Unusually High Chemical Compressibility of Normally Rigid Type-I Clathrate Framework: Synthesis and Structural Study of Sn24P19.3BrxI8-x Solid Solution, the Prospective Thermoelectric Material
Kirill A. Kovnir; Julia V. Zaikina; Lyudmila N. Reshetova; Andrei V. Olenev; Evgeny V. Dikarev; Andrei V. Shevelkov; Inorganic Chemistry 43 (2004) 3230–3236; doi:10.1021/ic035097f

data_4310979
_publ_contact_author
;
        Andrei V. Shevelkov
        Inorganic Synthesis Laboratory
        Moscow State University
        Leninskie Gory 1/3
        119992 Moscow
        Russia
;
_publ_section_title
;
 Unusually High Chemical Compressibility of Normally Rigid Type-I
 Clathrate Framework: Synthesis and Structural Study of Sn24P19.3BrxI8-x
 Solid Solution, the Prospective Thermoelectric Material
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3230
_journal_page_last               3236
_journal_paper_doi               10.1021/ic035097f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(Sn24P19.6), (Br8)'
_chemical_formula_sum            'Br8 P19.6 Sn24'
_chemical_formula_weight         4094.85
_chemical_melting_point          ?
_chemical_name_systematic        'tin phosphide bromide'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.8108(2)
_cell_length_b                   10.8108(2)
_cell_length_c                   10.8108(2)
_cell_measurement_reflns_used    8964
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.67
_cell_volume                     1263.49(4)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0061
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9849
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    18.574
_exptl_absorpt_correction_T_max  0.4569
_exptl_absorpt_correction_T_min  0.2857
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1774
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       0.00148(16)
_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_ref   1.582
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.582
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+33.7296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                310
_reflns_number_total             310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035097fsi20030917_071526_06.cif
_cod_data_source_block           xl6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with
'_publ_contact_author'.

'_atom_site_symetry_multiplicity' tag
replaced with '_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1263.50(4)
_cod_original_formula_sum        'Br8 P19.60 Sn24'
_cod_database_code               4310979