β-Polymorph of phenazepam: a powder study
Sergeev, Gleb B.; Sergeev, Boris M.; Morosov, Yurii N.; Chernyshev, Vladimir V.; Acta Crystallographica Section E 66 (2010) o2623–; doi:10.1107/S1600536810037402

data_2227782
_publ_section_title
;
 \b-Polymorph of phenazepam: a powder study
;
_journal_coeditor_code           LH5126
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2623
_journal_paper_doi               10.1107/S1600536810037402
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C15 H10 Br Cl N2 O'
_chemical_formula_moiety         'C15 H10 Br Cl N2 O'
_chemical_formula_sum            'C15 H10 Br Cl N2 O'
_chemical_formula_weight         349.61
_chemical_name_common            'Phenazepam, \b-polymorph'
_chemical_name_systematic
;
7-Bromo-5-(2-chlorophenyl)-1<i>H</i>-1,4-benzodiazepin-2(3<i>H</i>)-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.679(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8006(19)
_cell_length_b                   11.6756(14)
_cell_length_c                   8.4769(9)
_cell_measurement_reflns_used    862
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      39.99
_cell_measurement_theta_min      2.99
_cell_volume                     1461.8(3)
_computing_cell_refinement       '<i>MRIA</i> (Zlokazov & Chernyshev, 1992)'
_computing_data_collection
'<i>G670 Imaging Plate Guinier Camera Software</i> (Huber, 2002)'
_computing_data_reduction
'<i>G670 Imaging Plate Guinier Camera Software</i> (Huber, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'<i>MRIA</i> (Zlokazov & Chernyshev, 1992) and SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  '<i>MRIA</i> (Zlokazov & Chernyshev, 1992)'
_computing_structure_solution
'simulated annealing (Zhukov <i>et al.</i>, 2001)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Guinier camera G670'
_diffrn_radiation_monochromator  'Curved Germanium (111)'
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.54059
_exptl_absorpt_coefficient_mu    5.485
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_pd_block_diffractogram_id       beta_phenazepam
_pd_char_colour                  'light grey'
_pd_char_particle_morphology     'no specific habit'
_pd_instr_location
;
Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia
;
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        80.00
_pd_meas_2theta_range_min        5.00
_pd_meas_number_of_points        7501
_pd_meas_scan_method             cont
_pd_prep_pressure                '6.6 10^-6^'
_pd_prep_temperature             77
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        80.00
_pd_proc_2theta_range_min        5.00
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr
;
March-Dollase (Dollase, 1986); direction of preferred orientation 001,
texture parameter <i>r</i> = 0.93(1).
;
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0130
_pd_proc_ls_prof_wR_expected     0.0115
_pd_proc_ls_prof_wR_factor       0.0172
_pd_proc_wavelength              1.54059
_pd_spec_mounting
;
thin layer in the specimen holder of the camera
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.500
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     128
_refine_ls_number_restraints     64
_refine_ls_shift/su_max          .004
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            lh5126.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227782