8-Methyl-6-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
Marie-Rose Spirlet; Amaury Graulich; Jean-Francois Liégeois; Acta Crystallographica Section E 59 (2003) o1990–o1991; doi:10.1107/S1600536803026448

data_2202618
_publ_section_title
8-Methyl-6-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1990
_journal_page_last               o1991
_journal_paper_doi               10.1107/S1600536803026448
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C18 H21 N5'
_chemical_formula_moiety         'C18 H21 N5'
_chemical_formula_sum            'C18 H21 N5'
_chemical_formula_weight         307.40
_chemical_name_systematic
;
8-methyl-6-(4-methylpiperazin-1-yl)-11H-pyrido[2,3-b][1,4]benzodiazepine
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0331(19)
_cell_length_b                   15.610(3)
_cell_length_c                   16.514(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.49
_cell_measurement_theta_min      15.22
_cell_volume                     3359.7(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1991)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6621
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'NORTH et al. (1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0498
_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^)+(0.034P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                1441
_reflns_number_total             2952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6096.cif
_cod_data_source_block           I
_cod_database_code               2202618
_cod_database_fobs_code          2202618