8-Chloro-6-(3-dimethylaminopropylamino)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
Dupont, Léon; Eyrolles, Laurence; Evrard, Guy; Delarge, Jacques; Liégeois, Jean-François; Acta Crystallographica Section E 58 (2002) o69–o71; doi:10.1107/S1600536801021286

data_2200826
_publ_section_title
8-Chloro-6-(3-dimethylaminopropylamino)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o69
_journal_page_last               o71
_journal_paper_doi               10.1107/S1600536801021286
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C17 H20 Cl N5'
_chemical_formula_moiety         'C17 H20 Cl N5'
_chemical_formula_sum            'C17 H20 Cl N5'
_chemical_formula_weight         329.83
_chemical_name_systematic
;
8-Chloro-6-(3-dimethylaminopropylamino)-11H-pyrido[2,3-b][1,4]benzodiazepine
;
_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
;
H atoms were placed at standard calculated positions, except atoms H(N5)
and H(N16), which were obtained from difference map.
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.545(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0010(10)
_cell_length_b                   20.421(3)
_cell_length_c                   9.9350(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      20
_cell_volume                     1720.9(4)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0215
_diffrn_reflns_av_sigmaI/netI    .0328
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7197
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .229
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         .335
_refine_diff_density_min         -.158
_refine_ls_extinction_coef       .078(4)
_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   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          .0511
_refine_ls_R_factor_gt           .0436
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.2131P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1137
_refine_ls_wR_factor_ref         .1216
_reflns_number_gt                3036
_reflns_number_total             3511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6097.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200826
_cod_database_fobs_code          2200826