Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_XROPU_Osaka_Pref._Univ._(M _database_code_CSD 191668 _audit_creation_date 'Fri Aug 9 13:20:24 2002' _audit_creation_method 'by teXsan' _audit_update_record ? _journal_coden_Cambridge 182 loop_ _publ_author_name 'Toshikazu Takata' 'Nobuhiro Kilhara' 'Nobuhiro Watanabe' 'Takaya Yagi' _publ_contact_author_name 'Prof Toshikazu Takata' _publ_contact_author_address ; Department of Applied Chemistry Osaka Prefecture University Gakuen-cho, 1-1 Sakai, Osaka 599-8531 JAPAN ; _publ_contact_author_email 'TAKATA@CHEM.OSAKAFU-U.AC.JP' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Highly Efficient Synthesis of [3]- and [5]Rotaxanes Consisting of Crown Ether and sec-Ammonium Salt ; _publ_requested_journal test _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_references ; ENTER OTHER REFERENCES Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R. (1999). SIR97. A New Tool for Crystal Structure Determination and Refinement. J. App. Cryst., 32, 115-119. Johnson, C. K. (1976). ORTEP-II. A FORTRAN Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory. Tennessee, USA. MSC & Rigaku. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. Molecular Structure Corporation, Texsas, USA and Rigaku Corporation, Tokyo, Japan. Rigaku (1998). PROCESS-AUTO. Automatic Data Acquisition and Processing Package for Imaging Plate Diffractometer. Rigaku Corporation, Tokyo, Japan ; _publ_section_exptl_refinement ; Hydrogen atoms of EtOH disordered around a two-fold axis of the crystal were not located. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C90 H118 Cl3 F12 N2 O20.50 P2 ' _chemical_formula_moiety 'C40 H50 N2 O4 2+, 2(C24 H32 O8), 2(F6 P 1-), C H Cl3, 0.5(C2 H6 O)' _chemical_formula_weight 1952.21 _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 41.6032(9) _cell_length_b 16.1461(3) _cell_length_c 32.8652(7) _cell_angle_alpha 90 _cell_angle_beta 116.5971(3) _cell_angle_gamma 90 _cell_volume 19740.3(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 61019 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # 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 76981 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_max 25.25 _diffrn_measured_fraction_theta_max 0.9484 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.9484 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 #------------------------------------------------------------------------------ # 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 16980 _reflns_number_gt 8405 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.2882 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 16950 _refine_ls_number_parameters 1161 _refine_ls_goodness_of_fit_ref 1.442 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.11100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0280 _refine_diff_density_max 1.42 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # 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 Cl1 Cl 0.04713(9) 0.8060(2) 0.2550(1) 0.215(2) Uani 1.00 d . . . Cl2 Cl 0.0747(1) 0.7501(3) 0.1996(2) 0.275(2) Uani 1.00 d . . . Cl3 Cl 0.0103(1) 0.8481(2) 0.1668(2) 0.304(2) Uani 1.00 d . . . P1 P 0.12019(4) 0.0264(1) 0.23893(5) 0.0802(5) Uani 1.00 d . . . P2 P 0.29444(5) -0.01272(10) 0.44681(5) 0.0859(5) Uani 1.00 d . . . F1 F 0.1275(2) 0.0914(3) 0.2088(2) 0.170(2) Uani 1.00 d . . . F2 F 0.0995(1) 0.0945(3) 0.2515(2) 0.141(2) Uani 1.00 d . . . F3 F 0.1136(1) -0.0386(2) 0.2695(1) 0.126(2) Uani 1.00 d . . . F4 F 0.1422(2) -0.0370(3) 0.2266(2) 0.171(2) Uani 1.00 d . . . F5 F 0.0850(1) 0.0021(3) 0.1957(1) 0.145(2) Uani 1.00 d . . . F6 F 0.1548(1) 0.0550(4) 0.2815(2) 0.174(2) Uani 1.00 d . . . F7 F 0.3082(3) 0.0278(4) 0.4168(2) 0.270(4) Uani 1.00 d . . . F8 F 0.2884(2) 0.0733(3) 0.4614(2) 0.206(3) Uani 1.00 d . . . F9 F 0.2792(2) -0.0486(4) 0.4764(2) 0.238(4) Uani 1.00 d . . . F10 F 0.3039(3) -0.0948(3) 0.4335(2) 0.265(4) Uani 1.00 d . . . F11 F 0.2588(2) -0.0207(6) 0.4048(2) 0.276(4) Uani 1.00 d . . . F12 F 0.3310(1) -0.0025(5) 0.4875(2) 0.213(3) Uani 1.00 d . . . O1 O 0.03877(10) 0.6566(3) 0.0002(1) 0.092(1) Uani 1.00 d . . . O2 O 0.04776(8) 0.6080(2) 0.0679(1) 0.069(1) Uani 1.00 d . . . O3 O 0.51798(10) 0.2319(3) 0.6688(1) 0.081(1) Uani 1.00 d . . . O4 O 0.5392(1) 0.1286(3) 0.6438(2) 0.131(2) Uani 1.00 d . . . O5 O 0.1580(1) 0.3347(2) 0.3044(1) 0.080(1) Uani 1.00 d . . . O6 O 0.17254(10) 0.3612(2) 0.2259(1) 0.074(1) Uani 1.00 d . . . O7 O 0.22547(8) 0.4697(2) 0.22033(10) 0.064(1) Uani 1.00 d . . . O8 O 0.25958(8) 0.6122(2) 0.2753(1) 0.063(1) Uani 1.00 d . . . O9 O 0.2344(1) 0.7125(2) 0.3144(1) 0.077(1) Uani 1.00 d . . . O10 O 0.1638(1) 0.7196(3) 0.3105(2) 0.127(2) Uani 1.00 d . . . O11 O 0.1502(1) 0.5967(3) 0.3648(2) 0.104(2) Uani 1.00 d . . . O12 O 0.16131(10) 0.4217(3) 0.3720(1) 0.078(1) Uani 1.00 d . . . O13 O 0.38374(10) 0.3806(2) 0.4129(1) 0.075(1) Uani 1.00 d . . . O14 O 0.4367(1) 0.5134(4) 0.4468(2) 0.137(2) Uani 1.00 d . . . O15 O 0.4347(1) 0.6535(3) 0.4990(2) 0.129(2) Uani 1.00 d . . . O16 O 0.3926(1) 0.6706(2) 0.5486(1) 0.101(2) Uani 1.00 d . . . O17 O 0.3713(1) 0.5560(2) 0.5863(1) 0.092(1) Uani 1.00 d . . . O18 O 0.3948(1) 0.3963(2) 0.6136(1) 0.088(1) Uani 1.00 d . . . O19 O 0.37591(9) 0.2682(2) 0.5478(1) 0.065(1) Uani 1.00 d . . . O20 O 0.35807(9) 0.2826(2) 0.4540(1) 0.067(1) Uani 1.00 d . . . O21 O -0.0323(4) 0.1539(8) 0.2334(5) 0.173(5) Uiso 0.50 d P E A N1 N 0.2021(1) 0.5231(3) 0.2851(1) 0.073(1) Uani 1.00 d . . . N2 N 0.37707(9) 0.4381(2) 0.5199(1) 0.049(1) Uani 1.00 d . . . C1 C -0.0111(1) 0.6054(3) 0.0096(2) 0.056(1) Uani 1.00 d . . . C2 C -0.0366(1) 0.6298(3) -0.0338(2) 0.066(2) Uani 1.00 d . . . C3 C -0.0725(1) 0.6151(3) -0.0483(2) 0.073(2) Uani 1.00 d . . . C4 C -0.0834(1) 0.5731(4) -0.0191(2) 0.079(2) Uani 1.00 d . . . C5 C -0.0589(1) 0.5471(3) 0.0237(2) 0.071(2) Uani 1.00 d . . . C6 C -0.0226(1) 0.5634(3) 0.0381(2) 0.064(2) Uani 1.00 d . . . C7 C -0.1008(2) 0.6438(5) -0.0948(2) 0.105(2) Uani 1.00 d . . . C8 C -0.0712(2) 0.5016(4) 0.0540(2) 0.107(3) Uani 1.00 d . . . C9 C 0.0269(1) 0.6260(3) 0.0240(2) 0.063(2) Uani 1.00 d . . . C10 C 0.0858(1) 0.6268(3) 0.0851(2) 0.071(2) Uani 1.00 d . . . C11 C 0.1044(1) 0.6046(3) 0.1347(2) 0.057(1) Uani 1.00 d . . . C12 C 0.1359(1) 0.6457(3) 0.1627(2) 0.063(2) Uani 1.00 d . . . C13 C 0.1549(1) 0.6246(3) 0.2084(2) 0.061(1) Uani 1.00 d . . . C14 C 0.1430(1) 0.5620(3) 0.2270(1) 0.049(1) Uani 1.00 d . . . C15 C 0.1111(1) 0.5228(3) 0.1986(2) 0.062(2) Uani 1.00 d . . . C16 C 0.0921(1) 0.5437(3) 0.1533(2) 0.066(2) Uani 1.00 d . . . C17 C 0.1646(1) 0.5352(3) 0.2753(2) 0.058(1) Uani 1.00 d . . . C18 C 0.2267(1) 0.4758(4) 0.3260(2) 0.074(2) Uani 1.00 d . . . C19 C 0.2348(1) 0.5152(3) 0.3700(2) 0.068(2) Uani 1.00 d . . . C20 C 0.2654(1) 0.4620(4) 0.4075(2) 0.088(2) Uani 1.00 d . . . C21 C 0.2763(1) 0.4914(4) 0.4545(2) 0.092(2) Uani 1.00 d . . . C22 C 0.3102(1) 0.4492(3) 0.4884(2) 0.071(2) Uani 1.00 d . . . C23 C 0.3429(1) 0.4760(3) 0.4843(1) 0.056(1) Uani 1.00 d . . . C24 C 0.4096(1) 0.4694(3) 0.5179(2) 0.064(2) Uani 1.00 d . . . C25 C 0.4430(1) 0.4266(3) 0.5513(2) 0.054(1) Uani 1.00 d . . . C26 C 0.4651(1) 0.4621(3) 0.5925(2) 0.067(2) Uani 1.00 d . . . C27 C 0.4951(1) 0.4200(4) 0.6244(2) 0.068(2) Uani 1.00 d . . . C28 C 0.5027(1) 0.3425(3) 0.6154(2) 0.060(2) Uani 1.00 d . . . C29 C 0.4813(1) 0.3074(3) 0.5740(2) 0.061(2) Uani 1.00 d . . . C30 C 0.4520(1) 0.3485(3) 0.5418(2) 0.057(1) Uani 1.00 d . . . C31 C 0.5338(1) 0.2945(4) 0.6513(2) 0.086(2) Uani 1.00 d . . . C32 C 0.5214(1) 0.1520(4) 0.6612(2) 0.073(2) Uani 1.00 d . . . C33 C 0.4987(1) 0.0987(4) 0.6748(2) 0.066(2) Uani 1.00 d . . . C34 C 0.4748(1) 0.1311(3) 0.6889(2) 0.069(2) Uani 1.00 d . . . C35 C 0.4539(1) 0.0783(4) 0.7012(2) 0.077(2) Uani 1.00 d . . . C36 C 0.4583(2) -0.0051(5) 0.6991(2) 0.097(2) Uani 1.00 d . . . C37 C 0.4812(2) -0.0396(4) 0.6839(2) 0.101(2) Uani 1.00 d . . . C38 C 0.5023(2) 0.0134(4) 0.6725(2) 0.085(2) Uani 1.00 d . . . C39 C 0.4278(2) 0.1151(5) 0.7165(2) 0.110(3) Uani 1.00 d . . . C40 C 0.4847(3) -0.1320(5) 0.6812(4) 0.184(5) Uani 1.00 d . . . C41 C 0.1796(1) 0.3481(4) 0.3840(2) 0.076(2) Uani 1.00 d . . . C42 C 0.1980(2) 0.3191(6) 0.4270(2) 0.112(3) Uani 1.00 d . . . C43 C 0.2149(3) 0.2420(9) 0.4346(4) 0.151(4) Uani 1.00 d . . . C44 C 0.2118(3) 0.1966(7) 0.3990(6) 0.160(5) Uani 1.00 d . . . C45 C 0.1930(2) 0.2232(5) 0.3553(3) 0.120(3) Uani 1.00 d . . . C46 C 0.1771(1) 0.2991(4) 0.3469(2) 0.078(2) Uani 1.00 d . . . C47 C 0.1451(2) 0.2856(4) 0.2636(3) 0.127(3) Uani 1.00 d . . . C48 C 0.1642(3) 0.2833(5) 0.2400(3) 0.136(4) Uani 1.00 d . . . C49 C 0.1893(1) 0.3485(3) 0.1982(2) 0.068(2) Uani 1.00 d . . . C50 C 0.1977(1) 0.4257(3) 0.1827(2) 0.072(2) Uani 1.00 d . . . C51 C 0.2420(1) 0.5341(3) 0.2075(2) 0.071(2) Uani 1.00 d . . . C52 C 0.2731(1) 0.5656(3) 0.2492(2) 0.069(2) Uani 1.00 d . . . C53 C 0.2837(1) 0.6380(3) 0.3178(2) 0.059(2) Uani 1.00 d . . . C54 C 0.3193(1) 0.6130(3) 0.3403(2) 0.079(2) Uani 1.00 d . . . C55 C 0.3410(2) 0.6398(5) 0.3836(3) 0.107(3) Uani 1.00 d . . . C56 C 0.3275(2) 0.6923(6) 0.4045(2) 0.119(3) Uani 1.00 d . . . C57 C 0.2921(2) 0.7213(4) 0.3823(2) 0.097(2) Uani 1.00 d . . . C58 C 0.2700(2) 0.6927(3) 0.3388(2) 0.068(2) Uani 1.00 d . . . C59 C 0.2202(2) 0.7804(4) 0.3299(3) 0.115(3) Uani 1.00 d . . . C60 C 0.1816(2) 0.7853(4) 0.3029(3) 0.119(3) Uani 1.00 d . . . C61 C 0.1464(3) 0.7319(6) 0.3346(4) 0.168(5) Uani 1.00 d . . . C62 C 0.1299(2) 0.6681(6) 0.3483(3) 0.118(3) Uani 1.00 d . . . C63 C 0.1381(2) 0.5445(5) 0.3882(3) 0.106(3) Uani 1.00 d . . . C64 C 0.1622(2) 0.4735(5) 0.4076(2) 0.098(2) Uani 1.00 d . . . C65 C 0.3367(1) 0.2959(3) 0.4082(2) 0.059(2) Uani 1.00 d . . . C66 C 0.3029(2) 0.2590(4) 0.3835(2) 0.081(2) Uani 1.00 d . . . C67 C 0.2833(2) 0.2750(4) 0.3377(2) 0.091(2) Uani 1.00 d . . . C68 C 0.2969(2) 0.3266(4) 0.3164(2) 0.092(2) Uani 1.00 d . . . C69 C 0.3298(2) 0.3637(3) 0.3399(2) 0.073(2) Uani 1.00 d . . . C70 C 0.3500(1) 0.3478(3) 0.3861(2) 0.060(2) Uani 1.00 d . . . C71 C 0.4012(2) 0.4192(5) 0.3884(2) 0.102(3) Uani 1.00 d . . . C72 C 0.4356(2) 0.4494(6) 0.4182(3) 0.129(3) Uani 1.00 d . . . C73 C 0.4570(3) 0.5752(6) 0.4563(4) 0.157(5) Uani 1.00 d . . . C74 C 0.4622(2) 0.6344(6) 0.4895(3) 0.121(3) Uani 1.00 d . . . C75 C 0.4408(2) 0.7106(5) 0.5347(3) 0.113(3) Uani 1.00 d . . . C76 C 0.4081(2) 0.7369(4) 0.5362(3) 0.112(3) Uani 1.00 d . . . C77 C 0.3600(2) 0.6820(4) 0.5480(2) 0.089(2) Uani 1.00 d . . . C78 C 0.3375(3) 0.7522(4) 0.5278(2) 0.107(3) Uani 1.00 d . . . C79 C 0.3050(3) 0.7569(6) 0.5282(3) 0.142(4) Uani 1.00 d . . . C80 C 0.2937(3) 0.6968(7) 0.5460(3) 0.137(4) Uani 1.00 d . . . C81 C 0.3150(2) 0.6284(5) 0.5656(3) 0.111(3) Uani 1.00 d . . . C82 C 0.3481(2) 0.6228(4) 0.5673(2) 0.082(2) Uani 1.00 d . . . C83 C 0.3737(4) 0.5217(6) 0.6256(3) 0.216(5) Uani 1.00 d . . . C84 C 0.3891(4) 0.4538(5) 0.6408(3) 0.177(4) Uani 1.00 d . . . C85 C 0.3890(2) 0.3147(4) 0.6220(2) 0.091(2) Uani 1.00 d . . . C86 C 0.3976(2) 0.2558(3) 0.5944(2) 0.078(2) Uani 1.00 d . . . C87 C 0.3768(2) 0.2020(3) 0.5201(2) 0.081(2) Uani 1.00 d . . . C88 C 0.3489(2) 0.2126(3) 0.4730(2) 0.078(2) Uani 1.00 d . . . C89 C 0.0510(4) 0.8277(6) 0.2057(4) 0.193(5) Uani 1.00 d . . . C90 C 0.0000 0.108(2) 0.2500 0.33(1) Uiso 1.00 d S . . C91 C 0.0000 0.013(1) 0.2500 0.231(8) Uiso 1.00 d S . . H1 H -0.0289 0.6570 -0.0536 0.0794 Uiso 1.00 calc . . . H2 H -0.1082 0.5622 -0.0291 0.0941 Uiso 1.00 calc . . . H3 H -0.0055 0.5459 0.0674 0.0766 Uiso 1.00 calc . . . H4 H -0.0998 0.7024 -0.0967 0.1253 Uiso 1.00 calc . . . H5 H -0.0961 0.6194 -0.1179 0.1253 Uiso 1.00 calc . . . H6 H -0.1240 0.6277 -0.0988 0.1253 Uiso 1.00 calc . . . H7 H -0.0645 0.5320 0.0814 0.1280 Uiso 1.00 calc . . . H8 H -0.0966 0.4957 0.0390 0.1280 Uiso 1.00 calc . . . H9 H -0.0603 0.4485 0.0610 0.1280 Uiso 1.00 calc . . . H10 H 0.0957 0.5954 0.0689 0.0852 Uiso 1.00 calc . . . H11 H 0.0889 0.6842 0.0813 0.0852 Uiso 1.00 calc . . . H12 H 0.1447 0.6885 0.1505 0.0755 Uiso 1.00 calc . . . H13 H 0.1763 0.6537 0.2271 0.0731 Uiso 1.00 calc . . . H14 H 0.1020 0.4804 0.2106 0.0745 Uiso 1.00 calc . . . H15 H 0.0703 0.5157 0.1348 0.0790 Uiso 1.00 calc . . . H16 H 0.2021 0.4956 0.2596 0.0866 Uiso 1.00 calc . . . H17 H 0.2123 0.5768 0.2878 0.0866 Uiso 1.00 calc . . . H18 H 0.1552 0.4846 0.2802 0.0683 Uiso 1.00 calc . . . H19 H 0.1632 0.5765 0.2951 0.0683 Uiso 1.00 calc . . . H20 H 0.2160 0.4235 0.3252 0.0882 Uiso 1.00 calc . . . H21 H 0.2487 0.4679 0.3244 0.0882 Uiso 1.00 calc . . . H22 H 0.2429 0.5705 0.3705 0.0809 Uiso 1.00 calc . . . H23 H 0.2141 0.5156 0.3751 0.0809 Uiso 1.00 calc . . . H24 H 0.2569 0.4066 0.4052 0.1055 Uiso 1.00 calc . . . H25 H 0.2858 0.4631 0.4018 0.1055 Uiso 1.00 calc . . . H26 H 0.2804 0.5494 0.4556 0.1101 Uiso 1.00 calc . . . H27 H 0.2575 0.4803 0.4626 0.1101 Uiso 1.00 calc . . . H28 H 0.3135 0.4617 0.5182 0.0846 Uiso 1.00 calc . . . H29 H 0.3075 0.3911 0.4835 0.0846 Uiso 1.00 calc . . . H30 H 0.3448 0.5345 0.4872 0.0667 Uiso 1.00 calc . . . H31 H 0.3403 0.4604 0.4551 0.0667 Uiso 1.00 calc . . . H32 H 0.3788 0.4502 0.5491 0.0585 Uiso 1.00 calc . . . H33 H 0.3759 0.3798 0.5155 0.0585 Uiso 1.00 calc . . . H34 H 0.4072 0.4608 0.4881 0.0770 Uiso 1.00 calc . . . H35 H 0.4118 0.5270 0.5245 0.0770 Uiso 1.00 calc . . . H36 H 0.4599 0.5162 0.5993 0.0805 Uiso 1.00 calc . . . H37 H 0.5102 0.4458 0.6525 0.0810 Uiso 1.00 calc . . . H38 H 0.4868 0.2535 0.5673 0.0728 Uiso 1.00 calc . . . H39 H 0.4379 0.3234 0.5131 0.0682 Uiso 1.00 calc . . . H40 H 0.5489 0.3304 0.6751 0.1032 Uiso 1.00 calc . . . H41 H 0.5476 0.2688 0.6382 0.1032 Uiso 1.00 calc . . . H42 H 0.4724 0.1893 0.6902 0.0827 Uiso 1.00 calc . . . H43 H 0.4449 -0.0411 0.7087 0.1162 Uiso 1.00 calc . . . H44 H 0.5191 -0.0086 0.6632 0.1014 Uiso 1.00 calc . . . H45 H 0.4405 0.1484 0.7427 0.1320 Uiso 1.00 calc . . . H46 H 0.4107 0.1482 0.6928 0.1320 Uiso 1.00 calc . . . H47 H 0.4157 0.0718 0.7237 0.1320 Uiso 1.00 calc . . . H48 H 0.4690 -0.1591 0.6906 0.2206 Uiso 1.00 calc . . . H49 H 0.4786 -0.1472 0.6506 0.2206 Uiso 1.00 calc . . . H50 H 0.5088 -0.1481 0.7002 0.2206 Uiso 1.00 calc . . . H51 H 0.1994 0.3513 0.4520 0.1344 Uiso 1.00 calc . . . H52 H 0.2283 0.2221 0.4649 0.1806 Uiso 1.00 calc . . . H53 H 0.2232 0.1439 0.4046 0.1928 Uiso 1.00 calc . . . H54 H 0.1912 0.1890 0.3308 0.1441 Uiso 1.00 calc . . . H55 H 0.1431 0.2302 0.2719 0.1514 Uiso 1.00 calc . . . H56 H 0.1219 0.3060 0.2436 0.1514 Uiso 1.00 calc . . . H57 H 0.1511 0.2513 0.2134 0.1633 Uiso 1.00 calc . . . H58 H 0.1863 0.2564 0.2585 0.1633 Uiso 1.00 calc . . . H59 H 0.2110 0.3188 0.2149 0.0815 Uiso 1.00 calc . . . H60 H 0.1738 0.3169 0.1725 0.0815 Uiso 1.00 calc . . . H61 H 0.1766 0.4591 0.1697 0.0853 Uiso 1.00 calc . . . H62 H 0.2057 0.4145 0.1604 0.0853 Uiso 1.00 calc . . . H63 H 0.2501 0.5136 0.1866 0.0845 Uiso 1.00 calc . . . H64 H 0.2252 0.5776 0.1935 0.0845 Uiso 1.00 calc . . . H65 H 0.2877 0.6002 0.2409 0.0820 Uiso 1.00 calc . . . H66 H 0.2870 0.5204 0.2668 0.0820 Uiso 1.00 calc . . . H67 H 0.3288 0.5768 0.3255 0.0943 Uiso 1.00 calc . . . H68 H 0.3652 0.6218 0.3989 0.1281 Uiso 1.00 calc . . . H69 H 0.3424 0.7096 0.4348 0.1429 Uiso 1.00 calc . . . H70 H 0.2834 0.7601 0.3968 0.1161 Uiso 1.00 calc . . . H71 H 0.2256 0.7719 0.3609 0.1375 Uiso 1.00 calc . . . H72 H 0.2308 0.8308 0.3271 0.1375 Uiso 1.00 calc . . . H73 H 0.1763 0.7858 0.2716 0.1430 Uiso 1.00 calc . . . H74 H 0.1733 0.8352 0.3102 0.1430 Uiso 1.00 calc . . . H75 H 0.1632 0.7575 0.3621 0.2014 Uiso 1.00 calc . . . H76 H 0.1279 0.7701 0.3178 0.2014 Uiso 1.00 calc . . . H77 H 0.1082 0.6533 0.3227 0.1414 Uiso 1.00 calc . . . H78 H 0.1246 0.6896 0.3715 0.1414 Uiso 1.00 calc . . . H79 H 0.1366 0.5746 0.4121 0.1263 Uiso 1.00 calc . . . H80 H 0.1149 0.5246 0.3678 0.1263 Uiso 1.00 calc . . . H81 H 0.1546 0.4426 0.4264 0.1177 Uiso 1.00 calc . . . H82 H 0.1860 0.4928 0.4254 0.1177 Uiso 1.00 calc . . . H83 H 0.2935 0.2230 0.3984 0.0966 Uiso 1.00 calc . . . H84 H 0.2604 0.2501 0.3209 0.1084 Uiso 1.00 calc . . . H85 H 0.2834 0.3372 0.2848 0.1102 Uiso 1.00 calc . . . H86 H 0.3388 0.3999 0.3247 0.0868 Uiso 1.00 calc . . . H87 H 0.4036 0.3796 0.3686 0.1223 Uiso 1.00 calc . . . H88 H 0.3868 0.4640 0.3711 0.1223 Uiso 1.00 calc . . . H89 H 0.4467 0.4685 0.4003 0.1541 Uiso 1.00 calc . . . H90 H 0.4491 0.4046 0.4368 0.1541 Uiso 1.00 calc . . . H91 H 0.4803 0.5532 0.4643 0.1883 Uiso 1.00 calc . . . H92 H 0.4490 0.6055 0.4288 0.1883 Uiso 1.00 calc . . . H93 H 0.4692 0.6842 0.4803 0.1454 Uiso 1.00 calc . . . H94 H 0.4814 0.6153 0.5171 0.1454 Uiso 1.00 calc . . . H95 H 0.4559 0.6850 0.5629 0.1351 Uiso 1.00 calc . . . H96 H 0.4525 0.7580 0.5305 0.1351 Uiso 1.00 calc . . . H97 H 0.3916 0.7566 0.5070 0.1335 Uiso 1.00 calc . . . H98 H 0.4135 0.7803 0.5578 0.1335 Uiso 1.00 calc . . . H99 H 0.3451 0.7951 0.5143 0.1277 Uiso 1.00 calc . . . H100 H 0.2902 0.8039 0.5153 0.1703 Uiso 1.00 calc . . . H101 H 0.2707 0.7009 0.5455 0.1636 Uiso 1.00 calc . . . H102 H 0.3064 0.5851 0.5778 0.1323 Uiso 1.00 calc . . . H103 H 0.3858 0.5614 0.6489 0.2572 Uiso 1.00 calc . . . H104 H 0.3497 0.5153 0.6214 0.2572 Uiso 1.00 calc . . . H105 H 0.3752 0.4265 0.6532 0.2129 Uiso 1.00 calc . . . H106 H 0.4121 0.4669 0.6646 0.2129 Uiso 1.00 calc . . . H107 H 0.4036 0.3027 