2) 0.106(2) -0.028(1) 0.045(2) -0.005(1) O(1) 0.074(1) 0.065(1) 0.081(2) -0.0034(10) 0.041(1) 0.004(1) O(2) 0.068(2) 0.134(3) 0.094(2) -0.010(2) 0.014(1) -0.020(2) O(3) 0.141(3) 0.060(1) 0.117(3) -0.021(2) 0.066(2) -0.008(1) O(4) 0.110(3) 0.219(5) 0.176(5) -0.071(4) 0.000(3) 0.021(4) O(5) 0.122(3) 0.128(3) 0.086(2) 0.001(2) 0.029(2) 0.011(2) O(6) 0.116(3) 0.071(2) 0.135(3) 0.014(2) 0.041(2) 0.011(2) N(1) 0.050(1) 0.048(1) 0.050(1) -0.0021(8) 0.0160(9) -0.0038(9) N(2) 0.064(1) 0.061(1) 0.057(1) 0.003(1) 0.012(1) -0.002(1) N(3) 0.056(1) 0.051(1) 0.073(2) 0.0002(9) 0.022(1) -0.004(1) N(4) 0.072(2) 0.077(2) 0.075(2) -0.016(1) 0.023(1) -0.012(1) C(1) 0.069(2) 0.069(2) 0.078(2) -0.008(1) 0.021(2) -0.008(2) C(2) 0.066(2) 0.079(2) 0.099(3) 0.002(2) -0.007(2) -0.010(2) C(3) 0.094(3) 0.072(2) 0.075(2) -0.002(2) -0.012(2) 0.013(2) C(4) 0.082(2) 0.062(2) 0.059(2) -0.007(1) 0.008(2) 0.006(1) C(5) 0.064(2) 0.046(1) 0.054(1) 0.001(1) 0.011(1) -0.003(1) C(6) 0.062(2) 0.052(1) 0.062(2) -0.002(1) 0.016(1) 0.003(1) C(7) 0.071(2) 0.060(2) 0.103(3) -0.011(1) 0.025(2) 0.005(2) C(8) 0.091(3) 0.049(2) 0.119(4) 0.001(2) 0.022(3) -0.002(2) C(9) 0.077(2) 0.059(2) 0.121(4) 0.014(2) 0.021(2) -0.018(2) C(10) 0.065(2) 0.066(2) 0.083(2) 0.011(1) 0.026(2) -0.015(2) C(11) 0.052(1) 0.054(1) 0.061(2) 0.002(1) 0.013(1) -0.012(1) C(12) 0.071(2) 0.059(2) 0.055(2) 0.007(1) 0.024(1) -0.007(1) C(13) 0.074(2) 0.083(2) 0.063(2) -0.009(2) 0.022(2) -0.007(2) C(14) 0.079(2) 0.076(2) 0.058(2) 0.003(2) 0.006(2) -0.015(2) C(15) 0.076(2) 0.062(2) 0.077(2) -0.013(1) 0.006(2) -0.014(2) C(16) 0.052(1) 0.052(1) 0.058(2) -0.013(1) 0.012(1) -0.004(1) C(17) 0.047(1) 0.049(1) 0.058(1) -0.0033(10) 0.007(1) 0.000(1) C(18) 0.046(1) 0.058(1) 0.065(2) -0.002(1) 0.018(1) -0.003(1) C(19) 0.075(2) 0.078(2) 0.071(2) -0.001(2) 0.024(2) -0.002(2) C(20) 0.193(8) 0.085(3) 0.115(4) 0.006(4) 0.065(5) -0.010(3) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 S(1) O(1) 1.453(3) . . yes S(1) O(2) 1.432(3) . . yes S(1) O(3) 1.439(3) . . yes S(1) C(19) 1.812(4) . . yes S(2) O(4) 1.403(6) . . yes S(2) O(5) 1.427(4) . . yes S(2) O(6) 1.427(3) . . yes S(2) C(20) 1.807(9) . . yes P(1) F(7) 1.596(3) . . yes P(1) F(8) 1.579(3) . . yes P(1) F(9) 1.593(3) . . yes P(1) F(10) 1.596(3) . . yes P(1) F(11) 1.575(3) . . yes P(1) F(12) 1.602(3) . . yes F(1) F(2) 2.118(4) . . yes F(1) F(3) 2.162(5) . . yes F(1) C(19) 1.307(5) . . yes F(2) F(3) 2.139(4) . . yes F(2) C(19) 1.327(5) . . yes F(3) C(19) 1.331(6) . . yes F(4) F(5) 2.131(7) . . yes F(4) F(6) 2.170(7) . . yes F(4) C(20) 1.305(7) . . yes F(5) F(6) 2.217(9) . . yes F(5) C(20) 1.282(9) . . yes F(6) C(20) 1.41(1) . . yes F(7) F(8) 2.228(5) . . yes F(7) F(9) 2.263(4) . . yes F(7) F(11) 2.243(4) . . yes F(7) F(12) 2.262(4) . . yes F(8) F(9) 2.300(4) . . yes F(8) F(10) 2.250(4) . . yes F(8) F(12) 2.249(4) . . yes F(9) F(10) 2.285(4) . . yes F(9) F(11) 2.215(4) . . yes F(10) F(11) 2.252(5) . . yes F(10) F(12) 2.222(4) . . yes F(11) F(12) 2.214(4) . . yes O(1) O(2) 2.398(4) . . yes O(4) O(5) 2.330(7) . . yes N(1) C(6) 1.469(4) . . yes N(1) C(12) 1.474(4) . . yes N(1) C(18) 1.477(3) . . yes N(2) C(1) 1.345(4) . . yes N(2) C(2) 2.341(5) . . yes N(2) C(4) 2.333(5) . . yes N(2) C(5) 1.347(4) . . yes N(3) C(7) 1.358(4) . . yes N(3) C(8) 2.345(4) . . yes N(3) C(10) 2.336(5) . . yes N(3) C(11) 1.327(4) . . yes N(4) C(13) 1.382(5) . . yes N(4) C(14) 2.381(5) . . yes N(4) C(16) 2.329(4) . . yes N(4) C(17) 1.365(5) . . yes C(1) C(2) 1.372(6) . . yes C(1) C(3) 2.362(6) . . yes C(1) C(5) 2.374(5) . . yes C(2) C(3) 1.367(7) . . yes C(2) C(4) 2.386(6) . . yes C(3) C(4) 1.380(6) . . yes C(3) C(5) 2.386(5) . . yes C(4) C(5) 1.378(4) . . yes C(5) C(6) 1.500(4) . . yes C(7) C(8) 1.351(6) . . yes C(7) C(9) 2.343(7) . . yes C(7) C(11) 2.360(5) . . yes C(8) C(9) 1.368(7) . . yes C(8) C(10) 2.394(6) . . yes C(9) C(10) 1.385(5) . . yes C(9) C(11) 2.390(5) . . yes C(10) C(11) 1.390(5) . . yes C(11) C(12) 1.506(4) . . yes C(13) C(14) 1.368(5) . . yes C(13) C(15) 2.347(6) . . yes C(13) C(17) 2.391(5) . . yes C(14) C(15) 1.356(6) . . yes C(14) C(16) 2.351(5) . . yes C(15) C(16) 1.353(5) . . yes C(15) C(17) 2.378(5) . . yes C(16) C(17) 1.361(4) . . yes C(17) C(18) 1.500(4) . . 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 O(1) S(1) O(2) 112.4(2) . . . yes O(1) S(1) O(3) 112.8(2) . . . yes O(1) S(1) C(19) 103.1(2) . . . yes O(2) S(1) O(3) 118.0(2) . . . yes O(2) S(1) C(19) 103.8(2) . . . yes O(3) S(1) C(19) 104.8(2) . . . yes O(4) S(2) O(5) 110.8(3) . . . yes O(4) S(2) O(6) 118.3(3) . . . yes O(4) S(2) C(20) 102.9(4) . . . yes O(5) S(2) O(6) 115.5(2) . . . yes O(5) S(2) C(20) 103.9(3) . . . yes O(6) S(2) C(20) 103.0(3) . . . yes F(7) P(1) F(8) 89.2(2) . . . yes F(7) P(1) F(9) 90.5(2) . . . yes F(7) P(1) F(10) 178.0(2) . . . yes F(7) P(1) F(11) 90.0(2) . . . yes F(7) P(1) F(12) 90.0(2) . . . yes F(8) P(1) F(9) 92.9(2) . . . yes F(8) P(1) F(10) 90.3(2) . . . yes F(8) P(1) F(11) 178.1(2) . . . yes F(8) P(1) F(12) 90.0(2) . . . yes F(9) P(1) F(10) 91.5(1) . . . yes F(9) P(1) F(11) 88.7(2) . . . yes F(9) P(1) F(12) 177.1(2) . . . yes F(10) P(1) F(11) 90.5(2) . . . yes F(10) P(1) F(12) 88.0(2) . . . yes F(11) P(1) F(12) 88.4(2) . . . yes C(6) N(1) C(12) 110.2(2) . . . yes C(6) N(1) C(18) 109.4(2) . . . yes C(12) N(1) C(18) 109.8(2) . . . yes C(1) N(2) C(5) 123.8(3) . . . yes C(7) N(3) C(11) 123.0(3) . . . yes C(13) N(4) C(17) 121.0(3) . . . yes N(2) C(1) C(2) 119.0(4) . . . yes C(1) C(2) C(3) 119.2(4) . . . yes C(2) C(3) C(4) 120.6(4) . . . yes C(3) C(4) C(5) 119.7(4) . . . yes N(2) C(5) C(4) 117.7(3) . . . yes N(2) C(5) C(6) 119.5(3) . . . yes C(4) C(5) C(6) 122.7(3) . . . yes N(1) C(6) C(5) 112.5(2) . . . yes N(3) C(7) C(8) 119.9(4) . . . yes C(7) C(8) C(9) 119.0(4) . . . yes C(8) C(9) C(10) 120.7(4) . . . yes C(9) C(10) C(11) 118.8(4) . . . yes N(3) C(11) C(10) 118.5(3) . . . yes N(3) C(11) C(12) 118.8(3) . . . yes C(10) C(11) C(12) 122.6(3) . . . yes N(1) C(12) C(11) 113.1(3) . . . yes N(4) C(13) C(14) 119.9(4) . . . yes C(13) C(14) C(15) 119.0(4) . . . yes C(14) C(15) C(16) 120.4(3) . . . yes C(15) C(16) C(17) 122.3(3) . . . yes N(4) C(17) C(16) 117.4(3) . . . yes N(4) C(17) C(18) 124.0(3) . . . yes C(16) C(17) C(18) 118.6(3) . . . yes N(1) C(18) C(17) 111.7(2) . . . yes S(1) C(19) F(1) 111.7(3) . . . yes S(1) C(19) F(2) 110.3(3) . . . yes S(1) C(19) F(3) 110.4(3) . . . yes F(1) C(19) F(2) 107.0(3) . . . yes F(1) C(19) F(3) 110.1(4) . . . yes F(2) C(19) F(3) 107.1(4) . . . yes S(2) C(20) F(4) 111.3(6) . . . yes S(2) C(20) F(5) 111.8(6) . . . yes S(2) C(20) F(6) 105.9(5) . . . yes F(4) C(20) F(5) 110.9(6) . . . yes F(4) C(20) F(6) 106.0(6) . . . yes F(5) C(20) F(6) 110.6(8) . . . yes #------------------------------------------------------------------------------ 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 F(1) F(6) 2.981(7) . 