data_General _audit_creation_date '2009-05-12' _audit_creation_method 'by CrystalStructure 3.8' _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 'Takanori Shibata' _publ_contact_author_email 'tshibata@waseda.jp' _publ_contact_author_fax '+81-3-5286-8098' _publ_contact_author_phone '+81-3-5286-8098' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Organic Letters' _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_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Carruthers, J.R., Rollett,J.S., Betteridge, P.W., Kinna, D., Pearce, L., Larsen, A., and Gabe, E.(1999) CRYSTALS Issue 11, Chemical Crystallography Laboratory, Oxford, UK. ; _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__ca5-Br-1 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H31 Br2 N O2 ' _chemical_formula_moiety 'C33 H31 Br2 N O2 ' _chemical_formula_weight 633.42 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '1/2+X,1/2-Y,-Z' 3 '-X,1/2+Y,1/2-Z' 4 '1/2-X,-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 10.8453(11) _cell_length_b 11.9373(11) _cell_length_c 21.7419(19) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2814.8(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14963 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.89 _exptl_crystal_size_mid 0.81 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288.00 _exptl_absorpt_coefficient_mu 2.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.053 _exptl_absorpt_correction_T_max 0.230 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Ka' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 26568 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 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 6403 _reflns_number_gt 3266 _reflns_threshold_expression F^2^>2.0s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0790 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3298 _refine_ls_number_parameters 375 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0090 _refine_diff_density_max 1.72 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2804 Friedel Pairs' _refine_ls_abs_structure_Flack -0.015(11) 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) ; 'Br' 'Br' -0.290 2.459 ; 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) ; '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 THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.94844(6) 0.28225(6) 0.52089(3) 0.0639(2) Uani 1.00 1 d . . . Br(2) Br 0.01710(7) 1.16807(6) 0.69742(3) 0.0823(2) Uani 1.00 1 d . . . O(3) O 0.4492(3) 0.6959(2) 0.78815(14) 0.0493(12) Uani 1.00 1 d . . . O(4) O 0.2980(3) 0.5907(3) 0.50633(15) 0.0414(12) Uani 1.00 1 d . . . N(5) N 0.4488(3) 0.7773(3) 0.47179(17) 0.0307(12) Uani 1.00 1 d . . . C(6) C 0.3708(4) 0.7769(4) 0.6397(2) 0.0307(16) Uani 1.00 1 d . . . C(7) C 0.3981(4) 0.6906(4) 0.6817(2) 0.0306(16) Uani 1.00 1 d . . . C(8) C 0.3642(4) 0.7216(4) 0.4317(2) 0.0334(17) Uani 1.00 1 d . . . C(9) C 0.4222(4) 0.7681(4) 0.5806(2) 0.0274(15) Uani 1.00 1 d . . . C(10) C 0.5030(4) 0.6851(3) 0.5653(2) 0.0271(15) Uani 1.00 1 d . . . C(11) C 0.4708(5) 0.5976(4) 0.6635(2) 0.0303(16) Uani 1.00 1 d . . . C(12) C 0.7319(5) 0.4964(4) 0.6248(2) 0.0353(17) Uani 1.00 1 d . . . C(13) C 0.5321(4) 0.6000(3) 0.6058(2) 0.0276(16) Uani 1.00 1 d . . . C(14) C 0.7122(5) 0.3846(4) 0.5137(2) 0.0384(17) Uani 1.00 1 d . . . C(15) C 0.2191(5) 0.4981(4) 0.5972(2) 0.0381(17) Uani 1.00 1 d . . . C(16) C 0.6191(5) 0.4527(4) 0.5323(2) 