Crystal structure of 2,2,4-trimethyl-2,3,4,5-tetrahydro-1<i>H</i>-benzo[<i>b</i>][1,4]diazepine hemihydrate
Ezhilarasi, K. S.; Akila, A.; Ponnuswamy, S.; Revathi, B. K.; Usha, G.; Acta Crystallographica Section E 71 (2015) o570–o571; doi:10.1107/S2056989015013201

data_2240932
_publ_section_title
;
 Crystal structure of
 2,2,4-trimethyl-2,3,4,5-tetrahydro-1<i>H</i>-benzo[<i>b</i>][1,4]diazepine
 hemihydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o570
_journal_page_last               o571
_journal_paper_doi               10.1107/S2056989015013201
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C12 H18 N2 , 0.5H2 O'
_chemical_formula_moiety         'C12 H18 N2 , 0.5(H2 O)'
_chemical_formula_sum            'C12 H19 N2 O0.5'
_chemical_formula_weight         199.29
_chemical_name_systematic
;
2,2,4-Trimethyl-2,3,4,5-tetrahydro-1<i>H</i>-benzo[<i>b</i>][1,4]diazepine
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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.483(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.0548(10)
_cell_length_b                   23.246(2)
_cell_length_c                   11.5613(14)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.880
_cell_measurement_theta_min      1.75
_cell_volume                     2392.9(4)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2014/6 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22443
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.881
_diffrn_reflns_theta_min         2.287
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.204
_refine_ls_extinction_coef       0.0040(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4161
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0621P)^2^+0.8577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                2416
_reflns_number_total             4161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5164sup1.cif
_cod_data_source_block           I
_cod_database_code               2240932
_cod_database_fobs_code          2240932
_shelx_hkl_checksum              51811
_shelx_res_checksum              74395
_shelxl_version_number           2014/6