Air-stable Aryl Derivatives of the Pentafluoroorthotellurate
Wegener, Daniel; Hoffmann, Kurt F.; Pérez-Bitrián, Alberto; Bayindir, Ilayda; Hadi, Amiera Nadien; Wiesner, Anja; Riedel, Sebastian; Chemical Communications  (2022) –; doi:10.1039/D2CC03936B

data_7130488
_publ_section_title
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 Air-stable Aryl Derivatives of the Pentafluoroorthotellurate
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03936B
_journal_year                    2022
_chemical_formula_moiety         'C12 H2 F12 O2 Te, 0.8[C3H6O]'
_chemical_formula_sum            'C14.4 H6.8 F12 O2.8 Te'
_chemical_formula_weight         580.197
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-13 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.111(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4885(8)
_cell_length_b                   8.7591(4)
_cell_length_c                   11.8083(5)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.96
_cell_volume                     1817.53(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0072
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44869
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0414 after correction.
The Ratio of minimum to maximum transmission is 0.8964.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       block
_exptl_crystal_F_000             1102.047
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.4533
_refine_diff_density_min         -0.3644
_refine_diff_density_rms         0.0770
_refine_ls_d_res_high            0.7993
_refine_ls_d_res_low             8.7863
_refine_ls_goodness_of_fit_ref   1.0763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     206
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.0382
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+5.9194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -23
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1681
_reflns_number_total             1864
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cc03936b2.cif
_cod_data_source_block           run2_a
_cod_original_formula_sum        'C14.4 F12 H6.8 O2.8 Te1'
_cod_database_code               7130488
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 F2-C2 \\sim F2A-C2A
 with sigma of 0.02
 F3-C3 \\sim F3A-C3A
 with sigma of 0.02
 C1-C2 \\sim C1-C2A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C4-F4 \\sim C4A-F4A
 with sigma of 0.02
 C3-C2 \\sim C3A-C2A
 with sigma of 0.02
 F6-C1 \\sim F6A-C1
 with sigma of 0.04
 F2-C1 \\sim F2A-C1
 with sigma of 0.04
 F2-C3 \\sim F2A-C3A
 with sigma of 0.04
 F3-C4 \\sim F3A-C4A
 with sigma of 0.04
 F3-C2 \\sim F3A-C2A
 with sigma of 0.04
 F5-C4 \\sim F5A-C4A
 with sigma of 0.04
 C1-C3 \\sim C1-C3A
 with sigma of 0.04
 C4-C2 \\sim C4A-C2A
 with sigma of 0.04
 C3-F4 \\sim C3A-F4A
 with sigma of 0.04
 F6-C6 \\sim F6A-C6A
 with sigma of 0.02
 F5-C5 \\sim F5A-C5A
 with sigma of 0.02
 C1-C6 \\sim C1-C6A
 with sigma of 0.02
 C6-C5 \\sim C6A-C5A
 with sigma of 0.02
 C5-C4 \\sim C5A-C4A
 with sigma of 0.02
 F6-C5 \\sim F6A-C5A
 with sigma of 0.04
 F5-C6 \\sim F5A-C6A
 with sigma of 0.04
 C1-C5 \\sim C1-C5A
 with sigma of 0.04
 C6-C4 \\sim C6A-C4A
 with sigma of 0.04
 C5-C3 \\sim C5A-C3A
 with sigma of 0.04
 C5-F4 \\sim C5A-F4A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2A \\sim C3A \\sim C4A \\sim C6A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
C6A \\sim C5A \\sim C1 \\sim C2A \\sim C3A \\sim C4A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C6A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=
 Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F6)=Sof(F2)=Sof(F3)=Sof(F5)=Sof(C6)=Sof(C5)=Sof(C4)=Sof(C3)=Sof(C2)=
 Sof(F4)=FVAR(1)
5.a Free rotating group:
 O1(H1)
5.b Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'