Investigations on the structure of 4-methyldihydro-1,3,4-benzotriazepin-5-ones. Tautomer reassignment
Zahra, Jalal A.; El-Abadelah, Mustafa M.; Nazer, Musa Z.; Ebraheem, Kais A. K.; Boese, Roland; Organic & Biomolecular Chemistry 1 (2003) 1798–; doi:10.1039/b301047c

data_7150511
_publ_section_title
;
 Investigations on the structure of
 4-methyldihydro-1,3,4-benzotriazepin-5-ones. Tautomer reassignment
;
_journal_issue                   10
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              1798
_journal_paper_doi               10.1039/b301047c
_journal_volume                  1
_journal_year                    2003
_chemical_formula_sum            'C9 H9 N3 O'
_chemical_formula_weight         175.19
_chemical_name_common            4-Methyl-dihydro-1,3,4-benzotriazepin-5-ones
_chemical_name_systematic
; 
4-Methyl-dihydro-1,3,4-benzotriazepin-5-ones 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.368(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.906(8)
_cell_length_b                   14.087(7)
_cell_length_c                   7.001(4)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.81
_cell_volume                     1667.3(15)
_computing_cell_refinement       'BRUKER AXS SAINT program Vers.6.01'
_computing_data_collection       'BRUKER AXS SMART Vers. 5.054 1997/98'
_computing_data_reduction        'BRUKER AXS SAINT program Vers.6.01'
_computing_molecular_graphics    'BRUKER AXS SHELXTL Vers.6.12,98/NT/2000/ME'
_computing_publication_material  'BRUKER AXS SHELXTL Vers.6.12,98/NT/2000/ME'
_computing_structure_refinement  'BRUKER AXS SHELXTL Vers.6.12,98/NT/2000/ME'
_computing_structure_solution    'BRUKER AXS SHELXTL Vers.6.12,98/NT/2000/ME'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART CCD area detector system'
_diffrn_measurement_method
;
Fullsphere data collection 
in omega at 0.3 deg scan width, 
two runs with 720 frames, phi =  0, 270(deg) 
two runs with 436 frames, phi = 88, 180 deg) 
;
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9461
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
Siemens SADABS program multi-scan V2.03
R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment
;     
Riding model on idealized geometries
with the 1.2 fold (1.5 fold for methyl
groups) isotropic displacement
parameters of the equivalent Uij of the
corresponding carbon atom;
nitrogen hydrogen atom positions taken from
a Fourier-map and also refined as riding
group with the 1.2 fold isotropic
displacement parameters of the
equivalent Uij of the corresponding
nitrogen atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+0.0192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                1950
_reflns_number_total             2925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301047c.txt
_cod_data_source_block           tauaba0m
_cod_original_cell_volume        1667.3(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7150511