data_General _audit_creation_date '2007-06-02' _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 'ENTER NAME' _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 test _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 Johnson, C.K. (1976). ORTEP-II. A FORTRAN Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku (1998). PROCESS-AUTO. Automatic Data Acquisition and Processing Package for Imaging Plate Diffractometer. Rigaku Corporation, Tokyo 196-8666, Japan Rigaku/MSC and Rigaku Corporation. (2005). CrystalStructure (Version 3.70). Single Crystal Structure Analysis Software. Rigaku/MSC, TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXS97. Program for the Solution of Crystal Structures. University of Gottingen, Germany. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _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__RGK1451 #============================================================================== # CHEMICAL DATA _chemical_formula_sum _chemical_formula_moiety _chemical_formula_weight _chemical_melting_point _chemical_absolute_configuration 'C39 H51 Br1 O6 ' 'C39 H51 Br1 O6 ' 695.73 ? ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '1/2+X,1/2-Y,-Z' 3 '1/2-X,1/2+Y,-Z' 4 '-X,-Y,+Z' #----------------------------------------------------------------------------- _cell_length_a _cell_length_b _cell_length_c _cell_angle_alpha _cell_angle_beta _cell_angle_gamma _cell_volume _cell_formula_units_Z _cell_measurement_reflns_used _cell_measurement_theta_min _cell_measurement_theta_max _cell_measurement_temperature 16.6959(3) 22.8458(4) 9.30051(10) 90.0000 90.0000 90.0000 3547.51(10) 4 36654 4.7 68.2 103.1 #----------------------------------------------------------------------------- _exptl_crystal_description _exptl_crystal_colour _exptl_crystal_size_max _exptl_crystal_size_mid _exptl_crystal_size_min _exptl_crystal_density_diffrn _exptl_crystal_density_meas _exptl_crystal_density_method _exptl_crystal_F_000 _exptl_absorpt_coefficient_mu _exptl_absorpt_correction_type _exptl_absorpt_process_details 'block' 'colorless' 0.18 0.12 0.12 1.303 ? 'not measured' 1472.00 1.937 multi-scan ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.793 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type _diffrn_radiation_wavelength _diffrn_measurement_device_type _diffrn_measurement_method _diffrn_detector_area_resol_mean _diffrn_reflns_number _diffrn_reflns_av_R_equivalents _diffrn_reflns_theta_max _diffrn_measured_fraction_theta_max _diffrn_reflns_theta_full _diffrn_measured_fraction_theta_full _diffrn_reflns_limit_h_min _diffrn_reflns_limit_h_max _diffrn_reflns_limit_k_min _diffrn_reflns_limit_k_max _diffrn_reflns_limit_l_min _diffrn_reflns_limit_l_max 'Cu K¥a' 1.54187 'Rigaku RAXIS-RAPID' ¥w 10.00 42004 0.030 68.24 0.999 68.24 0.999 -19 20 -27 27 -11 11 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 _reflns_number_gt _reflns_threshold_expression _refine_ls_structure_factor_coef _refine_ls_R_factor_gt _refine_ls_wR_factor_ref _refine_ls_hydrogen_treatment _refine_ls_number_reflns _refine_ls_number_parameters _refine_ls_goodness_of_fit_ref _refine_ls_weighting_scheme _refine_ls_weighting_details 6491 6100 F^2^>2.0¥s(F^2^) Fsqd 0.0268 0.0602 constr 6491 424 1.097 calc 'w = 1/[¥s^2^(Fo^2^)+(0.0222P)^2^+1.2765P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.31 _refine_diff_density_min -0.28 _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 -0.023(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.018 0.009 ; 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' -0.676 1.280 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 2829 Friedel Pairs' ; 'O' 'O' 0.049 0.032 ; 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 0.322890(13) 0.813956(10) 0.66449(3) 0.02888(6) Uani 1.00 1 d . . . O(1) O 0.37067(9) 0.06708(6) -0.03518(16) 0.0224(3) Uani 1.00 1 d . . . O(2) O 0.39848(12) 0.08065(7) -0.26896(18) 0.0411(4) Uani 1.00 1 d . . . O(3) O 0.45375(8) 0.42221(6) 0.38506(17) 0.0240(3) Uani 1.00 1 d . . . O(4) O 0.71091(8) 0.57286(6) 0.43441(16) 0.0189(3) Uani 1.00 1 d . . . O(5) O 0.64605(8) 0.62982(5) 0.66890(17) 0.0202(3) Uani 1.00 1 d . . . O(6) O 0.70285(9) 0.71017(7) 0.7641(2) 0.0384(4) Uani 1.00 1 d . . . C(1) C 0.36401(13) 0.22505(9) 0.0927(2) 0.0196(4) Uani 1.00 1 d . . . C(2) C 0.33439(13) 0.16558(9) 0.0362(2) 0.0223(4) Uani 1.00 1 d . . . C(3) C 0.40387(13) 0.12425(8) 0.0040(2) 0.0187(4) Uani 1.00 1 d . . . C(4) C 0.46463(12) 0.11431(8) 0.1267(2) 0.0174(4) Uani 1.00 1 d . . . C(5) C 0.48806(11) 0.17662(8) 0.1794(2) 0.0163(4) Uani 1.00 1 d . . . C(6) C 0.55572(12) 0.18004(9) 0.2906(2) 0.0189(4) Uani 1.00 1 d . . . C(7) C 0.59964(12) 0.23932(8) 0.2803(2) 0.0177(4) Uani 1.00 1 d . . . C(8) C 0.54391(12) 0.29062(8) 0.2363(2) 0.0159(4) Uani 1.00 1 d . . . C(9) C 0.45735(12) 0.27399(8) 0.2843(2) 0.0156(4) Uani 1.00 1 d . . . C(10) C 0.41798(12) 0.21700(8) 0.2247(2) 0.0159(4) Uani 1.00 1 d . . . C(11) C 0.41097(12) 0.33100(8) 0.2783(2) 0.0203(4) Uani 1.00 1 d . . . C(12) C 0.47215(12) 0.37434(8) 0.3342(2) 0.0179(4) Uani 1.00 1 d . . . C(13) C 0.55426(11) 0.34909(8) 0.3178(2) 0.0157(4) Uani 1.00 1 d . . . C(14) C 0.62270(12) 0.37392(8) 0.3674(2) 0.0168(4) Uani 1.00 1 d . . . C(15) C 0.62110(12) 0.42817(9) 0.4531(2) 0.0173(4) Uani 1.00 1 d . . . C(16) C 0.67939(13) 0.44690(8) 0.5395(2) 0.0179(4) Uani 1.00 1 d . . . C(17) C 0.67420(13) 0.50212(8) 0.6254(2) 0.0171(4) Uani 1.00 1 d . . . C(18) C 0.70437(12) 0.34757(9) 0.3418(2) 0.0220(4) Uani 1.00 1 d . . . C(19) C 0.36615(12) 0.19443(9) 0.3513(2) 0.0206(4) Uani 1.00 1 d . . . C(20) C 0.73012(12) 0.55204(9) 0.5734(2) 0.0164(4) Uani 1.00 1 d . . . C(21) C 0.81861(13) 0.53468(9) 0.5687(2) 0.0196(4) Uani 1.00 1 d . . . C(22) C 0.72044(12) 0.59755(8) 0.6930(2) 0.0187(4) Uani 1.00 1 d . . . C(23) C 0.71317(12) 0.56196(8) 0.8323(2) 0.0211(4) Uani 1.00 1 d . . . C(24) C 0.69431(12) 0.49738(9) 0.7868(2) 0.0190(4) Uani 1.00 1 d . . . C(25) C 0.63225(13) 0.46881(9) 0.8822(2) 0.0230(4) Uani 1.00 1 d . . . C(26) C 0.65445(15) 0.46381(11) 1.0389(2) 0.0316(5) Uani 1.00 1 d . . . C(27) C 0.56250(13) 0.44921(9) 0.8347(2) 0.0274(4) Uani 1.00 1 d . . . C(28) C 0.53880(13) 0.08571(9) 0.0577(2) 0.0224(4) Uani 1.00 1 d . . . C(29) C 0.43317(13) 0.07319(9) 0.2437(2) 0.0222(4) Uani 1.00 1 d . . . C(30) C 0.55224(13) 0.30550(9) 0.0740(2) 0.0198(4) Uani 1.00 1 d . . . C(31) C 0.37400(12) 0.05024(9) -0.1732(2) 0.0209(4) Uani 1.00 1 d . . . C(32) C 0.34193(13) -0.01063(9) -0.1938(2) 0.0238(5) Uani 1.00 1 d . . . C(33) C 0.64563(12) 0.68576(10) 0.7133(2) 0.0200(4) Uani 1.00 1 d . . . C(34) C 0.56553(12) 0.71418(9) 0.6971(2) 0.0169(4) Uani 1.00 1 d . . . C(35) C 0.49523(11) 0.68299(9) 0.6789(2) 0.0201(4) Uani 1.00 1 d . . . C(36) C 0.42212(12) 0.71163(9) 0.6720(2) 0.0206(4) Uani 1.00 1 d . . . C(37) C 0.42102(12) 0.77220(9) 0.6797(2) 0.0198(4) Uani 1.00 1 d . . . C(38) C 0.49062(12) 0.80438(9) 0.6952(2) 0.0193(4) Uani 1.00 1 d . . . C(39) C 0.56293(13) 0.77513(9) 0.7051(2) 0.0190(4) Uani 1.00 1 d . . . H(1) H 0.3942 0.2454 0.0161 0.023 Uiso 1.00 1 c R . . H(2) H 0.3174 0.2497 0.1189 0.023 Uiso 1.00 1 c R . . H(3) H 0.2988 0.1474 0.1087 0.027 Uiso 1.00 1 c R . . H(4) H 0.3028 0.1718 -0.0525 0.027 Uiso 1.00 1 c R . . H(4O) H 0.6609 0.5733 0.4241 0.023 Uiso 1.00 1 c R . . H(5) H 0.4336 0.1399 -0.0810 0.022 Uiso 1.00 1 c R . . H(6) H 0.5109 0.1960 0.0921 0.020 Uiso 1.00 1 c R . . H(7) H 0.5942 0.1478 0.2737 0.023 Uiso 1.00 1 c R . . H(8) H 0.5332 0.1753 0.3883 0.023 Uiso 1.00 1 c R . . H(9) H 0.6434 0.2360 0.2090 0.021 Uiso 1.00 1 c R . . H(10) H 0.6241 0.2484 0.3747 0.021 Uiso 1.00 1 c R . . H(11) H 