Stabilization of poly-iodides: structural influences of the cationic disulfides of 2-mercapto-3,4,5,6-tetrahydro-pyrimidine and 2-mercatpo-pyrimidine
Owczarzak, Anita M.; Kubicki, Maciej; Kourkoumelis, Nikolaos; Hadjikakou, Sotiris K.; RSC Advances 2 (2012) 2856–; doi:10.1039/c2ra00013j

data_7238550
_publ_section_title
;
 Stabilization of poly-iodides: structural influences of the cationic
 disulfides of 2-mercapto-3,4,5,6-tetrahydro-pyrimidine and
 2-mercatpo-pyrimidine
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              2856
_journal_paper_doi               10.1039/c2ra00013j
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C4 H5 I2 N2 S'
_chemical_formula_weight         366.96
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-12-18 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.79(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2469(2)
_cell_length_b                   11.3129(2)
_cell_length_c                   10.3137(2)
_cell_measurement_reflns_used    19897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9195
_cell_measurement_theta_min      3.1401
_cell_volume                     921.21(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0108
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26655
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    6.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0160P)^2^+1.0236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0421
_reflns_number_gt                1922
_reflns_number_total             2120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra00013j.txt
_cod_data_source_block           shelxld
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7238550