#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:36:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179756 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/52/7005224.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_7005224
loop_
_publ_author_name
'Tyrra, Wieland'
'Naumann, Dieter'
'Buslei, Sigrid'
'Kremer, Silke'
'Pantenburg, Ingo'
'Scherer, Harald'
_publ_section_title
;
 Perfluoroalkyl(dithiocarbamato) tellurium(II) compounds.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1829
_journal_page_last               1837
_journal_paper_doi               10.1039/b618240b
_journal_year                    2007
_chemical_formula_moiety         'C60 H56 N4 S8 Te'
_chemical_formula_sum            'C60 H56 N4 S8 Te'
_chemical_formula_weight         1217.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4060(15)
_cell_length_b                   15.4060(15)
_cell_length_c                   12.1612(15)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.64
_cell_volume                     2886.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'IPDS I (Stoe & Cie)'
_diffrn_measurement_method       'φ 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  0.1002
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32889
_diffrn_reflns_theta_full        28.12
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.9051
_exptl_absorpt_correction_T_min  0.7781
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001)
was performed after optimizing the crystal shape
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            yollow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0436
_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/[σ²(Fo²)+(0.0366P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                2203
_reflns_number_total             3484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618240b.txt
_cod_data_source_block           ipwt103
_cod_database_code               7005224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y, x, -z'
'y, -x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 1.0000 0.0000 1.0000 0.04460(15) Uani 1 4 d S . .
S11 S 0.96141(8) 0.09594(8) 1.18483(11) 0.0564(3) Uani 1 1 d . . .
S12 S 0.92945(9) 0.15886(8) 0.95927(11) 0.0576(3) Uani 1 1 d . . .
C1 C 0.9348(3) 0.1787(3) 1.0978(4) 0.0486(11) Uani 1 1 d . . .
N1 N 0.9210(3) 0.2596(2) 1.1384(3) 0.0523(10) Uani 1 1 d . . .
C11 C 0.9329(4) 0.2790(3) 1.2550(5) 0.0601(14) Uani 1 1 d . . .
H11A H 0.9259 0.2261 1.2972 0.073(8) Uiso 1 1 calc R . .
H11B H 0.8882 0.3195 1.2783 0.073(8) Uiso 1 1 calc R . .
C12 C 1.0213(3) 0.3178(3) 1.2794(5) 0.0628(15) Uani 1 1 d . . .
C13 C 1.0312(5) 0.3725(5) 1.3681(7) 0.130(4) Uani 1 1 d . . .
H13 H 0.9830 0.3885 1.4094 0.139(9) Uiso 1 1 calc R . .
C14 C 1.1131(6) 0.4040(6) 1.3964(10) 0.157(4) Uani 1 1 d . . .
H14 H 1.1184 0.4394 1.4580 0.139(9) Uiso 1 1 calc R . .
C15 C 1.1837(5) 0.3853(5) 1.3383(8) 0.102(3) Uani 1 1 d . . .
H15 H 1.2374 0.4094 1.3557 0.139(9) Uiso 1 1 calc R . .
C16 C 1.1745(5) 0.3302(5) 1.2535(7) 0.0917(18) Uani 1 1 d . . .
H16 H 1.2233 0.3144 1.2133 0.139(9) Uiso 1 1 calc R . .
C17 C 1.0953(4) 0.2964(4) 1.2242(6) 0.082(2) Uani 1 1 d . . .
H17 H 1.0921 0.2580 1.1654 0.139(9) Uiso 1 1 calc R . .
C21 C 0.8987(3) 0.3333(3) 1.0680(5) 0.0610(14) Uani 1 1 d . . .
H21A H 0.9135 0.3192 0.9925 0.073(8) Uiso 1 1 calc R . .
H21B H 0.9332 0.3831 1.0897 0.073(8) Uiso 1 1 calc R . .
C22 C 0.8040(4) 0.3572(3) 1.0737(5) 0.0644(15) Uani 1 1 d . . .
C23 C 0.7436(4) 0.3108(4) 1.0150(7) 0.0807(18) Uani 1 1 d . . .
H23 H 0.7615 0.2642 0.9719 0.139(9) Uiso 1 1 calc R . .
C24 C 0.6567(4) 0.3323(5) 1.0192(8) 0.102(2) Uani 1 1 d . . .
H24 H 0.6168 0.3010 0.9777 0.139(9) Uiso 1 1 calc R . .
C25 C 0.6290(6) 0.3993(6) 1.0839(7) 0.116(3) Uani 1 1 d . . .
H25 H 0.5703 0.4133 1.0877 0.139(9) Uiso 1 1 calc R . .
C26 C 0.6888(6) 0.4457(6) 1.1432(7) 0.114(3) Uani 1 1 d . . .
