# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1539 data_1 _audit_creation_date 'Fri Oct 8 11:36:31 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #-------------------------------------------------------------------------- # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #-------------------------------------------------------------------------- # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #-------------------------------------------------------------------------- # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #-------------------------------------------------------------------------- # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; Higashi (1999). NUMABS. Program for Absorption Correction, Rigaku Corporation. Rigaku (1998). PROCESS-AUTO. RAXIS-RAPID Data Processing Software. Rigaku Corporation. MSC & Rigaku. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. Molecular Structure Corporation and Rigaku Corporation. SIR97: Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R. (1999) 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. Oak Ridge. Tennessee, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #-------------------------------------------------------------------------- data_XR0190raplt_Ehime_Univ._(P #-------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C26 H16 Br4 ' _chemical_formula_moiety '?' _chemical_formula_weight 648.03 _chemical_melting_point ? #-------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/c 21/c 2/n' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,y,1/2+z x,1/2-y,1/2+z _cell_length_a 16.173(2) _cell_length_b 16.512(1) _cell_length_c 18.024(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4813(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 46535 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 133.2 #-------------------------------------------------------------------------- _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 6.719 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_absorpt_correction_T_min 0.112 _exptl_absorpt_correction_T_max 0.365 #-------------------------------------------------------------------------- # 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 ? _diffrn_reflns_number 44574 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9989 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 #-------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5522 _reflns_number_gt 3159 _reflns_threshold_expression F^2^>2.0?s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0320 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3159 _refine_ls_number_parameters 272 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[?s^2^(Fo) + 0.00018|Fo|^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 0.43 _refine_diff_density_min -0.22 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00085(8) _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) ; 'Br' 'Br' -0.290 2.459 ;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 Br(1) Br 0.43494(4) 0.41394(4) 0.82964(3) 0.0429(2) Uani 1.00 d . . . Br(2) Br 0.43132(4) 0.43860(3) 0.26446(3) 0.0410(2) Uani 1.00 d . . . Br(3) Br 0.60510(4) 0.45125(3) 0.50888(3) 0.0321(1) Uani 1.00 d . . . Br(4) Br 0.53184(4) 0.39256(4) 1.07316(3) 0.0439(2) Uani 1.00 d . . . C(1) C 0.3869(3) 0.3732(3) 0.7409(2) 0.026(1) Uani 1.00 d . . . C(2) C 0.3858(3) 0.2899(3) 0.7303(3) 0.029(1) Uani 1.00 d . . . C(3) C 0.3512(3) 0.2591(3) 0.6660(2) 