0.4629 0.2661 0.3896 0.019 Uiso 1.00 1 c R . . H(12) H 0.3945 0.3405 0.1788 0.024 Uiso 1.00 1 c R . . H(13) H 0.3630 0.3297 0.3407 0.024 Uiso 1.00 1 c R . . H(14) H 0.5745 0.4518 0.4462 0.021 Uiso 1.00 1 c R . . H(15) H 0.7267 0.4240 0.5469 0.021 Uiso 1.00 1 c R . . H(16) H 0.6179 0.5167 0.6177 0.020 Uiso 1.00 1 c R . . H(17) H 0.7428 0.3788 0.3203 0.026 Uiso 1.00 1 c R . . H(18) H 0.7017 0.3204 0.2603 0.026 Uiso 1.00 1 c R . . H(19) H 0.7216 0.3264 0.4280 0.026 Uiso 1.00 1 c R . . H(20) H 0.3287 0.1647 0.3161 0.025 Uiso 1.00 1 c R . . H(21) H 0.3361 0.2271 0.3931 0.025 Uiso 1.00 1 c R . . H(22) H 0.4009 0.1772 0.4249 0.025 Uiso 1.00 1 c R . . H(23) H 0.8379 0.5276 0.6667 0.024 Uiso 1.00 1 c R . . H(24) H 0.8498 0.5664 0.5250 0.024 Uiso 1.00 1 c R . . H(25) H 0.8248 0.4990 0.5114 0.024 Uiso 1.00 1 c R . . H(26) H 0.7675 0.6246 0.6966 0.022 Uiso 1.00 1 c R . . H(27) H 0.6695 0.5777 0.8931 0.025 Uiso 1.00 1 c R . . H(28) H 0.7639 0.5637 0.8873 0.025 Uiso 1.00 1 c R . . H(29) H 0.7450 0.4743 0.7958 0.023 Uiso 1.00 1 c R . . H(30) H 0.6076 0.4512 1.0942 0.038 Uiso 1.00 1 c R . . H(31) H 0.6727 0.5020 1.0742 0.038 Uiso 1.00 1 c R . . H(32) H 0.6975 0.4350 1.0500 0.038 Uiso 1.00 1 c R . . H(33) H 0.5418 0.4482 0.7383 0.033 Uiso 1.00 1 c R . . H(34) H 0.5194 0.4314 0.8970 0.033 Uiso 1.00 1 c R . . H(35) H 0.5775 0.0756 0.1328 0.027 Uiso 1.00 1 c R . . H(36) H 0.5634 0.1132 -0.0101 0.027 Uiso 1.00 1 c R . . H(37) H 0.5226 0.0502 0.0064 0.027 Uiso 1.00 1 c R . . H(38) H 0.3785 0.0846 0.2700 0.027 Uiso 1.00 1 c R . . H(39) H 0.4678 0.0757 0.3285 0.027 Uiso 1.00 1 c R . . H(40) H 0.4330 0.0329 0.2075 0.027 Uiso 1.00 1 c R . . H(41) H 0.5118 0.3346 0.0472 0.024 Uiso 1.00 1 c R . . H(42) H 0.5444 0.2699 0.0168 0.024 Uiso 1.00 1 c R . . H(43) H 0.6058 0.3214 0.0554 0.024 Uiso 1.00 1 c R . . H(44) H 0.3822 -0.0347 -0.2425 0.029 Uiso 1.00 1 c R . . H(45) H 0.2932 -0.0091 -0.2525 0.029 Uiso 1.00 1 c R . . H(46) H 0.3294 -0.0278 -0.0999 0.029 Uiso 1.00 1 c R . . H(47) H 0.4971 0.6415 0.6711 0.024 Uiso 1.00 1 c R . . H(48) H 0.3737 0.6901 0.6621 0.025 Uiso 1.00 1 c R . . H(49) H 0.4888 0.8459 0.6991 0.023 Uiso 1.00 1 c R . . H(50) H 0.6111 0.7967 0.7175 0.023 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) 0.02033(10) 0.02895(11) 0.03737(14) 0.00622(10) -0.00201(11) -0.00445(12) O(1) 0.0314(8) 0.0176(7) 0.0180(8) -0.0079(6) -0.0004(6) -0.0042(6) O(2) 0.0692(13) 0.0324(9) 0.0217(9) -0.0215(9) 0.0050(9) -0.0033(7) O(3) 0.0192(7) 0.0171(7) 0.0356(9) 0.0001(6) 0.0019(6) -0.0085(6) O(4) 0.0169(7) 0.0194(7) 0.0203(8) 0.0010(6) -0.0017(6) 0.0029(6) O(5) 0.0183(6) 0.0133(6) 0.0288(8) 0.0012(5) -0.0037(7) -0.0042(7) O(6) 0.0220(8) 0.0239(8) 0.0693(13) 0.0016(6) -0.0114(8) -0.0185(8) C(1) 0.0196(10) 0.0166(10) 0.0224(12) -0.0003(8) -0.0044(9) -0.0034(8) C(2) 0.0220(11) 0.0207(10) 0.0241(12) -0.0028(8) -0.0055(9) -0.0042(8) C(3) 0.0249(11) 0.0142(9) 0.0170(11) -0.0038(8) -0.0015(9) -0.0037(8) C(4) 0.0208(10) 0.0138(9) 0.0175(11) -0.0018(8) -0.0003(8) -0.0023(8) C(5) 0.0169(9) 0.0147(9) 0.0173(10) -0.0006(7) 0.0017(8) 0.0022(9) C(6) 0.0207(9) 0.0159(9) 0.0201(11) 0.0004(8) -0.0018(8) 0.0008(9) C(7) 0.0196(10) 0.0157(9) 0.0179(11) -0.0014(8) -0.0003(8) -0.0024(8) C(8) 0.0161(10) 0.0136(9) 0.0180(10) -0.0007(8) -0.0014(8) -0.0001(8) C(9) 0.0171(10) 0.0147(9) 0.0149(10) -0.0022(8) -0.0014(8) -0.0023(8) C(10) 0.0172(10) 0.0146(9) 0.0158(10) -0.0019(8) 0.0002(8) -0.0012(8) C(11) 0.0174(10) 0.0197(10) 0.0238(11) 0.0008(8) -0.0024(8) -0.0037(8) C(12) 0.0200(9) 0.0171(9) 0.0165(10) -0.0010(7) 0.0006(9) 0.0012(9) C(13) 0.0192(10) 0.0138(8) 0.0142(10) 0.0006(7) 0.0006(9) -0.0007(8) C(14) 0.0197(10) 0.0137(9) 0.0171(11) -0.0004(8) 0.0022(8) 0.0032(8) C(15) 0.0174(10) 0.0149(9) 0.0196(11) -0.0008(8) 0.0012(8) 0.0020(8) C(16) 0.0198(9) 0.0131(8) 0.0208(11) 