#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:46:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179204 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/38/4313826.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313826
loop_
_publ_author_name
'Mark D. Smith'
'Gordon J. Miller'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0257P)²+11.5120P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ta1 Ta 0.7500 0.8568(3) 0.68160(13) 0.0116(4) Uani 0.510(4) d SP .
Ta2 Ta 0.60860(7) 0.2500 0.87665(14) 0.0127(4) Uani 0.517(4) d SP .
I1 I 0.58153(6) 0.7500 0.63999(13) 0.0181(3) Uani 1 d S .
I2 I 0.7500 0.2500 0.4229(2) 0.0282(5) Uani 1 d S .
I3 I 0.58430(7) 0.7500 0.12070(13) 0.0234(3) Uani 1 d S .
I4 I 0.2500 0.7500 0.1050(4) 0.0127(11) Uani 0.534(9) d SP .
S S 0.2500 0.7500 -0.9311(32) 0.0127(11) Uani 0.466(9) d SP .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ta1 Ta1 I4 130.83(6) 2_665 5_676 ?
Ta1 Ta1 S 126.5(4) 2_665 5_675 ?
I4 Ta1 S 4.4(4) 5_676 5_675 ?
Ta1 Ta1 I2 125.48(4) 2_665 1_565 ?
I4 Ta1 I2 103.70(8) 5_676 1_565 ?
S Ta1 I2 108.1(4) 5_675 1_565 ?
Ta1 Ta1 I1 81.54(2) 2_665 . ?
I4 Ta1 I1 100.87(3) 5_676 . ?
S Ta1 I1 100.70(3) 5_675 . ?
I2 Ta1 I1 89.19(3) 1_565 . ?
Ta1 Ta1 I1 81.54(2) 2_665 2_665 ?
I4 Ta1 I1 100.87(3) 5_676 2_665 ?
S Ta1 I1 100.70(3) 5_675 2_665 ?
I2 Ta1 I1 89.19(3) 1_565 2_665 ?
I1 Ta1 I1 157.95(5) . 2_665 ?
Ta1 Ta1 I4 36.86(6) 2_665 5_666 ?
I4 Ta1 I4 93.97(11) 5_676 5_666 ?
S Ta1 I4 89.6(3) 5_675 5_666 ?
I2 Ta1 I4 162.34(7) 1_565 5_666 ?
I1 Ta1 I4 87.46(3) . 5_666 ?
I1 Ta1 I4 87.46(3) 2_665 5_666 ?
Ta1 Ta1 Ta1 180.0(2) 2_665 2_675 ?
I4 Ta1 Ta1 49.17(6) 5_676 2_675 ?
S Ta1 Ta1 53.5(4) 5_675 2_675 ?
I2 Ta1 Ta1 54.53(4) 1_565 2_675 ?
I1 Ta1 Ta1 98.46(2) . 2_675 ?
I1 Ta1 Ta1 98.46(2) 2_665 2_675 ?
I4 Ta1 Ta1 143.14(6) 5_666 2_675 ?
Ta1 Ta1 I2 42.28(4) 2_665 . ?
I4 Ta1 I2 173.11(8) 5_676 . ?
S Ta1 I2 168.7(4) 5_675 . ?
I2 Ta1 I2 83.20(6) 1_565 . ?
I1 Ta1 I2 78.99(3) . . ?
I1 Ta1 I2 78.99(3) 2_665 . ?
I4 Ta1 I2 79.14(7) 5_666 . ?
Ta1 Ta1 I2 137.72(4) 2_675 . ?
Ta1 Ta1 Ta2 118.35(2) 2_665 2_665 ?
I4 Ta1 Ta2 46.33(2) 5_676 2_665 ?
S Ta1 Ta2 46.67(5) 5_675 2_665 ?
I2 Ta1 Ta2 97.67(4) 1_565 2_665 ?
I1 Ta1 Ta2 147.20(4) . 2_665 ?
I1 Ta1 Ta2 54.68(3) 2_665 2_665 ?
I4 Ta1 Ta2 94.51(5) 5_666 2_665 ?
Ta1 Ta1 Ta2 61.65(2) 2_675 2_665 ?
