Spectroscopic and Structural Studies on Polyfluorophenyl Tellurides and Tellurium(IV) Dihalides
Thomas M. Klapötke; Burkhard Krumm; Peter Mayer; Kurt Polborn; Oliver P. Ruscitti; Inorganic Chemistry 40 (2001) 5169–5176; doi:10.1021/ic010149r

data_4320283
_publ_section_title
;
 Spectroscopic and Structural Studies on Polyfluorophenyl Tellurides and
 Tellurium(IV) Dihalides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5169
_journal_page_last               5176
_journal_paper_doi               10.1021/ic010149r
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'provided by O. Ruscitti'
_chemical_formula_moiety         'Te Br2 F4 C12 H6'
_chemical_formula_sum            'C12 H6 Br2 F4 Te'
_chemical_formula_weight         513.58
_chemical_name_common            TeBr
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                Te_Br2_(C6F2H3)2_e023_klapoetke
_audit_creation_date             28-Jan-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3495(5)
_cell_length_b                   8.4819(4)
_cell_length_c                   28.2513(19)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.0
_cell_volume                     2719.6(3)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_molecular_graphics
;ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
  Plot Program for Crystal Structure Illustrations, Oak Ridge National
  Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
  Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
  Germany, 1995).
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)'
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            10149
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         3.08
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    8.092
_exptl_absorpt_correction_T_max  0.7912
_exptl_absorpt_correction_T_min  0.4860
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.5087(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                1991
_reflns_number_total             2504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010149r_2.cif
_cod_data_source_block           ar
_cod_database_code               4320283
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 100.2
_kl_diffrn_detector_area_phi_incr 0.6
_kl_diffrn_detector_area_expos_time 2.00_min
_kl_diffrn_detector_area_plate_dist 70.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.005
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 11
_kl_diffrn_detector_area_profile_max 17
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL   e023 in Pbca (61), sir97
CELL  0.71073   11.3495    8.4819   28.2513    90.000    90.000    90.000
ZERR  8          0.0005    0.0004    0.0019     0.000     0.000     0.000
LATT  1
SYMM   .50000-X,-Y,  .50000+Z
SYMM   .50000+X,  .50000-Y,-Z
SYMM -X,  .50000+Y,  .50000-Z
SFAC    C   H   F   BR  TE
UNIT    96  48  32  16   8
L.S.      8
FMAP      2
PLAN     -25
BOND $H
CONF
TEMP  -73
ACTA

WGHT    0.026100
FVAR       0.20052
TE    5   -0.110754    0.360687    0.103325    11.00000    0.01328    0.01561 =
          0.01331    0.00016   -0.00099    0.00093
BR1   4   -0.095546    0.667591    0.121918    11.00000    0.02768    0.01740 =
          0.03002   -0.00147   -0.00317    0.00066
BR2   4   -0.090916    0.056216    0.084979    11.00000    0.02118    0.01916 =
          0.03085   -0.00121    0.00170    0.00004
C11   1    0.066823    0.380709    0.081680    11.00000    0.01418    0.01709 =
          0.01825   -0.00061    0.00046   -0.00016
C21   1    0.089658    0.351457    0.034887    11.00000    0.02404    0.02241 =
          0.01975   -0.00199    0.00097   -0.00297
C31   1    0.199715    0.362328    0.015104    11.00000    0.03192    0.03920 =
          0.02052   -0.00834    0.01167   -0.00498
H31   2    0.209462    0.342416   -0.016704    11.00000    0.03273
C41   1    0.291868    0.408041    0.044087    11.00000    0.02144    0.04786 =
          0.04538   -0.00837    0.01315   -0.00541
H41   2    0.365553    0.405124    0.036717    11.00000    0.06914
C51   1    0.273601    0.440745    0.091119    11.00000    0.01976    0.04136 =
          0.03245   -0.00815   -0.00216   -0.00771
H51   2    0.327093    0.461193    0.109656    11.00000    0.04539
C61   1    0.161396    0.428999    0.109451    11.00000    0.02184    0.02848 =
          0.01649   -0.00234   -0.00084   -0.00129
F21   3   -0.002732    0.313442    0.006380    11.00000    0.02961    0.04522 =
          0.01573   -0.00547   -0.00403   -0.01043
F61   3    0.142936    0.466265    0.154874    11.00000    0.02471    0.04358 =
          0.01809   -0.00797   -0.00293   -0.00402
C12   1   -0.099414    0.313201    0.176342    11.00000    0.01859    0.02015 =
          0.01374    0.00026    0.00043   -0.00302
C22   1   -0.012546    0.226426    0.199421    11.00000    0.02368    0.02216 =
          0.01962    0.00039    0.00312    0.00381
C32   1   -0.013350    0.201754    0.246816    11.00000    0.03571    0.03365 =
          0.02827    0.01048   -0.00458    0.00886
H32   2    0.040948    0.153562    0.259754    11.00000    0.02908
C42   1   -0.103398    0.262667    0.273540    11.00000    0.04877    0.04134 =
          0.01116    0.00656   -0.00203   -0.00279
H42   2   -0.107497    0.259670    0.303791    11.00000    0.01967
C52   1   -0.194074    0.346657    0.252407    11.00000    0.02715    0.03402 =
          0.02262    0.00151    0.01005    0.00004
H52   2   -0.244928    0.381418    0.268488    11.00000    0.05560
C62   1   -0.189784    0.370372    0.204844    11.00000    0.01728    0.02097 =
          0.02270    0.00135    0.00278   -0.00332
F22   3    0.076557    0.165193    0.173350    11.00000    0.02855    0.03887 =
          0.02816    0.00216    0.00036    0.01516
F62   3   -0.276935    0.452292    0.183928    11.00000    0.01874    0.03453 =
          0.02568    0.00201    0.00111    0.00795
HKLF      4

REM    e023 in Pbca (61), sir97
REM R1 =  0.0211 for   1991 Fo > 4sig(Fo)  and  0.0320 for all   2504 data
REM    196 parameters refined using      0 restraints

END

WGHT      0.0261      0.0000
REM Highest difference peak  0.538,  deepest hole -0.538,  1-sigma level  0.101
Q1    1  -0.0815  0.4046  0.1016  11.00000  0.05    0.54
Q2    1  -0.0979  0.1057  0.1278  11.00000  0.05    0.52
Q3    1  -0.0802  0.7028  0.0812  11.00000  0.05    0.46
Q4    1  -0.1205  0.6702  0.1594  11.00000  0.05    0.43
Q5    1  -0.1376  0.3891  0.1039  11.00000  0.05    0.41
Q6    1   0.0185  0.3660  0.0865  11.00000  0.05    0.40
;