0.024(1) Uani 1.00 d . . . C(4) C 0.3180(3) 0.3096(3) 0.6122(2) 0.020(1) Uani 1.00 d . . . C(5) C 0.3208(3) 0.3941(3) 0.6244(2) 0.024(1) Uani 1.00 d . . . C(6) C 0.3559(3) 0.4251(3) 0.6891(3) 0.029(1) Uani 1.00 d . . . C(7) C 0.2802(3) 0.2778(2) 0.5421(2) 0.018(1) Uani 1.00 d . . . C(8) C 0.3149(3) 0.3140(2) 0.4726(2) 0.018(1) Uani 1.00 d . . . C(9) C 0.2650(3) 0.3537(3) 0.4209(3) 0.024(1) Uani 1.00 d . . . C(10) C 0.2991(4) 0.3902(3) 0.3584(2) 0.029(1) Uani 1.00 d . . . C(11) C 0.3836(3) 0.3864(3) 0.3482(2) 0.026(1) Uani 1.00 d . . . C(12) C 0.4342(3) 0.3467(3) 0.3974(3) 0.028(1) Uani 1.00 d . . . C(13) C 0.3993(3) 0.3112(3) 0.4601(2) 0.025(1) Uani 1.00 d . . . C(14) C 0.6409(3) 0.3965(3) 0.5963(2) 0.023(1) Uani 1.00 d . . . C(15) C 0.7243(3) 0.3945(3) 0.6126(3) 0.028(1) Uani 1.00 d . . . C(16) C 0.7507(3) 0.3555(3) 0.6768(2) 0.025(1) Uani 1.00 d . . . C(17) C 0.6932(3) 0.3191(2) 0.7242(2) 0.018(1) Uani 1.00 d . . . C(18) C 0.6094(3) 0.3242(3) 0.7064(3) 0.024(1) Uani 1.00 d . . . C(19) C 0.5829(3) 0.3619(3) 0.6417(2) 0.025(1) Uani 1.00 d . . . C(20) C 0.7208(3) 0.2796(3) 0.7946(2) 0.021(1) Uani 1.00 d . . . C(21) C 0.6791(3) 0.3085(3) 0.8627(2) 0.019(1) Uani 1.00 d . . . C(22) C 0.6636(3) 0.3895(3) 0.8753(2) 0.025(1) Uani 1.00 d . . . C(23) C 0.6219(3) 0.4164(3) 0.9383(3) 0.027(1) Uani 1.00 d . . . C(24) C 0.5935(3) 0.3599(3) 0.9879(2) 0.025(1) Uani 1.00 d . . . C(25) C 0.6074(3) 0.2780(3) 0.9780(3) 0.027(1) Uani 1.00 d . . . C(26) C 0.6502(3) 0.2535(3) 0.9151(2) 0.023(1) Uani 1.00 d . . . H(2) H 0.4084 0.2547 0.7667 0.0350 Uiso 1.00 calc . . . H(3) H 0.3503 0.2019 0.6588 0.0292 Uiso 1.00 calc . . . H(5) H 0.2983 0.4299 0.5884 0.0297 Uiso 1.00 calc . . . H(6) H 0.3589 0.4821 0.6966 0.0356 Uiso 1.00 calc . . . H(9) H 0.2068 0.3560 0.4287 0.0292 Uiso 1.00 calc . . . H(10) H 0.2649 0.4172 0.3234 0.0368 Uiso 1.00 calc . . . H(12) H 0.4921 0.3435 0.3889 0.0344 Uiso 1.00 calc . . . H(13) H 0.4339 0.2846 0.4950 0.0301 Uiso 1.00 calc . . . H(15) H 0.7635 0.4195 0.5806 0.0337 Uiso 1.00 calc . . . H(16) H 0.8077 0.3535 0.6887 0.0296 Uiso 1.00 calc . . . H(18) H 0.5695 0.3014 0.7390 0.0292 Uiso 1.00 calc . . . H(19) H 0.5258 0.3637 0.6294 0.0297 Uiso 1.00 calc . . . H(22) H 0.6818 0.4282 0.8400 0.0302 Uiso 1.00 calc . . . H(23) H 0.6136 0.4724 0.9467 0.0328 Uiso 1.00 calc . . . H(25) H 0.5886 0.2395 1.0134 0.0324 Uiso 1.00 calc . . . H(26) H 0.6604 0.1973 0.9077 0.0273 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) 0.0402(4) 0.0692(4) 0.0193(2) -0.0294(3) 0.0002(3) -0.0050(3) Br(2) 0.0636(5) 0.0339(3) 0.0254(3) -0.0148(3) 0.0135(3) 0.0016(2) Br(3) 0.0437(4) 0.0265(2) 0.0260(2) 0.0064(3) -0.0097(3) 0.0022(2) Br(4) 0.0472(4) 0.0539(4) 0.0306(3) 0.0146(3) 0.0093(3) -0.0104(3) C(1) 0.019(3) 0.044(3) 0.016(2) -0.015(2) 0.004(2) -0.006(2) C(2) 0.028(3) 0.036(3) 0.022(2) -0.007(2) -0.002(2) 0.011(2) C(3) 0.023(3) 0.018(2) 0.031(2) -0.006(2) -0.005(3) 0.006(2) C(4) 0.013(3) 0.027(2) 0.019(2) -0.007(2) 0.001(2) -0.003(2) C(5) 0.026(3) 0.023(2) 0.022(2) -0.002(2) -0.001(2) 0.006(2) C(6) 0.032(3) 0.030(3) 0.026(2) -0.009(2) 0.002(3) 0.001(2) C(7) 0.014(3) 0.022(2) 0.017(2) 0.002(2) -0.001(2) -0.002(2) C(8) 0.018(3) 0.019(2) 0.017(2) -0.003(2) -0.003(2) -0.001(2) C(9) 0.016(3) 0.026(2) 0.030(2) -0.003(2) -0.004(2) 0.003(2) C(10) 0.042(4) 0.025(3) 0.021(2) -0.002(3) -0.007(3) 0.004(2) C(11) 0.037(4) 0.022(2) 0.019(2) -0.012(2) 0.004(2) -0.001(2) C(12) 0.023(3) 0.031(3) 0.031(3) -0.004(2) 0.008(3) -0.003(2) C(13) 0.025(3) 