0.6533 0.1093 Uiso 1.00 calc . . . H108 H 0.3644 0.3082 0.6153 0.1093 Uiso 1.00 calc . . . H109 H 0.3940 0.2011 0.6022 0.0934 Uiso 1.00 calc . . . H110 H 0.4221 0.2627 0.6008 0.0934 Uiso 1.00 calc . . . H111 H 0.3997 0.2003 0.5203 0.0967 Uiso 1.00 calc . . . H112 H 0.3727 0.1514 0.5318 0.0967 Uiso 1.00 calc . . . H113 H 0.3262 0.2215 0.4727 0.0929 Uiso 1.00 calc . . . H114 H 0.3477 0.1646 0.4557 0.0929 Uiso 1.00 calc . . . H115 H 0.0646 0.8772 0.2110 0.2333 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 Cl1 0.193(3) 0.228(3) 0.236(4) -0.032(2) 0.106(3) 0.027(3) Cl2 0.269(4) 0.193(3) 0.442(7) 0.019(3) 0.228(5) -0.011(4) Cl3 0.271(4) 0.144(3) 0.312(5) -0.014(3) -0.034(4) 0.062(3) P1 0.091(1) 0.093(1) 0.0707(10) -0.0105(9) 0.0479(9) -0.0150(9) P2 0.114(1) 0.0680(10) 0.0650(10) -0.0164(9) 0.0310(10) -0.0046(8) F1 0.244(6) 0.152(4) 0.181(5) -0.049(4) 0.154(5) 0.003(3) F2 0.187(4) 0.137(3) 0.139(3) 0.042(3) 0.110(3) 0.009(3) F3 0.185(4) 0.115(3) 0.099(3) -0.013(3) 0.082(3) 0.012(2) F4 0.233(5) 0.173(4) 0.148(4) 0.073(4) 0.122(4) -0.011(3) F5 0.130(3) 0.175(4) 0.091(3) -0.037(3) 0.015(2) -0.009(3) F6 0.127(4) 0.223(5) 0.135(4) -0.028(4) 0.026(3) -0.055(4) F7 0.49(1) 0.227(7) 0.156(5) -0.193(8) 0.198(7) -0.057(4) F8 0.264(7) 0.111(4) 0.274(7) 0.025(4) 0.149(6) -0.015(4) F9 0.353(9) 0.224(6) 0.231(7) -0.148(6) 0.215(7) -0.049(5) F10 0.45(1) 0.112(4) 0.216(7) 0.041(6) 0.130(8) -0.054(4) F11 0.197(6) 0.37(1) 0.148(5) -0.065(7) -0.028(5) -0.006(6) F12 0.126(4) 0.344(9) 0.122(4) 0.020(5) 0.015(3) -0.054(5) O1 0.064(2) 0.129(3) 0.075(3) -0.008(2) 0.023(2) 0.034(2) O2 0.047(2) 0.089(2) 0.059(2) -0.003(2) 0.013(2) 0.014(2) O3 0.082(2) 0.085(3) 0.080(3) 0.006(2) 0.042(2) 0.011(2) O4 0.160(5) 0.108(3) 0.202(6) 0.032(3) 0.150(5) 0.023(3) O5 0.104(3) 0.071(2) 0.082(3) -0.014(2) 0.057(2) -0.011(2) O6 0.091(3) 0.071(2) 0.072(2) -0.019(2) 0.047(2) -0.018(2) O7 0.067(2) 0.079(2) 0.043(2) -0.017(2) 0.021(2) -0.011(2) O8 0.060(2) 0.066(2) 0.062(2) 0.000(2) 0.026(2) -0.012(2) O9 0.082(3) 0.070(2) 0.089(3) -0.006(2) 0.048(2) -0.021(2) O10 0.132(4) 0.079(3) 0.211(6) 0.011(3) 0.113(4) -0.009(3) O11 0.125(4) 0.105(3) 0.123(4) 0.014(3) 0.092(3) -0.002(3) O12 0.081(2) 0.091(3) 0.062(2) -0.017(2) 0.034(2) -0.013(2) O13 0.081(2) 0.089(2) 0.066(2) -0.025(2) 0.042(2) 0.002(2) O14 0.139(4) 0.193(5) 0.123(4) -0.112(4) 0.098(4) -0.064(4) O15 0.132(4) 0.105(4) 0.184(5) -0.052(3) 0.102(4) -0.025(4) O16 0.142(4) 0.068(3) 0.114(3) -0.005(3) 0.076(3) 0.016(2) O17 0.148(4) 0.065(2) 0.079(3) 0.013(2) 0.066(3) 0.012(2) O18 0.149(4) 0.072(2) 0.060(2) 0.015(2) 0.062(2) 0.014(2) O19 0.084(2) 0.057(2) 0.055(2) 0.000(2) 0.032(2) 0.006(2) O20 0.084(2) 0.061(2) 0.061(2) -0.021(2) 0.038(2) -0.001(2) N1 0.053(2) 0.111(3) 0.045(2) 0.007(2) 0.014(2) 0.000(2) N2 0.054(2) 0.053(2) 0.040(2) -0.006(2) 0.021(2) 0.009(2) C1 0.051(3) 0.056(3) 0.057(3) 0.001(2) 0.021(3) -0.008(2) C2 0.052(3) 0.079(4) 0.061(3) 0.002(3) 0.018(3) -0.006(3) C3 0.058(3) 0.080(4) 0.068(3) 0.006(3) 0.016(3) -0.020(3) C4 0.049(3) 0.083(4) 0.094(4) -0.008(3) 0.023(3) -0.030(4) C5 0.056(3) 0.074(4) 0.082(4) -0.009(3) 0.029(3) -0.009(3) C6 0.053(3) 0.066(3) 0.064(3) -0.001(2) 0.017(3) -0.001(3) C7 0.068(4) 0.145(6) 0.074(4) 0.014(4) 0.007(3) -0.010(4) C8 0.088(4) 0.122(5) 0.118(5) -0.030(4) 0.053(4) -0.007(4) C9 0.054(3) 0.066(3) 0.058(3) 0.000(3) 0.016(3) 0.007(3) C10 0.044(3) 0.095(4) 0.065(3) -0.014(3) 0.016(2) 0.014(3) C11 0.047(3) 0.062(3) 0.062(3) 0.002(2) 0.024(2) 0.010(3) C12 0.055(3) 0.062(3) 0.065(3) -0.009(2) 0.020(3) 0.016(3) C13 0.050(3) 0.058(3) 0.062(3) -0.008(2) 0.012(2) 0.004(3) C14 0.048(3) 0.051(3) 0.054(3) 0.004(2) 0.029(2) 0.004(2) C15 0.046(3) 0.069(3) 0.071(3) -0.002(2) 0.025(3) 0.019(3) C16 0.046(3) 0.078(4) 0.068(3) -0.008(2) 0.020(3) 0.012(3) C17 0.053(3) 0.061(3) 0.061(3) 0.009(2) 0.028(2) 0.010(2) C18 0.057(3) 0.096(4) 0.061(3) 0.005(3) 0.020(3) 0.009(3) C19 0.058(3) 0.085(4) 0.055(3) -0.008(3) 0.020(3) 0.009(3) C20 0.062(3) 0.128(5) 0.062(4) 0.000(3) 0.017(3) -0.001(3) C21 0.064(3) 0.138(5) 0.067(4) 0.003(3) 0.023(3) 0.017(4) C22 0.055(3) 0.094(4) 0.054(3) 0.000(3) 0.016(3) 0.010(3) C23 0.063(3) 0.056(3) 0.043(3) 0.006(2) 0.019(2) 0.012(2) C24 0.064(3) 0.070(3) 0.065(3) -0.008(3) 0.034(3) 0.016(3) C25 0.050(3) 0.064(3) 0.054(3) -0.012(2) 0.029(2) 0.004(3) C26 0.078(4) 0.064(3) 0.067(3) -0.011(3) 0.038(3) -0.009(3) C27 0.060(3) 0.083(4) 0.056(3) -0.012(3) 0.022(3) -0.011(3) C28 0.047(3) 0.072(3) 0.064(3) -0.005(3) 0.026(3) 0.008(3) C29 0.054(3) 0.061(3) 0.073(3) -0.004(2) 0.033(3) -0.006(3) C30 0.055(3) 0.066(3) 0.057(3) -0.018(3) 0.031(3) -0.012(3) C31 0.061(3) 0.089(4) 0.105(4) -0.007(3) 0.034(3) 0.024(4) C32 0.066(3) 0.079(4) 0.074(4) 0.017(3) 0.030(3) 0.020(3) C33 0.053(3) 0.088(4) 0.052(3) 0.013(3) 0.018(2) 0.015(3) C34 0.048(3) 0.093(4) 0.054(3) 0.007(3) 0.011(3) 0.010(3) C35 0.045(3) 0.119(5) 0.057(3) 0.005(3) 0.013(3) 0.018(3) C36 0.074(4) 0.104(5) 0.098(5) -0.006(4) 0.024(4) 0.028(4) C37 0.097(5) 0.080(5) 0.116(5) 0.009(4) 0.038(4) 0.024(4) C38 0.085(4) 0.077(4) 0.088(4) 0.011(3) 0.035(4) 0.014(3) C39 0.060(4) 0.186(7) 0.087(4) 0.004(4) 0.034(3) 0.029(5) C40 0.186(9) 0.086(6) 0.28(1) 0.011(6) 0.100(9) 0.037(7) C41 0.062(3) 0.085(4) 0.078(4) -0.025(3) 0.027(3) 0.006(4) C42 0.090(5) 0.129(6) 0.090(5) -0.032(5) 0.015(4) 0.028(5) C43 0.105(6) 0.17(1) 0.135(9) -0.025(7) 0.016(7) 0.071(8) C44 0.108(7) 0.136(9) 0.23(1) 0.032(6) 0.068(9) 0.102(10) C45 0.109(6) 0.097(5) 0.194(9) 0.016(5) 0.103(6) 0.038(6) C46 0.061(3) 0.075(4) 0.110(5) -0.008(3) 0.048(4) 0.012(4) C47 0.198(8) 0.084(5) 0.148(7) -0.061(5) 0.122(7) -0.054(5) C48 0.201(9) 0.111(6) 0.141(7) -0.069(6) 0.117(7) -0.050(5) C49 0.068(3) 0.067(3) 0.059(3) -0.004(3) 0.019(3) -0.018(3) C50 0.079(4) 