Synthesis and Structure of Ta4SI11: Disorder and Mixed Valency in the First Tantalum Sulfide Iodide
Mark D. Smith; Gordon J. Miller; Inorganic Chemistry 42 (2003) 4165–4170; doi:10.1021/ic034075q

data_4313826
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
Iowa State University
Ames, IA 50011
USA
;
_publ_contact_author_email       gjmiller@iastate.edu
_publ_contact_author_fax         '1 515 294 0105'
_publ_contact_author_name        'Professor Gordon J. Miller'
_publ_contact_author_phone       '1 515 294 6063'
_publ_section_title
;
 Synthesis and Structure of Ta4SI11: Disorder and Mixed Valency in the
 First Tantalum Sulfide Iodide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4165
_journal_page_last               4170
_journal_paper_doi               10.1021/ic034075q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'I11 S Ta4'
_chemical_formula_weight         2151.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                   16.135(3)
_cell_length_b                   3.8130(10)
_cell_length_c                   8.131(2)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      3.0
_cell_volume                     500.2(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2theta-omega 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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2629
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    38.854
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    7.143
_exptl_crystal_description       needle
_exptl_crystal_F_000             891
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.148
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.374
_refine_ls_extinction_coef       0.00149(14)
_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   1.054
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_restrained_S_obs      1.098
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_obs          0.0322
_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^)+(0.0257P)^2^+11.5120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0762
_refine_ls_wR_factor_obs         0.0695
_reflns_number_observed          533
_reflns_number_total             685
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034075qsi20030123_023942.cif
_cod_data_source_block           mds5452
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

'_symmetry_cell_setting' value 'Orthorhombic'
changed to 'orthorhombic' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+11.5120P] 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^)+(0.0257P)^2^+11.5120P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P m m  n'
_cod_database_code               4313826