4_545 ? F(1) F(5) 3.459(6) . 2_655 ? F(1) F(9) 3.591(4) . 2_655 ? F(2) F(9) 2.999(4) . 2_655 ? F(2) C(7) 3.148(4) . 2_655 ? F(2) C(8) 3.310(5) . 2_655 ? F(2) F(7) 3.392(4) . 2_655 ? F(3) C(4) 3.337(5) . 2_645 ? F(3) C(6) 3.403(4) . 2_645 ? F(3) C(5) 3.453(4) . 2_645 ? F(5) C(3) 3.502(6) . 1_545 ? F(6) C(7) 3.287(8) . 4_444 ? F(6) N(3) 3.485(8) . 4_444 ? F(7) C(13) 3.423(5) . 2_645 ? F(8) C(12) 3.445(5) . 3_755 ? F(9) C(13) 3.464(5) . 2_645 ? F(10) C(15) 3.266(4) . 4_454 ? F(11) F(11) 2.901(6) . 3_655 ? F(11) C(14) 3.339(5) . 4_454 ? F(11) C(14) 3.409(5) . 2_645 ? F(11) C(2) 3.411(5) . 3_655 ? F(12) C(10) 3.337(5) . 3_755 ? O(2) C(15) 3.271(5) . 2_645 ? O(2) C(14) 3.345(5) . 2_645 ? O(2) C(8) 3.491(6) . 2_655 ? O(3) N(2) 3.080(4) . 2_645 ? O(3) C(5) 3.211(5) . 2_645 ? O(3) C(6) 3.335(5) . 2_645 ? O(3) N(4) 3.393(5) . 2_645 ? O(3) C(13) 3.560(5) . 2_645 ? O(4) C(16) 3.389(8) . 3_755 ? O(4) C(6) 3.575(7) . 3_755 ? O(5) C(16) 2.856(5) . 3_755 ? O(5) C(15) 3.406(6) . 3_755 ? O(5) C(11) 3.449(5) . 4_444 ? O(5) C(10) 3.471(5) . 4_444 ? O(5) N(3) 3.499(5) . 4_444 ? O(5) C(18) 3.505(5) . 4_444 ? O(5) C(9) 3.569(6) . 4_444 ? O(6) C(17) 3.273(4) . 4_444 ? O(6) C(9) 3.324(6) . 3_745 ? O(6) C(3) 3.398(6) . 1_545 ? O(6) N(4) 3.407(5) . 4_444 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N(2) H(1) O(1) . . . 0.944 1.967 2.874(3) 160.354 no N(2) H(1) N(1) . . . 0.944 2.531 2.852(3) 100.101 no N(3) H(2) F(7) . . . 0.943 2.916 3.070(3) 90.341 no N(3) H(2) O(1) . . . 0.943 1.893 2.813(3) 164.547 no N(3) H(2) N(1) . . . 0.943 2.532 2.855(3) 100.265 no N(4) H(3) F(2) . . . 0.939 3.073 3.547(4) 113.036 no N(4) H(3) O(1) . . . 0.939 2.359 3.262(3) 161.278 no N(4) H(3) N(1) . . . 0.939 2.789 2.995(4) 93.414 no #------------------------------------------------------------------------------ #===END data_[tpaBrH3](PF6)2 _database_code_CSD 184349 #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C38 H50 Br2 F24 N9 O P4 ' _chemical_formula_moiety 'C38 H50 Br2 F24 N9 O P4 ' _chemical_formula_weight 1388.54 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 47.164(6) _cell_length_b 9.366(7) _cell_length_c 24.667(8) _cell_angle_alpha 90 _cell_angle_beta 90.25(2) _cell_angle_gamma 90 _cell_volume 10895(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_reflns_number 13424 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.44 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12492 _reflns_number_gt 5824 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2287 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5824 _refine_ls_number_parameters 698 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 1.34 _refine_diff_density_min -0.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.12493(2) 0.40477(8) 0.09155(3) 0.0387(2) Uani 1.00 d . . . Br(2) Br 0.12381(2) -0.09717(9) 0.09510(3) 0.0392(2) Uani 1.00 d . . . P(1) P 0.23404(4) 0.5255(3) 0.08154(9) 0.0530(6) Uani 1.00 d . . . P(2) P 0.08016(5) 0.4809(2) 0.40229(8) 0.0451(5) Uani 1.00 d . . . P(3) P 0.01415(5) 0.1093(3) 0.11485(9) 0.0585(6) Uani 1.00 d . . . P(4) P 0.15981(5) 0.0131(3) 0.29573(8) 0.0484(5) Uani 1.00 d . . . F(1) F 0.2362(2) 0.587(1) 0.1386(3) 0.175(5) Uani 1.00 d . . . F(2) F 0.2022(1) 0.488(1) 0.0842(4) 0.158(4) Uani 1.00 d . . . F(3) F 0.2375(3) 0.379(1) 0.0984(9) 0.34(1) Uani 1.00 d . . . F(4) F 0.2303(2) 0.480(1) 0.0212(3) 0.190(6) Uani 1.00 d . . . F(5) F 0.2658(2) 0.549(1) 0.0781(4) 0.175(5) Uani 1.00 d . . . F(6) F 0.2291(5) 0.667(1) 0.0639(7) 0.35(1) Uani 1.00 d . . . F(7) F 0.0709(1) 0.3224(5) 0.4148(2) 0.067(1) Uani 1.00 d . . . F(8) F 0.0943(1) 0.4966(6) 0.4607(2) 0.077(2) Uani 1.00 d . . . F(9) F 0.0516(1) 0.5370(7) 0.4257(3) 0.084(2) Uani 1.00 d . . . F(10) F 0.0894(1) 0.6409(6) 0.3885(2) 0.076(2) Uani 1.00 d . . . F(11) F 0.0669(1) 0.4683(6) 0.3428(2) 0.085(2) Uani 1.00 d . . . F(12) F 0.1095(1) 0.4249(8) 0.3793(3) 0.103(2) Uani 1.00 d . . . F(13) F 0.0289(2) 0.190(2) 0.1584(5) 0.264(9) Uani 1.00 d . . . F(14) F -0.0143(1) 0.1942(10) 0.1260(3) 0.123(3) Uani 1.00 d . . . F(15) F 0.0222(2) 0.2274(9) 0.0737(4) 0.146(4) Uani 1.00 d . . . F(16) F 0.0003(2) 0.034(1) 0.0672(5) 0.207(6) Uani 1.00 d . . . F(17) F 0.0422(1) 0.0222(7) 0.1033(2) 0.077(2) Uani 1.00 d . . . F(18) F 0.0069(3) 0.002(2) 0.1574(7) 0.33(1) Uani 1.00 d . . . F(19) F 0.1457(2) 0.149(1) 0.3178(5) 0.196(5) Uani 1.00 d . . . F(20) F 0.1344(2) -0.072(1) 0.3188(3) 0.164(4) Uani 1.00 d . . . F(21) F 0.1758(2) 0.0067(10) 0.3514(2) 0.133(3) Uani 1.00 d . . . F(22) F 0.1748(2) -0.1250(9) 0.2778(4) 0.153(4) Uani 1.00 d . . . F(23) F 0.1446(2) 0.003(1) 0.2394(3) 0.142(3) Uani 1.00 d . . . F(24) F 0.1849(2) 0.0993(9) 0.2736(3) 0.129(3) Uani 1.00 d . . . O(1) O 0.5000 0.085(3) 0.7500 0.2398(1) Uiso 1.00 d S . . N(1) N 0.1611(1) 0.2199(6) -0.0240(2) 0.032(1) Uani 1.00 d . . . N(2) N 0.1587(1) 0.5242(7) -0.0197(2) 0.041(1) Uani 1.00 d . . . N(3) N 0.1791(1) 0.1813(7) 0.0859(2) 0.039(1) Uani 1.00 d . . . N(4) N 0.1023(1) 0.1785(6) -0.0004(2) 0.036(1) Uani 1.00 d . . . N(5) N 0.0794(1) -0.2808(6) 0.2007(2) 0.032(1) Uani 1.00 d . . . N(6) N 0.0683(1) -0.3023(7) 0.0860(2) 0.039(1) Uani 1.00 d . . . N(7) N 0.1392(1) -0.3205(6) 0.1924(2) 0.038(1) Uani 1.00 d . . . N(8) N 0.0830(1) 0.0228(7) 0.1976(2) 0.037(1) Uani 1.00 d . . . N(9) N 0.2685(2) 0.100(1) 0.7060(4) 0.084(3) Uani 1.00 d . . . C(1) C 0.1656(2) 0.6600(9) -0.0083(3) 0.050(2) Uani 1.00 d . . . C(2) C 0.1829(2) 0.7356(9) -0.0422(4) 0.055(2) Uani 1.00 d . . . C(3) C 0.1930(2) 0.6711(9) -0.0881(4) 0.053(2) Uani 1.00 d . . . C(4) C 0.1859(2) 0.5289(9) -0.0994(3) 0.043(2) Uani 1.00 d . . . C(5) C 0.1682(1) 0.4568(8) -0.0649(3) 0.034(1) Uani 1.00 d . . . C(6) C 0.1588(2) 0.3055(8) -0.0736(3) 0.037(2) Uani 1.00 d . . . C(7) C 0.1812(2) 0.1361(9) 0.1368(3) 0.045(2) Uani 1.00 d . . . C(8) C 0.2015(2) 0.037(1) 0.1494(3) 0.055(2) Uani 1.00 d . . . C(9) C 0.2185(2) -0.0182(10) 0.1096(3) 0.053(2) Uani 1.00 d . . . C(10) C 0.2150(2) 0.0304(9) 0.0570(3) 0.045(2) Uani 1.00 d . . . C(11) C 0.1952(1) 0.1333(7) 0.0448(3) 0.035(2) Uani 1.00 d . . . C(12) C 0.1911(2) 0.1962(8) -0.0105(3) 0.039(2) Uani 1.00 d . . . C(13) C 0.0744(2) 0.1908(9) 0.0031(3) 0.041(2) Uani 1.00 d . . . C(14) C 0.0571(2) 