Oxime–Carboxyl Hydrogen Bonds: the Preferred Interaction Determining Crystal Packing of `Carboxyoximes'
Maurin, J. K.; Acta Crystallographica Section B 54 (1998) 866–871; doi:10.1107/S0108768198002171

data_2105528
_publ_section_title
;
 Oxime--Carboxyl Hydrogen Bonds: the Preferred Interaction Determining
 Crystal Packing of `Carboxyoximes'
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              866
_journal_page_last               871
_journal_paper_doi               10.1107/S0108768198002171
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C24 H39 N O3'
_chemical_formula_weight         389.56
_chemical_melting_point          442
_chemical_name_common            '5-\b-Cholanic acid -3-oxime'
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.564(3)
_cell_length_b                   14.564(3)
_cell_length_c                   20.282(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      8.25
_cell_volume                     3725.7(14)
_computing_cell_refinement       'CAD-4 Nonius software'
_computing_data_collection       'CAD-4 Nonius software'
_computing_data_reduction        'CAD-4 Nonius software'
_computing_molecular_graphics    'ORTEP (Johnson,1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'CAD-4 \k-axis diffractometer'
_diffrn_measurement_method       '\w-\q scans for individual reflections'
_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  0.029
_diffrn_reflns_av_sigmaI/netI    0.1232
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3614
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not applied'
_exptl_crystal_description       bipiramidal
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10.(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.914
_refine_ls_goodness_of_fit_obs   1.411
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.536
_refine_ls_restrained_S_obs      1.411
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_obs          0.0653
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2831
_refine_ls_wR_factor_obs         0.1489
_reflns_number_observed          888
_reflns_number_total             1680
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab0387.cif
_cod_data_source_block           w15j3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2105528