#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008382.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2008382 loop_ _publ_author_name 'Novoa de Armas, H.' 'Blaton, N. M.' 'Peeters, O. M.' 'De Ranter, C. J.' 'Pom\'es Hern\'andez, R.' 'Arteagas, M. A. I.' 'Gil, R. P.' 'Manchado, F. C.' _publ_section_title ; (25R)-6\b-Acetoxy-3\b-bromo-5\a-spirostan-23-one ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 601 _journal_page_last 603 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C29 H43 Br O5' _chemical_formula_sum 'C29 H43 Br O5' _chemical_formula_weight 551.54 _chemical_name_systematic (25R)-3beta-bromo-6beta-acetoxy-5alfa-spirostan-23-one _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.2654(12) _cell_length_b 10.6629(14) _cell_length_c 27.703(4) _cell_measurement_reflns_used 46 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 55.80 _cell_measurement_theta_min 6.45 _cell_volume 2736.9(6) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1996)' _computing_data_reduction XSCANS _computing_molecular_graphics 'DIAMOND (Bergerhoff, 1996)' _computing_publication_material ; PLATON (Spek, 1990), PARST (Nardelli, 1983, 1995) and PARSTCIF (Nardelli, 1991) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Siemens P4 four-circle' _diffrn_measurement_method 2\q/\w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 3629 _diffrn_reflns_reduction_process ; ; _diffrn_reflns_theta_full 69.17 _diffrn_reflns_theta_max 69.17 _diffrn_reflns_theta_min 3.19 _diffrn_standards_decay_% <1.0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.332 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1168.0 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.457 _refine_diff_density_min -0.756 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_extinction_coef 0.0030(3) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997a)' _refine_ls_goodness_of_fit_all 1.097 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 3410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.081 _refine_ls_R_factor_gt 0.061 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0633P)^2^+5.3297P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo^2^)+(0.0633P)^2^+5.3297P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.171 _refine_ls_wR_factor_ref 0.142 _reflns_number_gt 2651 _reflns_number_total 3410 _reflns_threshold_expression F>2\s(F) _[local]_cod_data_source_file na1383.cif _[local]_cod_data_source_block na1383 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_matrix_type' value 'Full' changed to 'full' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 2737.0(6) _cod_database_code 2008382 