0.033(3) 0.017(2) -0.001(2) -0.002(2) 0.002(2) C(14) 0.031(3) 0.018(2) 0.021(2) 0.006(2) -0.005(2) 0.000(2) C(15) 0.030(3) 0.027(3) 0.028(3) 0.002(2) 0.007(2) 0.003(2) C(16) 0.016(3) 0.029(2) 0.029(2) 0.006(2) -0.001(3) 0.003(2) C(17) 0.018(3) 0.018(2) 0.019(2) 0.009(2) 0.004(2) -0.002(2) C(18) 0.018(3) 0.030(2) 0.024(2) 0.002(2) 0.006(2) -0.001(2) C(19) 0.019(3) 0.031(3) 0.025(2) 0.005(2) -0.004(2) 0.000(2) C(20) 0.018(3) 0.024(2) 0.021(2) -0.002(2) -0.001(2) -0.001(2) C(21) 0.011(3) 0.025(2) 0.020(2) 0.005(2) -0.002(2) 0.002(2) C(22) 0.030(3) 0.021(2) 0.023(2) 0.004(2) -0.004(2) 0.001(2) C(23) 0.023(3) 0.023(2) 0.034(3) 0.008(2) -0.005(2) -0.009(2) C(24) 0.015(3) 0.036(3) 0.022(2) 0.007(2) -0.002(2) -0.006(2) C(25) 0.025(3) 0.027(2) 0.027(3) 0.002(2) -0.002(2) 0.007(2) C(26) 0.020(3) 0.020(2) 0.028(2) 0.003(2) 0.000(2) 0.002(2) #-------------------------------------------------------------------------- _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 Br(1) C(1) 1.902(4) . . yes Br(2) C(11) 1.902(5) . . yes Br(3) C(14) 1.907(4) . . yes Br(4) C(24) 1.909(4) . . yes C(1) C(2) 1.387(7) . . yes C(1) C(6) 1.363(7) . . yes C(2) C(3) 1.384(7) . . yes C(3) C(4) 1.387(6) . . yes C(4) C(5) 1.413(6) . . yes C(4) C(7) 1.499(6) . . yes C(5) C(6) 1.393(7) . . yes C(7) C(7) 1.340(8) . 2_555 yes C(7) C(8) 1.498(6) . . yes C(8) C(9) 1.395(6) . . yes C(8) C(13) 1.384(7) . . yes C(9) C(10) 1.392(7) . . yes C(10) C(11) 1.381(8) . . yes C(11) C(12) 1.373(7) . . yes C(12) C(13) 1.393(7) . . yes C(14) C(15) 1.381(7) . . yes C(14) C(19) 1.370(7) . . yes C(15) C(16) 1.391(6) . . yes C(16) C(17) 1.398(7) . . yes C(17) C(18) 1.396(7) . . yes C(17) C(20) 1.494(6) . . yes C(18) C(19) 1.390(6) . . yes C(20) C(20) 1.358(9) . 2_655 yes C(20) C(21) 1.481(6) . . yes C(21) C(22) 1.380(6) . . yes C(21) C(26) 1.390(6) . . yes C(22) C(23) 1.393(7) . . yes C(23) C(24) 1.370(7) . . yes C(24) C(25) 1.383(6) . . yes C(25) C(26) 1.388(6) . . 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 Br(1) C(1) C(2) 118.1(3) . 1_555 1_555 yes Br(1) C(1) C(6) 120.2(4) . 1_555 1_555 yes C(2) C(1) C(6) 121.6(4) . 1_555 1_555 yes C(1) C(2) C(3) 119.0(4) . 1_555 1_555 yes C(2) C(3) C(4) 121.4(4) . 1_555 1_555 yes C(3) C(4) C(5) 118.2(4) . 1_555 1_555 yes C(3) C(4) C(7) 122.4(4) . 1_555 1_555 yes C(5) C(4) C(7) 119.4(4) . 1_555 1_555 yes C(4) C(5) C(6) 120.4(4) . 1_555 1_555 yes C(1) C(6) C(5) 119.4(4) . 1_555 1_555 yes C(4) C(7) C(7) 122.5(2) . 1_555 2_555 yes C(4) C(7) C(8) 114.3(4) . 1_555 1_555 yes C(7) C(7) C(8) 123.1(2) . 2_555 1_555 yes C(7) C(8) C(9) 122.0(4) . 1_555 1_555 yes C(7) C(8) C(13) 119.5(4) . 1_555 1_555 yes C(9) C(8) C(13) 118.5(4) . 1_555 1_555 yes C(8) C(9) C(10) 121.0(5) . 1_555 1_555 yes C(9) C(10) C(11) 118.7(4) . 1_555 1_555 yes Br(2) C(11) C(10) 119.1(3) . 1_555 1_555 yes Br(2) C(11) C(12) 119.2(4) . 1_555 1_555 yes C(10) C(11) C(12) 121.7(4) . 1_555 1_555 yes C(11) C(12) C(13) 118.9(5) . 1_555 1_555 yes C(8) C(13) C(12) 121.2(4) . 1_555 1_555 yes Br(3) C(14) C(15) 118.9(3) . 1_555 1_555 yes Br(3) C(14) C(19) 118.9(4) . 1_555 1_555 yes C(15) C(14) C(19) 122.2(4) . 1_555 1_555 yes C(14) C(15) C(16) 119.1(4) . 1_555 1_555 yes C(15) C(16) C(17) 120.3(5) . 1_555 1_555 yes C(16) C(17) C(18) 118.6(4) . 1_555 1_555 yes C(16) C(17) C(20) 120.5(4) . 1_555 1_555 yes C(18) C(17) C(20) 120.8(4) . 1_555 1_555 yes C(17) C(18) C(19) 121.3(4) . 1_555 1_555 yes C(14) C(19) C(18) 118.4(5) . 1_555 1_555 yes C(17) C(20) C(20) 121.4(2) . 