0.1097(9) -0.0310(3) 0.044(2) Uani 1.00 d . . . C(15) C 0.0705(2) 0.0169(9) -0.0668(3) 0.049(2) Uani 1.00 d . . . C(16) C 0.0991(2) 0.0058(8) -0.0694(3) 0.043(2) Uani 1.00 d . . . C(17) C 0.1157(1) 0.0886(7) -0.0352(2) 0.031(1) Uani 1.00 d . . . C(18) C 0.1473(2) 0.0800(7) -0.0325(3) 0.034(1) Uani 1.00 d . . . C(19) C 0.0577(2) -0.2687(9) 0.0371(3) 0.048(2) Uani 1.00 d . . . C(20) C 0.0316(2) -0.312(1) 0.0233(3) 0.058(2) Uani 1.00 d . . . C(21) C 0.0161(2) -0.391(1) 0.0581(4) 0.063(3) Uani 1.00 d . . . C(22) C 0.0277(2) -0.428(1) 0.1088(3) 0.055(2) Uani 1.00 d . . . C(23) C 0.0544(2) -0.3835(7) 0.1223(3) 0.036(2) Uani 1.00 d . . . C(24) C 0.0691(2) -0.4124(8) 0.1749(3) 0.039(2) Uani 1.00 d . . . C(25) C 0.1652(2) -0.3638(9) 0.1783(3) 0.045(2) Uani 1.00 d . . . C(26) C 0.1787(2) -0.4685(10) 0.2077(3) 0.050(2) Uani 1.00 d . . . C(27) C 0.1651(2) -0.5289(10) 0.2511(3) 0.052(2) Uani 1.00 d . . . C(28) C 0.1382(2) -0.4825(8) 0.2651(3) 0.040(2) Uani 1.00 d . . . C(29) C 0.1252(1) -0.3751(7) 0.2354(3) 0.035(2) Uani 1.00 d . . . C(30) C 0.0969(2) -0.3123(8) 0.2487(3) 0.039(2) Uani 1.00 d . . . C(31) C 0.0920(2) 0.1585(9) 0.2046(3) 0.045(2) Uani 1.00 d . . . C(32) C 0.0825(2) 0.2335(8) 0.2483(3) 0.050(2) Uani 1.00 d . . . C(33) C 0.0640(2) 0.1706(9) 0.2847(3) 0.052(2) Uani 1.00 d . . . C(34) C 0.0553(2) 0.0318(9) 0.2753(3) 0.046(2) Uani 1.00 d . . . C(35) C 0.0648(1) -0.0435(8) 0.2322(3) 0.034(1) Uani 1.00 d . . . C(36) C 0.0555(1) -0.1903(8) 0.2175(3) 0.036(2) Uani 1.00 d . . . C(37) C 0.5000 -0.051(5) 0.7500 0.2423(2) Uiso 1.00 d S . . C(38) C 0.2396(3) 0.243(2) 0.7777(6) 0.113(5) Uani 1.00 d . . . C(39) C 0.2562(2) 0.163(1) 0.7372(5) 0.071(3) Uani 1.00 d . . . H(1) H 0.1931 0.4830 -0.1310 0.0516 Uiso 1.00 calc . . . H(2) H 0.2046 0.7232 -0.1117 0.0644 Uiso 1.00 calc . . . H(3) H 0.1876 0.8320 -0.0340 0.0676 Uiso 1.00 calc . . . H(4) H 0.1584 0.7031 0.0238 0.0587 Uiso 1.00 calc . . . H(5) H 0.1081 -0.0577 -0.0944 0.0495 Uiso 1.00 calc . . . H(6) H 0.0592 -0.0425 -0.0898 0.0594 Uiso 1.00 calc . . . H(7) H 0.0370 0.1185 -0.0298 0.0526 Uiso 1.00 calc . . . H(8) H 0.0662 0.2559 0.0281 0.0464 Uiso 1.00 calc . . . H(9) H 0.2264 -0.0088 0.0289 0.0508 Uiso 1.00 calc . . . H(10) H 0.2324 -0.0904 0.1178 0.0602 Uiso 1.00 calc . . . H(11) H 0.2039 0.0044 0.1860 0.0632 Uiso 1.00 calc . . . H(12) H 0.1690 0.1723 0.1639 0.0542 Uiso 1.00 calc . . . H(13) H 0.1745 -0.3225 0.1481 0.0513 Uiso 1.00 calc . . . H(14) H 0.1972 -0.4993 0.1976 0.0614 Uiso 1.00 calc . . . H(15) H 0.1741 -0.6023 0.2714 0.0595 Uiso 1.00 calc . . . H(16) H 0.1286 -0.5250 0.2949 0.0467 Uiso 1.00 calc . . . H(17) H 0.0424 -0.0100 0.2992 0.0550 Uiso 1.00 calc . . . H(18) H 0.0579 0.2201 0.3156 0.0615 Uiso 1.00 calc . . . H(19) H 0.0889 0.3287 0.2542 0.0582 Uiso 1.00 calc . . . H(20) H 0.1043 0.2011 0.1795 0.0521 Uiso 1.00 calc . . . H(21) H 0.0241 -0.2874 -0.0113 0.0700 Uiso 1.00 calc . . . H(22) H -0.0024 -0.4215 0.0485 0.0707 Uiso 1.00 calc . . . H(23) H 0.0171 -0.4864 0.1337 0.0633 Uiso 1.00 calc . . . H(24) H 0.0689 -0.2152 0.0122 0.0573 Uiso 1.00 calc . . . H(25) H 0.1708 0.2638 -0.1005 0.0432 Uiso 1.00 calc . . . H(26) H 0.1399 0.3049 -0.0860 0.0432 Uiso 1.00 calc . . . H(27) H 0.1543 0.0403 -0.0651 0.0395 Uiso 1.00 calc . . . H(28) H 0.1525 0.0191 -0.0029 0.0395 Uiso 1.00 calc . . . H(29) H 0.0850 -0.4730 0.1682 0.0461 Uiso 1.00 calc . . . H(30) H 0.0565 -0.4588 0.1988 0.0461 Uiso 1.00 calc . . . H(31) H 0.0424 -0.1840 0.1881 0.0414 Uiso 1.00 calc . . . H(32) H 0.0465 -0.2324 0.2477 0.0414 Uiso 1.00 calc . . . H(33) H 0.1993 0.1348 -0.0365 0.0458 Uiso 1.00 calc . . . H(34) H 0.2008 0.2867 -0.0116 0.0458 Uiso 1.00 calc . . . H(35) H 0.1002 -0.2261 0.2680 0.0478 Uiso 1.00 calc . . . H(36) H 0.0872 -0.3781 0.2711 0.0478 Uiso 1.00 calc . . . H(37) H 0.1472 0.4729 0.0049 0.0470 Uiso 1.00 calc . . . H(38) H 0.1652 0.2512 0.0779 0.0456 Uiso 1.00 calc . . . H(39) H 0.1137 0.2361 0.0229 0.0386 Uiso 1.00 calc . . . H(40) H 0.0865 -0.2668 0.0956 0.0454 Uiso 1.00 calc . . . H(41) H 0.1303 -0.2483 0.1711 0.0433 Uiso 1.00 calc . . . H(42) H 0.0896 -0.0280 0.1671 0.0444 Uiso 1.00 calc . . . 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 Br(1) 0.0386(4) 0.0422(4) 0.0354(4) 0.0008(4) 0.0051(3) -0.0096(3) Br(2) 0.0425(4) 0.0413(4) 0.0338(4) -0.0054(4) 0.0065(3) 0.0062(3) P(1) 0.041(1) 0.063(2) 0.055(1) -0.008(1) 0.0120(9) -0.009(1) P(2) 0.055(1) 0.045(1) 0.0355(10) -0.012(1) 0.0094(9) -0.0075(9) P(3) 0.037(1) 0.093(2) 0.046(1) 0.013(1) 0.0007(9) 0.009(1) P(4) 0.056(1) 0.055(1) 0.0346(10) -0.005(1) 0.0019(9) -0.0008(9) F(1) 0.115(6) 0.32(1) 0.086(5) -0.088(8) 0.043(4) -0.082(7) F(2) 0.065(4) 0.25(1) 0.162(7) -0.048(6) 0.039(4) -0.102(8) F(3) 0.30(2) 0.088(7) 0.63(3) -0.075(9) -0.30(2) 0.14(1) F(4) 0.128(6) 0.34(1) 0.104(6) -0.119(8) 0.062(5) -0.111(8) F(5) 0.069(4) 0.26(1) 0.190(9) -0.062(6) 0.047(5) -0.134(9) F(6) 0.61(3) 0.076(7) 0.35(2) 0.00(1) -0.33(2) 0.020(9) F(7) 0.102(4) 0.047(3) 0.052(3) -0.018(3) 0.009(3) 0.003(2) F(8) 0.088(4) 0.089(4) 0.055(3) -0.016(3) -0.020(3) -0.014(3) F(9) 0.059(3) 0.080(4) 0.113(5) 0.014(3) 0.028(3) 0.002(4) F(10) 0.112(5) 0.055(3) 0.060(3) -0.036(3) 0.011(3) -0.005(3) F(11) 0.147(5) 0.062(3) 0.045(3) -0.041(4) -0.021(3) 0.008(3) F(12) 0.094(5) 0.107(5) 0.109(5) 0.009(4) 0.057(4) -0.010(4) F(13) 0.21(1) 0.37(2) 0.21(1) 0.22(1) -0.162(9) -0.22(1) F(14) 0.062(4) 0.215(9) 0.092(4) 0.077(5) 0.022(3) 0.043(5) F(15) 0.120(6) 0.124(7) 0.195(8) 0.043(5) 0.095(6) 0.048(6) F(16) 0.128(7) 0.161(9) 0.33(1) 0.034(7) -0.145(9) -0.112(10) F(17) 0.065(3) 0.097(5) 0.069(3) 0.033(3) -0.009(3) -0.019(3) F(18) 0.24(1) 0.35(2) 0.40(2) 0.22(1) 0.25(1) 0.31(2) F(19) 0.170(9) 0.116(7) 0.30(1) 0.057(7) 0.060(9) -0.066(8) F(20) 0.162(7) 0.23(1) 0.097(5) -0.142(7) 0.060(5) -0.065(6) F(21) 0.140(6) 0.208(9) 0.050(3) -0.080(7) -0.017(4) 0.024(5) F(22) 0.136(7) 0.114(7) 0.208(10) 0.048(5) -0.027(7) -0.077(6) F(23) 0.119(6) 0.24(1) 0.064(4) -0.029(7) -0.033(4) 0.027(5) F(24) 0.155(7) 0.159(7) 0.072(4) -0.091(6) 0.043(4) -0.013(4) N(1) 0.031(3) 0.033(3) 0.031(3) -0.005(3) -0.001(2) 0.003(2) N(2) 0.045(4) 0.035(4) 0.042(3) -0.001(3) 0.007(3) -0.004(3) N(3) 0.037(3) 0.045(4) 0.034(3) 0.005(3) -0.001(2) -0.001(3) N(4) 0.036(3) 0.040(4) 0.031(3) -0.006(3) 0.000(2) -0.002(2) N(5) 0.033(3) 0.034(3) 0.027(3) 0.001(3) 0.000(2) -0.004(2) N(6) 0.036(3) 0.044(4) 0.037(3) -0.009(3) 0.002(2) -0.003(3) N(7) 0.038(3) 0.044(4) 0.031(3) 0.002(3) 0.001(2) 0.001(3) N(8) 0.041(3) 0.035(4) 0.036(3) 0.000(3) 0.004(2) -0.001(3) N(9) 0.067(6) 0.099(8) 