#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003272.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_2003272 loop_ _publ_author_name 'Guidetti-Grept, R.' 'Herzog, B.' 'Debrunner, B.' 'Siljegovic, V.' 'Keese, R.' 'Frey, H.-M.' 'Hauser, A.' 'K\"onig, O.' 'L\"uthi, S.' 'Birrer, J.' 'Nyffeler, D.' 'F\"ortsch, M.' 'B\"urgi, H.-B.' _publ_section_title ; A [5.5.5.5]Fenestrane Derivative ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 495 _journal_page_last 497 _journal_paper_doi 10.1107/S0108270194009455 _journal_volume 51 _journal_year 1995 _chemical_compound_source Synthesis _chemical_formula_sum 'C17 H22 O5' _chemical_formula_weight 306.36 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 108.33(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.274(4) _cell_length_b 7.746(2) _cell_length_c 15.080(5) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293 _cell_measurement_theta_max 19.5 _cell_measurement_theta_min 11 _cell_volume 1471.9(8) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2921 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.3 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.10 _exptl_absorpt_correction_T_max 0.9998 _exptl_absorpt_correction_T_min 0.9913 _exptl_absorpt_correction_type empirical _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.37 _exptl_crystal_description Plates _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.2026 _refine_diff_density_min -0.2277 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.534 _refine_ls_hydrogen_treatment refU _refine_ls_number_parameters 205 _refine_ls_number_reflns 1696 _refine_ls_R_factor_obs 0.040 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w=1/[\s^2^(F) + 0.000727F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.055 _reflns_number_observed 1696 _reflns_number_total 2245 _reflns_observed_criterion I>3.0\s(I) _cod_data_source_file ka1087.cif _cod_data_source_block ka1087a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w=1/[\s^2^(F) + 0.000727F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(F) + 0.000727F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1472.0(10) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2003272 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv C(1) .2326(2) .3864(3) .4150(2) 2.81(4) C(2) .3514(2) .4053(3) .4629(2) 3.03(4) C(3) .4037(2) .2441(3) .4389(2) 3.22(4) C(4) .3199(2) .0981(3) .4151(2) 2.72(4) C(5) .3143(2) .0043(4) .3235(2) 4.03(5) C(6) .1968(2) -.0248(3) .2743(2) 4.12(5) C(7) .1446(2) .1411(3) .2930(2) 3.51(4) C(8) .0306(2) .1159(3) .2919(2) 4.33(5) C(9) .0411(2) .0381(3) .3859(2) 4.01(5) C(10) .1327(2) .1395(3) .4534(2) 3.05(4) C(11) .0956(2) .3094(3) .4833(2) 4.03(5) C(12) .1805(2) .4394(3) .4882(2) 3.57(5) C(13) .2080(2) .1918(3) .3944(2) 2.58(4) C(14) .3346(2) -.0309(3) .4930(2) 3.04(5) C(15) .3907(3) -.0662(4) .6598(2) 5.63(7) C(16) .3029(3) -.0438(5) .6966(2) 7.01(9) C(17) .3618(2) .4184(3) .5647(2) 3.57(5) O(1) .4419(2) .4248(3) .6292(1) 5.48(4) O(2) .3071(2) -.1800(2) .4812(1) 4.76(4) O(3) .2656(1) .4228(2) .5769(1) 4.25(4) O(4) .3777(1) .0382(2) .5764(1) 4.14(3) O(5) .1409(2) .6058(2) .4823(2) 5.20(5) H .193(2) .675(4) .478(2) 4.5(1) H(1) .2078(2) .4549(3) .3571(2) 4.5(1) H(2) .3854(2) .5057(3) .4441(2) 4.5(1) H(31) .4280(2) .2673(3) .3847(2) 4.5(1) H(32) .4647(2) .2101(3) .4927(2) 4.5(1) H(51) .3523(2) -.1067(4) .3369(2) 4.5(1) H(52) .3455(2) .0763(4) .2850(2) 