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 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 0.0805(6) 0.0922(6) 0.0719(5) -0.0044(6) 0.0283(5) -0.0049(4) O1 0.062(3) 0.066(3) 0.042(2) 0.004(3) -0.007(2) 0.000(2) O2 0.109(5) 0.100(4) 0.051(3) 0.017(4) -0.010(3) -0.008(3) O3 0.050(3) 0.072(3) 0.0399(19) -0.001(2) -0.0070(19) 0.000(2) O4 0.050(3) 0.051(3) 0.058(2) 0.004(2) 0.001(2) 0.011(2) O5 0.079(4) 0.049(3) 0.098(4) 0.007(3) 0.005(4) -0.001(2) C1 0.043(4) 0.064(4) 0.052(3) 0.004(3) -0.007(3) -0.004(3) C2 0.055(4) 0.081(5) 0.066(4) 0.002(4) -0.006(4) -0.002(4) C3 0.053(4) 0.065(4) 0.070(4) 0.004(4) 0.011(4) 0.006(4) C4 0.059(4) 0.063(4) 0.049(3) 0.000(4) 0.006(3) -0.003(3) C5 0.056(4) 0.054(4) 0.045(3) 0.001(4) 0.000(3) 0.003(3) C6 0.050(4) 0.060(4) 0.046(3) 0.002(4) -0.002(3) -0.001(3) C7 0.056(4) 0.066(4) 0.043(3) -0.009(4) 0.000(3) -0.003(3) C8 0.047(4) 0.052(4) 0.042(3) 0.000(3) 0.001(3) 0.002(3) C9 0.047(4) 0.054(4) 0.043(3) 0.001(3) -0.002(3) 0.000(3) C10 0.039(3) 0.049(3) 0.042(3) 0.002(3) -0.001(3) -0.001(3) C11 0.052(4) 0.078(5) 0.049(3) -0.007(4) 0.004(3) -0.010(4) C12 0.054(4) 0.074(5) 0.038(3) -0.007(4) -0.005(3) -0.004(3) C13 0.045(4) 0.045(3) 0.045(3) -0.004(3) -0.006(3) 0.002(3) C14 0.044(4) 0.058(4) 0.040(3) -0.008(3) -0.005(3) -0.003(3) C15 0.054(4) 0.074(4) 0.045(3) -0.018(4) -0.002(3) -0.006(3) C16 0.049(4) 0.063(4) 0.041(3) -0.007(4) 0.002(3) -0.002(3) C17 0.048(4) 0.057(4) 0.034(3) -0.005(3) 0.002(3) 0.002(3) C18 0.075(5) 0.049(4) 0.051(3) 0.000(4) 0.007(4) 0.003(3) C19 0.057(4) 0.050(3) 0.052(3) -0.002(3) 0.003(3) 0.005(3) C20 0.049(4) 0.058(4) 0.045(3) 0.000(3) 0.002(3) 0.001(3) C21 0.060(4) 0.089(6) 0.045(3) -0.006(4) 0.007(3) -0.008(4) C22 0.055(4) 0.052(4) 0.044(3) 0.000(3) -0.001(3) 0.005(3) C23 0.054(4) 0.056(4) 0.057(3) 0.005(4) -0.006(3) 0.003(3) C24 0.054(4) 0.066(5) 0.085(5) 0.006(4) 0.003(4) -0.007(4) C25 0.050(4) 0.071(5) 0.059(4) -0.002(4) -0.002(3) -0.008(4) C26 0.050(4) 0.063(4) 0.061(4) -0.005(4) 0.008(3) 0.001(4) C27 0.055(5) 0.098(6) 0.076(5) -0.017(5) 0.010(4) -0.008(5) C28 0.061(5) 0.082(5) 0.042(3) 0.002(4) -0.007(3) 0.003(4) C29 0.097(7) 0.094(6) 0.056(4) 0.006(6) -0.010(5) 0.013(4) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Br 1.50646(11) 0.42482(9) -0.00871(3) 0.0815(3) Uani 1.000 O1 0.9246(5) 0.5164(5) 0.05147(15) 0.0567(16) Uani 1.000 O2 0.9254(8) 0.4301(6) -0.02254(18) 0.087(2) Uani 1.000 O3 0.5448(5) 0.4708(5) 0.28343(14) 0.0540(15) Uani 1.000 O4 0.5796(5) 0.3826(4) 0.35989(17) 0.0530(16) Uani 1.000 O5 0.5010(8) 0.6977(4) 0.3573(2) 0.075(2) Uani 1.000 C1 1.3442(7) 0.4862(7) 0.1328(2) 0.053(2) Uani 1.000 C2 1.4383(9) 0.4953(8) 0.0873(3) 0.067(3) Uani 1.000 C3 1.3879(8) 