First Tin Pnictide Halides Sn24P19.3I8 and Sn24As19.3I8: Synthesis and the Clathrate-I Type of the Crystal Structure
Mikhail M. Shatruk; Kirill A. Kovnir; Andrei V. Shevelkov; Igor A. Presniakov; Boris A. Popovkin; Inorganic Chemistry 38 (1999) 3455–3457; doi:10.1021/ic990153r

data_4322165
_publ_section_title
;
 First Tin Pnictide Halides Sn24P19.3I8 and Sn24As19.3I8: Synthesis and
 the Clathrate-I Type of the Crystal Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3455
_journal_page_last               3457
_journal_paper_doi               10.1021/ic990153r
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source
;
 prepared from tin, red phosphorus and tin(IV) iodide 
;
_chemical_formula_analytical     'Sn24 P19.29 I8'
_chemical_formula_moiety         '(Sn24 P19.29), 8 I'
_chemical_formula_structural     '(Sn24 P19.29) I8'
_chemical_formula_sum            'I8 P19.29 Sn24'
_chemical_formula_weight         4461.17
_chemical_melting_point          ?
_chemical_name_common            'tin(II) phosphide iodide'
_chemical_name_systematic        'tin(II) phosphide iodide'
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.9540(10)
_cell_length_b                   10.9540(10)
_cell_length_c                   10.9540(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.64
_cell_measurement_theta_min      13.62
_cell_volume                     1314.4(2)
_computing_cell_refinement       'CAD4 (Nonius)'
_computing_data_collection       'CAD4 (Nonius)'
_computing_data_reduction        'SDP (Nonius)'
_computing_molecular_graphics    'SHELXL-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4F'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1546
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    16.463
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9602
_exptl_absorpt_correction_type   'semiempirical via \y scans'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       cubooctahedron
_exptl_crystal_F_000             1913
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.0031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.266
_refine_ls_goodness_of_fit_obs   1.275
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.266
_refine_ls_restrained_S_obs      1.275
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.7116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0540
_refine_ls_wR_factor_obs         0.0540
_reflns_number_observed          287
_reflns_number_total             291
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990153r.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.7116P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.7116P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322165