#------------------------------------------------------------------------------ #$Date: 2014-07-15 13:46:19 +0300 (Tue, 15 Jul 2014) $ #$Revision: 120435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/33/7203346.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_7203346 loop_ _publ_author_name 'Nakano, Kazunori' 'Sada, Kazuki' 'Aburaya, Kazuaki' 'Nakagawa, Kenji' 'Yoswathananont, Nungruethai' 'Tohnai, Norimitsu' 'Miyata, Mikiji' _publ_section_title ; Guest-induced inversion of an asymmetric host layer in inclusion crystals of cholic acid ; _journal_issue 6 _journal_name_full CrystEngComm _journal_page_first 461 _journal_paper_doi 10.1039/b602862d _journal_volume 8 _journal_year 2006 _chemical_formula_moiety 'C32 H49 Cl O5 ' _chemical_formula_sum 'C32 H49 Cl O5' _chemical_formula_weight 549.19 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_date 'Thu Oct 28 11:18:34 2004' _audit_creation_method 'by teXsan' _cell_angle_alpha 90 _cell_angle_beta 111.031(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.078(1) _cell_length_b 8.0989(9) _cell_length_c 16.226(2) _cell_measurement_reflns_used 3227 _cell_measurement_temperature 203.2 _cell_measurement_theta_max 67.2 _cell_measurement_theta_min 4.0 _cell_volume 1481.5(3) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _diffrn_measured_fraction_theta_full 0.9396 _diffrn_measured_fraction_theta_max 0.9396 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 5334 _diffrn_reflns_theta_full 68.20 _diffrn_reflns_theta_max 68.20 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_T_max 0.539 _exptl_absorpt_correction_T_min 0.392 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.15 _refine_diff_density_min -0.48 _refine_ls_abs_structure_Flack 1.1(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 3.447 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 263 _refine_ls_number_reflns 2752 _refine_ls_R_factor_gt 0.1995 _refine_ls_shift/su_max 0.0041 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.4387 _reflns_number_gt 2386 _reflns_number_total 2752 _reflns_threshold_expression F^2^>2.0\s(F^2^) _[local]_cod_data_source_file b602862d.txt _[local]_cod_data_source_block 2cl-p-xylene _[local]_cod_chemical_formula_sum_orig 'C32 H49 Cl O5 ' _cod_original_cell_volume 1481.4(3) _cod_database_code 7203346 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z 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(1) O 0.6121(3) 0.4347(7) 0.5986(3) 0.0609(10) Uani 1.00 d . . . O(2) O 0.2551(3) 0.6628(7) 0.3807(2) 0.0550(9) Uani 1.00 d . . . O(3) O 0.1989(3) 0.1319(7) 0.2891(2) 0.0605(10) Uani 1.00 d . . . O(4) O -0.2175(8) 0.3633(9) -0.1759(4) 0.122(2) Uani 1.00 d . . . O(5) O -0.2738(4) 0.1105(9) -0.2214(3) 0.083(1) Uani 1.00 d . . . C(1) C 0.3305(5) 0.2319(8) 0.5960(3) 0.052(1) Uani 1.00 d . . . C(2) C 0.4496(5) 0.2468(8) 0.5849(3) 0.053(1) Uani 1.00 d . . . C(3) C 