#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100652.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100652 _publ_requested_journal 'X-ray Structure Analysis Online' _publ_section_title ; Structure of 7-\a-hydroxycholesterol ; loop_ _publ_author_name ' Fujii, Isao ' ' Hirayama, Noriaki ' _publ_section_abstract ; An X-ray analysis of 7-ƒ¿-hydroxycholesterol was undertaken in order to determine the inherent conformation and to understand the structure-f unction relationships. The bond distances and angles are within the expected ranges, except for those of the terminal part of the isoprenoid chain moiety. The A, B, C and D rings in the steroid skeleton take chair, half-chair, chair and envelope conformations, respectively. All rings of the steroid skele are trans connected. The isoprenoid chain moiety has an extended conformation. ; _chemical_formula_sum 'C28 H50 O3' _[local]_cod_chemical_formula_sum_orig 'C28 H50 O3 ' _chemical_formula_weight 434.70 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 14.5558(5) _cell_length_b 30.2416(6) _cell_length_c 6.2872(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2767.6(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 16.0 _cell_measurement_temperature 296.2 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.043 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type none _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type ? _diffrn_reflns_number 2759 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 65.00 _diffrn_measured_fraction_theta_max 0.2869 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.2869 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 0 _reflns_number_total 902 _reflns_number_gt 1254 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1447 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2725 _refine_ls_number_parameters 281 _refine_ls_goodness_of_fit_ref 1.546 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03600(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.35 _refine_diff_density_min -0.28 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.015(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 6.1.1.1) ; 'O' 'O' 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(3) O 0.4609(3) 0.2340(1) 0.8198(7) 0.126(2) Uani 1.00 d . . . O(7) O 0.0651(2) 0.3071(1) 0.4651(6) 0.076(1) Uani 1.00 d . . . O(100) O 0.5665(4) 0.2388(2) 0.1688(8) 0.145(2) Uani 1.00 d . . . C(1) C 0.3306(4) 0.3409(2) 0.8603(9) 0.082(2) Uani 1.00 d . . . C(2) C 0.4111(4) 0.3089(2) 0.895(1) 0.097(2) Uani 1.00 d . . . C(3) C 0.3887(4) 0.2649(2) 0.799(1) 0.086(2) Uani 1.00 d . . . C(4) C 0.3698(4) 0.2709(2) 0.563(1) 0.087(2) Uani 1.00 d . . . C(5) C 0.2931(4) 0.3035(2) 0.5205(9) 0.061(2) Uani 1.00 d . . . C(6) C 0.2237(4) 0.2935(2) 0.3995(9) 0.070(2) Uani 1.00 d . . . C(7) C 0.1436(4) 0.3226(2) 0.3479(9) 0.068(2) Uani 1.00 d . . . C(8) C 0.1652(4) 0.3699(2) 0.4012(9) 0.062(2) Uani 1.00 d . . . C(9) C 0.2120(3) 0.3743(2) 0.6179(8) 0.060(2) Uani 1.00 d . . . C(10) C 0.3029(4) 0.3486(2) 0.6249(9) 0.065(2) Uani 1.00 d . . . C(11) C 0.2215(4) 0.4223(2) 0.6917(9) 0.075(2) Uani 1.00 d . . . C(12) C 0.1338(4) 0.4499(2) 0.6700(9) 0.079(2) Uani 1.00 d . . . C(13) C 0.0939(4) 0.4479(2) 0.4443(9) 0.067(2) Uani 1.00 d . . . C(14) C 0.0802(4) 0.3989(2) 0.3899(8) 0.067(2) Uani 1.00 d . . . C(15) C 0.0212(4) 0.3992(2) 0.1924(10) 0.079(2) Uani 1.00 d . . . C(16) C -0.0375(4) 0.4414(2) 0.214(1) 0.096(2) Uani 1.00 