Hydrogen-bonded networks in crystals of 1-(diaminomethylene)thiouron-1-ium perchlorate, hydrogen sulfate, dihydrogen phosphate and dihydrogen arsenate
Janczak, Jan; Perpétuo, Genivaldo Julio; Acta Crystallographica Section C 64 (2008) o330–o334; doi:10.1107/S0108270108013504

data_2016633
_publ_section_title
;
 Hydrogen-bonded networks in crystals of
 1-(diaminomethylene)thiouron-1-ium perchlorate, hydrogen sulfate,
 dihydrogen phosphate and dihydrogen arsenate
;
_journal_coeditor_code           GA3088
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o330
_journal_page_last               o334
_journal_paper_doi               10.1107/S0108270108013504
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C2 H7 N4 S +, Cl O4 -'
_chemical_formula_moiety         'C2 H7 N4 S +, Cl O4 -'
_chemical_formula_sum            'C2 H7 Cl N4 O4 S'
_chemical_formula_weight         218.63
_chemical_name_systematic
;
1-(diaminomethylene)thiouron-1-ium perchlorate
;
_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                109.15(2)
_cell_angle_beta                 91.441(10)
_cell_angle_gamma                104.639(11)
_cell_formula_units_Z            2
_cell_length_a                   5.8011(9)
_cell_length_b                   8.4511(14)
_cell_length_c                   9.430(2)
_cell_measurement_reflns_used    1038
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      3.66
_cell_volume                     419.59(14)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction Poland, 2005)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction Poland, 2005)
;
_computing_data_reduction
;
CrysAlis Red (Oxford Diffraction Poland, 2005)
;
_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 0.938
_diffrn_measurement_device_type
'Kuma KM-4 diffractometer with CCD area 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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5108
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.7846
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(face-indexed; SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      1.73
_exptl_crystal_density_method    flotation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.348
_refine_ls_extinction_coef       0.017(5)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                1516
_reflns_number_total             2110
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3088.cif
_cod_data_source_block           Ia
_cod_original_cell_volume        419.59(15)
_cod_database_code               2016633
_cod_database_fobs_code          2016633