2,3,4,6,7,8,9,10-Octahydropyrimido[1,2-<i>a</i>]azepin-1-ium 2-cyano-1-(2,6-dimethylanilino)-2-(phenylsulfonyl)ethenethiolate
Svetlana V. Shishkina; Oleg V. Shishkin; Yuriy D. Vlasenko; Oleksiy O. Parkhomenko; Sergey M. Kovalenko; Acta Crystallographica Section E 64 (2008) o255–o255; doi:10.1107/S1600536807065518

data_2216885
_publ_section_title
;
 2,3,4,6,7,8,9,10-Octahydropyrimido[1,2-<i>a</i>]azepin-1-ium
 2-cyano-1-(2,6-dimethylanilino)-2-(phenylsulfonyl)ethenethiolate
;
_journal_coeditor_code           AV2006
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o255
_journal_page_last               o255
_journal_paper_doi               10.1107/S1600536807065518
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C9 H17 N2 +, C17 H15 N2 O2 S2 -'
_chemical_formula_moiety         'C9 H17 N2 +, C17 H15 N2 O2 S2 -'
_chemical_formula_sum            'C26 H32 N4 O2 S2'
_chemical_formula_weight         496.68
_chemical_name_systematic
;
2,3,4,6,7,8,9,10-Octahydropyrimido[1,2-<i>a</i>]azepin-1-ium
2-cyano-1-(2,6-dimethylanilino)-2-(phenylsulfonyl)ethenethiolate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.03(2)
_cell_angle_beta                 92.517(9)
_cell_angle_gamma                90.635(12)
_cell_formula_units_Z            2
_cell_length_a                   8.3278(5)
_cell_length_b                   11.348(4)
_cell_length_c                   13.661(3)
_cell_measurement_reflns_used    9472
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      2.8
_cell_volume                     1251.0(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'XP (Siemens, 1998)'
_computing_publication_material  'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11732
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0430P)^2^+0.3755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3564
_reflns_number_total             4319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            av2006.cif
_cod_data_source_block           I
_cod_original_cell_volume        1250.9(5)
_cod_database_code               2216885
_cod_database_fobs_code          2216885