0.084(6) 0.002(6) -0.008(5) -0.005(6) C(1) 0.053(5) 0.042(5) 0.055(5) 0.008(4) 0.007(4) -0.003(4) C(2) 0.055(5) 0.033(5) 0.076(6) 0.003(4) 0.002(4) 0.004(4) C(3) 0.054(5) 0.041(5) 0.063(5) -0.008(4) 0.005(4) 0.009(4) C(4) 0.044(4) 0.043(5) 0.042(4) 0.000(4) 0.005(3) 0.009(3) C(5) 0.034(4) 0.033(4) 0.036(3) 0.004(3) -0.003(3) 0.003(3) C(6) 0.041(4) 0.036(4) 0.035(3) -0.005(3) 0.002(3) 0.002(3) C(7) 0.042(4) 0.058(5) 0.034(3) 0.000(4) 0.006(3) -0.003(3) C(8) 0.058(5) 0.071(6) 0.036(4) -0.001(5) -0.004(4) 0.005(4) C(9) 0.046(4) 0.065(6) 0.047(4) 0.013(4) -0.007(4) 0.005(4) C(10) 0.043(4) 0.047(5) 0.044(4) 0.007(4) 0.001(3) -0.009(4) C(11) 0.033(3) 0.034(4) 0.037(3) 0.001(3) 0.003(3) -0.001(3) C(12) 0.034(4) 0.042(4) 0.040(4) -0.001(3) 0.006(3) 0.007(3) C(13) 0.038(4) 0.051(5) 0.035(4) -0.003(3) 0.003(3) -0.001(3) C(14) 0.036(4) 0.047(5) 0.051(4) -0.003(3) -0.002(3) -0.008(4) C(15) 0.047(4) 0.048(5) 0.051(5) -0.012(4) -0.010(4) -0.003(4) C(16) 0.055(5) 0.041(4) 0.033(4) -0.006(4) -0.005(3) 0.003(3) C(17) 0.034(3) 0.031(3) 0.028(3) -0.001(3) 0.001(2) 0.003(3) C(18) 0.041(4) 0.025(4) 0.037(3) 0.003(3) 0.000(3) -0.003(3) C(19) 0.057(5) 0.051(5) 0.037(4) 0.001(4) 0.004(3) 0.002(4) C(20) 0.055(5) 0.072(7) 0.047(5) 0.007(5) -0.008(4) -0.001(4) C(21) 0.043(4) 0.087(7) 0.057(5) -0.012(5) -0.019(4) -0.019(5) C(22) 0.048(5) 0.076(7) 0.042(4) -0.025(4) 0.005(3) -0.011(4) C(23) 0.039(4) 0.034(4) 0.034(3) -0.002(3) 0.002(3) -0.007(3) C(24) 0.045(4) 0.033(4) 0.038(4) -0.006(3) 0.002(3) -0.003(3) C(25) 0.047(4) 0.055(5) 0.033(3) -0.005(4) 0.003(3) 0.001(3) C(26) 0.043(4) 0.059(5) 0.049(4) 0.013(4) -0.002(3) 0.000(4) C(27) 0.051(5) 0.058(5) 0.047(4) 0.006(4) -0.008(4) 0.006(4) C(28) 0.037(4) 0.039(4) 0.044(4) 0.001(3) 0.003(3) 0.012(3) C(29) 0.036(4) 0.038(5) 0.030(3) -0.004(3) -0.001(3) -0.001(3) C(30) 0.046(4) 0.044(4) 0.027(3) 0.000(3) 0.004(3) -0.002(3) C(31) 0.039(4) 0.043(4) 0.052(4) -0.002(4) 0.001(3) 0.009(4) C(32) 0.058(5) 0.033(4) 0.060(5) 0.001(4) -0.004(4) -0.006(4) C(33) 0.068(5) 0.048(5) 0.040(4) 0.003(4) -0.002(4) -0.016(4) C(34) 0.043(4) 0.051(5) 0.045(4) 0.002(4) 0.012(3) -0.009(4) C(35) 0.030(3) 0.033(4) 0.039(4) -0.001(3) 0.004(3) -0.004(3) C(36) 0.032(3) 0.037(4) 0.038(4) -0.002(3) 0.003(3) -0.009(3) C(38) 0.11(1) 0.11(1) 0.12(1) 0.021(9) 0.002(8) -0.044(9) C(39) 0.062(7) 0.058(7) 0.092(8) -0.009(5) -0.030(6) 0.014(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 P(1) F(1) 1.524(9) . . yes P(1) F(2) 1.546(7) . . yes P(1) F(3) 1.44(1) . . yes P(1) F(4) 1.558(9) . . yes P(1) F(5) 1.517(8) . . yes P(1) F(6) 1.41(1) . . yes P(2) F(7) 1.579(5) . . yes P(2) F(8) 1.591(6) . . yes P(2) F(9) 1.558(6) . . yes P(2) F(10) 1.597(6) . . yes P(2) F(11) 1.597(5) . . yes P(2) F(12) 1.588(7) . . yes P(3) F(13) 1.49(1) . . yes P(3) F(14) 1.584(7) . . yes P(3) F(15) 1.549(9) . . yes P(3) F(16) 1.52(1) . . yes P(3) F(17) 1.581(6) . . yes P(3) F(18) 1.49(2) . . yes P(4) F(19) 1.54(1) . . yes P(4) F(20) 1.551(9) . . yes P(4) F(21) 1.565(7) . . yes P(4) F(22) 1.541(9) . . yes P(4) F(23) 1.563(7) . . yes P(4) F(24) 1.535(8) . . yes O(1) C(37) 1.26(6) . . yes N(1) C(6) 1.465(9) . . yes N(1) C(12) 1.470(9) . . yes N(1) C(18) 1.479(9) . . yes N(2) C(1) 1.34(1) . . yes N(2) C(5) 1.359(9) . . yes N(3) C(7) 1.328(9) . . yes N(3) C(11) 1.348(9) . . yes N(4) C(13) 1.326(9) . . yes N(4) C(17) 1.359(8) . . yes N(5) C(24) 1.468(9) . . yes N(5) C(30) 1.471(9) . . yes N(5) C(36) 1.472(9) . . yes N(6) C(19) 1.341(10) . . yes N(6) C(23) 1.349(9) . . yes N(7) C(25) 1.338(10) . . yes N(7) C(29) 1.354(9) . . yes N(8) C(31) 1.35(1) . . yes N(8) C(35) 1.360(9) . . yes N(9) C(39) 1.13(2) . . yes C(1) C(2) 1.37(1) . . yes C(2) C(3) 1.37(1) . . yes C(3) C(4) 1.40(1) . . yes C(4) C(5) 1.37(1) . . yes C(5) C(6) 1.50(1) . . yes C(7) C(8) 1.37(1) . . yes C(8) C(9) 1.37(1) . . yes C(9) C(10) 1.38(1) . . yes C(10) C(11) 1.37(1) . . yes C(11) C(12) 1.498(10) . . yes C(13) C(14) 1.39(1) . . yes C(14) C(15) 1.39(1) . . yes C(15) C(16) 1.36(1) . . yes C(16) C(17) 1.385(10) . . yes C(17) C(18) 1.494(9) . . yes C(19) C(20) 1.34(1) . . yes C(20) C(21) 1.35(1) . . yes C(21) C(22) 1.40(1) . . yes C(22) C(23) 1.37(1) . . yes C(23) C(24) 1.493(10) . . yes C(25) C(26) 1.37(1) . . yes C(26) C(27) 1.37(1) . . yes C(27) C(28) 1.39(1) . . yes C(28) C(29) 1.39(1) . . yes C(29) C(30) 1.49(1) . . yes C(31) C(32) 1.37(1) . . yes C(32) C(33) 1.39(1) . . yes C(33) C(34) 1.38(1) . . yes C(34) C(35) 1.36(1) . . yes C(35) C(36) 1.49(1) . . yes C(38) C(39) 1.47(2) . . 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 F(1) P(1) F(2) 96.2(5) . . . yes F(1) P(1) F(3) 94.8(9) . . . yes F(1) P(1) F(4) 173.1(6) . . . yes F(1) P(1) F(5) 86.4(5) . . . yes F(1) P(1) F(6) 86.7(8) . . . yes F(2) P(1) F(3) 83.2(7) . . . yes F(2) P(1) F(4) 82.6(5) . . . yes F(2) P(1) F(5) 175.0(6) . . . yes F(2) P(1) F(6) 93.9(10) . . . yes F(3) P(1) F(4) 91.7(10) . . . yes F(3) P(1) F(5) 92.3(8) . . . yes F(3) P(1) F(6) 176(1) . . . yes F(4) P(1) F(5) 95.4(5) . . . yes F(4) P(1) F(6) 86.6(8) . . . yes F(5) P(1) F(6) 90.6(10) . . . yes F(7) P(2) F(8) 91.4(3) . . . yes F(7) P(2) F(9) 90.2(3) . . . yes F(7) P(2) F(10) 178.9(3) . . . yes F(7) P(2) F(11) 90.2(3) . . . yes F(7) P(2) F(12) 90.1(3) . . . yes F(8) P(2) F(9) 89.6(3) . . . yes F(8) P(2) F(10) 89.6(3) . . . yes F(8) P(2) F(11) 177.9(3) . . . yes F(8) P(2) F(12) 89.5(3) . . . yes F(9) P(2) F(10) 89.9(3) . . . yes F(9) P(2) F(11) 91.8(3) . . . yes F(9) P(2) F(12) 179.0(4) . . . yes F(10) P(2) F(11) 88.8(3) . . . yes F(10) P(2) F(12) 89.7(3) . . . yes F(11) P(2) F(12) 89.2(3) . . . yes F(13) P(3) F(14) 90.8(6) . . . yes F(13) P(3) F(15) 89.7(6) . . . yes F(13) P(3) F(16) 175.4(7) . . . yes F(13) P(3) F(17) 90.2(5) . . . yes F(13) P(3) F(18) 86.6(8) . . . yes F(14) P(3) F(15) 88.0(4) . . . yes F(14) P(3) F(16) 90.2(5) . . . yes F(14) P(3) F(17) 178.9(4) . . . yes F(14) P(3) F(18) 91.0(6) . . . yes F(15) P(3) F(16) 85.9(5) . . . yes F(15) P(3) F(17) 92.5(4) . . . yes F(15) P(3) F(18) 176.2(7) . . . yes F(16) P(3) F(17) 88.8(4) . . . yes F(16) P(3) F(18) 97.8(8) . . . yes F(17) P(3) F(18) 88.5(6) . . . yes F(19) P(4) F(20) 87.8(6) . . . yes F(19) P(4) F(21) 85.9(6) . . . yes F(19) P(4) F(22) 175.9(6) . . . yes F(19) P(4) F(23) 99.5(6) . . . yes F(19) P(4) F(24) 91.5(5) . . . yes F(20) P(4) F(21) 91.5(4) . . . yes F(20) P(4) F(22) 91.7(5) . . . yes F(20) P(4) F(23) 86.9(4) . . . yes F(20) P(4) F(24) 179.1(4) . . . yes F(21) P(4) F(22) 90.0(5) . . . yes F(21) P(4) F(23) 174.3(5) . . . yes F(21) P(4) F(24) 