8-Chloro-5-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,5]benzodiazepine
Dupont, L.; Liégeois, J.-F.; Rogister, F.; Delarge, J.; Acta Crystallographica Section C 52 (1996) 391–393; doi:10.1107/S0108270195011942

data_2004533
_publ_section_title
8-Chloro-5-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,5]benzodiazepine
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              391
_journal_page_last               393
_journal_paper_doi               10.1107/S0108270195011942
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C17 H18 Cl1 N5'
_chemical_formula_sum            'C17 H18 Cl N5'
_chemical_formula_weight         327.81
_chemical_name_systematic
;
8-Chloro-5-(4-methylpiperazin-1-yl)-11H-pyrido[2,3-b][1,5]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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.836(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9739(12)
_cell_length_b                   10.2088(11)
_cell_length_c                   14.662(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.46
_cell_measurement_theta_min      24.30
_cell_volume                     1639.4(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1987a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1987b)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe-Siemens AED 4-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2170
_diffrn_reflns_theta_max         55.00
_diffrn_reflns_theta_min         4.05
_diffrn_standards_decay_%        5.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.5643
_exptl_absorpt_correction_T_min  0.5059
_exptl_absorpt_correction_type
'semi-empirical via \y scan (EMPIR; Stoe & Cie, 1987c)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.266
_refine_ls_extinction_coef       0.0061(5)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.965
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment
;
H atoms were restrained (included as riding atoms) except the H(N5) atom
which was kept fixed
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0684P)^2^ + 0.5308P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1313
_refine_ls_wR_factor_obs         0.1072
_reflns_number_observed          1428
_reflns_number_total             2055
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            pa1200.cif
_cod_data_source_block           pa1200
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C17 H18 Cl1 N5'
_cod_database_code               2004533