3-(2-Chloroethyl)-2-methyl-4-oxo-4<i>H</i>-pyrido[1,2-<i>a</i>]pyrimidinium 2,4,6-trinitrophenolate
Jasinski, Jerry P.; Butcher, Ray J.; Hakim Al-Arique, Q. N. M.; Yathirajan, H. S.; Narayana, B.; Acta Crystallographica Section E 65 (2009) o2201–o2202; doi:10.1107/S1600536809032693

data_2223131
_publ_section_title
;
 3-(2-Chloroethyl)-2-methyl-4-oxo-4<i>H</i>-pyrido[1,2-<i>a</i>]pyrimidinium
 2,4,6-trinitrophenolate
;
_journal_coeditor_code           IS2446
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2201
_journal_page_last               o2202
_journal_paper_doi               10.1107/S1600536809032693
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H12 Cl N2 O +, C6 H2 N3 O7 -'
_chemical_formula_moiety         'C11 H12 Cl N2 O +, C6 H2 N3 O7 -'
_chemical_formula_sum            'C17 H14 Cl N5 O8'
_chemical_formula_weight         451.78
_chemical_name_common
;
3-(2-Chloroethyl)-2-methyl-4<i>H</i>-pyrido[1,2-<i>a</i>] pyrimidinium-4-one
picrate
;
_chemical_name_systematic
;
3-(2-Chloroethyl)-2-methyl-4-oxo-4<i>H</i>-pyrido[1,2-<i>a</i>]pyrimidinium
2,4,6-trinitrophenolate
;
_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                 97.642(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2718(5)
_cell_length_b                   12.8159(9)
_cell_length_c                   19.940(3)
_cell_measurement_reflns_used    4324
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      74.1343
_cell_measurement_theta_min      4.1062
_cell_volume                     1841.8(3)
_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)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with a Ruby (Gemini Cu) detector
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6948
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.04
_diffrn_reflns_theta_min         4.11
_diffrn_standards_decay_%        <2%
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.575
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(<i>CrysAlis RED</i>; Oxford Diffraction, 2007)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max_lt       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^)+(0.063P)^2^+0.629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3198
_reflns_number_total             3616
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2446.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2223131
_cod_database_fobs_code          2223131