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_4320284
_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, 2(C7 F7)'
_chemical_formula_sum            'C14 F14 Te'
_chemical_formula_weight         561.73
_chemical_name_common            TeCF3
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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_(CF3C6F4)2_e033_klapoetke
_audit_creation_date             08-Feb-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 90.884(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.042(3)
_cell_length_b                   5.0180(6)
_cell_length_c                   10.3051(14)
_cell_measurement_reflns_used    4220
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      2.0
_cell_volume                     777.7(2)
_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 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2888
_diffrn_reflns_theta_full        23.83
_diffrn_reflns_theta_max         23.83
_diffrn_reflns_theta_min         1.98
_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    2.068
_exptl_absorpt_correction_T_max  0.9254
_exptl_absorpt_correction_T_min  0.8058
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.3987(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                1621
_reflns_number_total             1943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010149r_3.cif
_cod_data_source_block           ar
_cod_original_cell_volume        777.74(19)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4320284
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 120.0
_kl_diffrn_detector_area_phi_incr 1.2
_kl_diffrn_detector_area_expos_time 8.00_min
_kl_diffrn_detector_area_plate_dist 80.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.021
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 13
_kl_diffrn_detector_area_profile_max 27
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL  e033 in P21 (4), sir97
CELL  0.71073   15.0420    5.0180   10.3051    90.000    90.884    90.000
ZERR  2          0.0026    0.0006    0.0014     0.000     0.019     0.000
LATT -1
SYMM -X,  .50000+Y,-Z
SFAC    C   F   TE
UNIT    28  28   2
L.S.      8
FMAP      2
BOND
CONF
ACTA
TEMP -73
PLAN     -40
WGHT    0.075300
FVAR       0.57049   0.43987
MOLE  1
TE    3    0.812644    0.934154    0.238067    11.00000    0.03368    0.08210 =
          0.02870   -0.00076    0.00034    0.01218
C11   1    0.832773    0.914081    0.442130    11.00000    0.01941    0.03879 =
          0.03117   -0.01018   -0.00172   -0.01157
C21   1    0.887057    0.733277    0.494645    11.00000    0.03315    0.03696 =
          0.02960   -0.00734    0.00462    0.01523
C31   1    0.909198    0.725394    0.622042    11.00000    0.02583    0.03191 =
          0.05473    0.00362   -0.00157   -0.01254
C41   1    0.874195    0.912922    0.711582    11.00000    0.03165    0.05345 =
          0.02784    0.00375   -0.00022   -0.00890
C51   1    0.818748    1.093780    0.658282    11.00000    0.03274    0.03830 =
          0.04146   -0.01616    0.00993   -0.01426
C61   1    0.794439    1.113048    0.528511    11.00000    0.03263    0.02718 =
          0.03743    0.00611   -0.00982   -0.00275
C71   1    0.898502    0.898816    0.848791    11.00000    0.04628    0.02741 =
          0.06106    0.01136   -0.00144    0.00509
F21   2    0.925445    0.553173    0.414699    11.00000    0.04022    0.05403 =
          0.04459   -0.00637    0.00159    0.01640
F31   2    0.965797    0.534503    0.665150    11.00000    0.03822    0.05213 =
          0.05540    0.01597   -0.00690    0.01684
F51   2    0.779780    1.282850    0.734663    11.00000    0.05065    0.05143 =
          0.04221   -0.01382    0.00078    0.00787
F61   2    0.742187    1.299519    0.485826    11.00000    0.03922    0.04111 =
          0.04733    0.00265   -0.00755    0.01337
RESI 1
PART 1
F711  2    0.925594    1.123460    0.896410    21.00000    0.05423
F712  2    0.822813    0.854976    0.920116    21.00000    0.03837
F713  2    0.955387    0.706680    0.881133    21.00000    0.05892
RESI  2
PART 2
F711  2    0.888148    0.674186    0.906620   -21.00000    0.06626
F712  2    0.980929    1.002304    0.866231   -21.00000    0.06518
F713  2    0.856685    1.083445    0.923479   -21.00000    0.07473
RESI  0
PART 0
C12   1    0.680173    1.069380    0.234514    11.00000    0.02798    0.04278 =
          0.02672   -0.00921   -0.01082    0.00031
C22   1    0.652417    1.263048    0.149940    11.00000    0.04470    0.04516 =
          0.03596   -0.00679   -0.00367    0.00062
C32   1    0.569180    1.362165    0.145207    11.00000    0.04532    0.04564 =
          0.03348   -0.00202   -0.01923    0.01256
C42   1    0.504251    1.262065    0.229439    11.00000    0.02721    0.04352 =
          0.03935   -0.01072   -0.01021    0.01159
C52   1    0.532669    1.065650    0.316309    11.00000    0.03969    0.05910 =
          0.04210    0.00202   -0.00329   -0.00041
C62   1    0.615781    0.972186    0.319046    11.00000    0.03219    0.04514 =
          0.03340    0.00993   -0.00725   -0.00646
C72   1    0.412626    1.367069    0.230392    11.00000    0.02632    0.08997 =
          0.04336   -0.00745   -0.00492   -0.00439
F22   2    0.711521    1.361595    0.065488    11.00000    0.03785    0.08015 =
          0.04476    0.01726    0.00212   -0.00383
F32   2    0.548612    1.549331    0.059131    11.00000    0.04794    0.06987 =
          0.06803    0.02343   -0.00466    0.00967
F52   2    0.473499    0.969221    0.400184    11.00000    0.03470    0.07093 =
          0.05769    0.01007    0.00824    0.00032
F62   2    0.637717    0.780664    0.403707    11.00000    0.03831    0.07127 =
          0.05155    0.02322   -0.00425    0.00233
F721  2    0.387909    1.477256    0.338931    11.00000    0.07613
F722  2    0.358724    1.174275    0.198254    11.00000    0.12911
F733  2    0.392646    1.538394    0.134517    11.00000    0.09561
HKLF  4

REM   e033 in P21 (4), sir97
REM R1 =  0.0450 for   1621 Fo > 4sig(Fo)  and  0.0555 for all   1943 data
REM    245 parameters refined using      1 restraints

END

WGHT      0.0753      0.0000
REM Highest difference peak  0.657,  deepest hole -0.737,  1-sigma level  0.117
Q1    1   0.3748  1.4246  0.1084  11.00000  0.05    0.66
Q2    1   0.3405  1.1854  0.2901  11.00000  0.05    0.60
Q3    1   0.9209  0.5913  0.8842  11.00000  0.05    0.60
Q4    1   0.3979  1.6093  0.2929  11.00000  0.05    0.55
Q5    1   0.8337  0.6981  0.9153  11.00000  0.05    0.54
;