#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:57:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179271 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/91/4319143.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_4319143
loop_
_publ_author_name
'Holger Fleischer'
'Dieter Schollmeyer'
_publ_section_title
;
 Molecular Structure of Te(OMe)4.ClTe(OMe)3, a Model for Ligand Exchange
 between Te(IV) Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              324
_journal_page_last               328
_journal_paper_doi               10.1021/ic000374t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C7 H21 Cl O7 Te2'
_chemical_formula_weight         507.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.975(6)
_cell_angle_beta                 99.750(7)
_cell_angle_gamma                91.667(7)
_cell_formula_units_Z            2
_cell_length_a                   7.1309(6)
_cell_length_b                   10.3345(8)
_cell_length_c                   10.6899(8)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      4
_cell_volume                     763.28(11)
_computing_cell_refinement       'P4 Software'
_computing_data_collection       'P4 Software'
_computing_data_reduction        'P4 Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'euler cradle'
_diffrn_measurement_device_type  'P4 Siemens'
_diffrn_measurement_method       ω/2ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4121
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'sealed tube'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.014
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   'Psi scans'
_exptl_absorpt_process_details   Platon
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_obs          0.0445
_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)+(0.0540P)²+0.2185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0985
_refine_ls_wR_factor_ref         0.1116
_reflns_number_observed          2377
_reflns_number_total             3314
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000374t.cif
_cod_data_source_block           C7H21ClO7Te2
_cod_original_cell_volume        763.28(10)
_cod_database_code               4319143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_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 0.02067(7) 0.11139(4) 0.18898(5) 0.02930(16) Uani 1 1 d . . .
Te2 Te 0.41396(7) 0.41360(4) 0.32238(4) 0.02499(15) Uani 1 1 d . . .
Cl1 Cl -0.2330(5) 0.2067(3) 0.3439(3) 0.0653(7) Uani 1 1 d . . .
O11 O 0.2062(11) 0.0344(8) 0.0787(7) 0.061(2) Uani 1 1 d . . .
C11 C 0.331(2) -0.0327(9) 0.1184(11) 0.091(5) Uani 1 1 d . . .
H11A H 0.4050 -0.0607 0.0515 0.136 Uiso 1 1 calc R . .
H11B H 0.2744 -0.1093 0.1422 0.136 Uiso 1 1 calc R . .
H11C H 0.4134 0.0182 0.1934 0.136 Uiso 1 1 calc R . .
O12 O -0.0171(12) -0.0617(7) 0.2330(8) 0.070(2) Uani 1 1 d . . .
C12 C -0.1908(17) -0.1285(10) 0.2098(10) 0.061(3) Uani 1 1 d . . .
H12A H -0.1773 -0.2121 0.2389 0.092 Uiso 1 1 calc R . .
H12B H -0.2411 -0.1440 0.1179 0.092 Uiso 1 1 calc R . .
H12C H -0.2775 -0.0769 0.2559 0.092 Uiso 1 1 calc R . .
O13 O 0.2121(8) 0.1520(5) 0.3407(5) 0.0364(13) Uani 1 1 d . . .
C13 C 0.2262(19) 0.0863(11) 0.4430(10) 0.074(4) Uani 1 1 d . . .
H13A H 0.3346 0.1238 0.5083 0.111 Uiso 1 1 calc R . .
H13B H 0.2432 -0.0061 0.4133 0.111 Uiso 1 1 calc R . .
H13C H 0.1107 0.0947 0.4796 0.111 Uiso 1 1 calc R . .
O14 O 0.1624(8) 0.3085(5) 0.1813(5) 0.0351(13) Uani 1 1 d . . .
C14 C 0.0625(13) 0.3722(9) 0.0861(8) 0.042(2) Uani 1 1 d . . .
H14A H -0.0407 0.3134 0.0338 0.063 Uiso 1 1 calc R . .
H14B H 0.1488 0.3963 0.0317 0.063 Uiso 1 1 calc R . .
H14C H 0.0107 0.4509 0.1274 0.063 Uiso 1 1 calc R . .
O21 O 0.5071(8) 0.4471(5) 0.1724(5) 0.0337(12) Uani 1 1 d . . .
C21 C 0.5312(14) 0.3402(9) 0.0713(8) 0.044(2) Uani 1 1 d . . .
H21A H 0.5797 0.3750 0.0036 0.066 Uiso 1 1 calc R . .
H21B H 0.4093 0.2924 0.0360 0.066 Uiso 1 1 calc R . .
H21C H 0.6208 0.2812 0.1064 0.066 Uiso 1 1 calc R . .
O22 O 0.6168(8) 0.5431(5) 0.4264(5) 0.0332(12) Uani 1 1 d . . .
C22 C 0.8000(12) 0.5620(9) 0.3934(9) 0.044(2) Uani 1 1 d . . .
H22A H 0.8749 0.6301 0.4579 0.065 Uiso 1 1 calc R . .
H22B H 0.7853 0.5884 0.3097 0.065 Uiso 1 1 calc R . .