87.9(4) . . . yes F(22) P(4) F(23) 84.5(5) . . . yes F(22) P(4) F(24) 89.0(5) . . . yes F(23) P(4) F(24) 93.7(4) . . . yes C(6) N(1) C(12) 109.8(5) . . . yes C(6) N(1) C(18) 109.6(5) . . . yes C(12) N(1) C(18) 108.8(5) . . . yes C(1) N(2) C(5) 122.1(6) . . . yes C(7) N(3) C(11) 124.4(6) . . . yes C(13) N(4) C(17) 124.0(6) . . . yes C(24) N(5) C(30) 111.4(5) . . . yes C(24) N(5) C(36) 110.7(5) . . . yes C(30) N(5) C(36) 108.4(5) . . . yes C(19) N(6) C(23) 123.3(6) . . . yes C(25) N(7) C(29) 122.7(6) . . . yes C(31) N(8) C(35) 123.3(6) . . . yes N(2) C(1) C(2) 120.5(8) . . . yes C(1) C(2) C(3) 119.1(8) . . . yes C(2) C(3) C(4) 120.1(8) . . . yes C(3) C(4) C(5) 119.3(7) . . . yes N(2) C(5) C(4) 118.9(7) . . . yes N(2) C(5) C(6) 117.3(6) . . . yes C(4) C(5) C(6) 123.8(6) . . . yes N(1) C(6) C(5) 112.2(5) . . . yes N(3) C(7) C(8) 118.6(7) . . . yes C(7) C(8) C(9) 120.2(7) . . . yes C(8) C(9) C(10) 118.7(8) . . . yes C(9) C(10) C(11) 120.9(7) . . . yes N(3) C(11) C(10) 117.0(6) . . . yes N(3) C(11) C(12) 119.0(6) . . . yes C(10) C(11) C(12) 124.0(6) . . . yes N(1) C(12) C(11) 112.6(6) . . . yes N(4) C(13) C(14) 119.4(7) . . . yes C(13) C(14) C(15) 117.3(7) . . . yes C(14) C(15) C(16) 122.1(7) . . . yes C(15) C(16) C(17) 119.1(7) . . . yes N(4) C(17) C(16) 118.1(6) . . . yes N(4) C(17) C(18) 118.1(6) . . . yes C(16) C(17) C(18) 123.8(6) . . . yes N(1) C(18) C(17) 113.5(6) . . . yes N(6) C(19) C(20) 119.6(7) . . . yes C(19) C(20) C(21) 120.2(8) . . . yes C(20) C(21) C(22) 119.7(8) . . . yes C(21) C(22) C(23) 119.5(8) . . . yes N(6) C(23) C(22) 117.5(6) . . . yes N(6) C(23) C(24) 116.9(6) . . . yes C(22) C(23) C(24) 125.5(7) . . . yes N(5) C(24) C(23) 112.1(6) . . . yes N(7) C(25) C(26) 120.2(7) . . . yes C(25) C(26) C(27) 119.2(7) . . . yes C(26) C(27) C(28) 119.8(8) . . . yes C(27) C(28) C(29) 119.9(7) . . . yes N(7) C(29) C(28) 118.1(6) . . . yes N(7) C(29) C(30) 117.6(6) . . . yes C(28) C(29) C(30) 124.3(6) . . . yes N(5) C(30) C(29) 113.6(5) . . . yes N(8) C(31) C(32) 118.6(7) . . . yes C(31) C(32) C(33) 120.2(7) . . . yes C(32) C(33) C(34) 118.6(7) . . . yes C(33) C(34) C(35) 121.4(7) . . . yes N(8) C(35) C(34) 117.8(7) . . . yes N(8) C(35) C(36) 117.1(6) . . . yes C(34) C(35) C(36) 124.9(6) . . . yes N(5) C(36) C(35) 112.1(5) . . . yes N(9) C(39) C(38) 178(1) . . . yes #------------------------------------------------------------------------------ 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 Br(1) C(25) 3.586(8) . 1_565 ? F(1) C(26) 3.25(1) . 1_565 ? F(1) C(39) 3.50(2) . 4_564 ? F(1) C(25) 3.52(1) . 1_565 ? F(2) C(25) 3.23(1) . 1_565 ? F(2) C(26) 3.27(1) . 1_565 ? F(3) C(38) 3.43(2) . 7_556 ? F(4) C(10) 3.23(1) . 7_555 ? F(5) C(2) 3.27(1) . 7_565 ? F(5) C(3) 3.27(1) . 7_565 ? F(5) F(21) 3.28(1) . 6_555 ? F(5) C(12) 3.49(1) . 7_555 ? F(5) C(10) 3.53(1) . 7_555 ? F(6) C(9) 3.20(1) . 1_565 ? F(6) C(10) 3.48(1) . 1_565 ? F(7) F(14) 3.091(9) . 2_555 ? F(7) C(19) 3.122(9) . 4_555 ? F(7) C(15) 3.209(10) . 4_555 ? F(7) C(20) 3.26(1) . 4_555 ? F(7) C(16) 3.372(9) . 4_555 ? F(8) N(2) 3.079(8) . 4_565 ? F(8) N(4) 3.212(8) . 4_565 ? F(8) C(13) 3.250(10) . 4_565 ? F(8) C(19) 3.334(10) . 4_555 ? F(8) C(5) 3.569(9) . 4_565 ? F(9) C(21) 3.29(1) . 2_565 ? F(9) C(20) 3.34(1) . 4_555 ? F(9) C(13) 3.358(10) . 4_565 ? F(9) C(14) 3.49(1) . 4_565 ? F(10) N(4) 3.275(8) . 4_565 ? F(10) C(13) 3.317(9) . 4_565 ? F(10) C(17) 3.389(8) . 4_565 ? F(10) C(14) 3.427(10) . 4_565 ? F(10) C(6) 3.441(9) . 4_565 ? F(10) C(30) 3.496(8) . 1_565 ? F(10) C(16) 3.498(9) . 4_565 ? F(10) C(15) 3.506(10) . 4_565 ? F(11) C(30) 3.412(9) . 1_565 ? F(12) C(28) 3.247(10) . 1_565 ? F(12) C(5) 3.276(9) . 4_565 ? F(12) N(2) 3.430(9) . 4_565 ? F(13) O(1) 3.38(2) . 7_556 ? F(14) C(33) 3.23(1) . 2_555 ? F(14) C(34) 3.47(1) . 2_555 ? F(15) C(22) 3.35(1) . 1_565 ? F(15) C(20) 3.57(1) . 3_555 ? F(16) C(14) 3.15(1) . 3_555 ? F(16) C(15) 3.37(1) . 3_555 ? F(16) F(16) 3.38(3) . 3_555 ? F(18) C(34) 3.39(2) . 2_555 ? F(19) C(27) 3.56(1) . 1_565 ? F(20) C(16) 3.29(1) . 4_555 ? F(21) C(18) 3.269(9) . 4_555 ? F(21) C(3) 3.46(1) . 4_565 ? F(21) C(6) 3.55(1) . 4_555 ? F(21) C(2) 3.58(1) . 4_565 ? F(22) C(38) 3.25(2) . 4_554 ? F(24) C(39) 3.57(1) . 7_556 ? N(9) C(27) 3.37(1) . 7_546 ? N(9) C(38) 3.39(2) . 6_546 ? N(9) C(9) 3.43(1) . 4_555 ? N(9) C(4) 3.47(1) . 6_545 ? N(9) C(26) 3.49(1) . 7_546 ? N(9) C(3) 3.50(1) . 6_545 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N(2) H(37) Br(1) . . . 0.947 2.469 3.369(6) 158.862 no N(2) H(37) N(1) . . . 0.947 2.561 2.854(8) 98.199 no N(3) H(38) Br(1) . . . 0.947 2.405 3.304(5) 158.459 no N(3) H(38) F(2) . . . 0.947 2.825 3.07(1) 95.916 no N(3) H(38) N(1) . . . 0.947 2.538 2.860(7) 100.150 no N(4) H(39) Br(1) . . . 0.953 2.373 3.280(5) 158.700 no N(4) H(39) N(1) . . . 0.953 2.529 2.863(7) 100.685 no N(6) H(40) Br(2) . . . 0.948 2.372 3.254(6) 154.590 no N(6) H(40) N(5) . . . 0.948 2.617 2.882(7) 96.473 no N(7) H(41) Br(2) . . . 0.952 2.369 3.263(5) 156.198 no N(7) H(41) F(23) . . . 0.952 2.972 3.26(1) 98.822 no N(7) H(41) N(5) . . . 0.952 2.529 2.853(7) 100.002 no N(8) H(42) Br(2) . . . 0.947 2.488 3.378(5) 156.567 no N(8) H(42) F(17) . . . 0.947 2.770 3.013(7) 95.579 no N(8) H(42) N(5) . . . 0.947 2.555 2.849(8) 98.235 no #------------------------------------------------------------------------------ #===END data_tpaClPF6 _database_code_CSD 184350 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C36 H42 Cl2 F24 N8 P4 ' _chemical_formula_moiety 'C36 H42 Cl2 F24 N8 P4 ' _chemical_formula_weight 1237.54 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.1667(2) _cell_length_b 13.6026(2) _cell_length_c 26.5260(4) _cell_angle_alpha 90 _cell_angle_beta 100.9485(5) _cell_angle_gamma 90 _cell_volume 5018.6(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 55110 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 3.276 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.926 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 28095 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11447 _reflns_number_gt 6877 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1562 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6877 _refine_ls_number_parameters 667 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 1.49 _refine_diff_density_min -0.