The chloride, bromide and iodide salts of 1-(diaminomethylene)thiouron-1-ium
Perpétuo, Genivaldo Júlio; Janczak, Jan; Acta Crystallographica Section C 64 (2008) o264–o268; doi:10.1107/S0108270108008688

data_2016607
_publ_section_title
;
 The chloride, bromide and iodide salts of
 1-(diaminomethylene)thiouron-1-ium
;
_journal_coeditor_code           SK3208
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o264
_journal_page_last               o268
_journal_paper_doi               10.1107/S0108270108008688
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C2 H7 N4 S +, Br -'
_chemical_formula_moiety         'C2 H7 N4 S +, Br -'
_chemical_formula_sum            'C2 H7 Br N4 S'
_chemical_formula_weight         199.09
_chemical_name_systematic
;
1-(diaminomethylene)thiouron-1-ium bromide
;
_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                94.220(14)
_cell_angle_beta                 90.091(11)
_cell_angle_gamma                104.012(15)
_cell_formula_units_Z            2
_cell_length_a                   4.9661(9)
_cell_length_b                   7.4841(17)
_cell_length_c                   9.5739(19)
_cell_measurement_reflns_used    827
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.36
_cell_measurement_theta_min      3.40
_cell_volume                     344.24(12)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis Red (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Kuma KM-4 with area CCD detector'
_diffrn_measurement_method       \w-scan
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4034
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    6.181
_exptl_absorpt_correction_T_max  0.4414
_exptl_absorpt_correction_T_min  0.2441
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(face-indexed; SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      1.92
_exptl_crystal_density_method    flotation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             196
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.509
_refine_ls_extinction_coef       0.079(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                1295
_reflns_number_total             1737
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3208.cif
_cod_data_source_block           Ib
_cod_original_cell_volume        344.23(12)
_cod_database_code               2016607
_cod_database_fobs_code          2016607