1_555 2_655 yes C(17) C(20) C(21) 115.3(4) . 1_555 1_555 yes C(20) C(20) C(21) 123.3(2) . 2_655 1_555 yes C(20) C(21) C(22) 122.1(4) . 1_555 1_555 yes C(20) C(21) C(26) 120.4(4) . 1_555 1_555 yes C(22) C(21) C(26) 117.4(4) . 1_555 1_555 yes C(21) C(22) C(23) 122.0(4) . 1_555 1_555 yes C(22) C(23) C(24) 118.5(4) . 1_555 1_555 yes Br(4) C(24) C(23) 120.5(3) . 1_555 1_555 yes Br(4) C(24) C(25) 117.7(3) . 1_555 1_555 yes C(23) C(24) C(25) 121.8(4) . 1_555 1_555 yes C(24) C(25) C(26) 118.2(4) . 1_555 1_555 yes C(21) C(26) C(25) 122.1(4) . 1_555 1_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 Br(1) C(23) 3.603(5) . 1_555 yes Br(1) Br(2) 3.6721(8) . 5_666 yes Br(1) Br(4) 3.6834(8) . 5_667 yes Br(1) C(9) 3.762(5) . 7_555 yes Br(1) C(22) 3.810(5) . 1_555 yes Br(1) C(10) 3.840(6) . 7_555 yes Br(1) C(18) 3.885(5) . 1_555 yes Br(1) C(24) 3.938(5) . 1_555 yes Br(2) C(19) 3.711(5) . 5_666 yes Br(2) C(14) 3.883(4) . 5_666 yes Br(2) Br(4) 3.8871(8) . 1_554 yes Br(2) C(2) 3.894(5) . 8_554 yes Br(2) C(3) 3.935(4) . 8_554 yes Br(3) C(5) 3.705(5) . 5_666 yes Br(3) C(11) 3.722(4) . 5_666 yes Br(3) Br(3) 3.775(1) . 5_666 yes Br(3) C(12) 3.793(5) . 5_666 yes Br(3) C(25) 3.827(5) . 8_554 yes Br(3) C(12) 3.829(5) . 1_555 yes Br(3) C(26) 3.850(5) . 8_554 yes Br(3) C(10) 3.871(5) . 5_666 yes Br(3) C(13) 3.963(5) . 5_666 yes C(1) C(19) 3.645(7) . 1_555 yes C(1) C(10) 3.689(7) . 7_555 yes C(1) C(18) 3.740(7) . 1_555 yes C(2) C(11) 3.605(6) . 8_555 yes C(2) C(18) 3.685(7) . 1_555 yes C(2) C(19) 3.758(7) . 1_555 yes C(2) C(12) 3.843(7) . 8_555 yes C(6) C(19) 3.910(7) . 1_555 yes C(6) C(10) 3.992(7) . 7_555 yes C(10) C(15) 3.613(7) . 5_666 yes C(10) C(14) 3.744(6) . 5_666 yes C(11) C(14) 3.744(6) . 5_666 yes C(12) C(25) 3.768(7) . 8_554 yes C(12) C(26) 3.879(7) . 8_554 yes C(13) C(25) 3.688(7) . 8_554 yes C(14) C(25) 3.626(6) . 8_554 yes C(15) C(24) 3.750(7) . 7_654 yes C(19) C(25) 3.768(6) . 8_554 yes #-------------------------------------------------------------------------- _audit_creation_date 08-27-98 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; H. Irngartinger Organisch-Chemisches Institut Universit?"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; _publ_contact_author_email 'e56@ix.urz.uni-heidelberg.de' _publ_contact_author_fax '(+49) 6221 544205' _publ_contact_author_phone '(+49) 6221 548422' _publ_requested_journal '?' _publ_requested_coeditor_name ? _publ_contact_letter ; ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Tetra(p-bromophenyl)ethylene as a Novel Host Compound Which Form Chiral Inclusion Compounds with Various Kinds of Achiral Guests ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address Toda, Fumio' #<--'Last name, first name' ; Department of Applied Chemistry, Faculty of Engineering Ehime University, Matsuyama Ehime 790-8577 Japan ; Tanaka, Koichi' #<--'Last name, first name' ; Department of Applied Chemistry, Faculty of Engineering Ehime University, Matsuyama Ehime 790-8577 Japan ; 'Oeser, Thomas' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit?"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; 'Irngartinger, Hermann' #<--'Last name, first name' ; Organisch-Chemisches Institut Universit?"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; Enraf-Nonius, CAD4 Operations Manual, Delft, 1988. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, Vol. IV, The Kynoch Press, Birmingham, England, 1974 ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_611TODABREN _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetra(p-bromophenyl)ethylene * xylene (3) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Br4' _chemical_formula_weight 754.