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_2104115
_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_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_sum            'C58 H86 O8'
_chemical_formula_weight         911.27
_chemical_name_systematic
;
bis(23-methoxycarbonyl-24-nor-5beta-cholan
-3alpha-yl)terephtalate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   31.731(6)
_cell_length_b                   7.727(2)
_cell_length_c                   11.017(2)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.37
_cell_measurement_theta_min      16.03
_cell_volume                     2592.9(10)
_computing_cell_refinement       'Kuma KM-4 software (Kuma Diffraction, 1995)'
_computing_data_collection       'Kuma KM-4 software (Kuma Diffraction, 1995)'
_computing_data_reduction        'Kuma KM-4 software (Kuma Diffraction, 1995)'
_computing_molecular_graphics
;
Simens Analytical X-Ray Instruments (1989)
Mercury (Bruno at al. 2002)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KM-4 four circle diffractometer'
_diffrn_measurement_method       \Q--2\Q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1955
_diffrn_reflns_av_sigmaI/netI    0.2360
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4425
_diffrn_reflns_theta_full        65.82
_diffrn_reflns_theta_max         65.82
_diffrn_reflns_theta_min         5.72
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       0.00071(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         2419
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.2717
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                715
_reflns_number_total             2419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5073.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      C2
_cod_database_code               2104115
_cod_database_fobs_code          2104115