0.075(4) 0.054(3) -0.001(3) 0.024(3) -0.009(3) C51 0.085(4) 0.075(3) 0.064(3) -0.010(3) 0.045(3) -0.010(3) C52 0.069(3) 0.071(3) 0.076(4) -0.006(3) 0.042(3) -0.010(3) C53 0.063(3) 0.056(3) 0.058(3) -0.016(3) 0.026(3) -0.002(3) C54 0.065(4) 0.080(4) 0.084(4) -0.012(3) 0.026(3) -0.004(3) C55 0.076(4) 0.134(6) 0.096(5) -0.034(4) 0.026(4) -0.013(5) C56 0.107(6) 0.158(7) 0.069(4) -0.066(6) 0.018(4) -0.020(5) C57 0.114(5) 0.111(5) 0.080(4) -0.051(4) 0.055(4) -0.036(4) C58 0.074(4) 0.068(3) 0.067(3) -0.023(3) 0.037(3) -0.008(3) C59 0.119(6) 0.071(4) 0.183(8) -0.016(4) 0.093(6) -0.047(5) C60 0.142(7) 0.064(4) 0.194(8) 0.018(4) 0.113(7) 0.003(5) C61 0.21(1) 0.127(8) 0.24(1) 0.068(7) 0.160(10) 0.030(7) C62 0.106(5) 0.118(6) 0.159(7) 0.004(5) 0.085(5) -0.017(6) C63 0.107(5) 0.122(6) 0.112(5) -0.029(5) 0.071(5) -0.034(5) C64 0.124(5) 0.120(5) 0.073(4) -0.048(5) 0.064(4) -0.025(4) C65 0.068(3) 0.053(3) 0.061(3) -0.007(3) 0.032(3) -0.009(3) C66 0.075(4) 0.082(4) 0.094(5) -0.015(3) 0.045(4) -0.021(3) C67 0.072(4) 0.098(5) 0.087(5) -0.007(4) 0.021(4) -0.020(4) C68 0.092(5) 0.087(4) 0.068(4) 0.012(4) 0.010(4) -0.011(3) C69 0.090(4) 0.065(3) 0.065(4) 0.008(3) 0.038(3) 0.004(3) C70 0.065(3) 0.054(3) 0.068(3) -0.003(3) 0.036(3) -0.009(3) C71 0.110(5) 0.127(5) 0.099(5) -0.027(4) 0.074(4) -0.013(4) C72 0.106(5) 0.193(8) 0.126(6) -0.070(6) 0.087(5) -0.043(6) C73 0.156(8) 0.146(8) 0.25(1) -0.046(7) 0.161(9) -0.033(8) C74 0.080(5) 0.144(7) 0.151(7) -0.037(5) 0.061(5) -0.008(6) C75 0.134(6) 0.088(5) 0.099(5) -0.063(5) 0.037(5) -0.009(4) C76 0.134(6) 0.088(5) 0.130(6) -0.028(5) 0.075(5) -0.006(4) C77 0.121(6) 0.077(4) 0.073(4) -0.005(4) 0.048(4) -0.017(3) C78 0.140(7) 0.080(5) 0.089(5) 0.017(5) 0.042(5) 0.017(4) C79 0.138(8) 0.122(7) 0.132(7) 0.036(7) 0.029(6) 0.025(6) C80 0.140(7) 0.127(7) 0.133(7) 0.023(7) 0.052(6) -0.006(6) C81 0.130(6) 0.097(5) 0.118(6) 0.005(5) 0.068(5) 0.001(4) C82 0.125(6) 0.061(4) 0.067(4) -0.004(4) 0.048(4) -0.006(3) C83 0.44(2) 0.149(8) 0.096(6) 0.16(1) 0.153(9) 0.053(6) C84 0.38(2) 0.105(6) 0.097(6) 0.076(8) 0.146(8) 0.021(5) C85 0.126(5) 0.093(4) 0.061(4) -0.006(4) 0.047(4) 0.019(3) C86 0.099(4) 0.065(3) 0.071(4) 0.010(3) 0.039(3) 0.023(3) C87 0.112(5) 0.052(3) 0.094(4) -0.013(3) 0.060(4) 0.007(3) C88 0.107(4) 0.063(3) 0.075(4) -0.026(3) 0.052(4) -0.005(3) C89 0.23(1) 0.113(7) 0.20(1) -0.043(8) 0.063(10) 0.054(7) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'teXsan (MSC & Rigaku, 1999)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'teXsan (MSC & Rigaku, 1999)' _computing_publication_material 'teXsan (MSC & Rigaku, 1999)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' #------------------------------------------------------------------------------ _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 CL1 C89 1.73(1) . . yes CL2 C89 1.66(1) . . yes CL3 C89 1.63(1) . . yes P1 F1 1.563(4) . . yes P1 F2 1.561(4) . . yes P1 F3 1.560(4) . . yes P1 F4 1.544(4) . . yes P1 F5 1.566(4) . . yes P1 F6 1.562(4) . . yes P2 F7 1.494(6) . . yes P2 F8 1.527(5) . . yes P2 F9 1.495(5) . . yes P2 F10 1.502(5) . . yes P2 F11 1.512(6) . . yes P2 F12 1.518(5) . . yes O1 C9 1.204(6) . . yes O2 C9 1.340(6) . . yes O2 C10 1.455(5) . . yes O3 C31 1.458(6) . . yes O3 C32 1.332(7) . . yes O4 C32 1.184(7) . . yes O5 C46 1.385(7) . . yes O5 C47 1.441(7) . . yes O6 C48 1.436(8) . . yes O6 C49 1.389(6) . . yes O7 C50 1.446(6) . . yes O7 C51 1.411(6) . . yes O8 C52 1.433(6) . . yes O8 C53 1.368(5) . . yes O9 C58 1.368(6) . . yes O9 C59 1.445(7) . . yes O10 C60 1.379(8) . . yes O10 C61 1.30(1) . . yes O11 C62 1.389(9) . . yes O11 C63 1.380(8) . . yes O12 C41 1.370(7) . . yes O12 C64 1.425(7) . . yes O13 C70 1.386(6) . . yes O13 C71 1.443(7) . . yes O14 C72 1.383(9) . . yes O14 C73 1.254(9) . . yes O15 C74 1.352(9) . . yes O15 C75 1.422(9) . . yes O16 C76 1.402(8) . . yes O16 C77 1.358(8) . . yes O17 C82 1.394(7) . . yes O17 C83 1.367(9) . . yes O18 C84 1.383(8) . . yes O18 C85 1.391(7) . . yes O19 C86 1.402(6) . . yes O19 C87 1.415(6) . . yes O20 C65 1.381(6) . . yes O20 C88 1.422(6) . . yes O21 C90 1.41(2) . . yes N1 C17 1.459(6) . . yes N1 C18 1.484(6) . . yes N1 H16 0.950 . . no N1 H17 0.950 . . no N2 C23 1.509(5) . . yes N2 C24 1.474(6) . . yes N2 H32 0.950 . . no N2 H33 0.950 . . no C1 C2 1.400(6) . . yes C1 C6 1.401(7) . . yes C1 C9 1.472(7) . . yes C2 C3 1.370(7) . . yes C2 H1 0.950 . . no C3 C4 1.403(8) . . yes C3 C7 1.526(8) . . yes C4 C5 1.382(8) . . yes C4 H2 0.950 . . no C5 C6 1.391(7) . . yes C5 C8 1.500(8) . . yes C6 H3 0.950 . . no C7 H4 0.950 . . no C7 H5 0.949 . . no C7 H6 0.950 . . no C8 H7 0.951 . . no C8 H8 0.950 . . no C8 H9 0.950 . . no C10 C11 1.503(7) . . yes C10 H10 0.951 . . no C10 H11 0.950 . . no C11 C12 1.389(6) . . yes C11 C16 1.370(6) . . yes C12 C13 1.391(6) . . yes C12 H12 0.950 . . no C13 C14 1.383(6) . . yes C13 H13 0.950 . . no C14 C15 1.388(6) . . yes C14 C17 1.496(6) . . yes C15 C16 1.379(7) . . yes C15 H14 0.950 . . no C16 H15 0.950 . . no C17 H18 0.950 . . no C17 H19 0.950 . . no C18 C19 1.476(7) . . yes C18 H20 0.950 . . no C18 H21 0.950 . . no C19 C20 1.571(7) . . yes C19 H22 0.951 . . no C19 H23 0.950 . . no C20 C21 1.478(8) . . yes C20 H24 0.951 . . no C20 H25 0.950 . . no C21 C22 1.513(7) . . yes C21 H26 0.951 . . no C21 H27 0.950 . . no C22 C23 1.487(7) . . yes C22 H28 0.950 . . no C22 H29 0.951 . . no C23 H30 0.950 . . no C23 H31 0.951 . . no C24 C25 1.498(7) . . yes C24 H34 0.951 . . no C24 H35 0.950 . . no C25 C26 1.377(6) . . yes C25 C30 1.391(7) . . yes C26 C27 1.395(7) . . yes C26 H36 0.950 . . no C27 C28 1.356(7) . . yes C27 H37 0.950 . . no C28 C29 1.373(7) . . yes C28 C31 1.518(7) . . yes C29 C30 1.374(7) . . yes C29 H38 0.950 . . no C30 H39 0.951 . . no