0.0020(8) 0.0011(9) 0.0014(8) C(17) 0.0159(9) 0.0149(9) 0.0203(11) -0.0021(8) -0.0018(8) 0.0006(7) C(18) 0.0184(9) 0.0198(9) 0.0279(12) -0.0029(8) 0.0022(10) -0.0033(10) C(19) 0.0198(9) 0.0213(10) 0.0208(11) -0.0032(8) 0.0030(9) -0.0018(9) C(20) 0.0192(10) 0.0149(9) 0.0151(11) -0.0011(8) -0.0011(8) 0.0017(8) C(21) 0.0188(10) 0.0184(9) 0.0217(11) -0.0014(9) -0.0027(9) 0.0011(8) C(22) 0.0153(10) 0.0140(9) 0.0269(13) -0.0004(7) -0.0044(9) -0.0013(9) C(23) 0.0234(10) 0.0202(10) 0.0197(11) -0.0014(8) -0.0016(10) -0.0018(10) C(24) 0.0206(11) 0.0178(9) 0.0186(11) 0.0017(8) -0.0027(8) 0.0012(8) C(25) 0.0272(11) 0.0182(10) 0.0237(12) -0.0004(9) 0.0039(9) 0.0015(9) C(26) 0.0345(13) 0.0338(13) 0.0264(13) -0.0033(10) -0.0003(10) 0.0073(10) C(27) 0.0297(11) 0.0229(10) 0.0295(12) -0.0041(9) 0.0024(11) 0.0015(11) C(28) 0.0260(11) 0.0146(10) 0.0266(12) 0.0001(9) 0.0033(10) -0.0016(9) C(29) 0.0279(11) 0.0142(9) 0.0245(12) -0.0034(9) 0.0014(9) -0.0001(9) C(30) 0.0266(11) 0.0155(10) 0.0173(11) -0.0034(8) 0.0034(9) -0.0018(8) C(31) 0.0211(9) 0.0198(9) 0.0219(11) 0.0003(8) -0.0025(10) -0.0016(10) C(32) 0.0294(11) 0.0194(10) 0.0227(13) -0.0023(8) -0.0039(9) -0.0037(9) C(33) 0.0220(10) 0.0175(9) 0.0204(10) -0.0031(9) 0.0010(8) -0.0019(9) C(34) 0.0203(10) 0.0173(9) 0.0132(11) 0.0026(8) 0.0001(8) -0.0015(8) C(35) 0.0234(9) 0.0172(9) 0.0197(10) -0.0019(8) 0.0008(9) -0.0016(10) C(36) 0.0199(10) 0.0205(9) 0.0214(11) -0.0043(8) 0.0014(10) -0.0023(10) C(37) 0.0176(9) 0.0231(10) 0.0188(11) 0.0057(8) 0.0008(9) -0.0005(9) C(38) 0.0255(10) 0.0157(10) 0.0168(11) 0.0005(8) -0.0001(8) -0.0026(8) C(39) 0.0201(10) 0.0201(10) 0.0166(11) -0.0030(8) 0.0002(8) -0.0006(8) #============================================================================== _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (R/MSC, Rigaku, 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure (R/MSC, Rigaku, 2005)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' #============================================================================== # 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(37) 1.901(2) yes . . O(1) C(3) 1.465(2) yes . . O(1) C(31) 1.341(2) yes . . O(2) C(31) 1.201(2) yes . . O(3) C(12) 1.231(2) yes . . O(4) C(20) 1.415(2) yes . . O(5) C(22) 1.462(2) yes . . O(5) C(33) 1.343(2) yes . . O(6) C(33) 1.203(2) yes . . C(1) C(2) 1.539(2) yes . . C(1) C(10) 1.534(2) yes . . C(2) C(3) 1.525(2) yes . . C(3) C(4) 1.544(2) yes . . C(4) C(5) 1.555(2) yes . . C(4) C(28) 1.540(2) yes . . C(4) C(29) 1.530(2) yes . . C(5) C(6) 1.534(2) yes . . C(5) C(10) 1.548(2) yes . . C(6) C(7) 1.543(2) yes . . C(7) C(8) 1.551(2) yes . . C(8) C(9) 1.560(2) yes . . C(8) C(13) 1.546(2) yes . . C(8) C(30) 1.554(2) yes . . C(9) C(10) 1.560(2) yes . . C(9) C(11) 1.516(2) yes . . C(10) C(19) 1.550(2) yes . . C(11) C(12) 1.515(2) yes . . C(12) C(13) 1.495(2) yes . . C(13) C(14) 1.357(2) yes . . C(14) C(15) 1.474(2) yes . . C(14) C(18) 1.510(2) yes . . C(15) C(16) 1.332(2) yes . . C(16) C(17) 1.496(2) yes . . C(17) C(20) 1.551(2) yes . . C(17) C(24) 1.542(2) yes . . C(20) C(21) 1.530(2) yes . . C(20) C(22) 1.531(2) yes . . C(22) C(23) 1.534(3) yes . . C(23) C(24) 1.567(2) yes . . C(24) C(25) 1.512(2) yes . . C(25) C(26) 1.508(3) yes . . C(25) C(27) 1.324(3) yes . . C(31) C(32) 1.502(2) yes . . C(33) C(34) 1.494(2) yes . . C(34) C(35) 1.383(2) yes . . C(34) C(39) 1.395(2) yes . . C(35) C(36) 1.386(2) yes . . C(36) C(37) 1.386(2) yes . . C(37) C(38) 1.383(2) yes . . C(38) C(39) 1.383(2) yes . . O(4) H(4O) 0.840 no . . C(1) H(1) 0.990 no . . C(1) H(2) 0.990 no . . C(2) H(3) 0.990 no . . C(2) H(4) 0.990 no . . C(3) H(5) 1.000 no . . C(5) H(6) 1.000 no . . C(6) H(7) 0.990 no . . C(6) H(8) 0.990 no . . C(7) H(9) 0.990 no . . C(7) H(10) 0.990 no . . C(9) H(11) 1.000 no . . C(11) H(12) 0.990 no . . C(11) H(13) 