#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2101548.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_2101548 loop_ _publ_author_name 'Briozzo, P.' 'Kondo, T.' 'Sada, K.' 'Miyata, M.' 'Miki, K.' _publ_section_title ; Structures of three inclusion compounds of cholanamide with either (S)-enantiomer, (R)-enantiomer or an optically resolved mixture of butan-2-ol ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 728 _journal_page_last 733 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'C24 H41 N1 O4, C4 H10 O1' _chemical_formula_sum 'C28 H51 N O5' _[local]_cod_chemical_formula_sum_orig 'C28 H51 N1 O5' _chemical_formula_weight 481.71 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2y1' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.0 _cell_angle_beta 104.820(10) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 13.2510(10) _cell_length_b 7.8690(10) _cell_length_c 14.0450(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 29.3 _cell_measurement_theta_min 22.5 _cell_volume 1415.9(3) _diffrn_measurement_device 'Rigaku AFC-5R' _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 2888 _diffrn_reflns_theta_max 25.25 _diffrn_standards_decay_% 0.1 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.0708 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_type 'azimuthal scan' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_meas 1.10 _exptl_crystal_description prism _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.16 _refine_diff_density_min -0.22 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.06 _refine_ls_hydrogen_treatment ;H atoms of 2-butanol were not refined, positions of other H atoms were refined ; _refine_ls_number_parameters 438 _refine_ls_number_reflns 1473 _refine_ls_R_factor_obs 0.051 _refine_ls_shift/esd_max '0.07 for host, 1.03 for guest' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 4|F|^2^/\s^2^(F)' _refine_ls_wR_factor_obs 0.058 _reflns_number_observed 1473 _reflns_number_total 2766 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file as0702.cif loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy C1 1.1637(7) .860(2) .8944(6) 1.0 C2 1.1186(7) .829(2) .9815(6) 1.0 C3 1.1482(8) .655(2) 1.0257(6) 1.0 C4 1.1116(8) .522(2) .9484(5) 1.0 C5 1.1541(6) .545(2) .8572(6) 1.0 C6 1.1162(6) .401(2) .7831(6) 1.0 C7 1.0034(6) .418(2) .7247(6) 1.0 C8 .9812(6) .5950(10) .6781(5) 1.0 C9 1.0148(6) .740(2) .7540(6) 1.0 C10 1.1328(6) .7260(10) .8105(5) 1.0 C11 .9845(6) .9120(10) .7042(6) 1.0 C12 .8691(6) .930(2) .6496(5) 1.0 C13 0.8366(5) .7870(10) .5724(5) 1.0 C14 .8658(6) .617(2) .6267(6) 1.0 C15 .8145(7) .483(2) .5520(6) 1.0 C16 .7124(7) .565(2) .4963(7) 1.0 C17 .7181(6) .757(2) .5264(6) 1.0 C18 .8926(7) .811(2) .4916(6) 1.0 C19 1.2029(6) .753(2) .7389(6) 1.0 C20 .6582(6) .871(2) .4407(6) 1.0 C21 .6690(10) 1.062(2) .4621(8) 1.0 C22 .5424(7) .815(2) .4117(7) 1.0 C23 .4832(7) .867(2) .3098(7) 1.0 C24 .3719(8) .798(2) .2834(7) 1.0 O25 1.0990(7) .630 1.1052(5) 1.0 O26 .8087(6) .9290(10) .7205(5) 1.0 O27 .3544(6) .651(2) .3009(6) 1.0 N28 .2995(6) .900(2) .2411(6) 1.0 O29 .9312(5) .3950(10) .7832(4) 1.0 C1G .494(3) 1.350(3) .193(3) 1.0 C2G .393(2) 1.322(2) .128(3) 1.0 C3G .379(3) 1.200(3) .043(2) 1.0 C4GS .422(4) 1.262(4) -.037(3) 0.61 C4GR .517(5) 1.500(5) .153(7) 0.39 O5G .339(2) 1.247(2) .1900(10) 1.0 H1A 1.144 1.000 .871 1.0 H1B 1.229 .861 .912 