Redetermination of the structure of α-tetraphosphorus trisulfide diiodide at 180 K
Tattershall, B. W.; Kendall, N. L.; McCamley, A.; Clegg, W.; Acta Crystallographica Section C 49 (1993) 571–573; doi:10.1107/S0108270192011466

data_2001900
_publ_section_title
;
 Redetermination of the structure of \a-tetraphosphorus trisulfide
 diiodide at 180 K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              571
_journal_page_last               573
_journal_paper_doi               10.1107/S0108270192011466
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'I2 P4 S3'
_chemical_formula_weight         473.86
_chemical_name_systematic
;
2,5-diiodo-1,2,4,5-tetraphospha-3,6,7-trithiabicyclo[2.2.1]heptane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                94.43(6)
_cell_angle_beta                 90.31(6)
_cell_angle_gamma                90.90(6)
_cell_formula_units_Z            4
_cell_length_a                   7.268(4)
_cell_length_b                   7.342(4)
_cell_length_c                   19.553(11)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    180.0(5)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      11.46
_cell_volume                     1040.1(10)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-92 '
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      180.0(5)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method
'\w/\q scans, on-line profile fitting  (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3646
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    7.190
_exptl_absorpt_correction_T_max  0.048
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.026
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.58
_refine_diff_density_min         -1.41
_refine_ls_extinction_coef       0.0116(6)
_refine_ls_extinction_method     'SHELXL92 (Sheldrick, 1992)'
_refine_ls_goodness_of_fit_all   1.238
_refine_ls_goodness_of_fit_obs   1.238
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_restrained_S_obs      1.238
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_obs          0.0403
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;  calc w = 1/[\s^2^(F~o~^2^)+(0.0553P)^2^+4.9236P]
     where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1114
_refine_ls_wR_factor_obs         0.1112
_reflns_number_observed          3523
_reflns_number_total             3646
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            mu1018.cif
_cod_data_source_block           bwt3
_cod_original_formula_sum        'P4 S3 I2'
_cod_database_code               2001900