5,7-Dimethyl-2,3-dihydro-1<i>H</i>-1,4-diazepin-4-ium picrate
Jasinski, Jerry P.; Butcher, Ray J.; Yathirajan, H. S.; Narayana, B.; Prakash Kamath, K.; Acta Crystallographica Section E 66 (2010) o1187–o1188; doi:10.1107/S160053681001487X

data_2225907
_publ_section_title
;
 5,7-Dimethyl-2,3-dihydro-1<i>H</i>-1,4-diazepin-4-ium picrate
;
_journal_coeditor_code           IS2536
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1187
_journal_page_last               o1188
_journal_paper_doi               10.1107/S160053681001487X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C7 H13 N2 +, C6 H2 N3 O7-'
_chemical_formula_moiety         'C7 H13 N2 +, C6 H2 N3 O7-'
_chemical_formula_sum            'C13 H15 N5 O7'
_chemical_formula_weight         353.30
_chemical_name_systematic
;
5,7-Dimethyl-2,3-dihydro-1<i>H</i>-1,4-diazepin-4-ium picrate
;
_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                 110.611(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2341(3)
_cell_length_b                   27.6458(6)
_cell_length_c                   8.2831(3)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      34.6885
_cell_measurement_theta_min      4.6914
_cell_volume                     1550.52(10)
_computing_cell_refinement
'<i>CrysAlis RED</i> (Oxford Diffraction, 2007)'
_computing_data_collection
'<i>CrysAlis Pro</i> (Oxford Diffraction, 2007)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2007)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELXTL</i> (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f and \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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24773
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.77
_diffrn_reflns_theta_min         4.70
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.3582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                4493
_reflns_number_total             6353
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2536.cif
_cod_data_source_block           I
_cod_original_cell_volume        1550.52(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225907
_cod_database_fobs_code          2225907