C31 H40 0.950 . . no C31 H41 0.950 . . no C32 C33 1.485(8) . . yes C33 C34 1.375(7) . . yes C33 C38 1.392(8) . . yes C34 C35 1.399(7) . . yes C34 H42 0.949 . . no C35 C36 1.365(9) . . yes C35 C39 1.508(8) . . yes C36 C37 1.376(9) . . yes C36 H43 0.951 . . no C37 C38 1.393(9) . . yes C37 C40 1.51(1) . . yes C38 H44 0.949 . . no C39 H45 0.950 . . no C39 H46 0.950 . . no C39 H47 0.951 . . no C40 H48 0.949 . . no C40 H49 0.953 . . no C40 H50 0.948 . . no C41 C42 1.356(9) . . yes C41 C46 1.416(8) . . yes C42 C43 1.40(1) . . yes C42 H51 0.951 . . no C43 C44 1.34(1) . . yes C43 H52 0.952 . . no C44 C45 1.36(1) . . yes C44 H53 0.951 . . no C45 C46 1.362(9) . . yes C45 H54 0.950 . . no C47 C48 1.334(10) . . yes C47 H55 0.951 . . no C47 H56 0.951 . . no C48 H57 0.948 . . no C48 H58 0.952 . . no C49 C50 1.446(7) . . yes C49 H59 0.950 . . no C49 H60 0.951 . . no C50 H61 0.950 . . no C50 H62 0.950 . . no C51 C52 1.493(7) . . yes C51 H63 0.950 . . no C51 H64 0.950 . . no C52 H65 0.950 . . no C52 H66 0.950 . . no C53 C54 1.389(7) . . yes C53 C58 1.391(7) . . yes C54 C55 1.370(9) . . yes C54 H67 0.950 . . no C55 C56 1.36(1) . . yes C55 H68 0.949 . . no C56 C57 1.40(1) . . yes C56 H69 0.950 . . no C57 C58 1.388(8) . . yes C57 H70 0.951 . . no C59 C60 1.45(1) . . yes C59 H71 0.951 . . no C59 H72 0.950 . . no C60 H73 0.951 . . no C60 H74 0.950 . . no C61 C62 1.42(1) . . yes C61 H75 0.954 . . no C61 H76 0.949 . . no C62 H77 0.950 . . no C62 H78 0.950 . . no C63 C64 1.468(10) . . yes C63 H79 0.949 . . no C63 H80 0.950 . . no C64 H81 0.950 . . no C64 H82 0.951 . . no C65 C66 1.404(7) . . yes C65 C70 1.374(7) . . yes C66 C67 1.380(8) . . yes C66 H83 0.950 . . no C67 C68 1.362(9) . . yes C67 H84 0.950 . . no C68 C69 1.372(8) . . yes C68 H85 0.950 . . no C69 C70 1.391(7) . . yes C69 H86 0.950 . . no C71 C72 1.411(9) . . yes C71 H87 0.950 . . no C71 H88 0.951 . . no C72 H89 0.949 . . no C72 H90 0.950 . . no C73 C74 1.39(1) . . yes C73 H91 0.952 . . no C73 H92 0.948 . . no C74 H93 0.950 . . no C74 H94 0.951 . . no C75 C76 1.45(1) . . yes C75 H95 0.951 . . no C75 H96 0.949 . . no C76 H97 0.951 . . no C76 H98 0.951 . . no C77 C78 1.430(9) . . yes C77 C82 1.359(8) . . yes C78 C79 1.36(1) . . yes C78 H99 0.950 . . no C79 C80 1.33(1) . . yes C79 H100 0.949 . . no C80 C81 1.38(1) . . yes C80 H101 0.950 . . no C81 C82 1.358(10) . . yes C81 H102 0.951 . . no C83 C84 1.25(1) . . yes C83 H103 0.952 . . no C83 H104 0.949 . . no C84 H105 0.950 . . no C84 H106 0.952 . . no C85 C86 1.465(8) . . yes C85 H107 0.951 . . no C85 H108 0.951 . . no C86 H109 0.949 . . no C86 H110 0.951 . . no C87 C88 1.471(8) . . yes C87 H111 0.949 . . no C87 H112 0.950 . . no C88 H113 0.952 . . no C88 H114 0.950 . . no C89 H115 0.950 . . no C90 C91 1.52(3) . . 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 F1 P1 F2 88.8(3) . . . yes F1 P1 F3 179.1(3) . . . yes F1 P1 F4 88.4(3) . . . yes F1 P1 F5 87.8(3) . . . yes F1 P1 F6 90.3(3) . . . yes F2 P1 F3 91.6(2) . . . yes F2 P1 F4 176.5(3) . . . yes F2 P1 F5 90.8(3) . . . yes F2 P1 F6 87.2(3) . . . yes F3 P1 F4 91.1(3) . . . yes F3 P1 F5 93.0(2) . . . yes F3 P1 F6 88.9(3) . . . yes F4 P1 F5 91.2(3) . . . yes F4 P1 F6 90.7(3) . . . yes F5 P1 F6 177.2(3) . . . yes F7 P2 F8 88.5(4) . . . yes F7 P2 F9 176.4(5) . . . yes F7 P2 F10 88.1(5) . . . yes F7 P2 F11 86.8(5) . . . yes F7 P2 F12 90.3(4) . . . yes F8 P2 F9 88.4(4) . . . yes F8 P2 F10 174.7(5) . . . yes F8 P2 F11 97.6(5) . . . yes F8 P2 F12 82.2(4) . . . yes F9 P2 F10 95.1(4) . . . yes F9 P2 F11 91.9(5) . . . yes F9 P2 F12 90.9(4) . . . yes F10 P2 F11 86.3(5) . . . yes F10 P2 F12 93.7(5) . . . yes F11 P2 F12 177.1(5) . . . yes C9 O2 C10 116.2(4) . . . yes C31 O3 C32 119.5(5) . . . yes C46 O5 C47 121.2(5) . . . yes C48 O6 C49 110.3(5) . . . yes C50 O7 C51 114.6(4) . . . yes C52 O8 C53 117.8(4) . . . yes C58 O9 C59 118.4(5) . . . yes C60 O10 C61 118.7(7) . . . yes C62 O11 C63 114.4(6) . . . yes C41 O12 C64 117.8(5) . . . yes C70 O13 C71 115.5(4) . . . yes C72 O14 C73 125.3(6) . . . yes C74 O15 C75 118.8(6) . . . yes C76 O16 C77 118.5(6) . . . yes C82 O17 C83 118.7(6) . . . yes C84 O18 C85 114.3(5) . . . yes C86 O19 C87 114.0(4) . . . yes C65 O20 C88 115.7(4) . . . yes C17 N1 C18 120.3(4) . . . yes C17 N1 H16 106.7 . . . no C17 N1 H17 106.7 . . . no C18 N1 H16 106.7 . . . no C18 N1 H17 106.7 . . . no H16 N1 H17 109.4 . . . no C23 N2 C24 113.1(3) . . . yes C23 N2 H32 108.5 . . . no C23 N2 H33 108.6 . . . no C24 N2 H32 108.6 . . . no C24 N2 H33 108.6 . . . no H32 N2 H33 109.4 . . . no C2 C1 C6 119.2(4) . . . yes C2 C1 C9 118.6(5) . . . yes C6 C1 C9 122.2(4) . . . yes C1 C2 C3 121.0(5) . . . yes C1 C2 H1 119.5 . . . no C3 C2 H1 119.5 . . . no C2 C3 C4 118.7(5) . . . yes C2 C3 C7 121.7(6) . . . yes C4 C3 C7 119.5(5) . . . yes C3 C4 C5 121.8(5) . . . yes C3 C4 H2 119.1 . . . no C5 C4 H2 119.1 . . . no C4 C5 C6 118.7(5) . . . yes C4 C5 C8 120.8(5) . . . yes C6 C5 C8 120.5(5) . . . yes C1 C6 C5 120.5(5) . . . yes C1 C6 H3 119.8 . . . no C5 C6 H3 119.8 . . . no C3 C7 H4 109.4 . . . no C3 C7 H5 109.5 . . . no C3 C7 H6 109.5 . . . no H4 C7 H5 109.5 . . . no H4 C7 H6 109.4 . . . no H5 C7 H6 109.5 . . . no C5 C8 H7 109.5 . . . no C5 C8 H8 109.5 . . . no C5 C8 H9 109.5 . . . no H7 C8 H8 109.4 . . . no H7 C8 H9 109.4 . . . no H8 C8 H9 109.5 . . . no O1 C9 O2 122.1(5) . . . yes O1 C9 C1 125.4(5) . . . yes O2 C9 C1 112.5(5) . . . yes O2 C10 C11 108.2(4) . . . yes O2 C10 H10 109.8 . . . no O2 C10 H11 109.8 . . . no C11 C10 H10 109.8 . . . no C11 C10 H11 109.8 . . . no H10 C10 H11 109.4 . . . no C10 C11 C12 118.6(4) . . . yes C10 C11 C16 122.8(4) . . . yes C12 C11 C16 118.6(4) . . . yes C11 C12 C13 120.5(4) . . . yes C11 C12 H12 119.7 . . . no C13 C12 H12 119.7 . . . no C12 C13 