0.990 no . . C(15) H(14) 0.950 no . . C(16) H(15) 0.950 no . . C(17) H(16) 1.000 no . . C(18) H(17) 0.980 no . . C(18) H(18) 0.980 no . . C(18) H(19) 0.980 no . . C(19) H(20) 0.980 no . . C(19) H(21) 0.980 no . . C(19) H(22) 0.980 no . . C(21) H(23) 0.980 no . . C(21) H(24) 0.980 no . . C(21) H(25) 0.980 no . . C(22) H(26) 1.000 no . . C(23) H(27) 0.990 no . . C(23) H(28) 0.990 no . . C(24) H(29) 1.000 no . . C(26) H(30) 0.980 no . . C(26) H(31) 0.980 no . . C(26) H(32) 0.980 no . . C(27) H(33) 0.961 no . . C(27) H(34) 1.010 no . . C(28) H(35) 0.980 no . . C(28) H(36) 0.980 no . . C(28) H(37) 0.980 no . . C(29) H(38) 0.980 no . . C(29) H(39) 0.980 no . . C(29) H(40) 0.980 no . . C(30) H(41) 0.980 no . . C(30) H(42) 0.980 no . . C(30) H(43) 0.980 no . . C(32) H(44) 0.980 no . . C(32) H(45) 0.980 no . . C(32) H(46) 0.980 no . . C(35) H(47) 0.950 no . . C(36) H(48) 0.950 no . . C(38) H(49) 0.950 no . . C(39) H(50) 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(3) O(1) C(31) 118.56(15) yes . . . C(22) O(5) C(33) 115.93(14) yes . . . C(2) C(1) C(10) 110.88(16) yes . . . C(1) C(2) C(3) 111.67(17) yes . . . O(1) C(3) C(2) 108.24(16) yes . . . O(1) C(3) C(4) 107.54(14) yes . . . C(2) C(3) C(4) 116.46(17) yes . . . C(3) C(4) C(5) 105.28(14) yes . . . C(3) C(4) C(28) 106.41(16) yes . . . C(3) C(4) C(29) 112.97(16) yes . . . C(5) C(4) C(28) 108.50(15) yes . . . C(5) C(4) C(29) 115.10(16) yes . . . C(28) C(4) C(29) 108.17(15) yes . . . C(4) C(5) C(6) 116.38(15) yes . . . C(4) C(5) C(10) 116.16(15) yes . . . C(6) C(5) C(10) 110.04(16) yes . . . C(5) C(6) C(7) 110.67(16) yes . . . C(6) C(7) C(8) 113.23(16) yes . . . C(7) C(8) C(9) 107.23(15) yes . . . C(7) C(8) C(13) 117.14(16) yes . . . C(7) C(8) C(30) 111.60(16) yes . . . C(9) C(8) C(13) 100.00(15) yes . . . C(9) C(8) C(30) 114.48(16) yes . . . C(13) C(8) C(30) 106.12(15) yes . . . C(8) C(9) C(10) 119.47(16) yes . . . C(8) C(9) C(11) 104.68(15) yes . . . C(10) C(9) C(11) 119.25(16) yes . . . C(1) C(10) C(5) 107.31(16) yes . . . C(1) C(10) C(9) 115.58(15) yes . . . C(1) C(10) C(19) 108.66(16) yes . . . C(5) C(10) C(9) 105.99(15) yes . . . C(5) C(10) C(19) 115.50(15) yes . . . C(9) C(10) C(19) 104.05(15) yes . . . C(9) C(11) C(12) 101.80(15) yes . . . O(3) C(12) C(11) 123.00(17) yes . . . O(3) C(12) C(13) 127.66(17) yes . . . C(11) C(12) C(13) 109.35(15) yes . . . C(8) C(13) C(12) 106.31(15) yes . . . C(8) C(13) C(14) 128.49(17) yes . . . C(12) C(13) C(14) 125.20(17) yes . . . C(13) C(14) C(15) 121.35(17) yes . . . C(13) C(14) C(18) 122.70(17) yes . . . C(15) C(14) C(18) 115.93(17) yes . . . C(14) C(15) C(16) 125.65(18) yes . . . C(15) C(16) C(17) 123.41(19) yes . . . C(16) C(17) C(20) 114.76(16) yes . . . C(16) C(17) C(24) 116.63(16) yes . . . C(20) C(17) C(24) 102.94(15) yes . . . O(4) C(20) C(17) 113.30(16) yes . . . O(4) C(20) C(21) 106.25(15) yes . . . O(4) C(20) C(22) 114.30(16) yes . . . C(17) C(20) C(21) 113.55(16) yes . . . C(17) C(20) C(22) 102.10(15) yes . . . C(21) C(20) C(22) 107.39(16) yes . . . O(5) C(22) C(20) 108.73(16) yes . . . O(5) C(22) C(23) 109.23(15) yes . . . C(20) C(22) C(23) 105.17(15) yes . . . C(22) C(23) C(24) 106.68(17) yes . . . C(17) C(24) C(23) 103.91(16) yes . . . C(17) C(24) C(25) 116.89(17) yes . . . C(23) C(24) C(25) 112.69(17) yes . . . C(24) C(25) C(26) 115.55(18) yes . . . C(24) C(25) C(27) 123.6(2) yes . . . C(26) C(25) C(27) 120.9(2) yes . . . O(1) C(31) O(2) 123.90(19) yes . . . O(1) C(31) C(32) 111.89(18) yes . . . O(2) C(31) C(32) 124.2(2) yes . . . O(5) C(33) O(6) 123.90(19) yes . . . O(5) C(33) C(34) 112.78(16) yes . . . O(6) C(33) C(34) 123.3(2) yes . . . C(33) C(34) C(35) 123.22(18) yes . . . C(33) C(34) C(39) 117.14(18) yes . . . C(35) C(34) C(39) 119.62(18) yes . . . C(34) C(35) C(36) 120.63(19) yes . . . C(35) C(36) C(37) 