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_2022608
_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, C2 H6 O'
_chemical_formula_moiety         'C18 H14 Cl4 N2 O, C2 H6 O'
_chemical_formula_sum            'C20 H20 Cl4 N2 O2'
_chemical_formula_weight         462.18
_chemical_name_systematic
'(<i>RS</i>)-1-[2-(2,4-Dichlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl]-1<i>H</i>-imidazole ethanol monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                115.423(3)
_cell_angle_beta                 99.068(2)
_cell_angle_gamma                94.776(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0766(2)
_cell_length_b                   11.5926(3)
_cell_length_c                   13.0383(4)
_cell_measurement_reflns_used    11675
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6350
_cell_measurement_theta_min      2.6190
_cell_volume                     1073.06(6)
_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 0.987
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24180
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.1988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                3866
_reflns_number_total             5130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3025sup1.cif
_cod_data_source_block           MIC_EtOH
_cod_database_code               2022608
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              63203
_shelx_res_checksum              25622
_cod_database_fobs_code 2022608