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl -0.39762(6) 0.64182(6) 0.35156(3) 0.0319(2) Uani 1.00 d . . . Cl(2) Cl 0.10141(5) -0.07389(6) 0.35660(3) 0.0305(2) Uani 1.00 d . . . P(1) P 0.03621(6) 0.27827(6) 0.48475(3) 0.0259(2) Uani 1.00 d . . . P(2) P -0.26214(6) -0.00493(7) 0.28370(4) 0.0337(2) Uani 1.00 d . . . P(3) P 0.24977(6) 0.05844(7) 0.20572(3) 0.0301(2) Uani 1.00 d . . . P(4) P 0.40142(6) -0.17895(6) 0.50535(3) 0.0248(2) Uani 1.00 d . . . F(1) F 0.0247(2) 0.2171(2) 0.53413(8) 0.0451(5) Uani 1.00 d . . . F(2) F 0.1484(1) 0.2939(2) 0.50757(9) 0.0442(5) Uani 1.00 d . . . F(3) F 0.0606(1) 0.1789(1) 0.45734(8) 0.0382(5) Uani 1.00 d . . . F(4) F 0.0492(2) 0.3396(2) 0.43522(9) 0.0466(6) Uani 1.00 d . . . F(5) F -0.0755(1) 0.2634(1) 0.46097(8) 0.0369(5) Uani 1.00 d . . . F(6) F 0.0113(2) 0.3775(2) 0.51170(9) 0.0429(5) Uani 1.00 d . . . F(7) F -0.3112(2) 0.0252(2) 0.3309(1) 0.0689(8) Uani 1.00 d . . . F(8) F -0.2328(2) 0.1087(2) 0.2811(2) 0.100(1) Uani 1.00 d . . . F(9) F -0.3620(2) 0.0174(2) 0.24709(9) 0.0590(7) Uani 1.00 d . . . F(10) F -0.2138(2) -0.0223(4) 0.2375(1) 0.121(2) Uani 1.00 d . . . F(11) F -0.2964(2) -0.1119(2) 0.2913(2) 0.102(1) Uani 1.00 d . . . F(12) F -0.1629(2) -0.0314(2) 0.32025(9) 0.0612(7) Uani 1.00 d . . . F(13) F 0.2964(2) 0.1638(2) 0.2205(1) 0.0617(7) Uani 1.00 d . . . F(14) F 0.1955(2) 0.0618(2) 0.25316(9) 0.0604(7) Uani 1.00 d . . . F(15) F 0.1604(2) 0.1080(2) 0.1697(1) 0.0582(7) Uani 1.00 d . . . F(16) F 0.2040(2) -0.0473(2) 0.18991(9) 0.0459(5) Uani 1.00 d . . . F(17) F 0.3042(2) 0.0514(2) 0.15787(8) 0.0431(5) Uani 1.00 d . . . F(18) F 0.3404(2) 0.0086(2) 0.24077(8) 0.0455(5) Uani 1.00 d . . . F(19) F 0.3715(2) -0.2901(1) 0.48960(9) 0.0422(5) Uani 1.00 d . . . F(20) F 0.4911(1) -0.1885(2) 0.47719(8) 0.0356(5) Uani 1.00 d . . . F(21) F 0.4672(1) -0.2203(2) 0.55762(8) 0.0387(5) Uani 1.00 d . . . F(22) F 0.4336(2) -0.0701(1) 0.52212(8) 0.0369(5) Uani 1.00 d . . . F(23) F 0.3128(1) -0.1700(2) 0.53402(8) 0.0406(5) Uani 1.00 d . . . F(24) F 0.3367(1) -0.1392(2) 0.45361(7) 0.0362(5) Uani 1.00 d . . . N(1) N -0.2381(2) 0.4495(2) 0.4040(1) 0.0227(5) Uani 1.00 d . . . N(2) N -0.1828(2) 0.6167(2) 0.3522(1) 0.0252(6) Uani 1.00 d . . . N(3) N -0.3411(2) 0.5694(2) 0.4613(1) 0.0271(6) Uani 1.00 d . . . N(4) N -0.4146(2) 0.4175(2) 0.3324(1) 0.0256(6) Uani 1.00 d . . . N(5) N 0.2709(2) 0.1212(2) 0.39566(9) 0.0202(5) Uani 1.00 d . . . N(6) N 0.0827(2) 0.1477(2) 0.3367(1) 0.0246(5) Uani 1.00 d . . . N(7) N 0.1891(2) 0.0032(2) 0.4658(1) 0.0264(6) Uani 1.00 d . . . N(8) N 0.3116(2) -0.0576(2) 0.3460(1) 0.0223(5) Uani 1.00 d . . . C(1) C -0.1571(2) 0.7085(2) 0.3420(1) 0.0302(7) Uani 1.00 d . . . C(2) C -0.0615(3) 0.7305(3) 0.3458(1) 0.0328(8) Uani 1.00 d . . . C(3) C 0.0053(2) 0.6584(3) 0.3602(1) 0.0355(8) Uani 1.00 d . . . C(4) C -0.0233(2) 0.5637(3) 0.3703(1) 0.0299(7) Uani 1.00 d . . . C(5) C -0.1198(2) 0.5435(2) 0.3660(1) 0.0238(6) Uani 1.00 d . . . C(6) C -0.1603(2) 0.4435(2) 0.3738(1) 0.0259(6) Uani 1.00 d . . . C(7) C -0.4107(3) 0.6084(3) 0.4830(2) 0.0344(8) Uani 1.00 d . . . C(8) C -0.4137(3) 0.5878(3) 0.5328(2) 0.0381(8) Uani 1.00 d . . . C(9) C -0.3460(3) 0.5246(3) 0.5597(1) 0.0378(8) Uani 1.00 d . . . C(10) C -0.2747(2) 0.4858(3) 0.5364(1) 0.0307(7) Uani 1.00 d . . . C(11) C -0.2727(2) 0.5087(2) 0.4863(1) 0.0253(7) Uani 1.00 d . . . C(12) C -0.1974(2) 0.4731(2) 0.4577(1) 0.0270(7) Uani 1.00 d . . . C(13) C -0.4877(2) 0.4098(3) 0.2920(1) 0.0340(8) Uani 1.00 d . . . C(14) C -0.5128(3) 0.3202(3) 0.2707(1) 0.0403(9) Uani 1.00 d . . . C(15) C -0.4602(3) 0.2384(3) 0.2903(2) 0.0416(9) Uani 1.00 d . . . C(16) C -0.3849(3) 0.2485(3) 0.3319(1) 0.0328(8) Uani 1.00 d . . . C(17) C -0.3626(2) 0.3397(2) 0.3534(1) 0.0239(6) Uani 1.00 d . . . C(18) C -0.2891(2) 0.3546(2) 0.4017(1) 0.0262(7) Uani 1.00 d . . . C(19) C -0.0011(2) 0.1496(3) 0.3024(1) 0.0317(7) Uani 1.00 d . . . C(20) C -0.0326(3) 0.2373(3) 0.2794(1) 0.0363(8) Uani 1.00 d . . . C(21) C 0.0233(3) 0.3199(3) 0.2907(1) 0.0370(8) Uani 1.00 d . . . C(22) C 0.1094(2) 0.3152(2) 0.3256(1) 0.0304(7) Uani 1.00 d . . . C(23) C 0.1382(2) 0.2267(2) 0.3494(1) 0.0231(6) Uani 1.00 d . . . C(24) C 0.2243(2) 0.2178(2) 0.3922(1) 0.0232(6) Uani 1.00 d . . . C(25) C 0.1309(3) -0.0356(3) 0.4951(2) 0.0373(9) Uani 1.00 d . . . C(26) C 0.1395(3) -0.0066(3) 0.5450(2) 0.045(1) Uani 1.00 d . . . C(27) C 0.2076(3) 0.0627(3) 0.5642(2) 0.0445(10) Uani 1.00 d . . . C(28) C 0.2670(3) 0.1010(3) 0.5337(1) 0.0329(8) Uani 1.00 d . . . C(29) C 0.2571(2) 0.0707(2) 0.4834(1) 0.0237(6) Uani 1.00 d . . . C(30) C 0.3225(2) 0.1032(2) 0.4483(1) 0.0254(7) Uani 1.00 d . . . C(31) C 0.3349(2) -0.1513(2) 0.3384(1) 0.0270(7) Uani 1.00 d . . . C(32) C 0.4293(3) -0.1769(2) 0.3397(1) 0.0308(7) Uani 1.00 d . . . C(33) C 0.4986(2) -0.1048(3) 0.3496(1) 0.0319(7) Uani 1.00 d . . . C(34) C 0.4723(2) -0.0073(3) 0.3576(1) 0.0284(7) Uani 1.00 d . . . C(35) C 0.3769(2) 0.0154(2) 0.3550(1) 0.0213(6) Uani 1.00 d . . . C(36) C 0.3398(2) 0.1179(2) 0.3600(1) 0.0242(6) Uani 1.00 d . . . H(1) H -0.2478 0.6072 0.3489 0.0540 Uiso 1.00 calc . . . H(2) H -0.3419 0.5887 0.4278 0.0540 Uiso 1.00 calc . . . H(3) H -0.3949 0.4764 0.3472 0.0540 Uiso 1.00 calc . . . H(4) H 0.1019 0.0811 0.3510 0.0540 Uiso 1.00 calc . . . H(5) H 0.1770 -0.0198 0.4289 0.0540 Uiso 1.00 calc . . . H(6) H 0.2450 -0.0464 0.3474 0.0540 Uiso 1.00 calc . . . H(7) H -0.2048 0.7577 0.3325 0.0378 Uiso 1.00 calc . . . H(8) H -0.0419 0.7946 0.3384 0.0403 Uiso 1.00 calc . . . H(9) H 0.0719 0.6720 0.3631 0.0438 Uiso 1.00 calc . . . H(10) H 0.0229 0.5134 0.3805 0.0369 Uiso 1.00 calc . . . H(11) H -0.1098 0.4040 0.3920 0.0320 Uiso 1.00 calc . . . H(12) H -0.1844 0.4156 0.3414 0.0320 Uiso 1.00 calc . . . H(13) H -0.4571 0.6508 0.4638 0.0423 Uiso 1.00 calc . . . H(14) H -0.4610 0.6152 0.5490 0.0442 Uiso 1.00 calc . . . H(15) H -0.3481 0.5090 0.5940 0.0441 Uiso 1.00 calc . . . H(16) H -0.2280 0.4430 0.5549 0.0376 Uiso 1.00 calc . . . H(17) H -0.1688 0.4146 0.4741 0.0327 Uiso 1.00 calc . . . H(18) H -0.1497 0.5219 0.4588 0.0327 Uiso 1.00 calc . . . H(19) H -0.5225 0.4667 0.2788 0.0412 Uiso 1.00 calc . . . H(20) H -0.5641 0.3127 0.2425 0.0507 Uiso 1.00 calc . . . H(21) H -0.4754 0.1762 0.2757 0.0499 Uiso 1.00 calc . . . H(22) H -0.3486 0.1936 0.3454 0.0388 Uiso 1.00 calc . . . H(23) H -0.2434 0.3033 0.4040 0.0307 Uiso 1.00 calc . . . H(24) H -0.3211 0.3513 0.4301 0.0307 Uiso 1.00 calc . . . H(25) H -0.0375 0.0918 0.2946 0.0386 Uiso 1.00 calc . . . H(26) H -0.0922 0.2400 0.2555 0.0440 Uiso 1.00 calc . . . H(27) H 0.0026 0.3799 0.2747 0.0452 Uiso 1.00 calc . . . H(28) H 0.1481 0.3721 0.3331 0.0367 Uiso 1.00 calc . . . H(29) H 0.2043 0.2301 0.4235 0.0284 Uiso 1.00 calc . . . H(30) H 0.2700 0.2654 0.3865 0.0284 Uiso 1.00 calc . . . H(31) H 0.0832 -0.0834 0.4810 0.0451 Uiso 1.00 calc . . . H(32) H 0.0999 -0.0350 0.5660 0.0549 Uiso 1.00 calc . . . H(33) H 0.2131 0.0850 0.5981 0.0545 Uiso 1.00 calc . . . H(34) H 0.3137 0.1488 0.5472 0.0403 Uiso 1.00 calc . . . H(35) H 0.3690 0.0532 0.4474 0.0322 Uiso 1.00 calc . . . H(36) H 0.3532 0.1620 0.4614 0.0322 Uiso 1.00 calc . . . H(37) H 0.2861 -0.2002 0.3323 0.0336 Uiso 1.00 calc . . . H(38) H 0.4467 -0.2425 0.3334 0.0384 Uiso 1.00 calc . . . H(39) H 0.5640 -0.1216 0.3515 0.0402 Uiso 1.00 calc . . . H(40) H 0.5201 0.0421 0.3643 0.0329 Uiso 1.00 calc . . . H(41) H 0.3088 0.1406 0.3272 0.0303 Uiso 1.00 calc . . . H(42) H 0.3926 0.1602 0.3730 0.0303 Uiso 1.00 calc . . . 