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.762(1) _cell_length_b 14.942(2) _cell_length_c 23.472(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 3073.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 75 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.63 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 5.26 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK?a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NONIUS_CAD4 _diffrn_measurement_method ?w2?q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -2.7 _diffrn_reflns_number 4119 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 27.9 _reflns_number_total 4119 _reflns_number_gt 2148 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?s^2^(Fo^2^)+(0.0613P)^2^+0.5047P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calculated _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 4119 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.136 _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.128 _refine_ls_wR_factor_gt 0.096 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.977 _refine_ls_shift/su_mean 0.140 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.68796(13) 0.65731(7) 0.12456(4) 0.0549(3) Uani 1 1 d . . . Br2 Br 0.74911(17) 0.61723(8) 0.56912(4) 0.0815(5) Uani 1 1 d . . . Br3 Br 0.79012(12) 0.08295(7) 0.54496(4) 0.0500(3) Uani 1 1 d . . . Br4 Br 0.80414(16) 0.12250(7) 0.10947(4) 0.0583(3) Uani 1 1 d . . . C1 C 0.7660(8) 0.3307(5) 0.3352(3) 0.0205(17) Uani 1 1 d . . . C2 C 0.7549(8) 0.4202(5) 0.3391(3) 0.0215(17) Uani 1 1 d . . . C3 C 0.7355(9) 0.4788(5) 0.2865(3) 0.0239(18) Uani 1 1 d . . . C4 C 0.6290(10) 0.4590(6) 0.2445(3) 0.033(2) Uani 1 1 d . . . H4 H 0.5667 0.4082 0.2483 0.040 Uiso 1 1 calc R . . C5 C 0.6136(10) 0.5136(6) 0.1970(3) 0.035(2) Uani 1 1 d . . . H5 H 0.5368 0.5023 0.1700 0.042 Uiso 1 1 calc R . . C6 C 0.7119(10) 0.5844(6) 0.1900(3) 0.0315(19) Uani 1 1 d . . . C7 C 0.8157(10) 0.6080(5) 0.2309(3) 0.032(2) Uani 1 1 d . . . H7 H 0.8786 0.6584 0.2263 0.039 Uiso 1 1 calc R . . C8 C 0.8250(10) 0.5543(5) 0.2799(3) 0.034(2) Uani 1 1 d . . . H8 H 0.8938 0.5702 0.3090 0.040 Uiso 1 1 calc R . . C9 C 0.7569(10) 0.4700(5) 0.3936(3) 0.032(2) Uani 1 1 d . . . C10 C 0.8714(10) 0.4555(6) 0.4338(3) 0.035(2) Uani 1 1 d . . . H10 H 0.9500 0.4147 0.4254 0.042 Uiso 1 1 calc R . . C11 C 0.8729(12) 0.5001(6) 0.4866(3) 0.043(2) Uani 1 1 d . . . H11 H 0.9506 0.4899 0.5134 0.051 Uiso 1 1 calc R . . C12 C 0.7558(13) 0.5593(6) 0.4973(4) 0.050(3) Uani 1 1 d . . . C13 C 0.6408(11) 0.5765(6) 0.4585(4) 0.045(2) Uani 1 1 d . . . H13 H 0.5616 0.6167 0.4671 0.054 Uiso 1 1 calc R . . C14 C 0.6461(11) 0.5321(5) 0.4062(4) 0.035(2) Uani 1 1 d . . . H14 H 0.5715 0.5452 0.3786 0.041 Uiso 1 1 calc R . . C15 C 0.7691(10) 0.2723(5) 0.3869(3) 0.0252(19) Uani 1 1 d . . . C16 C 0.8859(11) 0.2088(5) 0.3927(4) 0.038(2) Uani 1 1 d . . . H16 H 0.9611 0.2040 0.3643 0.045 Uiso 1 1 calc R . . C17 C 0.8916(10) 0.1526(5) 0.4400(3) 0.032(2) Uani 1 1 d . . . H17 H 0.9702 0.1101 0.4436 0.038 Uiso 1 1 calc R . . C18 C 0.7823(10) 0.1598(5) 0.4811(3) 0.034(2) Uani 1 1 d . . . C19 C 0.6649(9) 0.2194(5) 0.4757(3) 0.030(2) Uani 1 1 d . . . H19 H 0.5875 0.2216 0.5034 0.036 Uiso 1 1 calc R . . C20 C 0.6602(10) 0.2773(5) 0.4286(3) 0.031(2) Uani 1 1 d . . . H20 H 0.5816 