3-Oxo-5β-24-norcholanic acid: acid-to-acid hydrogen-bonding catemers employing the rare <i>anti</i> carboxyl conformation in the aggregation of a steroid keto acid
Dufort, Marisa DeVita; Davison, Mark; Lalancette, Roger A.; Thompson, Hugh W.; Acta Crystallographica Section C 63 (2007) o646–o649; doi:10.1107/S0108270107047014

data_2016252
_publ_section_title
;
 3-Oxo-5\b-24-norcholanic acid: acid-to-acid hydrogen-bonding catemers
 employing the rare <i>anti</i> carboxyl conformation in the
 aggregation of a steroid keto acid
;
_journal_coeditor_code           GA3075
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o646
_journal_page_last               o649
_journal_paper_doi               10.1107/S0108270107047014
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C23 H36 O3'
_chemical_formula_moiety         'C23 H36 O3'
_chemical_formula_sum            'C23 H36 O3'
_chemical_formula_weight         360.52
_chemical_melting_point          457
_chemical_name_systematic
;
(5<i>R</i>,8<i>R</i>,9<i>S</i>,10<i>S</i>,13<i>R</i>,14<i>S</i>,
17<i>R</i>,20<i>R</i>)-3-oxo-5\b-24-norcholanic acid
;
_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                   7.47160(11)
_cell_length_b                   8.72260(12)
_cell_length_c                   30.2407(5)
_cell_measurement_reflns_used    13991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.14
_cell_measurement_theta_min      5.28
_cell_volume                     1970.84(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2004)'
_computing_publication_material  'SHELXTL (Sheldrick, 2004)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2004)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD APEXII area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.062
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            13991
_diffrn_reflns_theta_full        68.14
_diffrn_reflns_theta_max         68.14
_diffrn_reflns_theta_min         5.28
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.16
_refine_ls_abs_structure_details 'Flack (1983), 1475 Friedel pairs'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2004)'
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.040
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                2976
_reflns_number_total             3567
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3075.cif
_cod_data_source_block           I
_cod_database_code               2016252
_cod_database_fobs_code          2016252