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 Cl(1) 0.0256(4) 0.0270(4) 0.0427(5) 0.0095(3) 0.0052(3) 0.0116(3) Cl(2) 0.0227(4) 0.0232(4) 0.0447(5) -0.0065(3) 0.0040(3) -0.0031(3) P(1) 0.0242(4) 0.0213(4) 0.0313(5) 0.0038(3) 0.0029(3) 0.0000(3) P(2) 0.0249(4) 0.0458(6) 0.0288(5) -0.0061(4) 0.0009(4) 0.0108(4) P(3) 0.0302(4) 0.0300(5) 0.0284(5) 0.0031(4) 0.0017(4) -0.0005(4) P(4) 0.0226(4) 0.0218(4) 0.0295(5) 0.0017(3) 0.0038(3) 0.0038(3) F(1) 0.053(1) 0.046(1) 0.035(1) -0.002(1) 0.007(1) 0.0104(10) F(2) 0.025(1) 0.033(1) 0.069(2) 0.0034(9) -0.0045(10) -0.002(1) F(3) 0.037(1) 0.028(1) 0.049(1) 0.0088(9) 0.0052(9) -0.0066(9) F(4) 0.048(1) 0.042(1) 0.052(1) 0.009(1) 0.016(1) 0.020(1) F(5) 0.0256(10) 0.031(1) 0.050(1) 0.0032(8) -0.0006(9) -0.0043(9) F(6) 0.036(1) 0.030(1) 0.062(2) 0.0049(9) 0.006(1) -0.0157(10) F(7) 0.064(2) 0.089(2) 0.053(2) 0.025(2) 0.008(1) -0.002(1) F(8) 0.066(2) 0.050(2) 0.184(4) -0.013(2) 0.023(2) 0.014(2) F(9) 0.033(1) 0.095(2) 0.045(1) 0.006(1) -0.003(1) 0.020(1) F(10) 0.059(2) 0.276(5) 0.032(1) 0.070(3) 0.015(1) 0.011(2) F(11) 0.052(2) 0.031(1) 0.212(4) -0.002(1) -0.005(2) 0.013(2) F(12) 0.032(1) 0.099(2) 0.046(1) -0.005(1) -0.008(1) 0.026(1) F(13) 0.071(2) 0.034(1) 0.070(2) -0.007(1) -0.010(1) -0.008(1) F(14) 0.047(1) 0.093(2) 0.044(1) 0.010(1) 0.015(1) -0.017(1) F(15) 0.051(1) 0.055(2) 0.057(2) 0.025(1) -0.017(1) -0.006(1) F(16) 0.046(1) 0.038(1) 0.055(1) -0.011(1) 0.015(1) -0.004(1) F(17) 0.042(1) 0.056(1) 0.032(1) -0.012(1) 0.0104(9) 0.003(1) F(18) 0.042(1) 0.057(1) 0.034(1) 0.016(1) 0.0006(10) 0.007(1) F(19) 0.042(1) 0.023(1) 0.058(1) -0.0035(9) 0.001(1) -0.0026(9) F(20) 0.029(1) 0.041(1) 0.039(1) 0.0043(9) 0.0104(9) 0.0026(9) F(21) 0.037(1) 0.039(1) 0.037(1) 0.0055(9) -0.0012(9) 0.0094(9) F(22) 0.044(1) 0.0233(10) 0.043(1) -0.0032(9) 0.0060(9) 0.0004(9) F(23) 0.034(1) 0.040(1) 0.053(1) 0.0060(9) 0.0190(10) 0.014(1) F(24) 0.034(1) 0.039(1) 0.032(1) 0.0076(9) -0.0010(9) 0.0049(9) N(1) 0.022(1) 0.021(1) 0.024(1) -0.001(1) 0.003(1) 0.001(1) N(2) 0.022(1) 0.021(1) 0.032(2) -0.001(1) 0.006(1) 0.000(1) N(3) 0.028(1) 0.021(1) 0.032(2) 0.001(1) 0.005(1) 0.004(1) N(4) 0.022(1) 0.025(1) 0.029(1) -0.001(1) 0.004(1) 0.003(1) N(5) 0.019(1) 0.020(1) 0.021(1) 0.0006(10) 0.0028(10) -0.0014(10) N(6) 0.023(1) 0.023(1) 0.027(1) 0.000(1) 0.004(1) -0.001(1) N(7) 0.025(1) 0.021(1) 0.034(2) 0.004(1) 0.010(1) 0.006(1) N(8) 0.021(1) 0.020(1) 0.026(1) 0.001(1) 0.004(1) -0.001(1) C(1) 0.033(2) 0.024(2) 0.034(2) 0.000(1) 0.006(1) 0.000(1) C(2) 0.037(2) 0.028(2) 0.035(2) -0.013(2) 0.010(2) 0.000(1) C(3) 0.024(2) 0.044(2) 0.040(2) -0.011(2) 0.010(1) -0.009(2) C(4) 0.024(2) 0.038(2) 0.028(2) 0.004(1) 0.005(1) 0.000(1) C(5) 0.025(2) 0.024(2) 0.022(2) 0.000(1) 0.003(1) 0.000(1) C(6) 0.027(2) 0.021(2) 0.029(2) 0.004(1) 0.004(1) 0.002(1) C(7) 0.033(2) 0.025(2) 0.045(2) 0.005(1) 0.010(2) 0.000(1) C(8) 0.038(2) 0.036(2) 0.041(2) 0.004(2) 0.010(2) -0.009(2) C(9) 0.047(2) 0.041(2) 0.026(2) -0.002(2) 0.006(2) -0.006(2) C(10) 0.032(2) 0.030(2) 0.028(2) 0.001(1) 0.000(1) -0.002(1) C(11) 0.022(1) 0.019(2) 0.033(2) -0.003(1) 0.000(1) -0.003(1) C(12) 0.023(2) 0.028(2) 0.028(2) 0.001(1) 0.000(1) 0.001(1) C(13) 0.021(2) 0.046(2) 0.034(2) 0.002(2) 0.004(1) 0.009(2) C(14) 0.038(2) 0.052(2) 0.028(2) -0.010(2) -0.003(2) 0.002(2) C(15) 0.052(2) 0.040(2) 0.033(2) -0.013(2) 0.007(2) -0.009(2) C(16) 0.038(2) 0.031(2) 0.030(2) -0.001(1) 0.005(1) -0.002(1) C(17) 0.023(1) 0.024(2) 0.025(2) -0.002(1) 0.008(1) 0.005(1) C(18) 0.028(2) 0.019(2) 0.030(2) -0.001(1) 0.004(1) 0.005(1) C(19) 0.026(2) 0.035(2) 0.032(2) -0.002(1) 0.000(1) -0.008(1) C(20) 0.031(2) 0.043(2) 0.031(2) 0.009(2) -0.004(1) -0.001(2) C(21) 0.044(2) 0.034(2) 0.030(2) 0.012(2) 0.002(2) 0.009(2) C(22) 0.036(2) 0.024(2) 0.031(2) 0.001(1) 0.006(1) 0.004(1) C(23) 0.024(1) 0.022(2) 0.024(2) 0.000(1) 0.005(1) -0.001(1) C(24) 0.024(2) 0.021(1) 0.025(2) -0.001(1) 0.004(1) -0.002(1) C(25) 0.032(2) 0.030(2) 0.053(2) 0.006(2) 0.018(2) 0.016(2) C(26) 0.046(2) 0.046(2) 0.048(2) 0.018(2) 0.024(2) 0.024(2) C(27) 0.057(3) 0.048(2) 0.031(2) 0.025(2) 0.015(2) 0.013(2) C(28) 0.034(2) 0.036(2) 0.027(2) 0.012(2) 0.001(1) 0.000(1) C(29) 0.022(1) 0.022(2) 0.026(2) 0.008(1) 0.003(1) 0.004(1) C(30) 0.022(1) 0.027(2) 0.025(2) 0.000(1) 0.001(1) -0.001(1) C(31) 0.032(2) 0.019(2) 0.029(2) 0.001(1) 0.004(1) -0.001(1) C(32) 0.034(2) 0.026(2) 0.033(2) 0.008(1) 0.008(1) -0.001(1) C(33) 0.023(2) 0.037(2) 0.036(2) 0.010(1) 0.006(1) 0.003(1) C(34) 0.022(2) 0.033(2) 0.030(2) -0.001(1) 0.005(1) 0.000(1) C(35) 0.022(1) 0.023(2) 0.018(1) 0.000(1) 0.003(1) 0.001(1) C(36) 0.026(2) 0.020(2) 0.027(2) -0.003(1) 0.007(1) -0.001(1) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 P(1) F(1) 1.586(2) . . yes P(1) F(2) 1.604(2) . . yes P(1) F(3) 1.603(2) . . yes P(1) F(4) 1.596(3) . . yes P(1) F(5) 1.601(2) . . yes P(1) F(6) 1.597(2) . . yes P(2) F(7) 1.596(3) . . yes P(2) F(8) 1.606(3) . . yes P(2) F(9) 1.586(2) . . yes P(2) F(10) 1.531(3) . . yes P(2) F(11) 1.559(3) . . yes P(2) F(12) 1.590(2) . . yes P(3) F(13) 1.596(3) . . yes P(3) F(14) 1.595(3) . . yes P(3) F(15) 1.585(2) . . yes P(3) F(16) 1.600(2) . . yes P(3) F(17) 1.608(3) . . yes P(3) F(18) 1.588(2) . . yes P(4) F(19) 1.604(2) . . yes P(4) F(20) 1.597(2) . . yes P(4) F(21) 1.617(2) . . yes P(4) F(22) 1.588(2) . . yes P(4) F(23) 1.592(2) . . yes P(4) F(24) 1.593(2) . . yes F(1) F(2) 2.264(3) . . yes F(1) F(3) 2.251(3) . . yes F(1) F(5) 2.265(3) . . yes F(1) F(6) 2.260(3) . . yes F(2) F(3) 2.268(3) . . yes F(2) F(4) 2.241(3) . . yes F(2) F(6) 2.271(3) . . yes F(3) F(4) 2.262(3) . . yes F(3) F(5) 2.262(3) . . yes F(4) F(5) 2.262(3) . . yes F(4) F(6) 2.254(4) . . yes F(5) F(6) 2.258(3) . . yes F(7) F(8) 2.197(5) . . yes F(7) F(9) 2.205(3) . . yes F(7) F(11) 2.169(4) . . yes F(7) F(12) 2.304(4) . . yes F(8) F(9) 2.254(4) . . yes F(8) F(10) 2.169(6) . . yes