0.3199 0.4258 0.037 Uiso 1 1 calc R . . C21 C 0.7765(11) 0.2801(5) 0.2804(3) 0.030(2) Uani 1 1 d . . . C22 C 0.6840(11) 0.2057(5) 0.2717(3) 0.033(2) Uani 1 1 d . . . H22 H 0.6177 0.1866 0.3008 0.040 Uiso 1 1 calc R . . C23 C 0.6893(11) 0.1589(6) 0.2198(4) 0.039(2) Uani 1 1 d . . . H23 H 0.6258 0.1092 0.2132 0.047 Uiso 1 1 calc R . . C24 C 0.7903(12) 0.1881(5) 0.1789(3) 0.034(2) Uani 1 1 d . . . C25 C 0.8912(10) 0.2591(5) 0.1877(3) 0.032(2) Uani 1 1 d . . . H25 H 0.9644 0.2744 0.1602 0.038 Uiso 1 1 calc R . . C26 C 0.8802(9) 0.3060(5) 0.2383(3) 0.0291(19) Uani 1 1 d . . . H26 H 0.9433 0.3559 0.2445 0.035 Uiso 1 1 calc R . . C30 C 0.7523(11) 0.1129(7) -0.2310(4) 0.048(3) Uani 1 1 d . . . C31 C 0.8206(12) 0.1873(7) -0.2090(4) 0.049(3) Uani 1 1 d . . . H31 H 0.8642 0.2294 -0.2339 0.058 Uiso 1 1 calc R . . C32 C 0.8273(14) 0.2020(7) -0.1517(5) 0.059(3) Uani 1 1 d . . . H32 H 0.8745 0.2547 -0.1388 0.071 Uiso 1 1 calc R . . C33 C 0.7689(13) 0.1443(7) -0.1122(4) 0.055(3) Uani 1 1 d . . . C34 C 0.7023(14) 0.0689(7) -0.1337(4) 0.059(3) Uani 1 1 d . . . H34 H 0.6616 0.0269 -0.1081 0.071 Uiso 1 1 calc R . . C35 C 0.6922(13) 0.0515(6) -0.1917(4) 0.052(3) Uani 1 1 d . . . H35 H 0.6452 -0.0013 -0.2046 0.062 Uiso 1 1 calc R . . C36 C 0.7400(12) 0.0983(8) -0.2939(4) 0.072(4) Uani 1 1 d . . . H36A H 0.7200 0.1549 -0.3126 0.108 Uiso 1 1 calc R . . H36B H 0.6571 0.0570 -0.3017 0.108 Uiso 1 1 calc R . . H36C H 0.8349 0.0734 -0.3081 0.108 Uiso 1 1 calc R . . C37 C 0.7763(19) 0.1591(10) -0.0485(4) 0.106(5) Uani 1 1 d . . . H37A H 0.7069 0.2069 -0.0379 0.158 Uiso 1 1 calc R . . H37B H 0.8795 0.1755 -0.0378 0.158 Uiso 1 1 calc R . . H37C H 0.7473 0.1045 -0.0290 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0516(6) 0.0705(7) 0.0426(5) 0.0238(5) 0.0001(5) 0.0032(6) Br2 0.1226(14) 0.0844(9) 0.0376(5) -0.0294(6) -0.0056(7) 0.0220(8) Br3 0.0452(5) 0.0568(6) 0.0481(5) 0.0259(5) -0.0061(5) -0.0094(6) Br4 0.0977(8) 0.0489(6) 0.0283(4) -0.0145(4) 0.0011(6) -0.0003(7) C1 0.013(4) 0.033(5) 0.016(4) 0.004(3) 0.003(3) 0.008(3) C2 0.011(4) 0.021(4) 0.032(4) 0.001(3) -0.001(3) 0.002(3) C3 0.021(5) 0.018(4) 0.033(4) -0.001(3) 0.000(4) -0.003(4) C4 0.024(5) 0.043(5) 0.032(4) -0.005(4) 0.007(4) -0.010(4) C5 0.033(5) 0.052(6) 0.020(4) 0.003(4) -0.008(4) 0.003(5) C6 0.029(5) 0.034(4) 0.032(4) 0.001(4) 0.002(4) -0.008(5) C7 0.031(5) 0.015(4) 0.051(5) 0.004(3) 0.007(5) -0.004(4) C8 0.036(5) 0.039(5) 0.025(4) -0.002(4) -0.002(4) 0.002(4) C9 0.044(6) 0.033(5) 0.020(4) 0.000(3) -0.005(4) 0.003(4) C10 0.030(5) 0.040(5) 0.035(5) 0.000(4) 0.001(4) 0.001(4) C11 0.050(6) 0.054(6) 0.023(4) 0.000(4) -0.009(5) 0.003(5) C12 0.071(8) 0.039(6) 0.039(5) -0.011(4) 0.027(5) -0.011(5) C13 0.048(6) 0.044(6) 0.043(5) -0.009(5) -0.006(5) 0.013(5) C14 0.042(6) 0.026(4) 0.036(5) -0.004(4) -0.001(4) 0.010(4) C15 0.031(5) 0.025(4) 0.020(4) -0.003(3) -0.002(4) -0.001(4) C16 0.036(5) 0.037(5) 0.040(5) -0.005(4) 0.008(5) 0.001(4) C17 0.029(5) 0.031(5) 0.035(5) 0.004(4) -0.006(4) 0.006(4) C18 0.036(5) 0.031(4) 0.033(4) 0.003(4) 0.005(5) -0.009(4) C19 0.015(5) 0.043(5) 0.032(4) 0.000(4) 0.011(4) -0.006(4) C20 0.033(5) 0.019(4) 0.040(5) 0.000(3) 0.005(4) 0.007(4) C21 0.043(6) 0.025(4) 0.023(4) -0.004(3) 0.004(4) 0.000(4) C22 0.037(5) 0.031(4) 0.032(4) -0.004(3) 0.010(5) -0.009(4) C23 0.041(5) 0.040(5) 0.036(5) -0.004(4) 0.007(5) -0.008(5) C24 0.064(6) 0.022(4) 0.015(3) -0.009(3) -0.011(5) 0.018(5) C25 0.022(5) 0.040(5) 0.034(5) -0.001(4) 0.003(4) 0.003(4) C26 0.032(5) 0.031(4) 