<i>N</i>-(4-Methylpyridin-2-yl)-5<i>H</i>-dibenzo[<i>d</i>,<i>f</i>][1,3]diazepine-6-carboxamide toluene hemisolvate
Hodorowicz, Maciej; Stadnicka, Katarzyna; Trzewik, Bartosz; Zaleska, Barbara; Acta Crystallographica Section E 63 (2007) o4115–o4115; doi:10.1107/S1600536807042687

data_2215611
_publ_section_title
;<i>N</i>-(4-Methylpyridin-2-yl)-5<i>H</i>-dibenzo[<i>d</i>,<i>f</i>][1,3]diazepine-6-carboxamide
 toluene hemisolvate
;
_journal_coeditor_code           NG2316
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4115
_journal_page_last               o4115
_journal_paper_doi               10.1107/S1600536807042687
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H16 N4 O, 0.5C7 H8'
_chemical_formula_moiety         'C20 H16 N4 O, 0.5(C7 H8)'
_chemical_formula_sum            'C23.5 H20 N4 O'
_chemical_formula_weight         374.44
_chemical_name_systematic
;
<i>N</i>-(4-Methylpyridin-2-yl)-5<i>H</i>-dibenzo[d,f][1,3]diazepine-6-
carboxamide toluene hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.0500(10)
_cell_angle_beta                 87.5290(10)
_cell_angle_gamma                70.1910(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9323(2)
_cell_length_b                   9.6863(2)
_cell_length_c                   12.1478(3)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     963.08(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans to fill asymmetric unit'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17061
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9878
_exptl_absorpt_correction_T_min  0.9767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(DENZO and SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.184
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         <0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                5192
_reflns_number_total             8631
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2316.cif
_cod_data_source_block           I
_cod_database_code               2215611
_cod_database_fobs_code          2215611