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_7243697
_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         '0.5(C16 H14 F2 O4 Te)'
_chemical_formula_sum            'C8 H7 F O2 Te0.5'
_chemical_formula_weight         217.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   16.7448(2)
_cell_length_b                   16.7448(2)
_cell_length_c                   11.7851(3)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    114
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      3.2230
_cell_volume                     3304.40(10)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      114
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.915
_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    -21.00   4.00   0.50    7.38    --    3.50  15.00 103.00   50
  2  \w    -47.00   0.00   0.50    7.38    --   -4.40  15.00 103.00   94
  3  \w     -5.00  93.00   0.50    7.38    --    3.50  40.00  60.00  196
  4  \w     -1.00  86.00   0.50    7.38    --    3.50  40.00-180.00  174
  5  \w    -62.00 -35.00   0.50    7.38    --    3.50  40.00  60.00   54
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0078779000
_diffrn_orient_matrix_UB_12      0.0068840000
_diffrn_orient_matrix_UB_13      -0.0583131000
_diffrn_orient_matrix_UB_21      0.0317101000
_diffrn_orient_matrix_UB_22      -0.0280488000
_diffrn_orient_matrix_UB_23      0.0019821000
_diffrn_orient_matrix_UB_31      -0.0269751000
_diffrn_orient_matrix_UB_32      -0.0309846000
_diffrn_orient_matrix_UB_33      -0.0147123000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15815
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.346
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84373
_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    1.752
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.1625
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.0875
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1377 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.46(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3915
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+2.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0419
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.800
_reflns_number_gt                3247
_reflns_number_total             3915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           210422-pfph2teoac2-2
_cod_original_cell_volume        3304.40(12)
_cod_original_formula_sum        'C8 H7 F O2 Te0.50'
_cod_database_code               7243697
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H14 O4 Te1 F2'
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.755
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00C(H00F), C00E(H00E), C00G(H00G), C00I(H00I), C00K(H00K),
 C00L(H00M), C00M(H00N)
2.b Idealised Me refined as rotating group:
 C00J(H00H,H00J,H00L), C00N(H00B,H00C,H00D)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.950