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_4320287
_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 Cl2 F14 C14'
_chemical_formula_sum            'C14 Cl2 F14 Te'
_chemical_formula_weight         632.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                Te_Cl2_(C6F4CF3)2_e066_klapoetke
_audit_creation_date             15-Mar-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 108.971(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7666(7)
_cell_length_b                   6.5075(3)
_cell_length_c                   20.5438(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.2
_cell_volume                     1740.47(17)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8517
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         2.15
_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    2.160
_exptl_absorpt_correction_T_max  0.9317
_exptl_absorpt_correction_T_min  0.7029
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.4144(2)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2990
_reflns_number_total             3317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010149r_6.cif
_cod_data_source_block           ar
_cod_original_cell_volume        1740.47(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4320287
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 130.0
_kl_diffrn_detector_area_phi_incr 0.5
_kl_diffrn_detector_area_expos_time 6.00_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 13
_kl_diffrn_detector_area_profile_max 15
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL  e066 in P21/n (14), sir97
CELL  0.71073   13.7666    6.5075   20.5438    90.000   108.971    90.000
ZERR  4          0.0007    0.0003    0.0012     0.000     0.006     0.000
LATT  1
SYMM   .50000-X,  .50000+Y,  .50000-Z
SFAC    C   F   CL  TE
UNIT    56  56   8   4
L.S.     30
FMAP      2
PLAN     -50
BOND
CONF
TEMP  -73
ACTA
REM Wichtung aendert sich stets leicht, wR2 aber nicht
WGHT    0.049600    0.016700
FVAR       0.39047
TE    4    0.642424    0.234108    0.285125    11.00000    0.01779    0.01788 =
          0.02276    0.00192    0.00690    0.00101
CL1   3    0.630688   -0.053176    0.357168    11.00000    0.04101    0.02625 =
          0.03420    0.01209    0.01101    0.00109
CL2   3    0.624043    0.526771    0.202848    11.00000    0.02918    0.02342 =
          0.03410    0.00820    0.01170   -0.00061
C11   1    0.539129    0.399622    0.322304    11.00000    0.02132    0.01701 =
          0.02506   -0.00078    0.01130   -0.00051
C21   1    0.442599    0.470122    0.284042    11.00000    0.02272    0.02219 =
          0.02701    0.00073    0.00918   -0.00110
C31   1    0.387849    0.592179    0.314476    11.00000    0.02127    0.02497 =
          0.03363    0.00310    0.01129    0.00275
C41   1    0.427439    0.653280    0.382873    11.00000    0.02925    0.02596 =
          0.03746    0.00000    0.01917   -0.00029
C51   1    0.524447    0.583887    0.420486    11.00000    0.03056    0.02531 =
          0.02548   -0.00361    0.01343   -0.00544
C61   1    0.578472    0.458238    0.389844    11.00000    0.02006    0.02659 =
          0.02757    0.00239    0.00721   -0.00155
C71   1    0.364761    0.796357    0.411252    11.00000    0.04033    0.03605 =
          0.04203   -0.00795    0.02348    0.00412
F21   2    0.401528    0.424456    0.217491    11.00000    0.02768    0.03435 =
          0.02529   -0.00094    0.00370    0.00305
F31   2    0.294801    0.655849    0.276364    11.00000    0.02352    0.04244 =
          0.04325    0.00257    0.00952    0.01093
F51   2    0.570381    0.638427    0.485493    11.00000    0.03650    0.04588 =
          0.02903   -0.00981    0.01206   -0.00385
F61   2    0.673903    0.399511    0.427324    11.00000    0.02442    0.04058 =
          0.02786   -0.00339    0.00373    0.00234
F711  2    0.273620    0.717851    0.404631    11.00000    0.04079    0.07860 =
          0.08911   -0.02890    0.04186   -0.00373
F712  2    0.350165    0.973483    0.378030    11.00000    0.10344    0.04182 =
          0.08034    0.01654    0.05814    0.03542
F713  2    0.409114    0.837241    0.477318    11.00000    0.05663    0.05642 =
          0.05126   -0.01784    0.02472    0.00791
C12   1    0.545379    0.068543    0.200500    11.00000    0.02413    0.01599 =
          0.02059    0.00185    0.00407    0.00211
C22   1    0.583679    0.022658    0.147809    11.00000    0.02427    0.02072 =
          0.02469    0.00315    0.00609    0.00237
C32   1    0.530526   -0.099702    0.093124    11.00000    0.03385    0.02730 =
          0.02130    0.00325    0.00719    0.00715
C42   1    0.434610   -0.176553    0.088065    11.00000    0.03514    0.01925 =
          0.02632    0.00429   -0.00051    0.00310
C52   1    0.396434   -0.130633    0.141279    11.00000    0.02502    0.02164 =
          0.03304    0.00514    0.00642   -0.00148
C62   1    0.450878   -0.012744    0.196843    11.00000    0.02543    0.01994 =
          0.03066    0.00113    0.00941   -0.00012
C72   1    0.374529   -0.318156    0.031070    11.00000    0.04032    0.03522 =
          0.02929   -0.00597    0.00181    0.00031
F22   2    0.677585    0.089081    0.151210    11.00000    0.02544    0.03609 =
          0.02908    0.00026    0.01192    0.00028
F32   2    0.575907   -0.142677    0.046514    11.00000    0.04547    0.04638 =
          0.02567   -0.00613    0.01367    0.00455
F52   2    0.305427   -0.204185    0.140066    11.00000    0.02961    0.03663 =
          0.04910   -0.00030    0.00766   -0.01160
F62   2    0.411040    0.019608    0.247003    11.00000    0.02982    0.03345 =
          0.03466   -0.00190    0.01719   -0.00611
F721  2    0.279592   -0.259687    0.005470    11.00000    0.04670    0.13178 =
          0.08093   -0.06181   -0.02517    0.02279
F722  2    0.412715   -0.328657   -0.020390    11.00000    0.08228    0.06270 =
          0.03457   -0.01610    0.01444   -0.02149
F723  2    0.377181   -0.507990    0.053720    11.00000    0.11206    0.03758 =
          0.05327   -0.00786    0.01318   -0.03057
HKLF      4

REM   e066 in P21/n (14), sir97
REM R1 =  0.0247 for   2990 Fo > 4sig(Fo)  and  0.0281 for all   3317 data
REM    280 parameters refined using      0 restraints

END

WGHT      0.0496      0.0223
REM Highest difference peak  0.788,  deepest hole -0.456,  1-sigma level  0.109
Q1    1   0.3455 -0.2515 -0.0324  11.00000  0.05    0.79
Q2    1   0.2805 -0.3724  0.0336  11.00000  0.05    0.74
Q3    1   0.2848  0.8492  0.3891  11.00000  0.05    0.40
Q4    1   0.4050  0.4695  0.3041  11.00000  0.05    0.40
;