H26 H 0.6703 0.4912 1.1876 0.139(9) Uiso 1 1 calc R . .
C27 C 0.7753(5) 0.4260(4) 1.1380(6) 0.093(2) Uani 1 1 d . . .
H27 H 0.8151 0.4588 1.1777 0.139(9) Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
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
_geom_angle_publ_flag
S12 Te1 S12 91.896(10) 2_755 8_667 ?
S12 Te1 S12 91.896(10) 2_755 7_647 ?
S12 Te1 S12 159.04(6) 8_667 7_647 ?
S12 Te1 S12 159.04(6) 2_755 . ?
S12 Te1 S12 91.896(10) 8_667 . ?
S12 Te1 S12 91.896(10) 7_647 . ?
S12 Te1 S11 82.63(4) 2_755 7_647 ?
S12 Te1 S11 135.78(4) 8_667 7_647 ?
S12 Te1 S11 65.17(4) 7_647 7_647 ?
S12 Te1 S11 80.29(4) . 7_647 ?
S12 Te1 S11 135.78(4) 2_755 . ?
S12 Te1 S11 80.29(4) 8_667 . ?
S12 Te1 S11 82.63(4) 7_647 . ?
S12 Te1 S11 65.17(4) . . ?
S11 Te1 S11 131.73(3) 7_647 . ?
S12 Te1 S11 80.29(4) 2_755 8_667 ?
S12 Te1 S11 65.17(4) 8_667 8_667 ?
S12 Te1 S11 135.78(4) 7_647 8_667 ?
S12 Te1 S11 82.63(4) . 8_667 ?
S11 Te1 S11 70.66(6) 7_647 8_667 ?
S11 Te1 S11 131.73(4) . 8_667 ?
S12 Te1 S11 65.17(4) 2_755 2_755 ?
S12 Te1 S11 82.63(4) 8_667 2_755 ?
S12 Te1 S11 80.29(4) 7_647 2_755 ?
S12 Te1 S11 135.78(4) . 2_755 ?
S11 Te1 S11 131.73(4) 7_647 2_755 ?
S11 Te1 S11 70.66(6) . 2_755 ?
S11 Te1 S11 131.73(3) 8_667 2_755 ?
C1 S11 Te1 86.96(17) . . ?
C1 S12 Te1 87.87(17) . . ?
N1 C1 S11 119.9(4) . . ?
N1 C1 S12 121.0(4) . . ?
S11 C1 S12 119.1(3) . . ?
C1 N1 C11 121.5(4) . . ?
C1 N1 C21 122.4(4) . . ?
C11 N1 C21 116.0(4) . . ?
N1 C11 C12 112.5(4) . . ?
N1 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N1 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C17 C12 C13 116.2(6) . . ?
C17 C12 C11 124.1(5) . . ?
C13 C12 C11 119.5(5) . . ?
C12 C13 C14 120.4(7) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 122.3(8) . . ?
C15 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C14 C15 C16 117.3(7) . . ?
C14 C15 H15 121.4 . . ?
C16 C15 H15 121.4 . . ?
C15 C16 C17 122.2(7) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C12 C17 C16 121.5(7) . . ?
C12 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
N1 C21 C22 113.0(4) . . ?
N1 C21 H21A 109.0 . . ?
C22 C21 H21A 109.0 . . ?
N1 C21 H21B 109.0 . . ?
C22 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C23 C22 C27 118.3(6) . . ?
C23 C22 C21 120.3(5) . . ?
C27 C22 C21 121.3(6) . . ?
C22 C23 C24 120.9(7) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 120.4(9) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 119.1(8) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 121.0(8) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C22 120.3(7) . . ?
C26 C27 H27 119.8 . . ?
C22 C27 H27 119.8 . . ?
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
Te1 S12 2.7232(12) 2_755 ?
Te1 S12 2.7232(12) 8_667 ?
Te1 S12 2.7232(12) 7_647 ?
Te1 S12 2.7232(12) . ?
Te1 S11 2.7551(13) 7_647 ?
Te1 S11 2.7551(13) . ?
Te1 S11 2.7551(13) 8_667 ?
Te1 S11 2.7551(13) 2_755 ?
S11 C1 1.708(5) . ?
S12 C1 1.714(5) . ?
C1 N1 1.356(6) . ?
N1 C11 1.460(7) . ?
N1 C21 1.463(6) . ?
C11 C12 1.517(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C17 1.363(8) . ?
C12 C13 1.378(8) . ?
C13 C14 1.395(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.329(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.343(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.373(10) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C21 C22 1.506(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.373(8) . ?
C22 C27 1.390(8) . ?
C23 C24 1.380(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.368(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.370(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.368(10) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