0.024(4) -0.005(3) -0.001(4) -0.008(4) C30 0.036(6) 0.057(7) 0.051(6) -0.004(5) -0.013(5) 0.018(5) C31 0.051(7) 0.053(6) 0.043(5) 0.014(5) 0.005(6) 0.000(6) C32 0.065(8) 0.047(6) 0.064(7) -0.003(5) -0.004(7) 0.000(6) C33 0.062(8) 0.059(7) 0.045(6) 0.002(5) 0.009(6) 0.008(6) C34 0.068(7) 0.052(6) 0.059(7) 0.012(5) 0.002(7) 0.009(7) C35 0.048(6) 0.042(6) 0.066(7) -0.001(5) -0.004(6) 0.008(6) C36 0.059(8) 0.104(9) 0.054(6) -0.023(6) -0.010(6) 0.022(7) C37 0.155(15) 0.123(12) 0.038(6) -0.001(7) -0.011(9) 0.002(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C6 1.895(8) . ? Br2 C12 1.896(9) . ? Br3 C18 1.889(8) . ? Br4 C24 1.906(7) . ? C1 C2 1.343(10) . ? C1 C21 1.496(10) . ? C1 C15 1.494(10) . ? C2 C9 1.480(10) . ? C2 C3 1.525(10) . ? C3 C8 1.383(11) . ? C3 C4 1.389(11) . ? C4 C5 1.387(11) . ? C4 H4 0.9400 . ? C5 C6 1.375(12) . ? C5 H5 0.9400 . ? C6 C7 1.367(12) . ? C7 C8 1.405(11) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 C14 1.376(12) . ? C9 C10 1.394(11) . ? C10 C11 1.407(11) . ? C10 H10 0.9400 . ? C11 C12 1.378(13) . ? C11 H11 0.9400 . ? C12 C13 1.382(13) . ? C13 C14 1.396(11) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C20 1.370(11) . ? C15 C16 1.403(12) . ? C16 C17 1.394(11) . ? C16 H16 0.9400 . ? C17 C18 1.364(11) . ? C17 H17 0.9400 . ? C18 C19 1.367(11) . ? C19 C20 1.403(11) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.390(11) . ? C21 C26 1.396(11) . ? C22 C23 1.407(11) . ? C22 H22 0.9400 . ? C23 C24 1.376(12) . ? C23 H23 0.9400 . ? C24 C25 1.396(12) . ? C25 C26 1.382(10) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C30 C31 1.363(13) . ? C30 C35 1.405(13) . ? C30 C36 1.495(13) . ? C31 C32 1.364(13) . ? C31 H31 0.9400 . ? C32 C33 1.366(14) . ? C32 H32 0.9400 . ? C33 C34 1.366(14) . ? C33 C37 1.513(14) . ? C34 C35 1.388(13) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 124.6(7) . . ? C2 C1 C15 121.7(7) . . ? C21 C1 C15 113.7(6) . . ? C1 C2 C9 124.0(7) . . ? C1 C2 C3 121.6(7) . . ? C9 C2 C3 114.4(6) . . ? C8 C3 C4 118.4(7) . . ? C8 C3 C2 119.8(7) . . ? C4 C3 C2 121.9(7) . . ? C5 C4 C3 120.7(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 119.2(8) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.3 . . ? C7 C6 C5 122.1(7) . . ? C7 C6 Br1 119.6(6) . . ? C5 C6 Br1 118.1(6) . . ? C6 C7 C8 117.8(8) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.2 . . ? C3 C8 C7 121.6(8) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.2 . . ? C14 C9 C10 117.9(7) . . ? C14 C9 C2 121.1(7) . . ? C10 C9 C2 121.0(8) . . ? C9 C10 C11 121.9(9) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 117.3(9) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? C11 C12 C13 122.8(8) . . ? C11 C12 Br2 118.6(8) . . ? C13 C12 Br2 118.6(7) . . ? C12 C13 C14 117.9(9) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.1 . . ? C9 C14 C13 122.1(8) . . ? C9 C14 H14 119.0 . . ? C13 C14 H14 118.9 . . ? C20 C15 C16 118.4(7) . . ? C20 C15 C1 122.4(7) . . ? C16 C15 C1 119.2(7) . . ? C17 C16 C15 120.8(8) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 119.4(8) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.9(7) . . ? C17 C18 Br3 119.2(6) . . ? C19 C18 Br3 119.8(6) . . ? C18 C19 C20 119.8(7) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 120.6(7) . . ? C15 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C26 119.8(7) . . ? C22 C21 C1 119.6(7) . . ? C26 C21 C1 120.5(7) . . ? C21 C22 C23 120.3(8) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 