4.5(1) H(61) .1830(2) -.0418(3) .2068(2) 4.5(1) H(62) .1708(2) -.1256(3) .3005(2) 4.5(1) H(7) .1444(2) .2262(3) .2445(2) 4.5(1) H(81) -.0076(2) .0370(3) .2412(2) 4.5(1) H(82) -.0070(2) .2273(3) .2841(2) 4.5(1) H(91) -.0248(2) .0533(3) .4019(2) 4.5(1) H(92) .0585(2) -.0856(3) .3870(2) 4.5(1) H(10) .1657(2) .0684(3) .5091(2) 4.5(1) H(111) .0857(2) .2964(3) .5451(2) 4.5(1) H(112) .0282(2) .3460(3) .4374(2) 4.5(1) H(151) .4569(3) -.0316(4) .7080(2) 11.0(6) H(152) .3952(3) -.1887(4) .6439(2) 11.0(6) H(161) .3149(3) -.1161(5) .7527(2) 11.0(6) H(162) .2363(3) -.0789(5) .6491(2) 11.0(6) H(163) .2979(3) .0782(5) .7132(2) 11.0(6) 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 O(3) C(12) O(5) 108.1(2) yes O(3) C(12) C(1) 104.0(2) yes O(3) C(12) C(11) 109.9(2) yes O(5) C(12) C(1) 116.8(2) yes O(5) C(12) C(11) 111.0(2) yes C(1) C(12) C(11) 106.8(2) yes C(1) C(13) C(4) 106.2(2) yes C(1) C(13) C(7) 117.3(2) yes C(1) C(13) C(10) 105.4(2) yes C(4) C(13) C(7) 105.2(2) yes C(4) C(13) C(10) 119.1(2) yes C(7) C(13) C(10) 104.2(2) yes C(5) C(6) C(7) 103.9(2) no C(6) C(7) C(13) 105.0(2) no C(8) C(7) C(13) 106.0(2) no C(7) C(8) C(9) 104.1(2) no C(8) C(9) C(10) 103.8(2) no C(9) C(10) C(11) 112.1(2) no C(9) C(10) C(13) 105.5(2) no C(11) C(10) C(13) 105.4(2) no C(10) C(11) C(12) 106.6(2) no O(2) C(14) O(4) 123.3(2) no O(2) C(14) C(4) 124.0(2) no O(4) C(14) C(4) 112.6(2) no O(4) C(15) C(16) 111.8(3) no O(1) C(17) O(3) 121.8(3) no O(1) C(17) C(2) 127.4(3) no O(3) C(17) C(2) 110.8(2) no C(1) C(2) C(3) 106.8(2) no C(1) C(2) C(17) 103.9(2) no C(3) C(2) C(17) 113.3(2) no C(2) C(3) C(4) 107.8(2) no C(3) C(4) C(5) 112.4(2) no C(3) C(4) C(13) 105.7(2) no C(3) C(4) C(14) 113.3(2) no C(5) C(4) C(13) 105.1(2) no C(5) C(4) C(14) 110.1(2) no C(13) C(4) C(14) 109.8(2) no C(4) C(5) C(6) 105.1(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O(3) C(12) 1.460(3) yes O(5) C(12) 1.384(3) yes C(1) C(13) 1.553(3) yes C(4) C(13) 1.593(3) yes C(7) C(13) 1.546(3) yes C(10) C(13) 1.585(4) yes O(1) C(17) 1.197(3) no O(2) C(14) 1.207(3) no O(3) C(17) 1.345(4) no O(4) C(14) 1.321(3) no O(4) C(15) 1.459(4) no C(1) C(2) 1.521(3) no C(1) C(12) 1.531(4) no C(2) C(3) 1.526(4) no C(2) C(17) 1.500(4) no C(3) C(4) 1.547(3) no C(4) C(5) 1.541(4) no C(4) C(14) 1.507(3) no C(5) C(6) 1.519(3) no C(6) C(7) 1.528(4) no C(7) C(8) 1.520(4) no C(8) C(9) 1.507(4) no C(9) C(10) 1.533(3) no C(10) C(11) 1.523(4) no C(11) C(12) 1.496(4) no C(15) C(16) 1.451(6) 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 O(3) C(12) O(5) H 66.5(18) yes C(2) C(1) C(13) C(4) -10.1(3) no C(1) C(13) C(4) C(3) -4.5(2) no C(13) C(4) C(3) C(2) 17.5(2) no C(4) C(3) C(2) C(1) -24.2(3) no C(3) C(2) C(1) C(13) 21.2(3) no C(8) C(7) C(13) C(10) 16.2(2) no C(7) C(13) C(10) C(9) 8.7(2) no C(13) C(10) C(9) C(8) -30.5(2) no C(10) C(9) C(8) C(7) 41.0(3) no C(9) C(8) C(7) C(13) -35.8(2) no C(11) C(10) C(13) C(1) 14.1(2) no C(10) C(13) C(1) C(12) 4.0(2) no C(13) C(1) C(12) C(11) -21.2(2) no C(1) C(12) C(11) C(10) 30.6(2) no C(12) C(11) C(10) C(13) -27.5(2) no C(5) C(4) C(13) C(7) 1.6(2) no C(4) C(13) C(7) C(6) 22.0(2) no C(13) C(7) C(6) C(5) -37.9(3) no C(7) C(6) C(5) C(4) 39.0(3) no C(6) C(5) C(4) C(13) -24.8(3) no C(12) C(1) C(2) C(17) 15.2(2) no C(1) C(2) C(17) O(3) -4.8(2) no C(2) C(17) O(3) C(12) -8.5(3) no C(17) O(3) C(12) C(1) 17.9(2) no O(3) C(12) C(1) C(2) -19.8(2) no C(13) C(4) C(14) O(4) -88.0(2) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139054191