Channel-forming solvate crystals and isostructural solvent-free powder of 5-hydroxy-6-methyl-2-pyridone
Parkin, Sean R.; Behrman, Edward J.; Acta Crystallographica Section C 67 (2011) o324–o328; doi:10.1107/S0108270111026254

data_2018197
_publ_section_title
;
 Channel-forming solvate crystals and isostructural solvent-free powder
 of 5-hydroxy-6-methyl-2-pyridone
;
_journal_coeditor_code           MX3051
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o324
_journal_page_last               o328
_journal_paper_doi               10.1107/S0108270111026254
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H7 N O2 , 0.1667C3 H8 O'
_chemical_formula_moiety         'C6 H7 N O2, 0.1667(C3 H8 O)'
_chemical_formula_sum            'C6.5 H8.3333 N O2.1667'
_chemical_formula_weight         135.14
_chemical_name_systematic
;
5-hydroxy-6-methyl-2-pyridone propan-2-ol 0.167-solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   24.9208(5)
_cell_length_b                   24.9208(5)
_cell_length_c                   5.27380(10)
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      3.55
_cell_volume                     2836.47(10)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and local procedures'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            14474
_diffrn_reflns_theta_full        68.33
_diffrn_reflns_theta_max         68.33
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.297
_refine_ls_extinction_coef       0.00069(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1163
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0645P)^2^+5.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                908
_reflns_number_total             1163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mx3051.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C6.50 H8.3333 N O2.1667'
_cod_database_code               2018197
_cod_database_fobs_code          2018197