I2 Ta1 Ta2 133.57(2) . 2_665 ?
Ta1 Ta1 Ta2 118.35(2) 2_665 1_565 ?
I4 Ta1 Ta2 46.33(2) 5_676 1_565 ?
S Ta1 Ta2 46.67(5) 5_675 1_565 ?
I2 Ta1 Ta2 97.67(4) 1_565 1_565 ?
I1 Ta1 Ta2 54.68(3) . 1_565 ?
I1 Ta1 Ta2 147.20(4) 2_665 1_565 ?
I4 Ta1 Ta2 94.51(5) 5_666 1_565 ?
Ta1 Ta1 Ta2 61.65(2) 2_675 1_565 ?
I2 Ta1 Ta2 133.57(2) . 1_565 ?
Ta2 Ta1 Ta2 92.55(5) 2_665 1_565 ?
I4 Ta2 S 7.2(7) 5_666 5_665 ?
I4 Ta2 I1 101.80(7) 5_666 1_545 ?
S Ta2 I1 106.8(4) 5_665 1_545 ?
I4 Ta2 I1 101.80(7) 5_666 . ?
S Ta2 I1 106.8(4) 5_665 . ?
I1 Ta2 I1 88.03(5) 1_545 . ?
I4 Ta2 I3 95.41(7) 5_666 1_556 ?
S Ta2 I3 90.1(5) 5_665 1_556 ?
I1 Ta2 I3 162.71(5) 1_545 1_556 ?
I1 Ta2 I3 90.09(3) . 1_556 ?
I4 Ta2 I3 95.41(7) 5_666 1_546 ?
S Ta2 I3 90.1(5) 5_665 1_546 ?
I1 Ta2 I3 90.09(3) 1_545 1_546 ?
I1 Ta2 I3 162.71(5) . 1_546 ?
I3 Ta2 I3 86.61(5) 1_556 1_546 ?
I4 Ta2 I3 175.86(10) 5_666 5_666 ?
S Ta2 I3 168.6(6) 5_665 5_666 ?
I1 Ta2 I3 81.12(4) 1_545 5_666 ?
I1 Ta2 I3 81.12(4) . 5_666 ?
I3 Ta2 I3 81.60(4) 1_556 5_666 ?
I3 Ta2 I3 81.60(4) 1_546 5_666 ?
I4 Ta2 Ta1 46.50(7) 5_666 2_665 ?
S Ta2 Ta1 52.1(5) 5_665 2_665 ?
I1 Ta2 Ta1 95.32(5) 1_545 2_665 ?
I1 Ta2 Ta1 55.45(3) . 2_665 ?
I3 Ta2 Ta1 97.75(3) 1_556 2_665 ?
I3 Ta2 Ta1 141.83(5) 1_546 2_665 ?
I3 Ta2 Ta1 136.56(4) 5_666 2_665 ?
I4 Ta2 Ta1 46.50(7) 5_666 1_545 ?
S Ta2 Ta1 52.1(5) 5_665 1_545 ?
I1 Ta2 Ta1 55.45(3) 1_545 1_545 ?
I1 Ta2 Ta1 95.32(5) . 1_545 ?
I3 Ta2 Ta1 141.83(5) 1_556 1_545 ?
I3 Ta2 Ta1 97.75(3) 1_546 1_545 ?
I3 Ta2 Ta1 136.56(4) 5_666 1_545 ?
Ta1 Ta2 Ta1 56.70(5) 2_665 1_545 ?
Ta2 I1 Ta2 88.03(5) 1_565 . ?
Ta2 I1 Ta1 69.87(4) 1_565 . ?
Ta2 I1 Ta1 81.97(4) . . ?
Ta2 I1 Ta1 81.97(4) 1_565 2_665 ?
Ta2 I1 Ta1 69.87(4) . 2_665 ?
Ta1 I1 Ta1 16.92(5) . 2_665 ?
Ta1 I2 Ta1 70.95(7) 2_665 1_545 ?
Ta1 I2 Ta1 12.25(3) 2_665 . ?
Ta1 I2 Ta1 83.20(6) 1_545 . ?