0.4045(8) 0.0499(3) 0.063(2) Uani 1.000 C4 1.2301(8) 0.4181(8) 0.0373(2) 0.057(2) Uani 1.000 C5 1.1401(7) 0.4103(7) 0.0834(2) 0.052(2) Uani 1.000 C6 0.9782(7) 0.4010(7) 0.0738(2) 0.052(2) Uani 1.000 C7 0.8939(8) 0.3806(7) 0.1198(2) 0.055(2) Uani 1.000 C8 0.9293(7) 0.4749(7) 0.1595(2) 0.047(2) Uani 1.000 C9 1.0955(7) 0.4791(7) 0.1686(2) 0.048(2) Uani 1.000 C10 1.1825(7) 0.5083(6) 0.1222(2) 0.0433(17) Uani 1.000 C11 1.1322(8) 0.5628(8) 0.2114(2) 0.060(2) Uani 1.000 C12 1.0504(8) 0.5307(8) 0.2571(2) 0.055(2) Uani 1.000 C13 0.8884(8) 0.5289(6) 0.2490(2) 0.0450(19) Uani 1.000 C14 0.8544(7) 0.4414(7) 0.2065(2) 0.047(2) Uani 1.000 C15 0.6889(7) 0.4261(8) 0.2095(2) 0.058(2) Uani 1.000 C16 0.6689(7) 0.4078(7) 0.2632(2) 0.051(2) Uani 1.000 C17 0.8020(7) 0.4648(6) 0.2895(2) 0.046(2) Uani 1.000 C18 0.8351(10) 0.6616(6) 0.2395(3) 0.058(2) Uani 1.000 C19 1.1599(8) 0.6428(6) 0.1058(2) 0.0530(19) Uani 1.000 C20 0.7364(7) 0.5403(7) 0.3311(2) 0.051(2) Uani 1.000 C21 0.8188(8) 0.5351(8) 0.3778(2) 0.065(3) Uani 1.000 C22 0.5825(8) 0.4968(7) 0.3321(2) 0.050(2) Uani 1.000 C23 0.4705(8) 0.5869(7) 0.3517(2) 0.056(2) Uani 1.000 C24 0.3245(9) 0.5339(8) 0.3641(3) 0.068(3) Uani 1.000 C25 0.3346(8) 0.4071(7) 0.3888(3) 0.060(3) Uani 1.000 C26 0.4381(8) 0.3265(7) 0.3618(3) 0.058(2) Uani 1.000 C27 0.1853(9) 0.3441(9) 0.3921(3) 0.076(3) Uani 1.000 C28 0.9025(9) 0.5169(8) 0.0035(2) 0.062(3) Uani 1.000 C29 0.8510(11) 0.6405(9) -0.0128(3) 0.082(3) Uani 1.000 H1A 1.37690 0.54780 0.15610 0.0690 Uiso 1.000 H1B 1.35610 0.40380 0.14710 0.0690 Uiso 1.000 H2A 1.43360 0.57980 0.07440 0.0870 Uiso 1.000 H2B 1.53790 0.47750 0.09550 0.0870 Uiso 1.000 H3 1.40330 0.31950 0.06230 0.0810 Uiso 1.000 H4A 1.20160 0.35200 0.01530 0.0740 Uiso 1.000 H4B 1.21380 0.49810 0.02160 0.0740 Uiso 1.000 H5 1.16590 0.32930 0.09770 0.0670 Uiso 1.000 H6 0.96020 0.33050 0.05190 0.0680 Uiso 1.000 H7A 0.91350 0.29680 0.13170 0.0710 Uiso 1.000 H7B 0.79160 0.38570 0.11260 0.0710 Uiso 1.000 H8 0.89690 0.55830 0.14930 0.0610 Uiso 1.000 H9 1.12320 0.39400 0.17820 0.0620 Uiso 1.000 H11A 1.23480 0.55670 0.21780 0.0770 Uiso 1.000 H11B 1.11150 0.64920 0.20280 0.0770 Uiso 1.000 H12A 1.07340 0.59190 0.28180 0.0720 Uiso 1.000 H12B 1.08140 0.44900 0.26860 0.0720 Uiso 1.000 H14 0.89400 0.35970 0.21570 0.0610 Uiso 1.000 H15A 0.63910 0.50040 0.19810 0.0750 Uiso 1.000 H15B 0.65600 0.35370 0.19140 0.0750 Uiso 1.000 H16 0.66290 0.31800 0.27040 0.0660 Uiso 1.000 H17 0.86010 0.39640 0.30300 0.0600 Uiso 1.000 H18A 0.86040 0.71450 0.26630 0.0760 Uiso 1.000 H18B 0.73210 0.66080 0.23570 0.0760 Uiso 1.000 H18C 0.87920 0.69320 0.21060 0.0760 Uiso 1.000 H19A 1.21270 0.69830 0.12660 0.0690 Uiso 1.000 H19B 1.05900 