C14 121.1(4) . . . yes C12 C13 H13 119.5 . . . no C14 C13 H13 119.4 . . . no C13 C14 C15 117.3(4) . . . yes C13 C14 C17 121.2(4) . . . yes C15 C14 C17 121.4(4) . . . yes C14 C15 C16 121.9(4) . . . yes C14 C15 H14 119.1 . . . no C16 C15 H14 119.0 . . . no C11 C16 C15 120.6(4) . . . yes C11 C16 H15 119.7 . . . no C15 C16 H15 119.6 . . . no N1 C17 C14 110.4(4) . . . yes N1 C17 H18 109.2 . . . no N1 C17 H19 109.3 . . . no C14 C17 H18 109.3 . . . no C14 C17 H19 109.3 . . . no H18 C17 H19 109.4 . . . no N1 C18 C19 115.3(5) . . . yes N1 C18 H20 108.0 . . . no N1 C18 H21 108.0 . . . no C19 C18 H20 108.0 . . . no C19 C18 H21 108.0 . . . no H20 C18 H21 109.4 . . . no C18 C19 C20 106.5(5) . . . yes C18 C19 H22 110.3 . . . no C18 C19 H23 110.3 . . . no C20 C19 H22 110.2 . . . no C20 C19 H23 110.2 . . . no H22 C19 H23 109.4 . . . no C19 C20 C21 114.0(5) . . . yes C19 C20 H24 108.2 . . . no C19 C20 H25 108.3 . . . no C21 C20 H24 108.4 . . . no C21 C20 H25 108.5 . . . no H24 C20 H25 109.4 . . . no C20 C21 C22 112.0(5) . . . yes C20 C21 H26 108.9 . . . no C20 C21 H27 109.0 . . . no C22 C21 H26 108.8 . . . no C22 C21 H27 108.9 . . . no H26 C21 H27 109.4 . . . no C21 C22 C23 113.1(4) . . . yes C21 C22 H28 108.6 . . . no C21 C22 H29 108.5 . . . no C23 C22 H28 108.6 . . . no C23 C22 H29 108.6 . . . no H28 C22 H29 109.4 . . . no N2 C23 C22 113.2(4) . . . yes N2 C23 H30 108.6 . . . no N2 C23 H31 108.5 . . . no C22 C23 H30 108.5 . . . no C22 C23 H31 108.5 . . . no H30 C23 H31 109.4 . . . no N2 C24 C25 112.2(4) . . . yes N2 C24 H34 108.8 . . . no N2 C24 H35 108.8 . . . no C25 C24 H34 108.8 . . . no C25 C24 H35 108.8 . . . no H34 C24 H35 109.4 . . . no C24 C25 C26 121.4(5) . . . yes C24 C25 C30 120.6(4) . . . yes C26 C25 C30 118.0(4) . . . yes C25 C26 C27 121.1(5) . . . yes C25 C26 H36 119.5 . . . no C27 C26 H36 119.4 . . . no C26 C27 C28 120.2(4) . . . yes C26 C27 H37 119.9 . . . no C28 C27 H37 119.9 . . . no C27 C28 C29 119.2(4) . . . yes C27 C28 C31 120.2(5) . . . yes C29 C28 C31 120.6(5) . . . yes C28 C29 C30 121.4(5) . . . yes C28 C29 H38 119.3 . . . no C30 C29 H38 119.2 . . . no C25 C30 C29 120.1(4) . . . yes C25 C30 H39 120.0 . . . no C29 C30 H39 119.9 . . . no O3 C31 C28 106.3(4) . . . yes O3 C31 H40 110.3 . . . no O3 C31 H41 110.2 . . . no C28 C31 H40 110.3 . . . no C28 C31 H41 110.3 . . . no H40 C31 H41 109.4 . . . no O3 C32 O4 122.8(6) . . . yes O3 C32 C33 111.7(5) . . . yes O4 C32 C33 125.4(6) . . . yes C32 C33 C34 122.3(5) . . . yes C32 C33 C38 117.3(5) . . . yes C34 C33 C38 120.4(5) . . . yes C33 C34 C35 120.2(5) . . . yes C33 C34 H42 119.9 . . . no C35 C34 H42 119.9 . . . no C34 C35 C36 118.2(6) . . . yes C34 C35 C39 119.3(6) . . . yes C36 C35 C39 122.5(6) . . . yes C35 C36 C37 123.1(6) . . . yes C35 C36 H43 118.4 . . . no C37 C36 H43 118.4 . . . no C36 C37 C38 118.2(6) . . . yes C36 C37 C40 121.7(8) . . . yes C38 C37 C40 120.1(8) . . . yes C33 C38 C37 119.8(6) . . . yes C33 C38 H44 120.1 . . . no C37 C38 H44 120.1 . . . no C35 C39 H45 109.5 . . . no C35 C39 H46 109.5 . . . no C35 C39 H47 109.5 . . . no H45 C39 H46 109.5 . . . no H45 C39 H47 109.4 . . . no H46 C39 H47 109.4 . . . no C37 C40 H48 109.6 . . . no C37 C40 H49 109.3 . . . no C37 C40 H50 109.6 . . . no H48 C40 H49 109.3 . . . no H48 C40 H50 109.7 . . . no H49 C40 H50 109.3 . . . no O12 C41 C42 125.5(7) . . . yes O12 C41 C46 114.9(5) . . . yes C42 C41 C46 119.6(7) . . . yes C41 C42 C43 119.8(8) . . . yes C41 C42 H51 120.0 . . . no C43 C42 H51 120.2 . . . no C42 C43 C44 119.4(10) . . . yes C42 C43 H52 120.0 . . . no C44 C43 H52 120.6 . . . no C43 C44 C45 122(1) . . . yes C43 C44 H53 118.6 . . . no C45 C44 H53 119.1 . . . no C44 C45 C46 119.6(9) . . . yes C44 C45 H54 120.1 . . . no C46 C45 H54 120.3 . . . no O5 C46 C41 115.1(5) . . . yes O5 C46 C45 125.7(7) . . . yes C41 C46 C45 119.2(7) . . . yes O5 C47 C48 119.2(7) . . . yes O5 C47 H55 106.9 . . . no O5 C47 H56 106.9 . . . no C48 C47 H55 107.2 . . . no C48 C47 H56 107.1 . . . no H55 C47 H56 109.3 . . . no O6 C48 C47 117.1(7) . . . yes O6 C48 H57 107.6 . . . no O6 C48 H58 107.5 . . . no C47 C48 H57 107.6 . . . no C47 C48 H58 107.4 . . . no H57 C48 H58 109.4 . . . no O6 C49 C50 112.0(4) . . . yes O6 C49 H59 108.9 . . . no O6 C49 H60 108.8 . . . no C50 C49 H59 108.9 . . . no C50 C49 H60 108.9 . . . no H59 C49 H60 109.4 . . . no O7 C50 C49 110.3(4) . . . yes O7 C50 H61 109.3 . . . no O7 C50 H62 109.3 . . . no C49 C50 H61 109.3 . . . no C49 C50 H62 109.3 . . . no H61 C50 H62 109.4 . . . no O7 C51 C52 108.3(4) . . . yes O7 C51 H63 109.8 . . . no O7 C51 H64 109.8 . . . no C52 C51 H63 109.7 . . . no C52 C51 H64 109.8 . . . no H63 C51 H64 109.4 . . . no O8 C52 C51 108.5(4) . . . yes O8 C52 H65 109.6 . . . no O8 C52 H66 109.7 . . . no C51 C52 H65 109.7 . . . no C51 C52 H66 109.8 . . . no H65 C52 H66 109.5 . . . no O8 C53 C54 125.1(5) . . . yes O8 C53 C58 115.2(4) . . . yes C54 C53 C58 119.8(5) . . . yes C53 C54 C55 120.7(6) . . . yes C53 C54 H67 119.7 . . . no C55 C54 H67 119.6 . . . no C54 C55 C56 119.6(7) . . . yes C54 C55 H68 120.2 . . . no C56 C55 H68 120.2 . . . no C55 C56 C57 121.4(6) . . . yes C55 C56 H69 119.3 . . . no C57 C56 H69 119.3 . . . no C56 C57 C58 118.9(6) . . . yes C56 C57 H70 120.6 . . . no C58 C57 H70 120.5 . . . no O9 C58 C53 115.5(4) . . . yes O9 C58 C57 124.9(6) . . . yes C53 C58 C57 119.6(6) . . . yes O9 C59 C60 110.1(6) . . . yes O9 C59 H71 109.4 . . . no O9 C59 H72 109.4 . . . no C60 C59 H71 109.3 . . . no C60 C59 H72 109.3 . . . no H71 C59 H72 109.4 . . . no O10 C60 C59 112.6(7) . . . yes O10 C60 H73 108.7 . . . no O10 C60 H74 108.7 . . . no C59 C60 H73 108.6 . . . no C59 C60 H74 108.7 . . . no H73 C60 H74 109.4 . . . no O10 C61 C62 124.1(8) . . . yes O10 C61 H75 105.7 . . . no O10 