F(8) F(12) 2.303(4) . . yes F(9) F(10) 2.229(4) . . yes F(9) F(11) 2.218(4) . . yes F(10) F(11) 2.351(6) . . yes F(10) F(12) 2.179(3) . . yes F(11) F(12) 2.193(4) . . yes F(13) F(14) 2.279(4) . . yes F(13) F(15) 2.263(3) . . yes F(13) F(17) 2.276(3) . . yes F(13) F(18) 2.239(3) . . yes F(14) F(15) 2.265(4) . . yes F(14) F(16) 2.260(4) . . yes F(14) F(18) 2.259(3) . . yes F(15) F(16) 2.238(3) . . yes F(15) F(17) 2.255(3) . . yes F(16) F(17) 2.235(3) . . yes F(16) F(18) 2.267(3) . . yes F(17) F(18) 2.238(3) . . yes F(19) F(20) 2.258(3) . . yes F(19) F(21) 2.251(3) . . yes F(19) F(23) 2.263(3) . . yes F(19) F(24) 2.278(3) . . yes F(20) F(21) 2.264(3) . . yes F(20) F(22) 2.246(3) . . yes F(20) F(24) 2.259(3) . . yes F(21) F(22) 2.261(3) . . yes F(21) F(23) 2.264(3) . . yes F(22) F(23) 2.255(3) . . yes F(22) F(24) 2.263(3) . . yes F(23) F(24) 2.262(3) . . yes N(1) C(6) 1.482(4) . . yes N(1) C(12) 1.467(4) . . yes N(1) C(18) 1.474(4) . . yes N(2) C(1) 1.342(4) . . yes N(2) C(2) 2.342(4) . . yes N(2) C(4) 2.333(4) . . yes N(2) C(5) 1.341(4) . . yes N(3) C(7) 1.342(5) . . yes N(3) C(8) 2.338(5) . . yes N(3) C(10) 2.333(4) . . yes N(3) C(11) 1.348(4) . . yes N(4) C(13) 1.345(4) . . yes N(4) C(14) 2.345(4) . . yes N(4) C(16) 2.338(4) . . yes N(4) C(17) 1.349(4) . . yes N(5) C(24) 1.466(4) . . yes N(5) C(30) 1.468(4) . . yes N(5) C(36) 1.483(4) . . yes N(6) C(19) 1.351(4) . . yes N(6) C(20) 2.349(4) . . yes N(6) C(22) 2.337(4) . . yes N(6) C(23) 1.337(4) . . yes N(7) C(25) 1.344(5) . . yes N(7) C(26) 2.342(5) . . yes N(7) C(28) 2.339(4) . . yes N(7) C(29) 1.348(4) . . yes N(8) C(31) 1.341(4) . . yes N(8) C(32) 2.356(4) . . yes N(8) C(34) 2.341(4) . . yes N(8) C(35) 1.347(4) . . yes C(1) C(2) 1.372(5) . . yes C(1) C(3) 2.360(5) . . yes C(1) C(5) 2.365(4) . . yes C(2) C(3) 1.367(5) . . yes C(2) C(4) 2.394(5) . . yes C(3) C(4) 1.391(5) . . yes C(3) C(5) 2.390(5) . . yes C(4) C(5) 1.379(4) . . yes C(5) C(6) 1.505(4) . . yes C(7) C(8) 1.360(6) . . yes C(7) C(9) 2.360(5) . . yes C(7) C(11) 2.367(5) . . yes C(8) C(9) 1.381(5) . . yes C(8) C(10) 2.397(5) . . yes C(9) C(10) 1.385(6) . . yes C(9) C(11) 2.383(6) . . yes C(10) C(11) 1.370(5) . . yes C(11) C(12) 1.503(5) . . yes C(12) C(18) 2.400(4) . . yes C(13) C(14) 1.361(6) . . yes C(13) C(15) 2.365(6) . . yes C(13) C(17) 2.368(4) . . yes C(14) C(15) 1.385(6) . . yes C(14) C(16) 2.398(5) . . yes C(15) C(16) 1.388(5) . . yes C(15) C(17) 2.395(5) . . yes C(16) C(17) 1.377(5) . . yes C(17) C(18) 1.502(4) . . yes C(19) C(20) 1.375(5) . . yes C(19) C(21) 2.371(5) . . yes C(19) C(23) 2.370(4) . . yes C(20) C(21) 1.375(5) . . yes C(20) C(22) 2.395(5) . . yes C(21) C(22) 1.386(5) . . yes C(21) C(23) 2.392(4) . . yes C(22) C(23) 1.384(4) . . yes C(23) C(24) 1.503(4) . . yes C(25) C(26) 1.365(6) . . yes C(25) C(27) 2.361(5) . . yes C(25) C(29) 2.366(5) . . yes C(26) C(27) 1.375(6) . . yes C(26) C(28) 2.388(6) . . yes C(27) C(28) 1.377(6) . . yes C(27) C(29) 2.381(5) . . yes C(28) C(29) 1.377(5) . . yes C(29) C(30) 1.500(5) . . yes C(31) C(32) 1.377(5) . . yes C(31) C(33) 2.367(5) . . yes C(31) C(35) 2.364(4) . . yes C(32) C(33) 1.377(5) . . yes C(33) C(34) 1.403(5) . . yes C(33) C(35) 2.400(5) . . yes C(34) C(35) 1.376(4) . . yes C(35) C(36) 1.504(4) . . 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 ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ 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 Cl(1) C(32) 3.449(4) . 1_465 ? Cl(2) C(2) 3.498(4) . 1_545 ? F(1) C(2) 3.207(4) . 3_566 ? F(1) C(25) 3.302(4) . 3_556 ? F(1) C(3) 3.370(4) . 3_566 ? F(2) C(11) 3.198(4) . 3_566 ? F(2) N(3) 3.277(3) . 3_566 ? F(2) C(12) 3.336(4) . 3_566 ? F(5) C(25) 3.453(4) . 3_556 ? F(6) C(4) 3.204(4) . 3_566 ? F(6) C(12) 3.306(4) . 3_566 ? F(6) F(6) 3.395(4) . 3_566 ? F(6) C(3) 3.485(4) . 3_566 ? F(6) C(5) 3.486(4) . 3_566 ? F(7) C(27) 3.126(5) . 3_556 ? F(7) C(34) 3.306(4) . 1_455 ? F(7) C(33) 3.338(5) . 1_455 ? F(8) N(2) 3.513(5) . 2_445 ? F(9) C(5) 2.983(4) . 2_445 ? F(9) N(2) 3.131(4) . 2_445 ? F(9) C(4) 3.288(4) . 2_445 ? F(9) C(6) 3.433(4) . 2_445 ? F(9) C(21) 3.546(4) . 2_445 ? F(9) C(1) 3.559(4) . 2_445 ? F(10) N(4) 2.949(4) . 2_445 ? F(10) N(2) 3.173(4) . 2_445 ? F(10) C(6) 3.182(4) . 2_445 ? F(10) C(13) 3.235(5) . 2_445 ? F(10) C(5) 3.382(4) . 2_445 ? F(10) C(17) 3.392(5) . 2_445 ? F(11) C(1) 3.265(4) . 1_545 ? F(11) C(20) 3.446(5) . 2_445 ? F(11) C(33) 3.542(5) . 1_455 ? F(12) C(27) 3.272(5) . 3_556 ? F(12) C(2) 3.555(4) . 1_545 ? F(12) C(26) 3.564(5) . 3_556 ? F(12) C(1) 3.583(4) . 1_545 ? F(13) C(31) 3.336(4) . 2_555 ? F(13) C(14) 3.497(5) . 1_655 ? F(15) C(32) 3.180(4) . 2_555 ? F(15) C(31) 3.283(4) . 2_555 ? F(15) C(9) 3.417(5) . 4_554 ? F(16) C(13) 3.243(4) . 2_445 ? F(16) C(22) 3.327(4) . 2_545 ? F(16) C(9) 3.405(4) . 4_554 ? F(16) C(14) 3.571(5) . 2_445 ? F(17) C(3) 3.182(4) . 2_545 ? F(17) C(9) 3.205(4) . 4_554 ? F(17) C(10) 3.242(4) . 4_554 ? F(17) C(4) 3.332(4) . 2_545 ? F(17) C(22) 3.437(4) . 2_545 ? F(18) C(22) 3.317(4) . 2_545 ? F(18) C(21) 3.409(4) . 2_545 ? F(19) C(10) 3.015(4) . 3_556 ? F(19) C(11) 3.398(4) . 3_556 ? F(19) C(7) 3.414(4) . 1_645 ? F(19) C(18) 3.425(4) . 3_556 ? F(19) C(9) 3.441(4) . 3_556 ? F(19) C(8) 3.464(4) . 1_645 ? F(20) C(7) 3.084(4) . 1_645 ? F(20) C(30) 3.201(3) . 3_656 ? F(20) C(8) 3.536(4) . 1_645 ? F(21) C(8) 3.243(4) . 1_645 ? F(21) C(16) 3.374(4) . 3_556 ? F(21) C(30) 3.407(4) . 3_656 ? F(21) C(17) 3.426(4) . 3_556 ? F(21) C(18) 3.451(4) . 3_556 ? F(21) C(36) 3.452(3) . 3_656 ? F(22) F(22) 3.064(4) . 3_656 ? F(22) C(34) 3.384(4) . 3_656 ? F(22) C(30) 3.424(4) . 3_656 ? F(23) C(18) 3.090(4) . 3_556 ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N(2) H(1) N(1) . . . 0.919 2.581 2.837(4) 96.558 no N(3) H(2) N(1) . . . 0.926 2.549 2.819(4) 97.188 no N(4) H(3) N(1) . . . 0.910 2.459 2.863(3) 107.169 no N(6) H(4) N(5) . . . 0.995 2.520 2.847(3) 98.775 no N(7) H(5) N(5) . . . 1.010 2.583 2.863(4) 95.548 no N(8) H(6) N(5) . . . 0.966 2.601 2.879(3) 96.692 no N(2) H(1) Cl(1) . . 1_555 0.919 2.189 3.061(3) 158.203 no N(3) H(2) Cl(1) . . 1_555 0.926 2.151 3.034(3) 159.010 no N(4) H(3) Cl(1) . . 1_555 0.910 2.253 3.094(3) 153.359 no N(2) H(1) F(10) . . 2_455 0.919 2.864 3.179(4) 101.541 no N(6) H(4) Cl(2) . . 1_555 0.995 2.115 3.059(2) 157.451 no N(7) H(5) Cl(2) . . 1_555 1.010 2.142 3.109(2) 159.678 no N(8) H(6) Cl(2) . . 1_555 0.966 2.128 3.053(2) 159.670 no N(8) H(6) F(14) . . 1_555 0.966 2.872 3.149(3) 97.596 no #------------------------------------------------------------------------------ #==END