0.5019(4) 0.4192(8) 0.6148(3) 0.052(1) Uani 1.00 d . . . C(4) C 0.4150(4) 0.5479(8) 0.5624(3) 0.050(1) Uani 1.00 d . . . C(5) C 0.2928(4) 0.5310(8) 0.5694(3) 0.048(1) Uani 1.00 d . . . C(6) C 0.2104(4) 0.6702(8) 0.5167(3) 0.052(1) Uani 1.00 d . . . C(7) C 0.1639(4) 0.6447(8) 0.4178(3) 0.048(1) Uani 1.00 d . . . C(8) C 0.1100(4) 0.4732(8) 0.3947(3) 0.0445(10) Uani 1.00 d . . . C(9) C 0.1945(4) 0.3324(7) 0.4451(3) 0.0415(9) Uani 1.00 d . . . C(10) C 0.2376(4) 0.3584(8) 0.5470(3) 0.048(1) Uani 1.00 d . . . C(11) C 0.1383(4) 0.1666(8) 0.4134(3) 0.048(1) Uani 1.00 d . . . C(12) C 0.0948(5) 0.1384(8) 0.3126(3) 0.052(1) Uani 1.00 d . . . C(13) C 0.0095(4) 0.2735(8) 0.2627(3) 0.047(1) Uani 1.00 d . . . C(14) C 0.0711(4) 0.4432(8) 0.2950(3) 0.047(1) Uani 1.00 d . . . C(15) C -0.0109(5) 0.5661(9) 0.2334(4) 0.062(1) Uani 1.00 d . . . C(16) C -0.0595(5) 0.4737(10) 0.1438(4) 0.068(1) Uani 1.00 d . . . C(17) C -0.0198(4) 0.2965(9) 0.1615(3) 0.055(1) Uani 1.00 d . . . C(18) C -0.1070(4) 0.2545(8) 0.2801(3) 0.054(1) Uani 1.00 d . . . C(19) C 0.1333(5) 0.3397(9) 0.5800(3) 0.057(1) Uani 1.00 d . . . C(20) C -0.1078(5) 0.1790(10) 0.0959(3) 0.066(1) Uani 1.00 d . . . C(21) C -0.0718(9) -0.004(1) 0.1129(6) 0.101(2) Uani 1.00 d . . . C(22) C -0.1211(6) 0.229(1) 0.0005(4) 0.075(2) Uani 1.00 d . . . C(23) C -0.2261(6) 0.161(1) -0.0715(4) 0.084(2) Uani 1.00 d . . . C(24) C -0.2357(6) 0.224(1) -0.1596(4) 0.073(1) Uani 1.00 d . . . H(1) H 0.2999 0.1252 0.5757 0.0594 Uiso 1.00 calc . . . H(2) H 0.3438 0.2416 0.6570 0.0594 Uiso 1.00 calc . . . H(3) H 0.5031 0.1660 0.6196 0.0619 Uiso 1.00 calc . . . H(4) H 0.4403 0.2323 0.5245 0.0619 Uiso 1.00 calc . . . H(5) H 0.5162 0.4334 0.6761 0.0596 Uiso 1.00 calc . . . H(6) H 0.4462 0.6533 0.5836 0.0587 Uiso 1.00 calc . . . H(7) H 0.4067 0.5366 0.5024 0.0587 Uiso 1.00 calc . . . H(8) H 0.3045 0.5503 0.6296 0.0540 Uiso 1.00 calc . . . H(9) H 0.1447 0.6788 0.5357 0.0596 Uiso 1.00 calc . . . H(10) H 0.2532 0.7726 0.5293 0.0596 Uiso 1.00 calc . . . H(11) H 0.1028 0.7248 0.3909 0.0542 Uiso 1.00 calc . . . H(12) H 0.0413 0.4675 0.4100 0.0513 Uiso 1.00 calc . . . H(13) H 0.2628 0.3410 0.4290 0.0488 Uiso 1.00 calc . . . H(14) H 0.1952 0.0841 0.4399 0.0564 Uiso 1.00 calc . . . H(15) H 0.0720 0.1549 0.4309 0.0564 Uiso 1.00 calc . . . H(16) H 0.0548 0.0367 0.2994 0.0623 Uiso 1.00 calc . . . H(17) H 0.1414 0.4429 0.2817 0.0543 Uiso 1.00 calc . . . H(18) H -0.0735 0.5950 0.2535 0.0739 Uiso 1.00 calc . . . H(19) H 0.0311 0.6628 0.2294 0.0739 Uiso 1.00 calc . . . H(20) H -0.1441 0.4804 0.1199 0.0802 Uiso 1.00 calc . . . H(21) H -0.0288 0.5227 0.1029 0.0802 Uiso 1.00 calc . . . H(22) H 0.0530 0.2869 0.1518 0.0641 Uiso 1.00 calc . . . H(23) H -0.0912 0.2652 0.3415 0.0618 Uiso 1.00 calc . . . H(24) H -0.1608 0.3387 0.2490 0.0618 Uiso 1.00 calc . . . H(25) H -0.1405 0.1496 0.2602 0.0618 Uiso 1.00 calc . . . H(26) H 0.1600 0.3637 0.6416 