0.0345(17) Uani 1.00 1 d . . . C(17) C 0.3580(5) 0.7614(4) 0.3716(2) 0.0405(18) Uani 1.00 1 d . . . C(18) C 0.2861(5) 0.8708(4) 0.6542(2) 0.0308(17) Uani 1.00 1 d . . . C(19) C 0.5416(4) 0.7017(3) 0.49920(19) 0.0318(15) Uani 1.00 1 d . . . C(20) C 0.3928(4) 0.8396(4) 0.5244(2) 0.0350(16) Uani 1.00 1 d . . . C(21) C 0.3142(5) 0.4123(4) 0.6173(2) 0.0379(18) Uani 1.00 1 d . . . C(22) C 0.3296(5) 0.9800(4) 0.6595(2) 0.041(2) Uani 1.00 1 d . . . C(23) C 0.2093(5) 0.5846(4) 0.4044(2) 0.0432(19) Uani 1.00 1 d . . . C(24) C 0.2900(5) 0.6302(4) 0.4470(2) 0.0349(18) Uani 1.00 1 d . . . C(25) C 0.2772(5) 0.7160(5) 0.3285(2) 0.0456(19) Uani 1.00 1 d . . . C(26) C 0.2049(5) 0.5131(4) 0.5280(2) 0.0419(18) Uani 1.00 1 d . . . C(27) C 0.4670(5) 0.4896(3) 0.6996(2) 0.0358(16) Uani 1.00 1 d . . . C(28) C 0.3479(5) 0.4215(4) 0.6846(2) 0.0402(18) Uani 1.00 1 d . . . C(29) C 0.3489(5) 0.6953(4) 0.7465(2) 0.0402(18) Uani 1.00 1 d . . . C(30) C 0.0812(6) 0.9425(5) 0.6724(2) 0.056(2) Uani 1.00 1 d . . . C(31) C 0.2040(5) 0.6285(5) 0.3454(2) 0.045(2) Uani 1.00 1 d . . . C(32) C 0.6253(5) 0.5143(4) 0.5882(2) 0.0306(16) Uani 1.00 1 d . . . C(33) C 0.8166(5) 0.3722(4) 0.5495(2) 0.0403(19) Uani 1.00 1 d . . . C(34) C 0.1619(5) 0.8547(5) 0.6602(2) 0.048(2) Uani 1.00 1 d . . . C(35) C 0.8250(5) 0.4269(4) 0.6056(2) 0.0415(19) Uani 1.00 1 d . . . C(36) C 0.1267(6) 1.0505(5) 0.6791(2) 0.046(2) Uani 1.00 1 d . . . C(37) C 0.4080(6) 0.7038(4) 0.8501(2) 0.058(2) Uani 1.00 1 d . . . C(38) C 0.2486(6) 1.0683(5) 0.6730(2) 0.051(2) Uani 1.00 1 d . . . H(1) H 0.7370 0.5325 0.6636 0.042 Uiso 1.00 1 c R . . H(2) H 0.7056 0.3454 0.4758 0.046 Uiso 1.00 1 c R . . H(3) H 0.5472 0.4609 0.5078 0.041 Uiso 1.00 1 c R . . H(4) H 0.4101 0.8217 0.3598 0.048 Uiso 1.00 1 c R . . H(5) H 0.4152 0.9937 0.6541 0.050 Uiso 1.00 1 c R . . H(6) H 0.1569 0.5242 0.4156 0.052 Uiso 1.00 1 c R . . H(7) H 0.2726 0.7460 0.2881 0.055 Uiso 1.00 1 c R . . H(8) H -0.0047 0.9290 0.6766 0.067 Uiso 1.00 1 c R . . H(9) H 0.1500 0.5957 0.3161 0.054 Uiso 1.00 1 c R . . H(10) H 0.1303 0.7811 0.6553 0.058 Uiso 1.00 1 c R . . H(11) H 0.8961 0.4168 0.6305 0.050 Uiso 1.00 1 c R . . H(12) H 0.2801 1.1420 0.6777 0.061 Uiso 1.00 1 c R . . H(13) H 0.1416 0.4764 0.6138 0.046 Uiso 1.00 1 c R . . H(14) H 0.2423 0.5687 0.6137 0.046 Uiso 1.00 1 c R . . H(15) H 0.5430 0.6321 0.4780 0.038 Uiso 1.00 1 c R . . H(16) H 0.6211 0.7350 0.4975 0.038 Uiso 1.00 1 c R . . H(17) H 0.4290 0.9117 0.5285 0.042 Uiso 1.00 1 c R . . H(18) H 0.3063 0.8473 0.5191 0.042 Uiso 1.00 1 c R . . H(19) H 0.2832 0.3395 0.6089 0.046 Uiso 1.00 1 c R . . H(20) H 0.3873 0.4244 0.5941 0.045 Uiso 1.00 1 c R . . H(21) H 0.1250 0.5400 0.5180 0.050 Uiso 1.00 1 c R . . H(22) H 0.2175 0.4423 0.5090 0.050 Uiso 1.00 1 c R . . H(23) H 0.5363 0.4451 0.6888 0.043 Uiso 1.00 1 c R . . H(24) H 0.4700 0.5065 0.7423 0.043 Uiso 1.00 1 c R . . H(25) H 0.2811 0.4584 0.7044 0.048 Uiso 1.00 1 c R . . H(26) H 0.3563 0.3480 0.7009 0.048 Uiso 1.00 1 c R . . H(27) H 0.2989 0.6313 0.7538 0.048 Uiso 1.00 1 c R . . H(28) H 0.3010 0.7612 0.7519 0.048 Uiso 1.00 1 c R . . H(29) H 0.4016 0.7802 0.8619 0.070 Uiso 1.00 1 c R . . H(30) H 0.4654 0.6668 0.8762 0.069 Uiso 1.00 1 c R . . H(31) H 0.3296 0.6689 0.8537 0.069 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0499(4) 0.0594(4) 0.0824(4) 0.0171(4) 0.0105(3) -0.0163(3) Br(2) 0.0731(6) 0.0674(4) 0.1064(5) 0.0357(4) -0.0145(4) -0.0332(4) O(3) 0.050(2) 0.061(2) 0.038(2) 