Crystal structure and pseudosymmetry analysis of the triclinic prodrug cloxazolam (Z' = 4).
Garraza, María Soledad; Gimenez, María Emilia; Vega, Daniel Roberto; Baggio, Ricardo; Acta crystallographica. Section C, Structural chemistry 75 (2019) 851–858; doi:10.1107/S2053229619008404

data_2311997
_publ_section_title
;
 Crystal structure and pseudosymmetry analysis of the triclinic prodrug
 cloxazolam (Z' = 4).
;
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              851
_journal_page_last               858
_journal_paper_doi               10.1107/S2053229619008404
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C17 H14 Cl2 N2 O2'
_chemical_formula_sum            'C17 H14 Cl2 N2 O2'
_chemical_formula_weight         349.20
_chemical_name_systematic
13-Chloro-2-(2-chlorophenyl)-3-oxa-6,9-diazatricyclo[8.4.0.0^2,6^]tetradeca-1(10),11,13-trien-8-one
_space_group_IT_number           2
_space_group_name_Hall           '-B 1'
_space_group_name_H-M_alt        'B -1'
_symmetry_cell_setting           triclinic
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                78.897(2)
_cell_angle_beta                 100.411(4)
_cell_angle_gamma                90.042(3)
_cell_formula_units_Z            16
_cell_length_a                   16.7989(6)
_cell_length_b                   17.0054(7)
_cell_length_c                   22.1341(7)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      3.12
_cell_volume                     6098.8(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83792
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         26.445
_diffrn_reflns_theta_min         2.054
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SAINT; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12513
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0509P)^2^+3.6398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                7798
_reflns_number_total             12513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3730sup1.cif
_cod_data_source_block           I
_cod_database_code               2311997
_shelx_hkl_checksum              98127
_shelx_res_checksum              88421