0.66290 0.10720 0.0690 Uiso 1.000 H19C 1.19380 0.65220 0.07330 0.0690 Uiso 1.000 H20 0.73520 0.62830 0.32090 0.0660 Uiso 1.000 H21A 0.76590 0.57890 0.40240 0.0840 Uiso 1.000 H21B 0.91140 0.57400 0.37350 0.0840 Uiso 1.000 H21C 0.83180 0.44930 0.38720 0.0840 Uiso 1.000 H24A 0.26820 0.52530 0.33470 0.0890 Uiso 1.000 H24B 0.27430 0.59210 0.38510 0.0890 Uiso 1.000 H25 0.37160 0.41950 0.42160 0.0780 Uiso 1.000 H26A 0.44440 0.24520 0.37730 0.0750 Uiso 1.000 H26B 0.40270 0.31380 0.32920 0.0750 Uiso 1.000 H27A 0.14810 0.33090 0.36010 0.0990 Uiso 1.000 H27B 0.12060 0.39720 0.40980 0.0990 Uiso 1.000 H27C 0.19430 0.26490 0.40830 0.0990 Uiso 1.000 H29A 0.84340 0.64080 -0.04740 0.1070 Uiso 1.000 H29B 0.91790 0.70410 -0.00280 0.1070 Uiso 1.000 H29C 0.75800 0.65710 0.00100 0.1070 Uiso 1.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -1 2 2 4 -1 2 8 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 C6 O1 C28 118.2(6) yes C16 O3 C22 105.3(5) yes C22 O4 C26 112.8(5) yes C2 C1 C10 112.6(5) no C1 C2 C3 110.6(7) no Br C3 C2 109.0(5) yes Br C3 C4 109.8(5) yes C2 C3 C4 113.6(7) no C3 C4 C5 109.3(5) no C4 C5 C6 113.2(5) no C4 C5 C10 113.9(6) no C6 C5 C10 114.4(5) no O1 C6 C5 110.6(6) yes O1 C6 C7 107.6(5) yes C5 C6 C7 111.7(5) no C6 C7 C8 113.7(6) no C7 C8 C9 110.3(5) no C7 C8 C14 111.4(6) no C9 C8 C14 108.6(5) no C8 C9 C10 112.7(5) no C8 C9 C11 111.3(5) no C10 C9 C11 114.3(6) no C1 C10 C5 106.0(5) no C1 C10 C9 108.4(5) no C1 C10 C19 109.5(6) no C5 C10 C9 107.9(5) no C5 C10 C19 113.2(5) no C9 C10 C19 111.5(5) no C9 C11 C12 114.0(6) no C11 C12 C13 112.0(5) no C12 C13 C14 108.9(5) no C12 C13 C17 114.4(5) no C12 C13 C18 109.6(6) no C14 C13 C17 100.5(5) no C14 C13 C18 111.5(6) no C17 C13 C18 111.7(6) no C8 C14 C13 114.9(6) no C8 C14 C15 121.7(5) no C13 C14 C15 103.1(5) no C14 C15 C16 100.9(5) no O3 C16 C15 114.8(5) yes O3 C16 C17 105.5(5) yes C15 C16 C17 108.3(5) no C13 C17 C16 104.2(5) no C13 C17 C20 121.4(5) no C16 C17 C20 104.1(5) no C17 C20 C21 115.3(6) no C17 C20 C22 103.2(5) no C21 C20 C22 117.1(5) no O3 C22 O4 109.7(6) yes O3 C22 C20 106.1(5) yes O3 C22 C23 107.2(5) yes O4 C22 C20 106.8(5) yes O4 C22 C23 109.4(5) yes C20 C22 C23 117.5(6) no O5 C23 C22 119.9(7) yes O5 C23 C24 122.7(7) yes C22 C23 C24 117.3(6) no C23 C24 C25 112.4(7) no C24 C25 C26 109.1(7) no C24 C25 C27 111.1(7) no C26 C25 C27 110.9(6) no O4 C26 C25 111.4(6) yes O1 C28 O2 124.6(7) yes O1 C28 C29 110.9(7) yes O2 C28 C29 124.5(6) yes C2 C1 H1A 109.04 no C2 C1 H1B 109.14 no C10 C1 H1A 109.04 no C10 C1 H1B 109.03 no H1A C1 H1B 107.83 no C1 C2 H2A 109.60 no C1 C2 H2B 109.62 no C3 C2 H2A 109.42 no C3 C2 H2B 109.48 no H2A C2 H2B 108.12 no Br C3 H3 108.01 no C2 C3 H3 108.12 