2-Amino-4-(piperidin-1-yl)-11<i>H</i>-pyrimido[4,5-<i>b</i>][1,5]benzodiazepin-6-ium chloride monohydrate and 2-amino-4-[methyl(2-methylphenyl)amino]-11<i>H</i>-pyrimido[4,5-<i>b</i>][1,5]benzodiazepin-6-ium chloride–benzene-1,2-diamine (1/1): complex sheets generated by multiple hydrogen bonds
Quiroga, Jairo; Trilleras, Jorge; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 66 (2010) o154–o158; doi:10.1107/S0108270110006967

data_2017632
_publ_section_title
;
 2-Amino-4-(piperidin-1-yl)-11<i>H</i>-pyrimido[4,5-<i>b</i>][1,5]benzodiazepin-6-ium
 chloride monohydrate and
 2-amino-4-[methyl(2-methylphenyl)amino]-11<i>H</i>-pyrimido[4,5-<i>b</i>][1,5]benzodiazepin-6-ium
 chloride--benzene-1,2-diamine (1/1): complex sheets generated by
 multiple hydrogen bonds
;
_journal_coeditor_code           SK3368
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o154
_journal_page_last               o158
_journal_paper_doi               10.1107/S0108270110006967
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C16 H19 N6 + , Cl - , H2 O'
_chemical_formula_moiety         'C16 H19 N6 + , Cl - , H2 O'
_chemical_formula_sum            'C16 H21 Cl N6 O'
_chemical_formula_weight         348.84
_chemical_name_systematic
;
2-amino-4-(piperidin-1-yl)-11<i>H</i>-pyrimido[4,5-<i>b</i>][1,5]benzodiazepin-
6-ium chloride monohydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.925(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7831(14)
_cell_length_b                   7.5324(9)
_cell_length_c                   15.2987(12)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.41
_cell_volume                     1582.4(3)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22943
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0460P)^2^+1.3640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                2253
_reflns_number_total             3122
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3368.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017632
_cod_database_fobs_code          2017632