118.72(18) yes . . . Br(1) C(37) C(36) 120.57(15) yes . . . Br(1) C(37) C(38) 117.73(15) yes . . . C(36) C(37) C(38) 121.68(18) yes . . . C(37) C(38) C(39) 118.93(19) yes . . . C(34) C(39) C(38) 120.39(19) yes . . . C(20) O(4) H(4O) 109.5 no . . . C(2) C(1) H(1) 109.5 no . . . C(2) C(1) H(2) 109.5 no . . . C(10) C(1) H(1) 109.5 no . . . C(10) C(1) H(2) 109.5 no . . . H(1) C(1) H(2) 108.1 no . . . C(1) C(2) H(3) 109.3 no . . . C(1) C(2) H(4) 109.3 no . . . C(3) C(2) H(3) 109.3 no . . . C(3) C(2) H(4) 109.3 no . . . H(3) C(2) H(4) 108.0 no . . . O(1) C(3) H(5) 108.1 no . . . C(2) C(3) H(5) 108.1 no . . . C(4) C(3) H(5) 108.1 no . . . C(4) C(5) H(6) 104.2 no . . . C(6) C(5) H(6) 104.2 no . . . C(10) C(5) H(6) 104.2 no . . . C(5) C(6) H(7) 109.5 no . . . C(5) C(6) H(8) 109.5 no . . . C(7) C(6) H(7) 109.5 no . . . C(7) C(6) H(8) 109.5 no . . . H(7) C(6) H(8) 108.1 no . . . C(6) C(7) H(9) 108.9 no . . . C(6) C(7) H(10) 108.9 no . . . C(8) C(7) H(9) 108.9 no . . . C(8) C(7) H(10) 108.9 no . . . H(9) C(7) H(10) 107.7 no . . . C(8) C(9) H(11) 103.7 no . . . C(10) C(9) H(11) 103.7 no . . . C(11) C(9) H(11) 103.7 no . . . C(9) C(11) H(12) 111.4 no . . . C(9) C(11) H(13) 111.4 no . . . C(12) C(11) H(12) 111.4 no . . . C(12) C(11) H(13) 111.4 no . . . H(12) C(11) H(13) 109.3 no . . . C(14) C(15) H(14) 117.2 no . . . C(16) C(15) H(14) 117.2 no . . . C(15) C(16) H(15) 118.3 no . . . C(17) C(16) H(15) 118.3 no . . . C(16) C(17) H(16) 107.3 no . . . C(20) C(17) H(16) 107.3 no . . . C(24) C(17) H(16) 107.3 no . . . C(14) C(18) H(17) 109.5 no . . . C(14) C(18) H(18) 109.5 no . . . C(14) C(18) H(19) 109.5 no . . . H(17) C(18) H(18) 109.5 no . . . H(17) C(18) H(19) 109.5 no . . . H(18) C(18) H(19) 109.5 no . . . C(10) C(19) H(20) 109.5 no . . . C(10) C(19) H(21) 109.5 no . . . C(10) C(19) H(22) 109.5 no . . . H(20) C(19) H(21) 109.5 no . . . H(20) C(19) H(22) 109.5 no . . . H(21) C(19) H(22) 109.5 no . . . C(20) C(21) H(23) 109.5 no . . . C(20) C(21) H(24) 109.5 no . . . C(20) C(21) H(25) 109.5 no . . . H(23) C(21) H(24) 109.5 no . . . H(23) C(21) H(25) 109.5 no . . . H(24) C(21) H(25) 109.5 no . . . O(5) C(22) H(26) 111.2 no . . . C(20) C(22) H(26) 111.2 no . . . C(23) C(22) H(26) 111.2 no . . . C(22) C(23) H(27) 110.4 no . . . C(22) C(23) H(28) 110.4 no . . . C(24) C(23) H(27) 110.4 no . . . C(24) C(23) H(28) 110.4 no . . . H(27) C(23) H(28) 108.6 no . . . C(17) C(24) H(29) 107.6 no . . . C(23) C(24) H(29) 107.6 no . . . C(25) C(24) H(29) 107.6 no . . . C(25) C(26) H(30) 109.5 no . . . C(25) C(26) H(31) 109.5 no . . . C(25) C(26) H(32) 109.5 no . . . H(30) C(26) H(31) 109.5 no . . . H(30) C(26) H(32) 109.5 no . . . H(31) C(26) H(32) 109.5 no . . . C(25) C(27) H(33) 129.5 no . . . C(25) C(27) H(34) 124.9 no . . . H(33) C(27) H(34) 105.6 no . . . C(4) C(28) H(35) 109.5 no . . . C(4) C(28) H(36) 109.5 no . . . C(4) C(28) H(37) 109.5 no . . . H(35) C(28) H(36) 109.5 no . . . H(35) C(28) H(37) 109.5 no . . . H(36) C(28) H(37) 109.5 no . . . C(4) C(29) H(38) 109.5 no . . . C(4) C(29) H(39) 109.5 no . . . C(4) C(29) H(40) 109.5 no . . . H(38) C(29) H(39) 109.5 no . . . H(38) C(29) H(40) 109.5 no . . . H(39) C(29) H(40) 109.5 no . . . C(8) C(30) H(41) 109.5 no . . . C(8) C(30) H(42) 109.5 no . . . C(8) C(30) H(43) 109.5 no . . . H(41) C(30) H(42) 109.5 no . . . H(41) C(30) H(43) 109.5 no . . . H(42) C(30) H(43) 109.5 no . . . C(31) C(32) H(44) 109.5 no . . . C(31) C(32) H(45) 109.5 no . . . C(31) C(32) H(46) 109.5 no . . . H(44) C(32) H(45) 109.5 no . . . H(44) C(32) H(46) 109.5 no . . . H(45) C(32) H(46) 109.5 no . . . C(34) C(35) H(47) 119.7 no . . . C(36) C(35) H(47) 119.7 no . . . C(35) C(36) H(48) 120.6 no . . . C(37) C(36) H(48) 120.7 no . . . C(37) C(38) H(49) 120.5 no . . . C(39) C(38) H(49) 120.5 no . . . C(34) C(39) H(50) 119.8 no . . . C(38) C(39) H(50) 119.8 no . . . 