A comparison of three crystalline forms of miconazole: solvent-free, ethanol monosolvate and hemihydrate
Kaspiaruk, Hanna; Checińska, Lilianna; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622004909

data_2022609
_publ_section_title
;
 A comparison of three crystalline forms of miconazole: solvent-free,
 ethanol monosolvate and hemihydrate
;
_journal_coeditor_code           VP3025
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622004909
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C18 H14 Cl4 N2 O, 0.5 H2 O'
_chemical_formula_moiety         'C18 H14 Cl4 N2 O, 0.5(H2 O)'
_chemical_formula_sum            'C18 H15 Cl4 N2 O1.5'
_chemical_formula_weight         425.12
_chemical_name_systematic
'(<i>RS</i>)-1-[2-(2,4-Dichlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl]-1<i>H</i>-imidazole hemihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 117.864(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.0630(3)
_cell_length_b                   33.2610(16)
_cell_length_c                   16.5481(7)
_cell_measurement_reflns_used    11558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.0300
_cell_measurement_theta_min      2.6100
_cell_volume                     3923.4(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015<i>b</i>) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy Dualflex HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45202
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.449
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9339
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.3220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                6260
_reflns_number_total             9339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3025sup1.cif
_cod_data_source_block           MIC_0.5H2O
_cod_depositor_comments
;

2022-12-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H30 Cl8 N4 O3'
_cod_original_formula_weight         850.24
_cod_original_formula_moiety         '2(C18 H14 Cl4 N2 O), H2 O'
_cod_original_formula_iupac          '2C18 H14 Cl4 N2 O, H2 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022609
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.976
_shelx_hkl_checksum              76327
_shelx_res_checksum              28534
_cod_database_fobs_code 2022609