Synthesis and structural characteristics of lithocholate triads: steroid-type channels occupied by spacer fragments
Rychlewska, Urszula; Warżajtis, Beata; Joachimiak, Roman; Paryzek, Zdzisław; Acta Crystallographica Section B 64 (2008) 383–392; doi:10.1107/S0108768108006514

data_2104113
_publ_contact_author
;
Urszula Rychlewska
Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
_publ_section_title
;
 Synthesis and structural characteristics of lithocholate triads:
 steroid-type channels occupied by spacer fragments
;
_journal_coeditor_code           BK5073
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              383
_journal_page_last               392
_journal_paper_doi               10.1107/S0108768108006514
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'C56 H82 O8, 2(C5 H5 N)'
_chemical_formula_sum            'C66 H92 N2 O8'
_chemical_formula_weight         1041.42
_chemical_melting_point          320
_chemical_name_systematic
;
bis(23-carboxy-24-nor-5beta-cholan-3alpha-yl)terephtalate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.390(4)
_cell_angle_beta                 83.254(4)
_cell_angle_gamma                82.771(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8559(6)
_cell_length_b                   13.5462(7)
_cell_length_c                   17.4215(9)
_cell_measurement_reflns_used    22008
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.37
_cell_volume                     2900.9(3)
_computing_cell_refinement
'CrysAlis RED v.1.168 (Oxford Diffraction,2001)'
_computing_data_collection
'CrysAlis CCD v.1.168 (Oxford Diffraction,2001)'
_computing_data_reduction
'CrysAlis RED v.1.168 (Oxford Diffraction,2001)'
_computing_molecular_graphics    'Simens Analytical X-Ray Instruments (1989)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Kuma KM4CCD \k-geometry diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.1253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22008
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.37
_diffrn_standards_interval_count 'every 50 dc frames'
_diffrn_standards_number         '3 reference frames'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.191
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1381
_refine_ls_number_reflns         10239
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                6040
_reflns_number_total             10239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5073.cif
_cod_data_source_block           52Py120K
_cod_original_sg_symbol_H-M      P1
_cod_database_code               2104113
_cod_database_fobs_code          2104113