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) O(4) 3.3208(13) ? . 2_466 O(2) C(38) 3.231(2) ? . 4_664 O(2) C(39) 3.366(2) ? . 4_664 O(3) O(4) 2.7895(18) ? . 4_665 O(3) O(5) 3.340(2) ? . 4_665 O(3) C(17) 3.542(2) ? . 4_665 O(3) C(20) 3.583(2) ? . 4_665 O(4) C(11) 3.328(2) ? . 4_665 O(4) C(12) 3.415(2) ? . 4_665 O(4) C(32) 3.437(2) ? . 2_555 O(6) C(1) 3.575(2) ? . 4_666 O(6) C(7) 3.389(2) ? . 3_656 C(12) C(35) 3.506(3) ? . 4_665 C(13) C(35) 3.535(2) ? . 4_665 C(13) C(36) 3.595(3) ? . 4_665 C(14) C(36) 3.522(2) ? . 4_665 C(19) C(39) 3.566(2) ? . 4_665 C(21) C(29) 3.574(2) ? . 2_556 C(21) C(32) 3.551(3) ? . 2_555 C(27) C(27) 3.121(2) ? . 4_665 C(27) C(35) 3.486(3) ? . 4_665 C(28) C(32) 3.518(3) ? . 4_655 C(29) C(21) 3.574(2) ? . 2_456 Br(1) H(2) 3.421 ? . 3_556 Br(1) H(8) 3.526 ? . 4_665 Br(1) H(10) 3.174 ? . 4_665 Br(1) H(13) 3.124 ? . 3_556 Br(1) H(21) 3.356 ? . 3_556 Br(1) H(24) 3.284 ? . 2_466 O(1) H(29) 3.202 ? . 2_456 O(1) H(37) 3.240 ? . 4_655 O(1) H(32) 2.894 ? . 2_456 O(2) H(17) 2.800 ? . 2_455 O(2) H(25) 3.147 ? . 2_455 O(2) H(49) 2.539 ? . 4_664 O(2) H(50) 2.810 ? . 4_664 O(3) H(4O) 1.952 ? . 4_665 O(3) H(14) 2.971 ? . 4_665 O(3) H(16) 2.839 ? . 4_665 O(3) H(47) 3.142 ? . 4_665 O(4) H(12) 3.559 ? . 4_665 O(4) H(13) 2.691 ? . 4_665 O(4) H(44) 3.483 ? . 2_555 O(4) H(45) 2.622 ? . 2_555 O(5) H(13) 3.193 ? . 4_665 O(6) H(1) 3.025 ? . 4_666 O(6) H(2) 3.442 ? . 4_666 O(6) H(4) 3.193 ? . 4_666 O(6) H(9) 2.645 ? . 3_656 O(6) H(10) 3.282 ? . 3_656 O(6) H(18) 2.990 ? . 3_656 O(6) H(19) 3.439 ? . 3_656 C(1) H(50) 3.549 ? . 4_664 C(2) H(18) 3.552 ? . 2_455 C(2) H(50) 3.218 ? . 4_664 C(2) H(32) 3.339 ? . 2_456 C(3) H(49) 3.423 ? . 4_664 C(3) H(50) 3.229 ? . 4_664 C(6) H(24) 3.489 ? . 3_646 C(6) H(26) 3.214 ? . 3_646 C(7) H(26) 3.440 ? . 3_646 C(11) H(4O) 2.839 ? . 4_665 C(12) H(4O) 2.659 ? . 4_665 C(12) H(47) 3.196 ? . 4_665 C(13) H(47) 3.402 ? . 4_665 C(13) H(48) 3.536 ? . 4_665 C(13) H(30) 3.249 ? . 1_554 C(14) H(47) 3.479 ? . 4_665 C(14) H(48) 3.107 ? . 4_665 C(14) H(30) 3.104 ? . 1_554 C(14) H(32) 3.497 ? . 1_554 C(15) H(47) 3.247 ? . 4_665 C(15) H(48) 3.330 ? . 4_665 C(15) H(30) 3.387 ? . 1_554 C(16) H(45) 3.571 ? . 2_555 C(16) H(48) 3.448 ? . 4_665 C(18) H(4) 3.183 ? . 2_555 C(18) H(48) 3.364 ? . 4_665 C(18) H(50) 3.339 ? . 3_646 C(18) H(32) 3.372 ? . 1_554 C(19) H(19) 3.203 ? . 2_456 C(19) H(50) 3.433 ? . 4_665 C(20) H(45) 3.314 ? . 2_555 C(21) H(7) 3.308 ? . 3_656 C(21) H(35) 3.404 ? . 3_656 C(21) H(38) 3.268 ? . 2_556 C(21) H(40) 3.219 ? . 2_556 C(21) H(44) 3.215 ? . 2_555 C(21) H(45) 3.029 ? . 2_555 C(22) H(7) 3.315 ? . 3_656 C(23) H(35) 3.523 ? . 3_656 C(23) H(46) 3.251 ? . 2_556 C(25) H(34) 3.410 ? . 4_665 C(26) H(17) 3.578 ? . 1_556 C(26) H(43) 3.358 ? . 1_556 C(26) H(45) 3.222 ? . 2_556 C(26) H(46) 3.316 ? . 2_556 C(27) H(33) 3.054 ? . 4_665 C(27) H(34) 3.106 ? . 4_665 C(27) H(41) 3.388 ? . 1_556 C(27) H(47) 2.757 ? . 4_665 C(28) H(23) 3.546 ? . 3_646 C(28) H(28) 3.372 ? . 3_646 C(28) H(37) 3.304 ? . 4_655 C(28) H(40) 3.083 ? . 4_655 C(28) H(44) 3.300 ? . 4_655 C(28) H(46) 2.956 ? . 4_655 C(29) H(23) 2.920 ? . 2_456 C(29) H(25) 3.343 ? . 2_456 C(29) H(29) 3.345 ? . 2_456 C(29) H(35) 3.556 ? . 4_655 C(29) H(40) 3.314 ? . 4_655 C(30) H(34) 3.359 ? . 1_554 C(30) H(30) 3.459 ? . 1_554 C(31) H(17) 3.049 ? . 2_455 C(31) H(25) 3.440 ? . 2_455 C(31) H(37) 3.321 ? . 4_655 C(31) H(49) 3.505 ? . 4_664 C(31) H(32) 3.179 ? . 2_456 C(32) H(24) 3.335 ? . 2_455 C(32) H(25) 2.980 ? . 2_455 C(32) H(28) 3.360 ? . 2_456 C(32) H(36) 3.303 ? . 4_655 C(32) H(37) 3.065 ? . 4_655 C(32) H(31) 3.043 ? . 2_456 C(32) H(32) 3.253 ? . 2_456 C(33) H(1) 3.293 ? . 4_666 C(33) H(13) 3.486 ? . 4_665 C(33) H(21) 3.595 ? . 4_665 C(34) H(1) 3.179 ? . 4_666 C(34) H(11) 2.934 ? . 4_665 C(34) H(21) 3.534 ? . 4_665 C(34) H(22) 3.589 ? . 