0.0687 Uiso 1.00 calc . . . H(27) H 0.0725 0.4192 0.5498 0.0687 Uiso 1.00 calc . . . H(28) H 0.1013 0.2333 0.5690 0.0687 Uiso 1.00 calc . . . H(29) H -0.1819 0.1931 0.1022 0.0777 Uiso 1.00 calc . . . H(30) H -0.1326 -0.0691 0.0718 0.1190 Uiso 1.00 calc . . . H(31) H 0.0005 -0.0208 0.1040 0.1190 Uiso 1.00 calc . . . H(32) H -0.0642 -0.0319 0.1709 0.1190 Uiso 1.00 calc . . . H(33) H -0.1268 0.3478 -0.0035 0.0882 Uiso 1.00 calc . . . H(34) H -0.0521 0.1960 -0.0101 0.0882 Uiso 1.00 calc . . . H(35) H -0.2177 0.0455 -0.0704 0.1007 Uiso 1.00 calc . . . H(36) H -0.2944 0.1918 -0.0598 0.1007 Uiso 1.00 calc . . . H(37) H 0.6661 0.3525 0.6308 0.0707 Uiso 1.00 calc . . . H(38) H 0.2788 0.7660 0.3789 0.1077 Uiso 1.00 calc . . . H(39) H 0.1755 0.1090 0.2279 0.0710 Uiso 1.00 calc . . . H(40) H -0.2171 0.0966 -0.2492 0.0943 Uiso 1.00 calc . . . 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 O(1) 0.042(1) 0.070(2) 0.067(2) 0.002(2) 0.016(1) 0.000(2) O(2) 0.056(2) 0.059(2) 0.056(2) -0.003(2) 0.027(1) 0.008(2) O(3) 0.059(2) 0.075(2) 0.045(2) 0.020(2) 0.015(1) 0.003(2) O(4) 0.191(7) 0.094(3) 0.057(3) -0.051(4) 0.016(3) -0.002(3) O(5) 0.085(3) 0.106(4) 0.065(2) -0.002(3) 0.037(2) -0.008(2) C(1) 0.057(2) 0.057(3) 0.036(2) -0.003(2) 0.011(2) 0.007(2) C(2) 0.052(2) 0.058(2) 0.046(2) 0.010(2) 0.013(2) -0.002(2) C(3) 0.043(2) 0.064(2) 0.043(2) -0.002(2) 0.008(2) 0.002(2) C(4) 0.042(2) 0.055(3) 0.050(2) -0.007(2) 0.012(2) -0.002(2) C(5) 0.048(2) 0.061(2) 0.038(2) 0.007(2) 0.018(2) -0.002(2) C(6) 0.055(2) 0.051(3) 0.053(2) 0.006(2) 0.023(2) -0.009(2) C(7) 0.050(2) 0.047(2) 0.050(2) 0.002(2) 0.021(2) -0.001(2) C(8) 0.041(2) 0.050(2) 0.042(2) 0.003(2) 0.013(2) -0.001(2) C(9) 0.042(2) 0.053(2) 0.033(2) 0.006(2) 0.016(1) 0.004(2) C(10) 0.041(2) 0.066(2) 0.036(2) 0.000(2) 0.013(2) -0.005(2) C(11) 0.049(2) 0.052(2) 0.036(2) 0.000(2) 0.008(2) 0.007(2) C(12) 0.064(2) 0.054(3) 0.040(2) 0.001(2) 0.020(2) -0.001(2) C(13) 0.047(2) 0.059(2) 0.037(2) -0.003(2) 0.017(2) -0.001(2) C(14) 0.048(2) 0.055(2) 0.039(2) -0.003(2) 0.017(2) 0.007(2) C(15) 0.063(3) 0.063(3) 0.051(3) 0.014(2) 0.010(2) 0.009(2) C(16) 0.065(3) 0.081(3) 0.044(2) 0.003(3) 0.004(2) 0.014(2) C(17) 0.047(2) 0.080(3) 0.037(2) 0.006(2) 0.014(2) 0.012(2) C(18) 0.046(2) 0.065(3) 0.049(2) -0.008(2) 0.014(2) 0.006(2) C(19) 0.060(2) 0.075(4) 0.052(2) -0.011(3) 0.037(2) -0.005(2) C(20) 0.070(3) 0.086(3) 0.035(2) 0.003(3) 0.010(2) 0.002(2) C(21) 0.126(6) 0.080(3) 0.064(4) -0.008(4) -0.005(4) -0.008(3) C(22) 0.065(3) 0.124(6) 0.038(2) 0.001(3) 0.020(2) 0.004(3) C(23) 0.078(4) 0.121(6) 0.046(2) -0.015(4) 0.014(2) 0.011(3) C(24) 0.067(3) 0.097(3) 0.047(2) 0.000(3) 0.009(2) 0.016(2) 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) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O O 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag ? ? ? ? ? ? ? ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ?