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_4320339
_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. Ruscetti'
_chemical_formula_moiety         'Te2 C28 F32'
_chemical_formula_sum            'C14 F16 Te'
_chemical_formula_weight         599.72
_chemical_name_common            Te-F
_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_F16_C14_d121_klapoetke
_audit_creation_date             15-Dec-99
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 114.373(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8267(9)
_cell_length_b                   13.0023(14)
_cell_length_c                   12.0219(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.5
_cell_volume                     1683.9(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13150
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  0.8267
_exptl_absorpt_correction_T_min  0.5979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.3657(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         6150
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0284
_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          0.0730
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                5874
_reflns_number_total             6150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010149r_1.cif
_cod_data_source_block           ar
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4320339
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 199.5
_kl_diffrn_detector_area_phi_incr 1.5
_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 0.009
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 23
_kl_diffrn_detector_area_profile_max 19
_kl_archive_shelxl_comment       'release 97-2'
_kl_archive_shelxl_res
;
TITL  D121  STOE IPDS measurement
CELL  0.71073   11.8267   13.0023   12.0219    90.000   114.373    90.000
ZERR  2          0.0009    0.0014    0.0010     0.000     0.009     0.000
LATT  -1
SYMM  -x, 0.5+y, -z
SFAC  TE F C
UNIT  4 64 56