d . . . C(17) C -0.0032(4) 0.4665(2) 0.4115(10) 0.077(2) Uani 1.00 d . . . C(18) C 0.1599(4) 0.4704(2) 0.283(1) 0.094(2) Uani 1.00 d . . . C(19) C 0.3808(4) 0.3739(2) 0.509(1) 0.093(2) Uani 1.00 d . . . C(20) C -0.0199(5) 0.5161(2) 0.396(1) 0.095(3) Uani 1.00 d . . . C(21) C 0.0195(5) 0.5416(2) 0.589(1) 0.137(3) Uani 1.00 d . . . C(22) C -0.1197(5) 0.5268(2) 0.372(1) 0.122(3) Uani 1.00 d . . . C(23) C -0.1417(6) 0.5741(2) 0.301(2) 0.152(4) Uani 1.00 d . . . C(24) C -0.2331(6) 0.5858(3) 0.278(2) 0.175(4) Uani 1.00 d . . . C(25) C -0.2581(7) 0.6327(4) 0.216(3) 0.203(6) Uani 1.00 d . . . C(26) C -0.241(1) 0.6383(5) -0.010(3) 0.324(9) Uani 1.00 d . . . C(27) C -0.3381(9) 0.6458(4) 0.267(3) 0.314(8) Uani 1.00 d . . . C(100) C 0.6195(6) 0.2756(3) 0.192(2) 0.193(5) Uani 1.00 d . . . H(1) H 0.279 0.329 0.933 0.098 Uiso 1.00 calc . . . H(2) H 0.347 0.369 0.922 0.098 Uiso 1.00 calc . . . H(3) H 0.422 0.306 1.042 0.114 Uiso 1.00 calc . . . H(4) H 0.464 0.321 0.828 0.114 Uiso 1.00 calc . . . H(5) H 0.336 0.253 0.867 0.106 Uiso 1.00 calc . . . H(6) H 0.498 0.242 0.941 0.101 Uiso 1.00 calc . . . H(7) H 0.353 0.243 0.507 0.099 Uiso 1.00 calc . . . H(8) H 0.424 0.281 0.496 0.099 Uiso 1.00 calc . . . H(9) H 0.223 0.265 0.337 0.083 Uiso 1.00 calc . . . H(10) H 0.016 0.290 0.382 0.101 Uiso 1.00 calc . . . H(11) H 0.131 0.320 0.200 0.082 Uiso 1.00 calc . . . H(12) H 0.207 0.381 0.296 0.075 Uiso 1.00 calc . . . H(13) H 0.172 0.360 0.717 0.073 Uiso 1.00 calc . . . H(14) H 0.268 0.436 0.612 0.092 Uiso 1.00 calc . . . H(15) H 0.238 0.422 0.839 0.092 Uiso 1.00 calc . . . H(16) H 0.088 0.439 0.766 0.093 Uiso 1.00 calc . . . H(17) H 0.146 0.480 0.704 0.093 Uiso 1.00 calc . . . H(18) H 0.041 0.388 0.499 0.078 Uiso 1.00 calc . . . H(19) H -0.017 0.374 0.187 0.093 Uiso 1.00 calc . . . H(20) H 0.058 0.400 0.068 0.093 Uiso 1.00 calc . . . H(21) H -0.101 0.434 0.232 0.112 Uiso 1.00 calc . . . H(22) H -0.031 0.459 0.091 0.112 Uiso 1.00 calc . . . H(23) H -0.039 0.456 0.528 0.093 Uiso 1.00 calc . . . H(24) H 0.159 0.502 0.305 0.108 Uiso 1.00 calc . . . H(25) H 0.221 0.460 0.305 0.108 Uiso 1.00 calc . . . H(26) H 0.141 0.464 0.143 0.108 Uiso 1.00 calc . . . H(27) H 0.388 0.402 0.568 0.113 Uiso 1.00 calc . . . H(28) H 0.437 0.358 0.520 0.113 Uiso 1.00 calc . . . H(29) H 0.365 0.377 0.361 0.113 Uiso 1.00 calc . . . H(30) H 0.011 0.527 0.275 0.119 Uiso 1.00 calc . . . H(31) H -0.007 0.530 0.719 0.164 Uiso 1.00 calc . . . H(32) H 0.004 0.572 0.579 0.164 Uiso 1.00 calc . . . H(33) H 0.084 0.539 0.595 0.164 Uiso 1.00 calc . . . H(34) H -0.145 0.507 0.269 0.142 Uiso 1.00 calc . . . H(35) H -0.150 0.522 0.505 0.142 Uiso 1.00 calc . . . H(36) H -0.113 0.578 0.167 0.183 Uiso 1.00 calc . . . H(37) H -0.116 0.593 0.403 0.183 Uiso 1.00 calc . . . H(38) H -0.258 0.568 0.167 0.202 Uiso 1.00 calc . . . H(39) H -0.263 0.579 0.407 0.202 Uiso 1.00 calc . . . H(40) H -0.218 0.653 0.292 0.263 Uiso 1.00 calc . . . H(41) H -0.255 0.665 -0.057 0.396 Uiso 1.00 calc . . . H(42) H -0.180 0.629 -0.037 0.396 Uiso 1.00 calc . . . H(43) H -0.282 0.616 -0.079 0.396 Uiso 1.00 calc . . . H(44) H -0.354 0.675 0.219 0.377 Uiso 1.00 calc . . . H(45) H -0.351 0.645 0.418 0.377 Uiso 1.00 calc . . . H(46) H -0.385 0.626 0.202 0.377 Uiso 1.00 calc . . . H(47) H 0.622 0.285 0.337 0.233 Uiso 1.00 calc . . . H(48) H 0.681 0.270 0.147 0.233 Uiso 1.00 calc . . . H(49) H 0.596 0.299 0.108 0.233 Uiso 1.00 calc . . . H(50) H 0.550 0.224 0.259 0.101 Uiso 1.00 calc . . .