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_7243700
_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         'C16 H10 F6 O4 Te'
_chemical_formula_sum            'C16 H10 F6 O4 Te'
_chemical_formula_weight         507.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-27
_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                 117.086(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5971(8)
_cell_length_b                   10.3078(2)
_cell_length_c                   19.7804(8)
_cell_measurement_reflns_used    15939
_cell_measurement_temperature    108
_cell_measurement_theta_max      29.4340
_cell_measurement_theta_min      2.8620
_cell_volume                     3557.5(3)
_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      108
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.842
_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    0.92    --    3.50  20.00 -48.00   50
  2  \w     -5.00  20.00   0.50    0.92    --   -4.40  20.00 -48.00   50
  3  \w    -69.00 -37.00   0.50    0.92    --    3.50  45.00-180.00   64
  4  \w     -8.00  19.00   0.50    0.92    --    3.50  45.00-180.00   54
  5  \w    -71.00  90.00   0.50    0.92    --    3.50  45.00 -90.00  322
;
_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      0.0248559000
_diffrn_orient_matrix_UB_12      0.0542392000
_diffrn_orient_matrix_UB_13      0.0138969000
_diffrn_orient_matrix_UB_21      0.0311075000
_diffrn_orient_matrix_UB_22      -0.0421318000
_diffrn_orient_matrix_UB_23      0.0211058000
_diffrn_orient_matrix_UB_31      0.0081929000
_diffrn_orient_matrix_UB_32      -0.0043467000
_diffrn_orient_matrix_UB_33      -0.0313530000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31082
_diffrn_reflns_point_group_measured_fraction_full 0.880
_diffrn_reflns_point_group_measured_fraction_max 0.690
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.444
_diffrn_reflns_theta_min         2.318
_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    1.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66610
_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    1.896
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.625
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Flack x determined using 4631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.506(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         13640
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0813P)^2^+3.7091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.770
_reflns_Friedel_fraction_max     0.539
_reflns_number_gt                12579
_reflns_number_total             13640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           191227-3
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H40 F24 O16 Te4'
_cod_original_formula_weight         2031.36
_cod_original_formula_moiety         '4(C16 H10 F6 O4 Te)'
_cod_original_formula_units_Z            2
_cod_database_code               7243700
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Te F'
_chemical_oxdiff_usercomment     Ph2TeOTFA2
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.407
_reflns_odcompleteness_completeness 97.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C01E(H01E), C01G(H01G), C01H(H01H), C01K(H01K), C01M(H01M), C01O(H01O),
 C01Q(H01Q), C01S(H01S), C01U(H01U), C01V(H01V), C01X(H01X), C021(H021),
 C024(H024), C025(H025), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P),
 C02Q(H02Q), C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W),
 C02X(H02X), C02Y(H02Y), C02Z(H02Z), C030(H030)
;
_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 1.319
_oxdiff_exptl_absorpt_empirical_full_min 0.834