4_665 C(34) H(42) 3.513 ? . 4_666 C(35) H(11) 3.013 ? . 4_665 C(35) H(33) 3.110 ? . 4_665 C(35) H(34) 3.317 ? . 4_665 C(35) H(41) 3.451 ? . 4_666 C(35) H(42) 3.387 ? . 4_666 C(36) H(10) 3.013 ? . 4_665 C(36) H(11) 3.292 ? . 4_665 C(36) H(19) 3.415 ? . 4_665 C(36) H(42) 3.283 ? . 4_666 C(37) H(8) 3.060 ? . 4_665 C(37) H(10) 2.973 ? . 4_665 C(37) H(11) 3.435 ? . 4_665 C(37) H(42) 3.330 ? . 4_666 C(38) H(5) 2.747 ? . 4_666 C(38) H(8) 2.919 ? . 4_665 C(38) H(11) 3.358 ? . 4_665 C(38) H(22) 3.127 ? . 4_665 C(38) H(36) 3.445 ? . 4_666 C(38) H(42) 3.488 ? . 4_666 C(39) H(1) 3.016 ? . 4_666 C(39) H(4) 3.403 ? . 4_666 C(39) H(5) 2.779 ? . 4_666 C(39) H(8) 3.541 ? . 4_665 C(39) H(11) 3.113 ? . 4_665 C(39) H(21) 3.357 ? . 4_665 C(39) H(22) 2.888 ? . 4_665 C(39) H(42) 3.560 ? . 4_666 H(1) H(50) 2.940 ? . 4_664 H(3) H(29) 3.055 ? . 2_456 H(3) H(32) 2.930 ? . 2_456 H(4) H(17) 2.922 ? . 2_455 H(4) H(18) 2.572 ? . 2_455 H(4) H(43) 3.292 ? . 2_455 H(4) H(50) 2.676 ? . 4_664 H(4) H(32) 3.007 ? . 2_456 H(4O) H(12) 3.153 ? . 4_665 H(4O) H(13) 2.383 ? . 4_665 H(4O) H(45) 3.095 ? . 2_555 H(5) H(49) 2.443 ? . 4_664 H(5) H(50) 2.483 ? . 4_664 H(7) H(23) 3.022 ? . 3_646 H(7) H(24) 2.800 ? . 3_646 H(7) H(26) 2.385 ? . 3_646 H(7) H(28) 3.399 ? . 3_646 H(8) H(24) 3.265 ? . 3_646 H(8) H(49) 2.953 ? . 4_665 H(9) H(26) 3.075 ? . 3_646 H(10) H(26) 3.421 ? . 3_646 H(10) H(48) 3.020 ? . 4_665 H(11) H(47) 3.428 ? . 4_665 H(11) H(50) 3.590 ? . 4_665 H(12) H(27) 3.419 ? . 4_664 H(14) H(14) 3.321 ? . 4_665 H(14) H(47) 3.218 ? . 4_665 H(14) H(30) 3.320 ? . 1_554 H(15) H(20) 2.937 ? . 2_556 H(15) H(38) 3.060 ? . 2_556 H(15) H(45) 3.537 ? . 2_555 H(15) H(48) 3.280 ? . 4_665 H(16) H(33) 3.002 ? . 4_665 H(17) H(45) 3.157 ? . 2_555 H(17) H(50) 3.097 ? . 3_646 H(17) H(30) 3.501 ? . 1_554 H(17) H(32) 2.923 ? . 1_554 H(18) H(50) 3.179 ? . 3_646 H(18) H(32) 3.269 ? . 1_554 H(19) H(20) 2.983 ? . 2_556 H(19) H(21) 2.814 ? . 2_556 H(19) H(22) 3.292 ? . 2_556 H(19) H(48) 2.724 ? . 4_665 H(19) H(50) 3.176 ? . 3_646 H(20) H(48) 3.434 ? . 3_546 H(21) H(50) 3.190 ? . 4_665 H(22) H(49) 3.189 ? . 4_665 H(22) H(50) 2.793 ? . 4_665 H(23) H(35) 2.583 ? . 3_656 H(23) H(38) 2.717 ? . 2_556 H(23) H(39) 3.206 ? . 2_556 H(23) H(39) 3.425 ? . 3_656 H(23) H(40) 2.408 ? . 2_556 H(24) H(35) 3.413 ? . 3_656 H(24) H(39) 3.343 ? . 3_656 H(24) H(44) 2.778 ? . 2_555 H(24) H(45) 3.005 ? . 2_555 H(25) H(38) 2.930 ? . 2_556 H(25) H(39) 3.291 ? . 2_556 H(25) H(40) 3.260 ? . 2_556 H(25) H(44) 2.801 ? . 2_555 H(25) H(45) 2.476 ? . 2_555 H(26) H(35) 3.235 ? . 3_656 H(27) H(34) 3.162 ? . 4_665 H(27) H(46) 3.482 ? . 2_556 H(28) C(28) 3.372 ? . 3_656 H(28) H(35) 2.669 ? . 3_656 H(28) H(36) 3.302 ? . 3_656 H(28) H(46) 2.404 ? . 2_556 H(29) H(38) 2.676 ? . 2_556 H(29) H(40) 3.144 ? . 2_556 H(29) H(46) 3.388 ? . 2_556 H(30) H(41) 3.137 ? . 1_556 H(30) H(43) 2.988 ? . 1_556 H(31) H(45) 2.612 ? . 2_556 H(31) H(46) 2.693 ? . 2_556 H(32) H(43) 3.016 ? . 1_556 H(32) H(45) 2.993 ? . 2_556 H(32) H(46) 3.091 ? . 2_556 H(33) H(33) 2.748 ? . 4_665 H(33) H(34) 3.285 ? . 4_665 H(33) H(47) 2.240 ? . 4_665 H(33) H(48) 3.533 ? . 4_665 H(34) H(34) 3.201 ? . 4_665 H(34) H(41) 2.619 ? . 1_556 H(34) H(43) 3.252 ? . 1_556 H(34) H(47) 2.696 ? . 4_665 H(35) H(37) 3.526 ? . 4_655 H(35) H(40) 2.580 ? . 4_655 H(35) H(46) 2.880 ? . 4_655 H(36) H(44) 2.951 ? . 4_655 H(36) H(46) 2.776 ? . 4_655 H(36) H(49) 2.991 ? . 4_664 H(37) H(37) 2.413 ? . 4_655 H(37) H(40) 2.765 ? . 4_655 H(37) H(44) 2.829 ? . 4_655 H(37) H(46) 2.709 ? . 4_655 H(39) H(40) 3.188 ? . 4_655 H(40) H(40) 2.695 ? . 4_655 H(41) H(47) 3.543 ? . 4_664 H(44) H(49) 3.301 ? . 1_544 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O(4) H(4O) O(3) . . 4_665 2.7895(18) 0.840 1.952 175.2 no #===END========================================================================