no C4 C3 H3 108.11 no C3 C4 H4A 109.85 no C3 C4 H4B 109.82 no C5 C4 H4A 109.73 no C5 C4 H4B 109.75 no H4A C4 H4B 108.40 no C4 C5 H5 104.65 no C6 C5 H5 104.65 no C10 C5 H5 104.60 no O1 C6 H6 108.98 no C5 C6 H6 108.95 no C7 C6 H6 108.89 no C6 C7 H7A 108.83 no C6 C7 H7B 108.89 no C8 C7 H7A 108.78 no C8 C7 H7B 108.74 no H7A C7 H7B 107.73 no C7 C8 H8 108.92 no C9 C8 H8 108.82 no C14 C8 H8 108.71 no C8 C9 H9 106.00 no C10 C9 H9 105.97 no C11 C9 H9 105.84 no C9 C11 H11A 108.80 no C9 C11 H11B 108.73 no C12 C11 H11A 108.83 no C12 C11 H11B 108.71 no H11A C11 H11B 107.60 no C11 C12 H12A 109.14 no C11 C12 H12B 109.20 no C13 C12 H12A 109.29 no C13 C12 H12B 109.25 no H12A C12 H12B 107.90 no C8 C14 H14 105.15 no C13 C14 H14 105.32 no C15 C14 H14 105.31 no C14 C15 H15A 111.63 no C14 C15 H15B 111.62 no C16 C15 H15A 111.57 no C16 C15 H15B 111.56 no H15A C15 H15B 109.42 no O3 C16 H16 109.29 no C15 C16 H16 109.48 no C17 C16 H16 109.36 no C13 C17 H17 108.84 no C16 C17 H17 108.85 no C20 C17 H17 108.77 no C13 C18 H18A 109.44 no C13 C18 H18B 109.47 no C13 C18 H18C 109.42 no H18A C18 H18B 109.40 no H18A C18 H18C 109.53 no H18B C18 H18C 109.56 no C10 C19 H19A 109.41 no C10 C19 H19B 109.45 no C10 C19 H19C 109.54 no H19A C19 H19B 109.54 no H19A C19 H19C 109.41 no H19B C19 H19C 109.49 no C17 C20 H20 106.91 no C21 C20 H20 106.81 no C22 C20 H20 106.90 no C20 C21 H21A 109.48 no C20 C21 H21B 109.33 no C20 C21 H21C 109.44 no H21A C21 H21B 109.50 no H21A C21 H21C 109.59 no H21B C21 H21C 109.49 no C23 C24 H24A 109.06 no C23 C24 H24B 109.13 no C25 C24 H24A 109.08 no C25 C24 H24B 109.22 no H24A C24 H24B 107.81 no C24 C25 H25 108.62 no C26 C25 H25 108.56 no C27 C25 H25 108.54 no O4 C26 H26A 109.42 no O4 C26 H26B 109.33 no C25 C26 H26A 109.42 no C25 C26 H26B 109.29 no H26A C26 H26B 107.93 no C25 C27 H27A 109.33 no C25 C27 H27B 109.52 no C25 C27 H27C 109.47 no H27A C27 H27B 109.49 no H27A C27 H27C 109.47 no H27B C27 H27C 109.54 no C28 C29 H29A 109.42 no C28 C29 H29B 109.55 no C28 C29 H29C 109.51 no H29A C29 H29B 109.44 no H29A C29 H29C 109.33 no H29B C29 H29C 109.56 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Br C3 1.972(8) yes O1 C6 1.464(9) yes O1 C28 1.345(7) yes O2 C28 1.192(10) yes O3 C16 1.445(8) yes O3 C22 1.420(7) yes O4 C22 1.441(8) yes O4 C26 1.442(9) yes O5 C23 1.225(9) yes C1 C2 1.536(10) no C1 C10 1.545(9) no C2 C3 1.493(12) no C3 C4 1.510(10) no C4 C5 1.528(8) no C5 C6 1.527(9) no C5 C10 1.550(9) no C6 C7 1.510(8) no C7 C8 1.526(9) no C8 C9 1.561(9) no C8 C14 1.518(8) no C9 C10 1.549(8) no C9 C11 1.523(9) no C10 C19 1.519(9) no C11 C12 1.515(9) no C12 C13 1.518(10) no C13 C14 1.535(9) no C13 C17 1.538(9) no C13 C18 1.522(9) no C14 C15 