117.9(8) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.1 . . ? C23 C24 C25 123.0(7) . . ? C23 C24 Br4 118.3(7) . . ? C25 C24 Br4 118.5(7) . . ? C26 C25 C24 117.9(8) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.0 . . ? C25 C26 C21 120.8(8) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C31 C30 C35 116.6(9) . . ? C31 C30 C36 121.6(10) . . ? C35 C30 C36 121.7(10) . . ? C32 C31 C30 121.6(10) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 123.5(10) . . ? C31 C32 H32 118.3 . . ? C33 C32 H32 118.3 . . ? C34 C33 C32 115.5(10) . . ? C34 C33 C37 120.3(10) . . ? C32 C33 C37 124.2(11) . . ? C33 C34 C35 123.0(10) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C34 C35 C30 119.9(10) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.1 . . ? C30 C36 H36A 109.3 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.6 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.6 . . ? C33 C37 H37B 109.4 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.4 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 C1 C2 C9 -174.9(8) . . . . ? C15 C1 C2 C9 5.0(13) . . . . ? C21 C1 C2 C3 6.4(12) . . . . ? C15 C1 C2 C3 -173.7(7) . . . . ? C1 C2 C3 C8 -132.9(8) . . . . ? C9 C2 C3 C8 48.3(10) . . . . ? C1 C2 C3 C4 47.5(11) . . . . ? C9 C2 C3 C4 -131.3(8) . . . . ? C8 C3 C4 C5 0.3(12) . . . . ? C2 C3 C4 C5 179.9(8) . . . . ? C3 C4 C5 C6 4.3(13) . . . . ? C4 C5 C6 C7 -6.2(13) . . . . ? C4 C5 C6 Br1 179.8(7) . . . . ? C5 C6 C7 C8 3.3(13) . . . . ? Br1 C6 C7 C8 177.2(6) . . . . ? C4 C3 C8 C7 -3.3(12) . . . . ? C2 C3 C8 C7 177.1(8) . . . . ? C6 C7 C8 C3 1.6(12) . . . . ? C1 C2 C9 C14 -129.2(9) . . . . ? C3 C2 C9 C14 49.5(10) . . . . ? C1 C2 C9 C10 50.9(12) . . . . ? C3 C2 C9 C10 -130.3(8) . . . . ? C14 C9 C10 C11 2.1(13) . . . . ? C2 C9 C10 C11 -178.0(8) . . . . ? C9 C10 C11 C12 0.0(13) . . . . ? C10 C11 C12 C13 -0.7(14) . . . . ? C10 C11 C12 Br2 177.5(7) . . . . ? C11 C12 C13 C14 -0.7(14) . . . . ? Br2 C12 C13 C14 -179.0(7) . . . . ? C10 C9 C14 C13 -3.7(13) . . . . ? C2 C9 C14 C13 176.5(8) . . . . ? C12 C13 C14 C9 3.0(14) . . . . ? C2 C1 C15 C20 52.6(12) . . . . ? C21 C1 C15 C20 -127.5(8) . . . . ? C2 C1 C15 C16 -128.6(8) . . . . ? C21 C1 C15 C16 51.3(10) . . . . ? C20 C15 C16 C17 -0.6(12) . . . . ? C1 C15 C16 C17 -179.4(8) . . . . ? C15 C16 C17 C18 -0.1(13) . . . . ? C16 C17 C18 C19 2.0(12) . . . . ? C16 C17 C18 Br3 179.7(6) . . . . ? C17 C18 C19 C20 -3.2(12) . . . . ? Br3 C18 C19 C20 179.1(6) . . . . ? C16 C15 C20 C19 -0.7(12) . . . . ? C1 C15 C20 C19 178.1(7) . . . . ? C18 C19 C20 C15 2.6(12) . . . . ? C2 C1 C21 C22 -132.4(9) . . . . ? C15 C1 C21 C22 47.7(11) . . . . ? C2 C1 C21 C26 48.7(12) . . . . ? C15 C1 C21 C26 -131.2(8) . . . . ? C26 C21 C22 C23 -3.0(13) . . . . ? C1 C21 C22 C23 178.1(8) . . . . ? C21 C22 C23 C24 1.3(14) . . . . ? C22 C23 C24 C25 2.8(14) . . . . ? C22 C23 C24 Br4 177.6(7) . . . . ? C23 C24 C25 C26 -5.1(13) . . . . ? Br4 C24 C25 C26 -179.9(6) . . . . ? C24 C25 C26 C21 3.2(13) . . . . ? C22 C21 C26 C25 0.6(13) . . . . ? C1 C21 C26 C25 179.5(8) . . . . ? C35 C30 C31 C32 -1.4(16) . . . . ? C36 C30 C31 C32 177.8(10) . . . . ? C30 C31 C32 C33 0.8(19) . . . . ? C31 C32 C33 C34 0.3(18) . . . . ? C31 C32 C33 C37 179.5(12) . . . . ? C32 C33 C34 C35 -0.7(17) . . . . ? C37 C33 C34 C35 -179.9(12) . . . . ? C33 C34 C35 C30 0.1(17) . . . . ? C31 C30 C35 C34 0.9(15) . . . . ? C36 C30 C35 C34 -178.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.635 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.128 #===END