0.003(2) -0.010(2) -0.0140(19) O(4) 0.040(2) 0.043(2) 0.040(2) -0.016(2) -0.0088(19) 0.0077(18) N(5) 0.027(2) 0.030(2) 0.035(2) 0.004(2) -0.000(2) -0.004(2) C(6) 0.028(3) 0.024(3) 0.040(3) -0.001(2) -0.007(2) -0.003(2) C(7) 0.028(3) 0.033(3) 0.031(2) -0.009(2) 0.003(2) -0.006(2) C(8) 0.023(3) 0.040(3) 0.038(3) 0.007(3) 0.006(2) -0.003(2) C(9) 0.024(3) 0.025(3) 0.033(2) -0.007(2) 0.003(2) -0.001(2) C(10) 0.024(3) 0.025(3) 0.032(2) -0.001(2) -0.002(2) -0.003(2) C(11) 0.030(3) 0.031(3) 0.030(2) 0.001(2) -0.006(2) -0.000(2) C(12) 0.026(3) 0.033(3) 0.047(3) 0.003(3) -0.001(2) -0.003(2) C(13) 0.021(3) 0.027(3) 0.035(3) 0.001(2) -0.002(2) -0.010(2) C(14) 0.041(4) 0.029(3) 0.046(3) -0.001(3) 0.011(3) -0.015(2) C(15) 0.032(3) 0.043(3) 0.039(3) -0.012(3) -0.004(2) -0.000(2) C(16) 0.027(3) 0.032(3) 0.044(3) -0.008(2) 0.002(2) -0.003(2) C(17) 0.046(4) 0.037(3) 0.039(3) 0.001(3) 0.008(3) 0.004(2) C(18) 0.029(3) 0.031(3) 0.033(3) 0.002(3) 0.002(2) -0.004(2) C(19) 0.025(3) 0.029(3) 0.042(2) 0.001(2) -0.002(2) 0.001(2) C(20) 0.028(3) 0.032(3) 0.045(3) 0.003(2) 0.002(2) -0.001(2) C(21) 0.039(4) 0.035(3) 0.040(3) -0.012(3) 0.005(2) -0.001(2) C(22) 0.036(4) 0.041(3) 0.048(3) 0.001(3) 0.003(2) -0.001(2) C(23) 0.047(4) 0.037(3) 0.045(3) -0.007(3) -0.001(3) -0.008(2) C(24) 0.030(3) 0.037(3) 0.038(3) 0.003(3) -0.004(3) -0.005(2) C(25) 0.054(4) 0.053(4) 0.030(3) 0.002(4) -0.002(3) 0.001(3) C(26) 0.034(3) 0.039(3) 0.053(3) -0.008(3) -0.005(2) 0.000(2) C(27) 0.036(3) 0.040(3) 0.031(2) 0.000(3) 0.003(2) 0.001(2) C(28) 0.039(4) 0.036(3) 0.045(3) -0.005(3) 0.005(2) 0.002(2) C(29) 0.046(4) 0.034(3) 0.040(3) 0.000(3) 0.002(2) -0.005(2) C(30) 0.022(4) 0.060(4) 0.086(4) 0.003(3) 0.002(3) -0.027(3) C(31) 0.041(4) 0.055(4) 0.041(3) 0.004(3) -0.009(3) -0.010(3) C(32) 0.029(3) 0.025(3) 0.038(3) -0.004(2) 0.007(2) 0.005(2) C(33) 0.039(4) 0.026(3) 0.055(3) 0.003(3) 0.011(3) -0.004(2) C(34) 0.032(4) 0.041(4) 0.071(4) 0.000(3) -0.003(3) -0.016(3) C(35) 0.039(4) 0.037(3) 0.048(3) 0.003(3) -0.007(2) 0.001(2) C(36) 0.034(4) 0.062(4) 0.043(3) 0.005(3) -0.004(2) -0.015(3) C(37) 0.086(5) 0.053(4) 0.034(3) 0.003(4) -0.003(3) -0.004(2) C(38) 0.056(5) 0.031(3) 0.065(4) 0.003(3) -0.002(3) -0.013(3) #============================================================================== _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) C(33) 1.893(5) yes . . Br(2) C(36) 1.882(6) yes . . O(3) C(29) 1.416(6) yes . . O(3) C(37) 1.423(5) yes . . O(4) C(24) 1.377(6) yes . . O(4) C(26) 1.448(6) yes . . N(5) C(8) 1.430(6) yes . . N(5) C(19) 1.478(6) yes . . N(5) C(20) 1.495(6) yes . . C(6) C(7) 1.409(7) yes . . C(6) C(9) 1.404(6) yes . . C(6) C(18) 1.482(7) yes . . C(7) C(11) 1.418(7) yes . . C(7) C(29) 1.507(6) yes . . C(8) C(17) 1.393(7) yes . . C(8) C(24) 1.396(7) yes . . C(9) C(10) 1.364(6) yes . . C(9) C(20) 1.524(6) yes . . C(10) C(13) 1.380(6) yes . . C(10) C(19) 1.511(6) yes . . C(11) C(13) 1.420(6) yes . . C(11) C(27) 1.510(6) yes . . C(12) C(32) 1.419(7) yes . . C(12) C(35) 1.372(8) yes . . C(13) C(32) 1.488(7) yes . . C(14) C(16) 1.358(7) yes . . C(14) C(33) 1.382(8) yes . . C(15) C(21) 1.518(7) yes . . C(15) C(26) 1.523(6) yes . . C(16) C(32) 1.422(6) yes . . C(17) C(25) 1.392(7) yes . . C(18) C(22) 1.392(7) yes . . C(18) C(34) 1.367(8) yes . . C(21) C(28) 1.514(7) yes . . C(22) C(38) 1.403(8) yes . . C(23) C(24) 1.385(7) yes . . C(23) C(31) 1.387(7) yes . . C(25) C(31) 1.363(8) yes . . C(27) C(28) 1.561(7) yes . . C(30) C(34) 1.390(8) yes . . C(30) C(36) 1.388(8) yes . . C(33) C(35) 1.388(7) yes . . C(36) C(38) 1.345(9) yes . . C(12) H(1) 0.950 no . . C(14) H(2) 0.950 no . . C(15) H(13) 0.950 no . . C(15) H(14) 0.950 no . . C(16) H(3) 0.950 no . . C(17) H(4) 0.950 no . . C(19) H(15) 0.950 no . . C(19) H(16) 0.950 no . . C(20) H(17) 0.950 no . . C(20) H(18) 0.950 no . . C(21) H(19) 0.950 no . . C(21) H(20) 0.950 no . . C(22) H(5) 0.950 no . . C(23) H(6) 0.950 no . . C(25) H(7) 0.950 no . . C(26) H(21) 0.950 no . . C(26) H(22) 0.950 no . . C(27) H(23) 0.950 no . . C(27) H(24) 0.950 no . . C(28) H(25) 0.950 no . . C(28) H(26) 0.950 no . . C(29) H(27) 0.950 no . . C(29) H(28) 0.950 no . . C(30) H(8) 0.950 no . . C(31) H(9) 0.950 no . . C(34) H(10) 0.950 no . . C(35) H(11) 0.950 no . . C(37) H(29) 0.950 no . . C(37) H(30) 0.950 no . . C(37) H(31) 0.950 no . . C(38) H(12) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(29) O(3) C(37) 111.4(4) yes . . . C(24) O(4) C(26) 118.6(4) yes . . . C(8) N(5) C(19) 113.5(3) yes . . . C(8) N(5) C(20) 115.9(3) yes . . . C(19) N(5) C(20) 105.8(3) yes . . . C(7) C(6) C(9) 117.0(4) yes . . . C(7) C(6) C(18) 122.9(4) yes . . . C(9) C(6) C(18) 119.9(4) yes . . . C(6) C(7) C(11) 120.5(4) yes . . . C(6) C(7) C(29) 120.3(4) yes . . . C(11) C(7) C(29) 119.2(4) yes . . . N(5) C(8) C(17) 116.4(4) yes . . . N(5) C(8) C(24) 126.1(4) yes . . . C(17) C(8) C(24) 117.5(4) yes . . . C(6) C(9) C(10) 122.2(4) yes . . . C(6) C(9) C(20) 127.4(4) yes . . . C(10) C(9) C(20) 110.3(4) yes . . . C(9) C(10) C(13) 121.7(4) yes . . . C(9) C(10) C(19) 108.3(3) yes . . . C(13) C(10) C(19) 129.8(4) yes . . . C(7) C(11) C(13) 119.4(4) yes . . . C(7) C(11) C(27) 120.5(4) yes . . . C(13) C(11) C(27) 119.3(4) yes . . . C(32) C(12) C(35) 121.4(4) yes . . . C(10) C(13) C(11) 118.1(4) yes . . . C(10) C(13) C(32) 119.8(4) yes . . . C(11) C(13) C(32) 122.1(4) yes . . . C(16) C(14) C(33) 120.4(4) yes . . . C(21) C(15) C(26) 115.6(4) yes . . . C(14) C(16) C(32) 122.0(4) yes . . . C(8) C(17) C(25) 121.9(5) yes . . . C(6) C(18) C(22) 121.0(5) yes . . . C(6) C(18) C(34) 121.7(5) yes . . . C(22) C(18) C(34) 117.2(5) yes . . . N(5) C(19) C(10) 106.0(3) yes . . . N(5) C(20) C(9) 104.4(3) yes . . . C(15) C(21) C(28) 113.2(4) yes . . . C(18) C(22) C(38) 120.6(5) yes . . . C(24) C(23) C(31) 119.7(5) yes . . . O(4) C(24) C(8) 117.0(4) yes . . . O(4) C(24) C(23) 122.1(4) yes . . . C(8) C(24) C(23) 120.8(4) yes . . . C(17) C(25) C(31) 118.9(4) yes . . . O(4) C(26) C(15) 109.0(4) yes . . . C(11) C(27) C(28) 111.0(4) yes . . . C(21) C(28) C(27) 116.0(4) yes . . . O(3) C(29) C(7) 109.0(4) yes . . . C(34) C(30) C(36) 119.8(6) yes . . . C(23) C(31) C(25) 121.0(5) yes . . . C(12) C(32) C(13) 120.9(4) yes . . . C(12) C(32) C(16) 116.1(4) yes . . . C(13) C(32) C(16) 122.9(4) yes . . . Br(1) C(33) C(14) 119.7(4) yes . . . Br(1) C(33) C(35) 120.4(4) yes . . . C(14) C(33) C(35) 119.9(5) yes . . . C(18) C(34) C(30) 122.2(5) yes . . . C(12) C(35) C(33) 120.2(5) yes . . . Br(2) C(36) C(30) 119.3(5) yes . . . Br(2) C(36) C(38) 121.6(4) yes . . . C(30) C(36) C(38) 119.0(5) yes . . . C(22) C(38) C(36) 121.2(5) yes . . . C(32) C(12) H(1) 118.5 no . . . C(35) C(12) H(1) 120.0 no . . . C(16) C(14) H(2) 119.8 no . . . C(33) C(14) H(2) 119.8 no . . . C(21) C(15) H(13) 107.9 no . . . C(21) C(15) H(14) 108.0 no . . . C(26) C(15) H(13) 108.6 no . . . C(26) C(15) H(14) 107.2 no . . . H(13) C(15) H(14) 109.5 no . . . C(14) C(16) H(3) 120.3 no . . . C(32) C(16) H(3) 