1.544(9) no C15 C16 1.512(8) no C16 C17 1.556(9) no C17 C20 1.532(9) no C20 C21 1.503(8) no C20 C22 1.500(10) no C22 C23 1.515(10) no C23 C24 1.506(11) no C24 C25 1.518(11) no C25 C26 1.489(11) no C25 C27 1.541(11) no C28 C29 1.473(13) no C1 H1A 0.9695 no C1 H1B 0.9701 no C2 H2A 0.9703 no C2 H2B 0.9691 no C3 H3 0.9797 no C4 H4A 0.9685 no C4 H4B 0.9694 no C5 H5 0.9798 no C6 H6 0.9803 no C7 H7A 0.9696 no C7 H7B 0.9701 no C8 H8 0.9802 no C9 H9 0.9798 no C11 H11A 0.9692 no C11 H11B 0.9707 no C12 H12A 0.9693 no C12 H12B 0.9710 no C14 H14 0.9790 no C15 H15A 0.9697 no C15 H15B 0.9697 no C16 H16 0.9797 no C17 H17 0.9806 no C18 H18A 0.9614 no C18 H18B 0.9602 no C18 H18C 0.9599 no C19 H19A 0.9600 no C19 H19B 0.9599 no C19 H19C 0.9588 no C20 H20 0.9800 no C21 H21A 0.9606 no C21 H21B 0.9604 no C21 H21C 0.9588 no C24 H24A 0.9715 no C24 H24B 0.9695 no C25 H25 0.9801 no C26 H26A 0.9692 no C26 H26B 0.9703 no C27 H27A 0.9615 no C27 H27B 0.9594 no C27 H27C 0.9600 no C29 H29A 0.9611 no C29 H29B 0.9596 no C29 H29C 0.9592 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br C21 3.562(6) 2_764 no Br H21A 3.2426 2_764 no Br H27B 3.1755 2_664 no Br H6 3.0045 4_555 no O1 C19 2.972(8) . no O2 C4 3.276(10) . no O3 O5 3.195(7) . no O5 O3 3.195(7) . no O5 C1 3.405(9) 3_755 no O1 H8 2.7587 . no O1 H19B 2.5248 . no O1 H4B 2.8112 . no O2 H4A 2.8882 . no O2 H6 2.3419 . no O2 H21A 2.7340 2_664 no O2 H25 2.9162 2_664 no O2 H3 2.8877 4_455 no O3 H26B 2.4787 . no O4 H29A 2.6772 2_665 no O4 H16 2.6863 . no O4 H21C 2.5571 . no O4 H19A 2.7759 3_745 no O5 H20 2.5046 . no O5 H1B 2.5686 3_755 no O5 H3 2.7265 3_755 no O5 H15B 2.5890 3_655 no C1 O5 3.405(9) 3_745 no C4 C28 3.347(11) . no C4 O2 3.276(10) . no C16 C26 3.576(10) . no C19 O1 2.972(8) . no C21 Br 3.562(6) 2_765 no C26 C16 3.576(10) . no C28 C4 3.347(11) . no C1 H11A 2.6716 . no C2 H5 3.0961 . no C2 H19C 2.8428 . no C2 H26A 3.0403 3_755 no C4 H19C 2.7090 . no C6 H19B 3.0357 . no C7 H15B 2.9792 . no C8 H19B 2.7499 . no C8 H18C 2.7636 . no C11 H1A 2.7410 . no C11 H18C 2.7256 . no C11 H19A 2.8570 . no C11 H14 3.0944 . no C12 H24A 2.9491 1_655 no C15 H7B 2.8805 . no C15 H18B 2.6363 . no C16 H18B 2.8637 . no C18 H20 2.4633 . no C18 H15A 2.7510 . no C18 H11B 2.7586 . no C18 H8 2.7902 . no C19 H2A 2.7639 . no C19 H4B 2.8410 . no C19 H11B 2.7252 . no C19 H8 2.8639 . no C20 H18B 2.9389 . no C20 H18A 2.8272 . no C23 H21A 3.0775 . no C23 H26B 3.0435 . no C27 H19B 2.9761 3_645 no C28 H4B 2.9344 . no H1A C11 2.7410 . no H1A H11A 2.1597 . no H1A H19A 2.3575 . no H1B H3 2.5530 . no H1B H5 2.3684 . no H1B H9 2.3259 . no H1B O5 2.5686 3_745 no H2A C19 2.7639 . no H2A H19C 2.3523 . no H2A H26A 2.4857 3_755 no H2B H7B 