1.0 H2A 1.141 .923 1.030 1.0 H2B 1.040 .840 .963 1.0 H3 1.217 .656 1.056 1.0 H4A 1.131 .410 .975 1.0 H4B 1.028 .536 .930 1.0 H5 1.229 .525 .883 1.0 H6A 1.158 .382 .736 1.0 H6B 1.125 .284 .825 1.0 H7 .986 .319 .669 1.0 H8 1.020 .607 .631 1.0 H9 .976 .727 .801 1.0 H11A .997 .986 .744 1.0 H11B 1.036 .951 .646 1.0 H12 .860 1.045 .615 1.0 H14 .830 .611 .674 1.0 H15A .856 .457 .507 1.0 H15B .809 .380 .584 1.0 H16A .696 .551 .415 1.0 H16B .651 .506 .509 1.0 H17 .691 .762 .572 1.0 H18A .966 .806 .519 1.0 H18B .872 .723 .444 1.0 H18C .875 .918 .461 1.0 H19A 1.274 .739 .774 1.0 H19B 1.185 .673 .687 1.0 H19C 1.192 .865 .712 1.0 H20 .691 .850 .393 1.0 H21A .740 1.092 .480 1.0 H21B .634 1.123 .405 1.0 H21C .638 1.088 .515 1.0 H22A .547 .695 .421 1.0 H22B .506 .848 .459 1.0 H23A .481 .988 .306 1.0 H23B .519 .825 .264 1.0 H25 1.124 .561 1.136 1.0 H26 .769 .992 .710 1.0 H28A .224 .908 .232 1.0 H28B .314 1.033 .221 1.0 H29 .942 .307 .814 1.0 H1GA .491 1.364 .259 1.0 H1GB .542 1.262 .189 1.0 H2G .362 1.428 .105 1.0 H3GA .413 1.096 .067 1.0 H3GB .306 1.180 .018 1.0 H4GSA .494 1.282 -.012 1.0 H4GSB .411 1.179 -.088 1.0 H4GSC .388 1.365 -.062 1.0 H4GRA .584 1.538 .188 1.0 H4GRB .517 1.482 .086 1.0 H4GRC .466 1.583 .156 1.0 H5G .288 1.309 .221 1.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.512(12) no C1 C10 1.556(12) no C2 C3 1.513(13) no C3 C4 1.497(12) no C3 O25 1.443(11) no C4 C5 1.536(11) no C5 C6 1.534(12) no C5 C10 1.563(12) no C6 C7 1.516(11) no C7 C8 1.535(12) no C7 O29 1.423(9) no C8 C9 1.547(10) no C8 C14 1.525(10) no C9 C10 1.566(10) no C9 C11 1.529(11) no C10 C19 1.548(11) no C11 C12 1.532(11) no C12 C13 1.545(11) no C12 O26 1.428(10) no C13 C14 1.539(11) no C13 C17 1.556(10) no C13 C18 1.518(11) no C14 C15 1.520(11) no C15 C16 1.522(12) no C16 C17 1.565(13) no C17 C20 1.548(11) no C20 C21 1.532(15) no C20 C22 1.548(12) no C22 C23 1.502(12) no C23 C24 1.526(13) no C24 O27 1.217(15) no C24 N28 1.275(16) no C1G C2G 1.43(5) no C1G C4GR 1.38(6) no C2G C3G 1.51(4) no C2G O5G 1.39(4) no C3G C4GS 1.47(5) 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 C2 C1 C10 114.9(8) no C1 C2 C3 111.3(8) no C2 C3 C4 109.5(7) no C2 C3 O25 108.7(8) no C4 C3 O25 109.8(8) no C3 C4 C5 113.7(8) no C4 C5 C6 110.6(8) no C4 C5 C10 113.1(7) no C6 C5 C10 113.3(7) no C5 C6 C7 114.1(8) no C6 C7 C8 111.5(8) no C6 C7 O29 113.1(6) no C8 C7 O29 106.1(7) no C7 C8 C9 112.7(6) no C7 C8 C14 111.4(7) no C9 C8 C14 108.6(6) no C8 C9 C10 111.8(7) no C8 C9 C11 110.0(6) no C10 C9 C11 113.9(6) no C1 C10 C5 108.4(6) no C1 C10 C9 111.8(6) no C1 C10 C19 108.3(7) no C5 C10 C9 109.1(7) no C5 C10 C19 108.9(7) no C9 C10 C19 110.4(6) no C9 C11 C12 115.0(7) no C11 C12 C13 110.3(7) no C11 C12 O26 108.4(6) no C13 C12 O26 112.3(6) no C12 C13 C14 107.2(5) no C12 C13 C17 118.2(7) no C12 C13 C18 109.4(7) no C14 C13 C17 100.0(6) no C14 C13 C18 111.7(7) no C17 C13 C18 110.1(6) no C8 C14 C13 115.3(7) no C8 C14 C15 117.7(7) no C13 C14 C15 104.5(6) no C14 C15 C16 104.0(7) no C15 C16 C17 107.2(7) no C13 C17 C16 103.4(7) no C13 C17 C20 119.8(7) no C16 C17 C20 111.7(7) no C17 C20 C21 114.4(8) no C17 C20 C22 108.4(8) no C21 C20 C22 111.6(9) no C20 C22 C23 114.5(8) no C22 C23 C24 111.8(9) no C23 C24 O27 120.8(13) no C23 C24 N28 117.0(13) no O27 C24 N28 122.2(11) no C2G C1G C4GR 98(6) no C1G C2G C3G 121(4) no C1G C2G O5G 102(4) no C3G C2G O5G 104(3) no C2G C3G C4GS 114(5) no