4-Phenyl-2,5,5a,6,7,8,9,9a-hexahydro-1<i>H</i>-1,5-benzodiazepine-2-thione ethanol monosolvate
Al Garadi, Wedad; Ramli, Youssef; El Ghayati, Lhoussaine; El Hafi, Mohamed; Moussaif, Ahmed; Essassi, El Mokhtar; Mague, Joel T.; IUCrData 3 (2018) x181276–; doi:10.1107/S2414314618012762

data_1549951
_publ_section_title
;
 4-Phenyl-2,5,5a,6,7,8,9,9a-hexahydro-1<i>H</i>-1,5-benzodiazepine-2-thione
 ethanol monosolvate
;
_journal_coeditor_code           HB4260
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x181276
_journal_paper_doi               10.1107/S2414314618012762
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          'C15 H18 N2 S, C2 H6 O'
_chemical_formula_moiety         'C15 H18 N2 S, C2 H6 O'
_chemical_formula_sum            'C17 H24 N2 O S'
_chemical_formula_weight         304.44
_chemical_name_systematic
;
4-Phenyl-2,5,5a,6,7,8,9,9a-hexahydro-1<i>H</i>-1,5-benzodiazepine-2-thione
ethanol monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 95.8130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0255(2)
_cell_length_b                   8.9303(2)
_cell_length_c                   15.8822(3)
_cell_measurement_reflns_used    8452
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      70.144
_cell_measurement_theta_min      4.858
_cell_volume                     1696.84(6)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12459
_diffrn_reflns_theta_full        70.100
_diffrn_reflns_theta_max         70.138
_diffrn_reflns_theta_min         4.857
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0531P)^2^+0.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                2613
_reflns_number_total             3209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4260sup1.cif
_cod_data_source_block           I
_cod_database_code               1549951
_cod_database_fobs_code          1549951
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.931
_shelx_hkl_checksum              67666
_shelx_res_checksum              88195