H22C H 0.8644 0.4804 0.3902 0.065 Uiso 1 1 calc R . .
O23 O 0.2427(8) 0.5511(5) 0.3209(5) 0.0356(13) Uani 1 1 d . . .
C23 C 0.3001(17) 0.6825(9) 0.3132(11) 0.057(3) Uani 1 1 d . . .
H23A H 0.1913 0.7367 0.3137 0.086 Uiso 1 1 calc R . .
H23B H 0.3496 0.6825 0.2341 0.086 Uiso 1 1 calc R . .
H23C H 0.3985 0.7178 0.3867 0.086 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O13 Te1 O12 87.7(3) . . ?
O13 Te1 O11 93.1(3) . . ?
O12 Te1 O11 88.3(4) . . ?
O13 Te1 O14 74.2(2) . . ?
O12 Te1 O14 160.3(3) . . ?
O11 Te1 O14 85.2(3) . . ?
O13 Te1 Cl1 86.4(2) . . ?
O12 Te1 Cl1 89.2(3) . . ?
O11 Te1 Cl1 177.5(2) . . ?
O14 Te1 Cl1 97.00(16) . . ?
O23 Te2 O21 93.8(2) . . ?
O23 Te2 O22 88.9(2) . . ?
O21 Te2 O22 87.4(2) . . ?
O23 Te2 O14 79.8(2) . . ?
O21 Te2 O14 85.2(2) . . ?
O22 Te2 O14 166.1(2) . . ?
C11 O11 Te1 121.7(7) . . ?
C12 O12 Te1 123.0(7) . . ?
C13 O13 Te1 124.3(6) . . ?
C14 O14 Te2 120.2(5) . . ?
C14 O14 Te1 113.2(5) . . ?
Te2 O14 Te1 126.1(2) . . ?
C21 O21 Te2 120.7(5) . . ?
C22 O22 Te2 124.0(5) . . ?
C23 O23 Te2 122.8(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
Te1 O13 1.910(5) . ?
Te1 O12 1.949(6) . ?
Te1 O11 2.009(7) . ?
Te1 O14 2.268(5) . ?
Te1 Cl1 2.746(3) . ?
Te2 O23 1.901(5) . ?
Te2 O21 1.916(5) . ?
Te2 O22 1.987(5) . ?
Te2 O14 2.253(5) . ?
O11 C11 1.209(14) . ?
O12 C12 1.363(12) . ?
O13 C13 1.376(10) . ?
O14 C14 1.411(9) . ?
O21 C21 1.441(9) . ?
O22 C22 1.426(10) . ?
O23 C23 1.427(10) . ?
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
O13 Te1 O11 C11 39.5(11) . . . . ?
O12 Te1 O11 C11 -48.0(11) . . . . ?
O14 Te1 O11 C11 113.4(11) . . . . ?
Cl1 Te1 O11 C11 -38(6) . . . . ?
O13 Te1 O12 C12 145.1(9) . . . . ?
O11 Te1 O12 C12 -121.8(9) . . . . ?
O14 Te1 O12 C12 167.6(7) . . . . ?
Cl1 Te1 O12 C12 58.7(9) . . . . ?
O12 Te1 O13 C13 -20.1(9) . . . . ?
O11 Te1 O13 C13 -108.3(9) . . . . ?
O14 Te1 O13 C13 167.6(9) . . . . ?
Cl1 Te1 O13 C13 69.3(9) . . . . ?
O23 Te2 O14 C14 42.7(6) . . . . ?
O21 Te2 O14 C14 -52.1(6) . . . . ?
O22 Te2 O14 C14 6.0(13) . . . . ?
O23 Te2 O14 Te1 -128.9(4) . . . . ?
O21 Te2 O14 Te1 136.3(4) . . . . ?
O22 Te2 O14 Te1 -165.6(7) . . . . ?
O13 Te1 O14 C14 -168.3(6) . . . . ?
O12 Te1 O14 C14 168.3(10) . . . . ?
O11 Te1 O14 C14 97.2(6) . . . . ?
Cl1 Te1 O14 C14 -84.0(6) . . . . ?
O13 Te1 O14 Te2 3.9(3) . . . . ?
O12 Te1 O14 Te2 -19.5(11) . . . . ?
O11 Te1 O14 Te2 -90.7(4) . . . . ?
Cl1 Te1 O14 Te2 88.1(3) . . . . ?
O23 Te2 O21 C21 -135.5(6) . . . . ?
O22 Te2 O21 C21 135.8(6) . . . . ?
O14 Te2 O21 C21 -56.0(6) . . . . ?
O23 Te2 O22 C22 -127.5(6) . . . . ?
O21 Te2 O22 C22 -33.7(6) . . . . ?
O14 Te2 O22 C22 -91.5(11) . . . . ?
O21 Te2 O23 C23 -50.9(7) . . . . ?
O22 Te2 O23 C23 36.4(7) . . . . ?
O14 Te2 O23 C23 -135.4(7) . . . . ?