117.7 no . . . C(8) C(17) H(4) 118.8 no . . . C(25) C(17) H(4) 119.2 no . . . N(5) C(19) H(15) 110.4 no . . . N(5) C(19) H(16) 110.3 no . . . C(10) C(19) H(15) 110.6 no . . . C(10) C(19) H(16) 110.1 no . . . H(15) C(19) H(16) 109.5 no . . . N(5) C(20) H(17) 110.7 no . . . N(5) C(20) H(18) 110.8 no . . . C(9) C(20) H(17) 110.3 no . . . C(9) C(20) H(18) 111.1 no . . . H(17) C(20) H(18) 109.5 no . . . C(15) C(21) H(19) 108.8 no . . . C(15) C(21) H(20) 108.2 no . . . C(28) C(21) H(19) 109.6 no . . . C(28) C(21) H(20) 107.5 no . . . H(19) C(21) H(20) 109.5 no . . . C(18) C(22) H(5) 118.8 no . . . C(38) C(22) H(5) 120.6 no . . . C(24) C(23) H(6) 120.3 no . . . C(31) C(23) H(6) 120.0 no . . . C(17) C(25) H(7) 120.6 no . . . C(31) C(25) H(7) 120.5 no . . . O(4) C(26) H(21) 110.3 no . . . O(4) C(26) H(22) 109.1 no . . . C(15) C(26) H(21) 110.9 no . . . C(15) C(26) H(22) 108.1 no . . . H(21) C(26) H(22) 109.5 no . . . C(11) C(27) H(23) 109.1 no . . . C(11) C(27) H(24) 109.0 no . . . C(28) C(27) H(23) 108.2 no . . . C(28) C(27) H(24) 110.0 no . . . H(23) C(27) H(24) 109.5 no . . . C(21) C(28) H(25) 106.7 no . . . C(21) C(28) H(26) 108.4 no . . . C(27) C(28) H(25) 107.1 no . . . C(27) C(28) H(26) 108.9 no . . . H(25) C(28) H(26) 109.5 no . . . O(3) C(29) H(27) 109.6 no . . . O(3) C(29) H(28) 109.7 no . . . C(7) C(29) H(27) 109.1 no . . . C(7) C(29) H(28) 109.9 no . . . H(27) C(29) H(28) 109.5 no . . . C(34) C(30) H(8) 120.5 no . . . C(36) C(30) H(8) 119.7 no . . . C(23) C(31) H(9) 119.4 no . . . C(25) C(31) H(9) 119.6 no . . . C(18) C(34) H(10) 118.3 no . . . C(30) C(34) H(10) 119.5 no . . . C(12) C(35) H(11) 120.2 no . . . C(33) C(35) H(11) 119.6 no . . . O(3) C(37) H(29) 110.0 no . . . O(3) C(37) H(30) 109.1 no . . . O(3) C(37) H(31) 109.2 no . . . H(29) C(37) H(30) 109.5 no . . . H(29) C(37) H(31) 109.5 no . . . H(30) C(37) H(31) 109.5 no . . . C(22) C(38) H(12) 119.6 no . . . C(36) C(38) H(12) 119.2 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(37) O(3) C(29) C(7) 178.2(4) ? . . . . C(24) O(4) C(26) C(15) -169.8(4) ? . . . . C(26) O(4) C(24) C(8) 166.7(4) ? . . . . C(26) O(4) C(24) C(23) -11.1(7) ? . . . . C(8) N(5) C(19) C(10) -105.2(4) ? . . . . C(19) N(5) C(8) C(17) -122.6(4) ? . . . . C(19) N(5) C(8) C(24) 55.9(6) ? . . . . C(8) N(5) C(20) C(9) 106.9(4) ? . . . . C(20) N(5) C(8) C(17) 114.6(5) ? . . . . C(20) N(5) C(8) C(24) -67.0(6) ? . . . . C(19) N(5) C(20) C(9) -19.9(4) ? . . . . C(20) N(5) C(19) C(10) 23.1(4) ? . . . . C(7) C(6) C(9) C(10) -5.1(7) ? . . . . C(7) C(6) C(9) C(20) 170.4(4) ? . . . . C(9) C(6) C(7) C(11) -2.3(7) ? . . . . C(9) C(6) C(7) C(29) 178.6(4) ? . . . . C(7) C(6) C(18) C(22) 112.9(5) ? . . . . C(7) C(6) C(18) C(34) -70.2(7) ? . . . . C(18) C(6) C(7) C(11) 174.2(5) ? . . . . C(18) C(6) C(7) C(29) -4.9(7) ? . . . . C(9) C(6) C(18) C(22) -70.6(6) ? . . . . C(9) C(6) C(18) C(34) 106.2(6) ? . . . . C(18) C(6) C(9) C(10) 178.3(4) ? . . . . C(18) C(6) C(9) C(20) -6.2(8) ? . . . . C(6) C(7) C(11) C(13) 9.9(7) ? . . . . C(6) C(7) C(11) C(27) -160.2(4) ? . . . . C(6) C(7) C(29) O(3) -120.1(5) ? . . . . C(11) C(7) C(29) O(3) 60.8(6) ? . . . . C(29) C(7) C(11) C(13) -171.0(4) ? . . . . C(29) C(7) C(11) C(27) 19.0(7) ? . . . . N(5) C(8) C(17) C(25) -178.5(5) ? . . . . N(5) C(8) C(24) O(4) 0.8(8) ? . . . . N(5) C(8) C(24) C(23) 178.6(5) ? . . . . C(17) C(8) C(24) O(4) 179.2(4) ? . . . . C(17) C(8) C(24) C(23) -2.9(8) ? . . . . C(24) C(8) C(17) C(25) 