Ta1 I2 Ta1 83.20(6) 2_665 2_655 ?
Ta1 I2 Ta1 12.25(3) 1_545 2_655 ?
Ta1 I2 Ta1 95.45(7) . 2_655 ?
Ta2 I3 Ta2 86.61(5) 1_554 1_564 ?
Ta2 I3 Ta2 98.39(4) 1_554 5_666 ?
Ta2 I3 Ta2 98.39(4) 1_564 5_666 ?
Ta2 I4 Ta2 172.5(2) 5_666 6_566 ?
Ta2 I4 Ta1 87.17(7) 5_666 5_676 ?
Ta2 I4 Ta1 87.17(7) 6_566 5_676 ?
Ta2 I4 Ta1 87.17(7) 5_666 6_556 ?
Ta2 I4 Ta1 87.17(7) 6_566 6_556 ?
Ta1 I4 Ta1 81.66(12) 5_676 6_556 ?
Ta2 I4 Ta1 87.76(6) 5_666 6_566 ?
Ta2 I4 Ta1 87.76(6) 6_566 6_566 ?
Ta1 I4 Ta1 12.31(4) 5_676 6_566 ?
Ta1 I4 Ta1 93.97(12) 6_556 6_566 ?
Ta2 I4 Ta1 87.76(6) 5_666 5_666 ?
Ta2 I4 Ta1 87.76(6) 6_566 5_666 ?
Ta1 I4 Ta1 93.97(12) 5_676 5_666 ?
Ta1 I4 Ta1 12.31(4) 6_556 5_666 ?
Ta1 I4 Ta1 106.28(12) 6_566 5_666 ?
Ta2 S Ta2 158.0(13) 5_665 6_565 ?
Ta2 S Ta1 81.2(6) 5_665 5_675 ?
Ta2 S Ta1 81.2(6) 6_565 5_675 ?
Ta2 S Ta1 81.2(6) 5_665 6 ?
Ta2 S Ta1 81.2(6) 6_565 6 ?
Ta1 S Ta1 72.9(7) 5_675 6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 Ta1 0.815(2) 2_665 ?
Ta1 I4 2.293(3) 5_676 ?
Ta1 S 2.52(2) 5_675 ?
Ta1 I2 2.583(2) 1_565 ?
Ta1 I1 2.7694(10) . ?
Ta1 I1 2.7694(10) 2_665 ?
Ta1 I4 2.892(2) 5_666 ?
Ta1 Ta1 2.998(2) 2_675 ?
Ta1 I2 3.127(2) . ?
Ta1 Ta2 3.1572(13) 2_665 ?
Ta1 Ta2 3.1572(13) 1_565 ?
Ta2 I4 2.2864(12) 5_666 ?
Ta2 S 2.324(5) 5_665 ?
Ta2 I1 2.7438(12) 1_545 ?
Ta2 I1 2.7438(12) . ?
Ta2 I3 2.7796(13) 1_556 ?
Ta2 I3 2.7796(13) 1_546 ?
Ta2 I3 3.112(2) 5_666 ?
Ta2 Ta1 3.1572(13) 2_665 ?
Ta2 Ta1 3.1572(13) 1_545 ?
I1 Ta2 2.7438(12) 1_565 ?
I1 Ta1 2.7694(10) 2_665 ?
I2 Ta1 2.583(2) 2_665 ?
I2 Ta1 2.583(2) 1_545 ?
I2 Ta1 3.127(2) 2_655 ?
I3 Ta2 2.7796(13) 1_554 ?
I3 Ta2 2.7796(13) 1_564 ?
I3 Ta2 3.112(2) 5_666 ?
I4 Ta2 2.2865(12) 5_666 ?
I4 Ta2 2.2865(12) 6_566 ?
I4 Ta1 2.293(3) 5_676 ?
I4 Ta1 2.293(3) 6_556 ?
I4 Ta1 2.892(2) 6_566 ?
I4 Ta1 2.892(2) 5_666 ?
S Ta2 2.324(5) 5_665 ?
S Ta2 2.324(5) 6_565 ?
S Ta1 2.52(2) 5_675 ?
S Ta1 2.52(2) 6 ?
