#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:55:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179906 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/02/7020208.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_7020208
loop_
_publ_author_name
'Hector, Andrew L.'
'Jolleys, Andrew'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 TeX4 (X = F, Cl, Br) as Lewis acids--complexes with soft thio- and
 seleno-ether ligands.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10988
_journal_page_last               10999
_journal_paper_doi               10.1039/c2dt30968h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C5 H12 Cl4 S2 Te'
_chemical_formula_sum            'C5 H12 Cl4 S2 Te'
_chemical_formula_weight         405.67
_chemical_name_systematic
;
tetrachloro(1,3-Bis(methylsulfanyl)propane-S,S')tellurium(IV)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-30
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.881(3)
_cell_length_b                   9.881(3)
_cell_length_c                   26.388(8)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      2.9
_cell_volume                     2576.4(14)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12'
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, HF VariMax'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            12362
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ SuperBright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.416
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R.A. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+19.5788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                1575
_reflns_number_total             1596
_reflns_threshold_expression     I>σ(I)
_cod_data_source_file            c2dt30968h.txt
_cod_data_source_block           11aj0108
_cod_database_code               7020208
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-y+3/4, x+1/4, z+1/4'
4 'y+3/4, -x+3/4, z+3/4'
5 'x+1/2, y+1/2, z+1/2'
6 '-x+1, -y+1/2, z+1'
7 '-y+5/4, x+3/4, z+3/4'
8 'y+5/4, -x+5/4, z+5/4'
9 '-x, -y, -z'
10 'x-1/2, y, -z-1/2'
11 'y-3/4, -x-1/4, -z-1/4'
12 '-y-3/4, x-3/4, -z-3/4'
13 '-x+1/2, -y+1/2, -z+1/2'
14 'x, y+1/2, -z'
15 'y-1/4, -x+1/4, -z+1/4'
16 '-y-1/4, x-1/4, -z-1/4'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Te1 Te 0.5000 0.2500 0.622475(16) 0.01375(11) Uani 1 2 d S
Cl1 Cl 0.57617(15) 0.08777(15) 0.55938(5) 0.0218(3) Uani 1 1 d .
Cl2 Cl 0.72479(14) 0.36620(15) 0.62623(5) 0.0210(3) Uani 1 1 d .
S1 S 0.59825(14) 0.08623(14) 0.70421(5) 0.0170(3) Uani 1 1 d .
C1 C 0.5000 0.2500 0.7809(2) 0.0215(14) Uani 1 2 d S
H1A H 0.5780 0.2293 0.8031 0.026 Uiso 0.50 1 calc PR
H1B H 0.4220 0.2707 0.8031 0.026 Uiso 0.50 1 calc PR
C2 C 0.4666(5) 0.1237(5) 0.7505(2) 0.0200(12) Uani 1 1 d .
H2A H 0.3793 0.1369 0.7328 0.024 Uiso 1 1 calc R
H2B H 0.4565 0.0460 0.7739 0.024 Uiso 1 1 calc R
C3 C 0.5422(6) -0.0785(5) 0.6844(2) 0.0200(12) Uani 1 1 d .
H3A H 0.5506 -0.1422 0.7126 0.030 Uiso 1 1 calc R
H3B H 0.5981 -0.1096 0.6560 0.030 Uiso 1 1 calc R
H3C H 0.4474 -0.0735 0.6736 0.030 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te1 0.0148(2) 0.0153(2) 0.01112(18) 0.000 0.000 0.0001(2)
Cl1 0.0281(8) 0.0190(7) 0.0184(6) -0.0026(5) 0.0064(5) 0.0008(6)
Cl2 0.0170(6) 0.0245(7) 0.0214(6) -0.0014(6) 0.0002(5) -0.0028(6)
S1 0.0152(6) 0.0189(7) 0.0168(6) 0.0005(5) 0.0002(5) 0.0026(6)
C1 0.026(4) 0.025(4) 0.013(3) 0.000 0.000 0.004(4)
C2 0.023(3) 0.022(3) 0.015(2) 0.004(2) 0.005(2) 0.005(2)
C3 0.023(3) 0.012(3) 0.025(3) 0.002(2) -0.002(2) 0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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
Cl1 Te1 Cl1 93.53(7) 6_554 .
Cl1 Te1 Cl2 89.96(5) 6_554 .
Cl1 Te1 Cl2 93.15(5) . .
Cl1 Te1 Cl2 93.15(5) 6_554 6_554
Cl1 Te1 Cl2 89.96(5) . 6_554
Cl2 Te1 Cl2 175.46(6) . 6_554
Cl1 Te1 S1 173.12(5) 6_554 .
Cl1 Te1 S1 92.19(5) . .
Cl2 Te1 S1 85.90(4) . .
Cl2 Te1 S1 90.68(4) 6_554 .
Cl1 Te1 S1 92.19(5) 6_554 6_554
Cl1 Te1 S1 173.12(5) . 6_554
Cl2 Te1 S1 90.68(4) . 6_554
Cl2 Te1 S1 85.90(4) 6_554 6_554
S1 Te1 S1 82.37(6) . 6_554
C3 S1 C2 99.2(3) . .
C3 S1 Te1 100.81(18) . .
C2 S1 Te1 98.52(18) . .
C2 C1 C2 116.3(6) . 6_554
C2 C1 H1A 108.2 . .
C2 C1 H1A 108.2 6_554 .
C2 C1 H1B 108.2 . .
C2 C1 H1B 108.2 6_554 .
H1A C1 H1B 107.4 . .
C1 C2 S1 111.4(3) . .
C1 C2 H2A 109.3 . .
S1 C2 H2A 109.3 . .
C1 C2 H2B 109.3 . .
S1 C2 H2B 109.3 . .
H2A C2 H2B 108.0 . .
S1 C3 H3A 109.5 . .
S1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
S1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 Cl1 2.4307(15) 6_554
Te1 Cl1 2.4307(15) .
Te1 Cl2 2.5023(16) .
Te1 Cl2 2.5023(16) 6_554
Te1 S1 2.8658(15) .
Te1 S1 2.8658(15) 6_554
S1 C3 1.798(6) .
S1 C2 1.824(5) .
C1 C2 1.519(6) .
C1 C2 1.519(6) 6_554
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Cl1 Te1 S1 C3 -43.8(2) .
Cl2 Te1 S1 C3 -136.78(19) .
Cl2 Te1 S1 C3 46.2(2) 6_554
S1 Te1 S1 C3 132.0(2) 6_554
Cl1 Te1 S1 C2 -144.91(18) .
Cl2 Te1 S1 C2 122.09(18) .
Cl2 Te1 S1 C2 -54.92(18) 6_554
S1 Te1 S1 C2 30.86(18) 6_554
C2 C1 C2 S1 52.8(2) 6_554
C3 S1 C2 C1 170.4(4) .
Te1 S1 C2 C1 -87.1(3) .