2.9(8) ? . . . . C(6) C(9) C(10) C(13) 4.9(7) ? . . . . C(6) C(9) C(10) C(19) -178.9(4) ? . . . . C(6) C(9) C(20) N(5) -166.5(4) ? . . . . C(10) C(9) C(20) N(5) 9.5(5) ? . . . . C(20) C(9) C(10) C(13) -171.4(4) ? . . . . C(20) C(9) C(10) C(19) 4.9(5) ? . . . . C(9) C(10) C(13) C(11) 2.9(7) ? . . . . C(9) C(10) C(13) C(32) -177.1(4) ? . . . . C(9) C(10) C(19) N(5) -17.6(5) ? . . . . C(13) C(10) C(19) N(5) 158.2(5) ? . . . . C(19) C(10) C(13) C(11) -172.4(4) ? . . . . C(19) C(10) C(13) C(32) 7.6(8) ? . . . . C(7) C(11) C(13) C(10) -10.1(7) ? . . . . C(7) C(11) C(13) C(32) 169.9(4) ? . . . . C(7) C(11) C(27) C(28) 77.4(5) ? . . . . C(13) C(11) C(27) C(28) -92.7(5) ? . . . . C(27) C(11) C(13) C(10) 160.1(4) ? . . . . C(27) C(11) C(13) C(32) -19.9(7) ? . . . . C(32) C(12) C(35) C(33) 0.0(7) ? . . . . C(35) C(12) C(32) C(13) -172.6(4) ? . . . . C(35) C(12) C(32) C(16) 2.4(7) ? . . . . C(10) C(13) C(32) C(12) 122.3(5) ? . . . . C(10) C(13) C(32) C(16) -52.4(7) ? . . . . C(11) C(13) C(32) C(12) -57.7(7) ? . . . . C(11) C(13) C(32) C(16) 127.6(5) ? . . . . C(16) C(14) C(33) Br(1) -177.2(4) ? . . . . C(16) C(14) C(33) C(35) 1.9(8) ? . . . . C(33) C(14) C(16) C(32) 0.8(8) ? . . . . C(21) C(15) C(26) O(4) -84.0(5) ? . . . . C(26) C(15) C(21) C(28) 165.3(4) ? . . . . C(14) C(16) C(32) C(12) -2.9(7) ? . . . . C(14) C(16) C(32) C(13) 172.1(4) ? . . . . C(8) C(17) C(25) C(31) -1.4(8) ? . . . . C(6) C(18) C(22) C(38) 179.7(4) ? . . . . C(6) C(18) C(34) C(30) -178.3(4) ? . . . . C(22) C(18) C(34) C(30) -1.3(7) ? . . . . C(34) C(18) C(22) C(38) 2.7(7) ? . . . . C(15) C(21) C(28) C(27) -96.8(5) ? . . . . C(18) C(22) C(38) C(36) -2.3(7) ? . . . . C(24) C(23) C(31) C(25) 0.1(7) ? . . . . C(31) C(23) C(24) O(4) 179.2(5) ? . . . . C(31) C(23) C(24) C(8) 1.5(8) ? . . . . C(17) C(25) C(31) C(23) -0.2(7) ? . . . . C(11) C(27) C(28) C(21) 45.0(5) ? . . . . C(34) C(30) C(36) Br(2) -178.5(4) ? . . . . C(34) C(30) C(36) C(38) 0.8(8) ? . . . . C(36) C(30) C(34) C(18) -0.4(7) ? . . . . Br(1) C(33) C(35) C(12) 176.8(4) ? . . . . C(14) C(33) C(35) C(12) -2.3(8) ? . . . . Br(2) C(36) C(38) C(22) 179.8(2) ? . . . . C(30) C(36) C(38) C(22) 0.5(8) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) C(14) 3.566(5) ? . 2_556 Br(1) C(16) 3.554(5) ? . 2_556 O(3) C(28) 3.528(6) ? . 3_656 C(9) C(23) 3.591(7) ? . 2_566 C(12) C(17) 3.199(7) ? . 2_566 C(14) Br(1) 3.566(5) ? . 2_456 C(16) Br(1) 3.554(5) ? . 2_456 C(17) C(12) 3.199(7) ? . 2_466 C(17) C(30) 3.564(8) ? . 2_566 C(19) C(24) 3.557(7) ? . 2_566 C(23) C(9) 3.591(7) ? . 2_466 C(24) C(19) 3.557(7) ? . 2_466 C(28) O(3) 3.528(6) ? . 3_646 C(28) C(31) 3.590(7) ? . 4_565 C(30) C(17) 3.564(8) ? . 2_466 C(31) C(28) 3.590(7) ? . 4_564 Br(1) H(2) 3.178 ? . 2_556 Br(1) H(3) 3.156 ? . 2_556 Br(1) H(20) 3.574 ? . 2_556 Br(1) H(22) 3.498 ? . 1_655 Br(1) H(30) 3.339 ? . 4_664 Br(2) H(7) 3.185 ? . 4_575 Br(2) H(11) 3.557 ? . 1_465 O(3) H(5) 3.092 ? . 3_646 O(3) H(12) 3.095 ? . 3_646 O(3) H(23) 3.021 ? . 3_656 O(3) H(26) 2.793 ? . 3_656 O(4) H(16) 2.832 ? . 2_466 N(5) H(10) 3.464 ? . 2_566 N(5) H(21) 2.908 ? . 2_566 C(6) H(9) 3.523 ? . 2_566 C(8) H(8) 3.287 ? . 2_566 C(8) H(10) 3.451 ? . 2_566 C(8) H(16) 3.096 ? . 2_466 C(9) H(6) 3.555 ? . 2_566 C(12) H(4) 2.927 ? . 2_566 C(12) H(29) 2.973 ? . 3_646 C(14) H(17) 3.504 ? . 2_566 C(14) H(18) 3.433 ? . 2_566 C(14) H(29) 3.224 ? . 3_646 C(16) H(18) 3.327 ? . 2_566 C(16) H(29) 3.095 ? . 3_646 C(17) H(1) 2.891 ? . 2_466 C(17) H(8) 2.913 ? . 