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_7243698
_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         'C22 H28 O4 Te'
_chemical_formula_sum            'C22 H28 O4 Te'
_chemical_formula_weight         484.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-28
_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                115.288(3)
_cell_angle_beta                 104.367(3)
_cell_angle_gamma                91.682(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5423(3)
_cell_length_b                   11.0370(3)
_cell_length_c                   11.4973(3)
_cell_measurement_reflns_used    13161
_cell_measurement_temperature    108
_cell_measurement_theta_max      29.4640
_cell_measurement_theta_min      2.5800
_cell_volume                     1047.86(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.858
_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     -4.00  93.00   0.50    0.50    --    3.50  14.00 -90.00  194
  2  \w    -86.00  68.00   0.50    0.50    --    3.50  45.00 -90.00  308
  3  \w    -86.00 -25.00   0.50    0.50    --    3.50  43.00 150.00  122
  4  \w     -8.00  19.00   0.50    0.50    --    3.50  43.00 150.00   54
  5  \w     42.00  93.00   0.50    0.50    --    3.50  43.00 150.00  102
  6  \w    -64.00   4.00   0.50    0.50    --    3.50  43.00  30.00  136
  7  \w     54.00  83.00   0.50    0.50    --    3.50  43.00  30.00   58
  8  \w    -85.00 -29.00   0.50    0.50    --    3.50  14.00 -90.00  112
;
_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      -0.0176137000
_diffrn_orient_matrix_UB_12      -0.0339977000
_diffrn_orient_matrix_UB_13      0.0359461000
_diffrn_orient_matrix_UB_21      0.0179777000
_diffrn_orient_matrix_UB_22      0.0623211000
_diffrn_orient_matrix_UB_23      0.0594674000
_diffrn_orient_matrix_UB_31      -0.0734737000
_diffrn_orient_matrix_UB_32      0.0116490000
_diffrn_orient_matrix_UB_33      -0.0157914000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.419
_diffrn_reflns_theta_min         2.159
_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    1.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83761
_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    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.617
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+1.1127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4630
_reflns_number_total             4969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           191028-mes2teoac2
_cod_database_code               7243698
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Te'
_reflns_odcompleteness_completeness 99.70
_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:
 C00C(H00g), C00F(H00h), C00H(H00i), C00K(H00m)
2.b Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C00B(H00d,H00e,H00f), C00I(H00j,H00k,H00l), C00N(H00n,
 H00o,H00p), C00O(H00q,H00r,H00s), C00P(H00t,H00u,H00v), C00Q(H00w,H00x,H00y),
 C00R(H00z,H,Ha)
;
_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 1.163
_oxdiff_exptl_absorpt_empirical_full_min 0.904