8-Chloro-5-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,5]benzoxazepine
Dupont, Léon; Liégeois, Jean-François; Acta Crystallographica Section E 59 (2003) o1962–o1963; doi:10.1107/S1600536803025844

data_2202627
_publ_section_title
8-Chloro-5-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,5]benzoxazepine
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1962
_journal_page_last               o1963
_journal_paper_doi               10.1107/S1600536803025844
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C17 H17 Cl N4 O'
_chemical_formula_moiety         'C17 H17 Cl N4 O'
_chemical_formula_sum            'C17 H17 Cl N4 O'
_chemical_formula_weight         328.80
_chemical_name_systematic
;
8-chloro-5-(4-methylpiperazin-1-yl)-11H-pyrido[2,3-b][1,5]benzoxazepine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.347(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5531(8)
_cell_length_b                   10.6765(8)
_cell_length_c                   17.2457(12)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.94
_cell_measurement_theta_min      20.17
_cell_volume                     1572.1(2)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1987)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe-Siemens AED four-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4860
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.8231
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(EMPIR; Stoe & Cie, 1987)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.234
_refine_ls_extinction_coef       0.0278(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.1871P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                2865
_reflns_number_total             4581
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6107.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2202627
_cod_database_fobs_code          2202627