2_566 C(17) H(10) 3.053 ? . 2_566 C(19) H(10) 3.501 ? . 2_566 C(19) H(18) 2.956 ? . 2_566 C(19) H(21) 3.234 ? . 2_566 C(20) H(6) 3.542 ? . 2_566 C(20) H(16) 3.115 ? . 2_466 C(20) H(21) 3.043 ? . 2_566 C(21) H(12) 3.504 ? . 1_545 C(21) H(29) 3.492 ? . 3_646 C(22) H(24) 3.063 ? . 3_656 C(22) H(30) 3.243 ? . 3_656 C(23) H(5) 3.559 ? . 2_466 C(23) H(8) 3.570 ? . 2_566 C(23) H(16) 3.179 ? . 2_466 C(23) H(17) 3.373 ? . 2_466 C(23) H(31) 3.248 ? . 4_564 C(24) H(8) 3.560 ? . 2_566 C(24) H(16) 2.721 ? . 2_466 C(25) H(1) 3.038 ? . 2_466 C(25) H(8) 2.933 ? . 2_566 C(25) H(25) 3.466 ? . 4_564 C(25) H(26) 3.221 ? . 4_564 C(26) H(16) 3.189 ? . 2_466 C(26) H(17) 3.356 ? . 2_466 C(27) H(5) 3.428 ? . 3_646 C(27) H(9) 3.009 ? . 4_565 C(27) H(29) 3.173 ? . 3_646 C(28) H(7) 3.281 ? . 4_565 C(28) H(9) 2.865 ? . 4_565 C(28) H(12) 3.419 ? . 1_545 C(28) H(29) 3.354 ? . 3_646 C(29) H(23) 3.523 ? . 3_656 C(30) H(15) 3.413 ? . 2_466 C(31) H(5) 3.455 ? . 2_466 C(31) H(8) 3.268 ? . 2_566 C(31) H(24) 3.344 ? . 4_564 C(31) H(25) 3.240 ? . 4_564 C(31) H(26) 3.221 ? . 4_564 C(31) H(31) 3.574 ? . 4_564 C(32) H(18) 3.468 ? . 2_566 C(32) H(29) 3.011 ? . 3_646 C(33) H(17) 3.319 ? . 2_566 C(33) H(29) 3.243 ? . 3_646 C(33) H(31) 3.583 ? . 3_646 C(34) H(4) 3.475 ? . 2_466 C(34) H(15) 3.274 ? . 2_466 C(35) H(4) 3.228 ? . 2_566 C(35) H(13) 3.489 ? . 1_655 C(35) H(29) 3.099 ? . 3_646 C(36) H(7) 3.565 ? . 4_575 C(37) H(5) 3.158 ? . 3_646 C(37) H(6) 3.152 ? . 4_565 C(37) H(12) 3.515 ? . 3_646 C(37) H(23) 3.062 ? . 3_656 C(37) H(26) 3.275 ? . 3_656 C(38) H(1) 3.581 ? . 3_656 C(38) H(2) 3.428 ? . 2_466 C(38) H(7) 3.351 ? . 4_575 C(38) H(19) 3.544 ? . 1_565 C(38) H(26) 3.589 ? . 1_565 C(38) H(30) 3.486 ? . 3_656 H(1) C(17) 2.891 ? . 2_566 H(1) C(25) 3.038 ? . 2_566 H(1) C(38) 3.581 ? . 3_646 H(1) H(4) 2.610 ? . 2_566 H(1) H(7) 2.870 ? . 2_566 H(1) H(29) 3.412 ? . 3_646 H(2) Br(1) 3.178 ? . 2_456 H(2) C(38) 3.428 ? . 2_566 H(2) H(12) 3.438 ? . 2_566 H(2) H(19) 2.996 ? . 2_556 H(2) H(22) 3.452 ? . 2_556 H(3) Br(1) 3.156 ? . 2_456 H(4) C(12) 2.927 ? . 2_466 H(4) C(34) 3.475 ? . 2_566 H(4) C(35) 3.228 ? . 2_466 H(4) H(1) 2.610 ? . 2_466 H(4) H(8) 3.231 ? . 2_566 H(4) H(10) 2.704 ? . 2_566 H(4) H(11) 3.133 ? . 2_466 H(4) H(13) 3.528 ? . 2_566 H(5) O(3) 3.092 ? . 3_656 H(5) C(23) 3.559 ? . 2_566 H(5) C(27) 3.428 ? . 3_656 H(5) C(31) 3.455 ? . 2_566 H(5) C(37) 3.158 ? . 3_656 H(5) H(6) 3.035 ? . 2_566 H(5) H(9) 2.837 ? . 2_566 H(5) H(23) 3.504 ? . 3_656 H(5) H(24) 2.579 ? . 3_656 H(5) H(30) 2.526 ? . 3_656 H(5) H(31) 3.473 ? . 3_656 H(6) C(9) 3.555 ? . 2_466 H(6) C(20) 3.542 ? . 2_466 H(6) C(37) 3.152 ? . 4_564 H(6) H(5) 3.035 ? . 2_466 H(6) H(16) 3.461 ? . 2_466 H(6) H(17) 2.859 ? . 2_466 H(6) H(30) 2.774 ? . 4_564 H(6) H(31) 2.674 ? . 4_564 H(7) Br(2) 3.185 ? . 4_574 H(7) C(28) 3.281 ? . 4_564 H(7) C(36) 3.565 ? . 4_574 H(7) C(38) 3.351 ? . 4_574 H(7) H(1) 2.870 ? . 2_466 H(7) H(8) 3.285 ? . 2_566 H(7) H(12) 2.806 ? . 4_574 H(7) H(25) 3.099 ? . 4_564 H(7) H(26) 2.609 ? . 4_564 H(8) C(8) 3.287 ? . 2_466 H(8) C(17) 2.913 ? . 2_466 H(8) C(23) 3.570 ? . 2_466 H(8) C(24) 3.560 ? . 2_466 H(8) C(25) 2.933 ? . 2_466 H(8) C(31) 3.268 ? . 2_466 H(8) H(4) 3.231 ? . 2_466 H(8) H(7) 3.285 ? . 2_466 H(8) H(15) 3.479 ? . 2_466 H(9) C(6) 3.523 ? . 2_466 H(9) C(27) 3.009 ? . 4_564 H(9) C(28) 2.865 ? . 4_564 H(9) H(5) 2.837 ? . 2_466 H(9) H(23) 3.460 ? . 4_564 H(9) H(24) 2.399 ? . 4_564 H(9) H(25) 2.620 ? . 4_564 H(9) H(26) 2.594 ? . 4_564 H(9) H(27) 3.080 ? . 