3-Methyl-6-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
Dupont, L.; Liégeois, J.-F.; Rogister, F.; Delarge, J.; Acta Crystallographica Section C 51 (1995) 1889–1891; doi:10.1107/S0108270195003337

data_2003871
_publ_section_title
3-Methyl-6-(4-methylpiperazin-1-yl)-11<i>H</i>-pyrido[2,3-<i>b</i>][1,4]benzodiazepine
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1889
_journal_page_last               1891
_journal_paper_doi               10.1107/S0108270195003337
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C18 H21 N5'
_chemical_formula_weight         307.40
_chemical_name_systematic
;
 3-methyl-6-(4-methylpiperazin-1-yl)-11H-pyrido[2,3-b][1,4]benzodiazepine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.039(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3352(6)
_cell_length_b                   19.2342(10)
_cell_length_c                   9.3903(7)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.59
_cell_measurement_theta_min      37.15
_cell_volume                     1683.71(19)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe-Siemens AED four-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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2594
_diffrn_reflns_theta_max         58.94
_diffrn_reflns_theta_min         4.60
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.8261
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_type   'semi-empirical via \y scan'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.14
_refine_ls_extinction_coef       0.0059(4)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   0.897
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment
;
H atoms were constrained (included as riding atoms) except H(N5) which
was kept fixed.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_obs          0.0385
_refine_ls_shift/esd_max         0.006
_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^) + (0.0677P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1043
_refine_ls_wR_factor_obs         0.0940
_reflns_number_observed          1399
_reflns_number_total             2426
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1002.cif
_cod_data_source_block           sm0140
_cod_original_cell_volume        1683.7(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2003871