#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:48:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179264 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318446.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_4318446
loop_
_publ_author_name
'Holger Fleischer'
'Dieter Schollmeyer'
_publ_section_title
;
 Conformation versus Coordination: Synthesis and Structural Investigations
 of Tellurium(II) Dithiolates Derived from β-Donor-Substituted Thiols
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4739
_journal_page_last               4747
_journal_paper_doi               10.1021/ic020277v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C8 H14 O2 S4 Te'
_chemical_formula_weight         398.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.1470(3)
_cell_length_b                   8.6904(5)
_cell_length_c                   31.7950(18)
_cell_measurement_reflns_used    4139
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     1422.17(14)
_computing_cell_refinement       'Saint V6'
_computing_data_collection       'Smart V6'
_computing_data_reduction        'Saint V6'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       θ/φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            11721
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.659
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Mulabs Blessing'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.848
_refine_diff_density_min         -2.652
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0401
_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)+(0.0258P)²+5.2555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0817
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                1372
_reflns_number_total             1768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020277v_2.cif
_cod_data_source_block           2
_cod_database_code               4318446
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
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 0.02898(5) 0.2500 0.02336(13) Uani 1 2 d S . .
S2 S 1.2523(2) 0.20154(14) 0.20724(3) 0.0271(3) Uani 1 1 d . . .
C3 C 1.0165(10) 0.2751(5) 0.16950(14) 0.0269(9) Uani 1 1 d . . .
H3A H 0.8661 0.3180 0.1850 0.045(11) Uiso 1 1 calc R . .
H3B H 1.0969 0.3598 0.1533 0.045(11) Uiso 1 1 calc R . .
C4 C 0.9211(9) 0.1530(5) 0.13926(15) 0.0270(10) Uani 1 1 d . . .
H4A H 0.8572 0.0633 0.1554 0.035(10) Uiso 1 1 calc R . .
H4B H 1.0676 0.1181 0.1215 0.035(10) Uiso 1 1 calc R . .
S5 S 0.6629(2) 0.22457(16) 0.10594(4) 0.0323(3) Uani 1 1 d . . .
C6 C 0.8470(9) 0.3145(6) 0.06552(15) 0.0312(11) Uani 1 1 d . . .
C7 C 0.6850(10) 0.3891(7) 0.03258(15) 0.0380(13) Uani 1 1 d . . .
H7A H 0.5008 0.3747 0.0393 0.100(16) Uiso 1 1 calc R . .
H7B H 0.7229 0.3423 0.0052 0.100(16) Uiso 1 1 calc R . .
H7C H 0.7246 0.4993 0.0315 0.100(16) Uiso 1 1 calc R . .
O8 O 1.0812(7) 0.3135(6) 0.06526(12) 0.0493(11) Uani 1 1 d . . .
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 0.0277(2) 0.0229(2) 0.01953(19) 0.000 -0.00481(19) 0.000
S2 0.0261(5) 0.0301(6) 0.0252(5) 0.0005(5) -0.0045(5) -0.0051(5)
C3 0.032(2) 0.025(2) 0.023(2) -0.0001(17) -0.002(2) 0.003(2)
C4 0.028(2) 0.026(2) 0.027(2) 0.0002(19) -0.0071(19) 0.0003(19)
S5 0.0246(6) 0.0428(7) 0.0293(6) 0.0048(5) -0.0046(5) -0.0022(5)
C6 0.029(3) 0.038(3) 0.027(2) -0.001(2) -0.002(2) 0.002(2)
C7 0.033(3) 0.052(3) 0.029(3) 0.008(2) -0.007(2) 0.001(3)
O8 0.0253(18) 0.083(3) 0.039(2) 0.018(2) 0.0009(16) 0.003(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'
O O 0.0106 0.0060 '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
S2 Te1 S2 102.85(6) 4_755 . ?
C3 S2 Te1 103.37(16) . . ?
C4 C3 S2 112.9(3) . . ?
C3 C4 S5 111.7(3) . . ?
C6 S5 C4 100.5(2) . . ?
O8 C6 C7 124.0(5) . . ?
O8 C6 S5 122.3(4) . . ?
C7 C6 S5 113.7(4) . . ?
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 S2 2.4050(12) 4_755 ?
Te1 S2 2.4050(12) . ?
S2 C3 1.822(5) . ?
C3 C4 1.514(6) . ?
C4 S5 1.810(5) . ?
S5 C6 1.778(5) . ?
C6 O8 1.205(6) . ?
C6 C7 1.487(6) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 Te1 S2 C3 -74.25(15) 4_755 . . . ?
Te1 S2 C3 C4 -67.5(4) . . . . ?
S2 C3 C4 S5 173.9(2) . . . . ?
C3 C4 S5 C6 84.4(4) . . . . ?
C4 S5 C6 O8 1.3(6) . . . . ?
C4 S5 C6 C7 -179.0(4) . . . . ?