4_564 H(9) H(31) 3.271 ? . 4_564 H(10) N(5) 3.464 ? . 2_466 H(10) C(8) 3.451 ? . 2_466 H(10) C(17) 3.053 ? . 2_466 H(10) C(19) 3.501 ? . 2_466 H(10) H(4) 2.704 ? . 2_466 H(10) H(15) 3.221 ? . 2_466 H(10) H(16) 3.329 ? . 2_466 H(11) Br(2) 3.557 ? . 1_645 H(11) H(4) 3.133 ? . 2_566 H(11) H(13) 2.780 ? . 1_655 H(12) O(3) 3.095 ? . 3_656 H(12) C(21) 3.504 ? . 1_565 H(12) C(28) 3.419 ? . 1_565 H(12) C(37) 3.515 ? . 3_656 H(12) H(2) 3.438 ? . 2_466 H(12) H(7) 2.806 ? . 4_575 H(12) H(19) 2.791 ? . 1_565 H(12) H(26) 2.642 ? . 1_565 H(12) H(30) 3.014 ? . 3_656 H(13) C(35) 3.489 ? . 1_455 H(13) H(4) 3.528 ? . 2_466 H(13) H(11) 2.780 ? . 1_455 H(15) C(30) 3.413 ? . 2_566 H(15) C(34) 3.274 ? . 2_566 H(15) H(8) 3.479 ? . 2_566 H(15) H(10) 3.221 ? . 2_566 H(15) H(18) 2.867 ? . 2_566 H(16) O(4) 2.832 ? . 2_566 H(16) C(8) 3.096 ? . 2_566 H(16) C(20) 3.115 ? . 2_566 H(16) C(23) 3.179 ? . 2_566 H(16) C(24) 2.721 ? . 2_566 H(16) C(26) 3.189 ? . 2_566 H(16) H(6) 3.461 ? . 2_566 H(16) H(10) 3.329 ? . 2_566 H(16) H(18) 2.264 ? . 2_566 H(16) H(21) 2.706 ? . 2_566 H(17) C(14) 3.504 ? . 2_466 H(17) C(23) 3.373 ? . 2_566 H(17) C(26) 3.356 ? . 2_566 H(17) C(33) 3.319 ? . 2_466 H(17) H(6) 2.859 ? . 2_566 H(17) H(21) 2.423 ? . 2_566 H(18) C(14) 3.433 ? . 2_466 H(18) C(16) 3.327 ? . 2_466 H(18) C(19) 2.956 ? . 2_466 H(18) C(32) 3.468 ? . 2_466 H(18) H(15) 2.867 ? . 2_466 H(18) H(16) 2.264 ? . 2_466 H(19) C(38) 3.544 ? . 1_545 H(19) H(2) 2.996 ? . 2_456 H(19) H(12) 2.791 ? . 1_545 H(19) H(29) 3.547 ? . 3_646 H(19) H(30) 3.434 ? . 3_646 H(20) Br(1) 3.574 ? . 2_456 H(20) H(29) 3.020 ? . 3_646 H(20) H(30) 3.525 ? . 3_646 H(21) N(5) 2.908 ? . 2_466 H(21) C(19) 3.234 ? . 2_466 H(21) C(20) 3.043 ? . 2_466 H(21) H(16) 2.706 ? . 2_466 H(21) H(17) 2.423 ? . 2_466 H(22) Br(1) 3.498 ? . 1_455 H(22) H(2) 3.452 ? . 2_456 H(23) O(3) 3.021 ? . 3_646 H(23) C(29) 3.523 ? . 3_646 H(23) C(37) 3.062 ? . 3_646 H(23) H(5) 3.504 ? . 3_646 H(23) H(9) 3.460 ? . 4_565 H(23) H(28) 3.096 ? . 3_646 H(23) H(29) 2.354 ? . 3_646 H(24) C(22) 3.063 ? . 3_646 H(24) C(31) 3.344 ? . 4_565 H(24) H(5) 2.579 ? . 3_646 H(24) H(9) 2.399 ? . 4_565 H(25) C(25) 3.466 ? . 4_565 H(25) C(31) 3.240 ? . 4_565 H(25) H(7) 3.099 ? . 4_565 H(25) H(9) 2.620 ? . 4_565 H(26) O(3) 2.793 ? . 3_646 H(26) C(25) 3.221 ? . 4_565 H(26) C(31) 3.221 ? . 4_565 H(26) C(37) 3.275 ? . 3_646 H(26) C(38) 3.589 ? . 1_545 H(26) H(7) 2.609 ? . 4_565 H(26) H(9) 2.594 ? . 4_565 H(26) H(12) 2.642 ? . 1_545 H(26) H(29) 3.068 ? . 3_646 H(26) H(30) 3.350 ? . 3_646 H(27) H(9) 3.080 ? . 4_565 H(28) H(23) 3.096 ? . 3_656 H(29) C(12) 2.973 ? . 3_656 H(29) C(14) 3.224 ? . 3_656 H(29) C(16) 3.095 ? . 3_656 H(29) C(21) 3.492 ? . 3_656 H(29) C(27) 3.173 ? . 3_656 H(29) C(28) 3.354 ? . 3_656 H(29) C(32) 3.011 ? . 3_656 H(29) C(33) 3.243 ? . 3_656 H(29) C(35) 3.099 ? . 3_656 H(29) H(1) 3.412 ? . 3_656 H(29) H(19) 3.547 ? . 3_656 H(29) H(20) 3.020 ? . 3_656 H(29) H(23) 2.354 ? . 3_656 H(29) H(26) 3.068 ? . 3_656 H(30) Br(1) 3.339 ? . 4_665 H(30) C(22) 3.243 ? . 3_646 H(30) C(38) 3.486 ? . 3_646 H(30) H(5) 2.526 ? . 3_646 H(30) H(6) 2.774 ? . 4_565 H(30) H(12) 3.014 ? . 3_646 H(30) H(19) 3.434 ? . 3_656 H(30) H(20) 3.525 ? . 3_656 H(30) H(26) 3.350 ? . 3_656 H(31) C(23) 3.248 ? . 4_565 H(31) C(31) 3.574 ? . 4_565 H(31) C(33) 3.583 ? . 3_656 H(31) H(5) 3.473 ? . 3_646 H(31) H(6) 2.674 ? . 4_565 H(31) H(9) 3.271 ? . 4_565 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================