One-pot synthesis, structural analysis, and oxidation applications of a series of diaryltellurium dicarboxylates
Shibuya, Yuga; Toyoda, Anna; Ohmura, Shiori; Higashikawa, Go; Koguchi, Shinichi; RSC Advances 11 (2021) 32837–32840; doi:10.1039/D1RA06150J

data_7243696
_publ_section_title
;
 One-pot synthesis, structural analysis, and oxidation applications of a
 series of diaryltellurium dicarboxylates
;
_journal_issue                   52
_journal_name_full               'RSC Advances'
_journal_page_first              32837
_journal_page_last               32840
_journal_paper_doi               10.1039/D1RA06150J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C8 H8 O2 Te0.5'
_chemical_formula_sum            'C8 H8 O2 Te0.5'
_chemical_formula_weight         199.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.9927(4)
_cell_length_b                   15.9927(4)
_cell_length_c                   12.1188(4)
_cell_measurement_reflns_used    3503
_cell_measurement_temperature    101
_cell_measurement_theta_max      29.4190
_cell_measurement_theta_min      2.5470
_cell_volume                     3099.58(15)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00 -23.00   0.50   13.81    --    3.50  28.00 -77.00   54
  2  \w    -37.00  80.00   0.50   13.81    --    3.50  50.00-150.00  234
  3  \w      8.00  33.00   0.50   13.81    --    3.50  28.00 -77.00   50
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8462
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.309
_diffrn_reflns_theta_min         2.547
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.111
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1891
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+85.9728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1609
_reflns_number_total             1891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           200320
_cod_original_cell_volume        3099.58(19)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C8 H8 O2 Te0.50'
_cod_database_code               7243696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C005, C00B, C007, C008, C009, C004
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C007(H007), C009(H009), C00B(H00D)
3.b Idealised Me refined as rotating group:
 C00A(H00A,H00B,H00C)
;
_shelx_res_checksum              68127
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;