Two-dimensional hydrogen-bonded networks in 1-(diaminomethylene)thiouron-1-ium nitrate and bis[1-(diaminomethylene)thiouron-1-ium] phosphonate monohydrate
Janczak, Jan; Perpétuo, Genivaldo Julio; Acta Crystallographica Section C 65 (2009) o118–o120; doi:10.1107/S0108270109006325

data_2017002
_publ_section_title
;
 Two-dimensional hydrogen-bonded networks in
 1-(diaminomethylene)thiouron-1-ium nitrate and
 bis[1-(diaminomethylene)thiouron-1-ium] phosphonate monohydrate
;
_journal_coeditor_code           FG3078
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o118
_journal_page_last               o120
_journal_paper_doi               10.1107/S0108270109006325
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '2C2 H7 N4 S +, H P O3 2-, H2 O'
_chemical_formula_moiety         '2(C2 H7 N4 S +), H O3 P 2-, H2 O'
_chemical_formula_sum            'C4 H17 N8 O4 P S2'
_chemical_formula_weight         336.35
_chemical_name_systematic
;
bis[1-(diaminomethylene)thiouron-1-ium] phosphonate monohydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.700(16)
_cell_angle_beta                 72.961(15)
_cell_angle_gamma                85.842(14)
_cell_formula_units_Z            2
_cell_length_a                   7.6109(12)
_cell_length_b                   7.8771(14)
_cell_length_c                   12.758(2)
_cell_measurement_reflns_used    852
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.85
_cell_volume                     698.1(2)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis CCD (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 0.905
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8542
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.9231
_exptl_absorpt_correction_T_min  0.8502
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      1.594
_exptl_crystal_density_method    floatation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                1950
_reflns_number_total             3529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3078.cif
_cod_data_source_block           II
_cod_database_code               2017002
_cod_database_fobs_code          2017002