C61 H76 106.1 . . . no C62 C61 H75 105.4 . . . no C62 C61 H76 105.7 . . . no H75 C61 H76 109.3 . . . no O11 C62 C61 115.5(7) . . . yes O11 C62 H77 108.0 . . . no O11 C62 H78 107.9 . . . no C61 C62 H77 107.8 . . . no C61 C62 H78 108.1 . . . no H77 C62 H78 109.4 . . . no O11 C63 C64 111.7(6) . . . yes O11 C63 H79 108.9 . . . no O11 C63 H80 108.9 . . . no C64 C63 H79 108.9 . . . no C64 C63 H80 108.8 . . . no H79 C63 H80 109.6 . . . no O12 C64 C63 109.8(5) . . . yes O12 C64 H81 109.4 . . . no O12 C64 H82 109.3 . . . no C63 C64 H81 109.5 . . . no C63 C64 H82 109.5 . . . no H81 C64 H82 109.4 . . . no O20 C65 C66 123.5(5) . . . yes O20 C65 C70 117.1(4) . . . yes C66 C65 C70 119.4(5) . . . yes C65 C66 C67 120.0(6) . . . yes C65 C66 H83 120.1 . . . no C67 C66 H83 119.9 . . . no C66 C67 C68 119.8(6) . . . yes C66 C67 H84 120.1 . . . no C68 C67 H84 120.1 . . . no C67 C68 C69 121.2(6) . . . yes C67 C68 H85 119.4 . . . no C69 C68 H85 119.4 . . . no C68 C69 C70 119.7(5) . . . yes C68 C69 H86 120.1 . . . no C70 C69 H86 120.2 . . . no O13 C70 C65 115.5(4) . . . yes O13 C70 C69 124.5(5) . . . yes C65 C70 C69 120.0(5) . . . yes O13 C71 C72 111.7(6) . . . yes O13 C71 H87 109.0 . . . no O13 C71 H88 108.9 . . . no C72 C71 H87 108.9 . . . no C72 C71 H88 108.9 . . . no H87 C71 H88 109.4 . . . no O14 C72 C71 116.4(7) . . . yes O14 C72 H89 107.6 . . . no O14 C72 H90 107.5 . . . no C71 C72 H89 107.9 . . . no C71 C72 H90 107.8 . . . no H89 C72 H90 109.5 . . . no O14 C73 C74 126.4(7) . . . yes O14 C73 H91 105.1 . . . no O14 C73 H92 105.3 . . . no C74 C73 H91 104.8 . . . no C74 C73 H92 105.0 . . . no H91 C73 H92 109.5 . . . no O15 C74 C73 119.1(6) . . . yes O15 C74 H93 106.9 . . . no O15 C74 H94 106.8 . . . no C73 C74 H93 107.2 . . . no C73 C74 H94 107.2 . . . no H93 C74 H94 109.4 . . . no O15 C75 C76 113.3(6) . . . yes O15 C75 H95 108.5 . . . no O15 C75 H96 108.6 . . . no C76 C75 H95 108.4 . . . no C76 C75 H96 108.6 . . . no H95 C75 H96 109.5 . . . no O16 C76 C75 110.4(6) . . . yes O16 C76 H97 109.2 . . . no O16 C76 H98 109.3 . . . no C75 C76 H97 109.3 . . . no C75 C76 H98 109.3 . . . no H97 C76 H98 109.3 . . . no O16 C77 C78 123.9(7) . . . yes O16 C77 C82 117.9(6) . . . yes C78 C77 C82 118.3(7) . . . yes C77 C78 C79 119.2(8) . . . yes C77 C78 H99 120.5 . . . no C79 C78 H99 120.3 . . . no C78 C79 C80 121.0(9) . . . yes C78 C79 H100 119.4 . . . no C80 C79 H100 119.6 . . . no C79 C80 C81 120.7(9) . . . yes C79 C80 H101 119.7 . . . no C81 C80 H101 119.6 . . . no C80 C81 C82 119.9(8) . . . yes C80 C81 H102 120.1 . . . no C82 C81 H102 120.0 . . . no O17 C82 C77 115.4(7) . . . yes O17 C82 C81 123.8(6) . . . yes C77 C82 C81 120.8(7) . . . yes O17 C83 C84 122.7(8) . . . yes O17 C83 H103 106.0 . . . no O17 C83 H104 106.2 . . . no C84 C83 H103 106.0 . . . no C84 C83 H104 106.1 . . . no H103 C83 H104 109.4 . . . no O18 C84 C83 122.2(7) . . . yes O18 C84 H105 106.3 . . . no O18 C84 H106 106.2 . . . no C83 C84 H105 106.2 . . . no C83 C84 H106 106.2 . . . no H105 C84 H106 109.3 . . . no O18 C85 C86 112.3(5) . . . yes O18 C85 H107 108.9 . . . no O18 C85 H108 108.8 . . . no C86 C85 H107 108.7 . . . no C86 C85 H108 108.7 . . . no H107 C85 H108 109.4 . . . no O19 C86 C85 111.6(4) . . . yes O19 C86 H109 109.0 . . . no O19 C86 H110 108.9 . . . no C85 C86 H109 109.0 . . . no C85 C86 H110 108.9 . . . no H109 C86 H110 109.5 . . . no O19 C87 C88 110.7(5) . . . yes O19 C87 H111 109.2 . . . no O19 C87 H112 109.1 . . . no C88 C87 H111 109.1 . . . no C88 C87 H112 109.2 . . . no H111 C87 H112 109.5 . . . no O20 C88 C87 108.3(4) . . . yes O20 C88 H113 109.7 . . . no O20 C88 H114 109.8 . . . no C87 C88 H113 109.8 . . . no C87 C88 H114 109.9 . . . no H113 C88 H114 109.3 . . . no CL1 C89 CL2 105.6(6) . . . yes CL1 C89 CL3 106.0(9) . . . yes CL1 C89 H115 107.2 . . . no CL2 C89 CL3 121.4(8) . . . yes CL2 C89 H115 108.6 . . . no CL3 C89 H115 107.3 . . . no O21 C90 O21 116(2) . . 2_555 yes O21 C90 C91 121(1) . . . yes O21 C90 C91 121(1) 2_555 . . 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 F1 C54 3.291(8) . 6_545 ? F1 C48 3.404(8) . . ? F1 C47 3.525(8) . . ? F2 O21 3.20(1) . 2_555 ? F2 C84 3.444(8) . 7_556 ? F2 C47 3.549(8) . . ? F3 C83 3.258(8) . 7_556 ? F3 C84 3.296(8) . 7_556 ? F3 C89 3.31(1) . 1_545 ? F4 C69 3.314(7) . 6_545 ? F4 C71 3.457(8) . 6_545 ? F5 C89 3.234(10) . 1_545 ? F5 C71 3.347(8) . 6_545 ? F5 C72 3.551(9) . 6_545 ? F6 C45 3.512(10) . . ? F6 C52 3.570(8) . 6_545 ? F7 C88 3.518(8) . . ? F7 C50 3.572(8) . 6_545 ? F8 C88 3.268(8) . . ? F8 C44 3.53(1) . . ? F9 C79 3.50(1) . 1_545 ? F10 C57 3.339(8) . 1_545 ? F12 C64 3.360(8) . 7_556 ? O1 C29 3.277(6) . 6_555 ? O1 C30 3.482(6) . 6_555 ? O1 C5 3.566(7) . 3_565 ? O3 O21 3.52(1) . 7_556 ? O4 C16 3.474(7) . 8_555 ? O4 C2 3.567(7) . 6_545 ? O4 C7 3.591(8) . 6_545 ? O5 C39 3.415(7) . 7_556 ? O5 C17 3.422(6) . . ? O5 C18 3.472(6) . . ? O6 N1 3.161(5) . . ? O6 C17 3.334(6) . . ? O6 C14 3.473(6) . . ? O6 C15 3.478(6) . . ? O6 C18 3.560(6) . . ? O7 N1 2.842(5) . . ? O7 C18 3.451(6) . . ? O8 N1 2.928(5) . . ? O8 C18 3.396(6) . . ? O9 N1 3.304(6) . . ? O10 C17 3.199(7) . . ? O10 C14 3.553(7) . . ? O10 C13 3.555(8) . . ? O11 C17 3.401(6) . . ? O12 C19 3.438(6) . . ? O12 C39 3.593(7) . 7_556 ? O13 C24 3.434(6) . . ? O14 C24 3.096(6) . . ? O15 C24 3.299(6) . . ? O16 C24 3.565(7) . . ? O17 N2 2.986(5) . . ? O17 C23 3.279(6) . . ? O17 C22 3.530(6) . . ? O17 C24 3.572(7) . . ? O18 N2 2.906(5) . . ? O18 C26 3.461(7) . . ? O18 C25 3.482(6) . . ? O19 N2 2.899(4) . . ? O19 C30 3.507(6) . . ? O20 N2 3.176(5) . . ? O20 C23 3.421(6) . . ? N1 C53 3.584(6) . . ? C19 C58 3.571(7) . . ? C23 C82 3.546(7) . . ? C33 C39 3.520(8) . 2_656 ? C36 C37 3.573(9) . 2_656 ? C36 C36 3.58(1) . 2_656 ? C49 C58 3.537(7) . 6_545 ?