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_7238552
_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            'C16 H32 Cl I9 N8 S4'
_chemical_formula_weight         1642.29
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.59(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.502(2)
_cell_length_b                   12.310(2)
_cell_length_c                   12.354(2)
_cell_measurement_reflns_used    3487
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9555
_cell_measurement_theta_min      2.4827
_cell_volume                     2050.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Eos'
_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  0.0627
_diffrn_reflns_av_sigmaI/netI    0.1860
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14097
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    7.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0014P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                2441
_reflns_number_total             4792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra00013j.txt
_cod_data_source_block           shelxlb
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7238552