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_2017633
_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          'C19 H19 N6 + , Cl - , C6 H8 N2'
_chemical_formula_moiety         'C19 H19 N6 + , Cl - , C6 H8 N2'
_chemical_formula_sum            'C25 H27 Cl N8'
_chemical_formula_weight         475.00
_chemical_name_systematic
;
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)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                102.894(12)
_cell_angle_beta                 112.176(14)
_cell_angle_gamma                107.512(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9559(13)
_cell_length_b                   11.2372(13)
_cell_length_c                   11.432(2)
_cell_measurement_reflns_used    4532
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.11
_cell_volume                     1149.0(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30475
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0402P)^2^+0.6732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                3349
_reflns_number_total             4532
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3368.cif
_cod_data_source_block           II
_cod_original_cell_volume        1149.0(3)
_cod_database_code               2017633
_cod_database_fobs_code          2017633