L.S. 20
TEMP  -73
BOND
CONF
ACTA
FMAP 2
PLAN -50

DFIX  1.5 0.01 C44 C74
DFIX  -1.25 0.01 C74 F714
DFIX  1.25 0.01 C74 F734

WGHT    0.056400
FVAR       0.47463
MOLE   1
TE1   1    0.289412    0.581996    0.994935    11.00000    0.03152    0.03357 =
          0.02915   -0.00018    0.01298    0.00439
F1    2    0.244117    0.436507    0.966092    11.00000    0.05691    0.03389 =
          0.04574   -0.00343    0.02349    0.00761
F2    2    0.296140    0.731401    1.034782    11.00000    0.04862    0.03567 =
          0.03230   -0.00627    0.01746   -0.00401
C11   3    0.263626    0.562609    1.156380    11.00000    0.04027    0.03042 =
          0.02947    0.00558    0.01438    0.00676
C21   3    0.165982    0.510540    1.163635    11.00000    0.04752    0.03701 =
          0.02874    0.00277    0.01510    0.00594
C31   3    0.155397    0.499525    1.273098    11.00000    0.04262    0.04097 =
          0.04394    0.00889    0.01989    0.00319
C41   3    0.239030    0.543284    1.377820    11.00000    0.06537    0.04526 =
          0.03233    0.00600    0.02522    0.01443
C51   3    0.337961    0.595199    1.373331    11.00000    0.05997    0.03992 =
          0.02909   -0.00203    0.00833    0.01020
C61   3    0.353592    0.602999    1.265015    11.00000    0.04030    0.03250 =
          0.03050    0.00080    0.00980    0.00628
C71   3    0.226086    0.539744    1.498723    11.00000    0.08757    0.05668 =
          0.03743    0.00031    0.03396    0.00769
F21   2    0.076038    0.472386    1.063504    11.00000    0.04653    0.05301 =
          0.03950    0.00216    0.01366   -0.01034
F31   2    0.056754    0.444462    1.270952    11.00000    0.05803    0.07649 =
          0.06088    0.01233    0.03386   -0.00585
F51   2    0.422939    0.639524    1.471721    11.00000    0.07516    0.06656 =
          0.03350   -0.01048    0.01142   -0.00500
F61   2    0.453279    0.648493    1.263944    11.00000    0.04347    0.05970 =
          0.04383   -0.00572    0.00989   -0.00449
F711  2    0.188516    0.627362    1.519841    11.00000    0.20230    0.05161 =
          0.08879    0.00104    0.10448    0.02967
F721  2    0.321332    0.504769    1.587070    11.00000    0.12814    0.15332 =
          0.04902    0.03962    0.04970    0.05233
F731  2    0.137731    0.472578    1.495540    11.00000    0.16012    0.08645 =
          0.07540   -0.01787    0.08265   -0.04197
C12   3    0.105007    0.614058    0.874145    11.00000    0.03031    0.03394 =
          0.03002    0.00274    0.01374    0.00206
C22   3    0.022513    0.674124    0.902112    11.00000    0.04498    0.02826 =
          0.03019   -0.00112    0.01590    0.00212
C32   3   -0.091351    0.700076    0.812773    11.00000    0.04288    0.02787 =
          0.04909    0.00425    0.01747    0.00330
C42   3   -0.127413    0.669374    0.693069    11.00000    0.03806    0.03258 =
          0.04087    0.00496    0.01084   -0.00061
C52   3   -0.044675    0.610450    0.664133    11.00000    0.04227    0.03687 =
          0.02939    0.00344    0.00970   -0.00312
C62   3    0.069680    0.582091    0.756021    11.00000    0.03372    0.03298 =
          0.03087   -0.00135    0.01441   -0.00028
C72   3   -0.251740    0.697940    0.596106    11.00000    0.04237    0.04350 =
          0.05805    0.00873    0.00760    0.00488
F22   2    0.052113    0.705532    1.015787    11.00000    0.04712    0.05237 =
          0.03915   -0.00869    0.01822    0.01093
F32   2   -0.166475    0.757542    0.844769    11.00000    0.04742    0.04975 =
          0.06927   -0.00055    0.02604    0.01546
F52   2   -0.072267    0.580152    0.550847    11.00000    0.05996    0.06287 =
          0.02851   -0.00427    0.00749   -0.00397
F62   2    0.147241    0.525956    0.724967    11.00000    0.04468    0.05196 =
          0.03825   -0.00767    0.02106    0.00417
F712  2   -0.336295    0.707641    0.638685    11.00000    0.05243    0.30554 =
          0.08031   -0.01713   -0.00021    0.05067
F722  2   -0.248711    0.784339    0.546179    11.00000    0.08971    0.09435 =
          0.15243    0.07538   -0.04457   -0.01372
F732  2   -0.296526    0.630931    0.509335    11.00000    0.06914    0.09289 =
          0.09733   -0.03626   -0.02857    0.01401
TE2   1    0.336487    0.861262    0.854507    11.00000    0.03654    0.03295 =
          0.03472   -0.00180    0.01394   -0.00106
F3    2    0.436072    0.988882    0.881901    11.00000    0.05465    0.02977 =
          0.04652   -0.00266    0.01325   -0.00565
F4    2    0.277461    0.719395    0.800938    11.00000    0.05042    0.03973 =
          0.03986   -0.00326    0.02077   -0.01448
C13   3    0.326541    0.869032    0.675789    11.00000    0.04149    0.03305 =
          0.03506    0.00590    0.01584   -0.00022
C23   3    0.424953    0.882328    0.643452    11.00000    0.04474    0.02922 =
          0.04215    0.00205    0.01724   -0.00250
C33   3    0.407446    0.887736    0.524596    11.00000    0.05743    0.03281 =
          0.04166    0.00057    0.02607   -0.00268
C43   3    0.288862    0.882138    0.429466    11.00000    0.07660    0.02681 =
          0.04301   -0.00188    0.02272    0.00096
C53   3    0.190571    0.869337    0.460682    11.00000    0.05465    0.03530 =
          0.03423   -0.00564    0.00349   -0.00344
C63   3    0.209097    0.863225    0.582315    11.00000    0.04021    0.03895 =
          0.03827   -0.00192    0.00923   -0.00021
C73   3    0.267815    0.888738    0.296749    11.00000    0.09022    0.04689 =
          0.03803   -0.00362    0.02256    0.01832
F23   2    0.540891    0.887524    0.730946    11.00000    0.04008    0.05682 =
          0.05070    0.00281    0.01451   -0.01308
F33   2    0.506154    0.901230    0.499745    11.00000    0.07525    0.06569 =
          0.06555    0.00946    0.04426    0.00390
F53   2    0.074632    0.864310    0.375685    11.00000    0.06164    0.06954 =
          0.04401   -0.00516   -0.00672   -0.00009
F63   2    0.110106    0.851614    0.607894    11.00000    0.03657    0.07171 =
          0.05226    0.00295    0.01110   -0.00147
F713  2    0.360918    0.865331    0.276854    11.00000    0.13695    0.31094 =
          0.06310   -0.01098    0.05508    0.05959
F723  2    0.209859    0.962627    0.244649    11.00000    0.44200    0.14874 =
          0.08013    0.06747    0.15345    0.18787
F733  2    0.207295    0.806029    0.238858    11.00000    0.25984    0.11914 =
          0.06550   -0.02680    0.04961    0.00522
C14   3    0.507218    0.790050    0.958172    11.00000    0.03481    0.03171 =
          0.04285    0.00552    0.01601   -0.00257
C24   3    0.561994    0.820352    1.080035    11.00000    0.04819    0.04199 =
          0.03721    0.00808    0.01028   -0.00894
C34   3    0.669018    0.776096    1.160760    11.00000    0.05272    0.06706 =
          0.05525    0.02756    0.00148   -0.02035
C44   3    0.725552    0.699049    1.121049    11.00000    0.03828    0.06771 =
          0.11186    0.05073    0.02117    0.00004
C54   3    0.669082    0.668718    0.998198    11.00000    0.04356    0.04872 =
          0.12823    0.03404    0.04619    0.01536
C64   3    0.562953    0.714298    0.919782    11.00000    0.05165    0.03669 =
          0.06963    0.00642    0.03751    0.00019
C74   3    0.841996    0.648315    1.207678    11.00000    0.02980    0.11403 =
          0.19202    0.10786    0.01742    0.00325
F24   2    0.509966    0.894349    1.120391    11.00000    0.08032    0.05997 =
          0.03946   -0.00581    0.02147   -0.00007
F34   2    0.715852    0.809028    1.274718    11.00000    0.11257    0.11218 =
          0.05824    0.02825   -0.02375   -0.04851
F54   2    0.719038    0.593806    0.958703    11.00000    0.10352    0.05854 =
          0.22757    0.03662    0.11319    0.03579
F64   2    0.512333    0.682493    0.803862    11.00000    0.09392    0.04762 =
          0.07712   -0.00977    0.05658    0.00259
F714  2    0.918854    0.636936    1.165655    11.00000    0.15506    0.75749 =
          0.31265    0.42173    0.17420    0.28845
F724  2    0.828734    0.570938    1.257706    11.00000    0.06314    0.08830 =
          0.10924    0.05404   -0.00225   -0.00528
F734  2    0.908394    0.701130    1.295183    11.00000    0.12310    0.11303 =
          0.67145    0.15400   -0.23048   -0.06299
HKLF  4

REM   D121  STOE IPDS measurement
REM R1 =  0.0284 for   5874 Fo > 4sig(Fo)  and  0.0299 for all   6150 data
REM    559 parameters refined using      4 restraints

END

WGHT      0.0564      0.0000
REM Highest difference peak  0.803,  deepest hole -0.617,  1-sigma level  0.084
Q1    1   0.8823  0.7042  1.3399  11.00000  0.05    0.80
Q2    1   0.1489  0.8779  0.2133  11.00000  0.05    0.75
Q3    1   0.9319  0.6778  1.2035  11.00000  0.05    0.73
Q4    1   0.3379  0.9820  0.2962  11.00000  0.05    0.69
;