2.5900 1_655 no H3 H1B 2.5530 . no H3 H5 2.4106 . no H3 O5 2.7265 3_745 no H3 O2 2.8877 4_555 no H4A O2 2.8882 . no H4A H6 2.4664 . no H4B O1 2.8112 . no H4B C19 2.8410 . no H4B C28 2.9344 . no H4B H19C 2.1876 . no H5 C2 3.0961 . no H5 H1B 2.3684 . no H5 H3 2.4106 . no H5 H7A 2.5448 . no H5 H9 2.3677 . no H6 O2 2.3419 . no H6 H4A 2.4664 . no H6 Br 3.0045 4_455 no H7A H5 2.5448 . no H7A H9 2.5512 . no H7A H14 2.4285 . no H7B C15 2.8805 . no H7B H2B 2.5900 1_455 no H7B H15B 2.5417 . no H8 O1 2.7587 . no H8 C18 2.7902 . no H8 C19 2.8639 . no H8 H18C 2.2316 . no H8 H19B 2.2045 . no H9 H1B 2.3259 . no H9 H5 2.3677 . no H9 H7A 2.5512 . no H9 H14 2.3922 . no H9 H18A 2.4598 3_745 no H11A C1 2.6716 . no H11A H1A 2.1597 . no H11B C18 2.7586 . no H11B C19 2.7252 . no H11B H18C 2.2135 . no H11B H19A 2.3684 . no H12A H18A 2.4059 . no H12A H24A 2.4310 1_655 no H12B H14 2.4636 . no H12B H17 2.3296 . no H14 C11 3.0944 . no H14 H7A 2.4285 . no H14 H9 2.3922 . no H14 H12B 2.4636 . no H14 H17 2.4700 . no H15A C18 2.7510 . no H15A H18B 2.1801 . no H15B C7 2.9792 . no H15B H7B 2.5417 . no H15B O5 2.5890 3_645 no H16 O4 2.6863 . no H17 H12B 2.3296 . no H17 H14 2.4700 . no H17 H21C 2.4141 . no H18A C20 2.8272 . no H18A H12A 2.4059 . no H18A H20 2.1162 . no H18A H9 2.4598 3_755 no H18B C15 2.6363 . no H18B C16 2.8637 . no H18B C20 2.9389 . no H18B H15A 2.1801 . no H18B H20 2.3858 . no H18C C8 2.7636 . no H18C C11 2.7256 . no H18C H8 2.2316 . no H18C H11B 2.2135 . no H18C H27A 2.4609 3_655 no H19A C11 2.8570 . no H19A H1A 2.3575 . no H19A H11B 2.3684 . no H19A O4 2.7759 3_755 no H19B O1 2.5248 . no H19B C6 3.0357 . no H19B C8 2.7499 . no H19B H8 2.2045 . no H19B C27 2.9761 3_655 no H19C C2 2.8428 . no H19C C4 2.7090 . no H19C H2A 2.3523 . no H19C H4B 2.1876 . no H20 O5 2.5046 . no H20 C18 2.4633 . no H20 H18A 2.1162 . no H20 H18B 2.3858 . no H21A C23 3.0775 . no H21A Br 3.2426 2_765 no H21A O2 2.7340 2_665 no H21C O4 2.5571 . no H21C H17 2.4141 . no H24A C12 2.9491 1_455 no H24A H12A 2.4310 1_455 no H24A H26B 2.5811 . no H24A H27A 2.4556 . no H25 O2 2.9162 2_665 no H26A H27C 2.4802 . no H26A C2 3.0403 3_745 no H26A H2A 2.4857 3_745 no H26B O3 2.4787 . no H26B C23 3.0435 . no H26B H24A 2.5811 . no H26B H27A 2.5161 . no H27A H24A 2.4556 . no H27A H26B 2.5161 . no H27A H18C 2.4609 3_645 no H27B Br 3.1755 2_665 no H27C H26A 2.4802 . no H29A O4 2.6772 2_664 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C1 H1B O5 3_745 0.97 2.57 3.405(9) 145 yes C6 H6 O2 . 0.98 2.34 2.731(8) 103 yes C15 H15B O5 3_645 0.97 2.59 3.529(9) 163 yes C19 H19B O1 . 0.96 2.53 2.972(8) 108 yes C20 H20 O5 . 0.98 2.50 2.846(9) 100 yes C26 H26B O3 . 