Methyl 3-[(chloromethoxy)carbonyloxy]-7-hydroxycholan-24-oate
Zhong, Jia-Liang; Sun, Wen-Xia; Zhang, Fu-Li; Liu, Li-Hong; Liu, He; Acta Crystallographica Section E 69 (2013) o1186–; doi:10.1107/S160053681301725X

data_2238190
_publ_section_title
;
 Methyl 3-[(chloromethoxy)carbonyloxy]-7-hydroxycholan-24-oate
;
_journal_coeditor_code           IM2434
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1186
_journal_paper_doi               10.1107/S160053681301725X
_journal_volume                  69
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C27 H43 Cl O6'
_chemical_formula_moiety         'C27 H43 Cl O6'
_chemical_formula_sum            'C27 H43 Cl O6'
_chemical_formula_weight         499.06
_chemical_name_systematic
; 
Methyl 3-[(chloromethoxy)carbonyloxy]-7-hydroxycholan-24-oate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8896(13)
_cell_length_b                   10.9493(17)
_cell_length_c                   30.683(5)
_cell_measurement_reflns_used    2869
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      20.23
_cell_measurement_theta_min      2.29
_cell_volume                     2650.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15292
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack (1983), 2309 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.10(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.1843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                3191
_reflns_number_total             5411
_reflns_threshold_expression     I>2sigma(I)
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            im2434.cif
_cod_data_source_block           I
_cod_database_code               2238190
_cod_database_fobs_code          2238190