0.97 2.48 2.839(9) 102 yes 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 C28 O1 C6 C5 100.8(7) no C28 O1 C6 C7 -136.8(6) no C6 O1 C28 O2 -1.1(11) no C6 O1 C28 C29 -179.1(6) no C22 O3 C16 C15 -151.3(6) no C22 O3 C16 C17 -32.2(6) no C16 O3 C22 O4 -73.4(6) no C16 O3 C22 C20 41.6(7) no C16 O3 C22 C23 167.9(6) no C26 O4 C22 O3 -62.5(7) no C26 O4 C22 C20 -177.1(5) no C26 O4 C22 C23 54.8(7) no C22 O4 C26 C25 -66.1(8) no C10 C1 C2 C3 -56.9(8) no C2 C1 C10 C5 56.6(7) no C2 C1 C10 C9 172.3(6) no C2 C1 C10 C19 -65.9(7) no C1 C2 C3 C4 54.8(9) no C1 C2 C3 Br 177.6(5) no Br C3 C4 C5 -176.5(5) no C2 C3 C4 C5 -54.1(9) no C3 C4 C5 C6 -170.3(6) no C3 C4 C5 C10 56.6(8) no C10 C5 C6 O1 67.0(6) no C4 C5 C10 C9 -173.4(6) no C10 C5 C6 C7 -52.9(8) no C4 C5 C10 C1 -57.4(7) no C6 C5 C10 C9 54.1(7) no C6 C5 C10 C19 -69.8(7) no C4 C5 C10 C19 62.7(8) no C6 C5 C10 C1 170.1(5) no C4 C5 C6 O1 -65.8(7) no C4 C5 C6 C7 174.4(6) no C5 C6 C7 C8 51.6(8) no O1 C6 C7 C8 -70.0(7) no C6 C7 C8 C9 -52.9(7) no C6 C7 C8 C14 -173.6(6) no C7 C8 C14 C13 177.9(6) no C7 C8 C14 C15 -56.6(9) no C14 C8 C9 C11 -52.0(8) no C9 C8 C14 C15 -178.3(6) no C7 C8 C9 C11 -174.4(6) no C9 C8 C14 C13 56.2(8) no C7 C8 C9 C10 55.7(7) no C14 C8 C9 C10 178.1(6) no C8 C9 C10 C1 -169.6(6) no C11 C9 C10 C19 -58.7(7) no C8 C9 C11 C12 53.0(8) no C10 C9 C11 C12 -178.0(6) no C8 C9 C10 C5 -55.3(7) no C8 C9 C10 C19 69.7(7) no C11 C9 C10 C1 62.0(7) no C11 C9 C10 C5 176.4(6) no C9 C11 C12 C13 -54.2(9) no C11 C12 C13 C18 -68.7(8) no C11 C12 C13 C14 53.5(8) no C11 C12 C13 C17 165.0(6) no C12 C13 C14 C15 168.2(5) no C17 C13 C14 C8 -177.7(5) no C17 C13 C14 C15 47.7(6) no C12 C13 C14 C8 -57.2(7) no C14 C13 C17 C16 -32.5(6) no C14 C13 C17 C20 -149.1(6) no C18 C13 C17 C16 85.8(7) no C18 C13 C14 C8 63.8(8) no C18 C13 C14 C15 -70.8(7) no C12 C13 C17 C16 -149.0(6) no C12 C13 C17 C20 94.4(7) no C18 C13 C17 C20 -30.8(8) no C13 C14 C15 C16 -43.5(7) no C8 C14 C15 C16 -174.2(7) no C14 C15 C16 O3 140.0(6) no C14 C15 C16 C17 22.4(7) no O3 C16 C17 C20 11.1(6) no C15 C16 C17 C13 6.3(7) no C15 C16 C17 C20 134.5(6) no O3 C16 C17 C13 -117.1(5) no C13 C17 C20 C21 -101.8(7) no C13 C17 C20 C22 129.3(6) no C16 C17 C20 C21 141.6(6) no C16 C17 C20 C22 12.7(6) no C17 C20 C22 O4 83.8(5) no C17 C20 C22 C23 -153.0(5) no C17 C20 C22 O3 -33.2(7) no C21 C20 C22 C23 79.2(8) no C21 C20 C22 O3 -161.0(6) no C21 C20 C22 O4 -44.0(8) no O3 C22 C23 C24 75.4(7) no O4 C22 C23 O5 135.8(6) no O4 C22 C23 C24 -43.5(7) no C20 C22 C23 O5 13.9(8) no O3 C22 C23 O5 -105.3(7) no C20 C22 C23 C24 -165.4(6) no O5 C23 C24 C25 -138.4(7) no C22 C23 C24 C25 40.9(8) no C23 C24 C25 C27 -169.0(6) no C23 C24 C25 C26 -46.5(9) no C24 C25 C26 O4 59.3(8) no C27 C25 C26 O4 -178.0(6) no