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_7243701
_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         'C18 H20 O6 Te'
_chemical_formula_sum            'C18 H20 O6 Te'
_chemical_formula_weight         459.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-30
_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                 101.416(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4353(3)
_cell_length_b                   11.8064(4)
_cell_length_c                   16.9075(5)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    112.3
_cell_measurement_theta_max      29.0790
_cell_measurement_theta_min      2.8510
_cell_volume                     1846.18(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      112.3
_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 0.895
_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     52.00  77.00   0.50   15.64    --   -4.20  53.00  77.00   50
  2  \w    -85.00 -60.00   0.50   15.64    --   -4.20  53.00  77.00   50
  3  \w    -83.00  92.00   0.50   15.64    --    3.40  14.00 120.00  350
  4  \w    -13.00  22.00   0.50   15.64    --    3.40  40.00  30.00   70
  5  \w     27.00  60.00   0.50   15.64    --    3.40  40.00  30.00   66
  6  \w    -24.00   2.00   0.50   15.64    --    3.40  29.00-120.00   52
  7  \w     15.00  41.00   0.50   15.64    --    3.40  29.00-120.00   52
  8  \w    -71.00  20.00   0.50   15.64    --    3.40  40.00 -30.00  182
  9  \w    -21.00   4.00   0.50   15.64    --    3.40  53.00  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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0150749000
_diffrn_orient_matrix_UB_12      -0.0468152000
_diffrn_orient_matrix_UB_13      0.0265552000
_diffrn_orient_matrix_UB_21      0.0751691000
_diffrn_orient_matrix_UB_22      0.0102125000
_diffrn_orient_matrix_UB_23      0.0040330000
_diffrn_orient_matrix_UB_31      -0.0016032000
_diffrn_orient_matrix_UB_32      0.0362578000
_diffrn_orient_matrix_UB_33      0.0333198000
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.330
_diffrn_reflns_theta_min         2.458
_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    1.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91957
_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    1.655
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0224P)^2^+2.7421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3840
_reflns_number_total             4525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           210429-an2teoac2
_cod_database_code               7243701
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H20 O6 Te1'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.821
_reflns_odcompleteness_completeness 99.75
_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(H00C), C00D(H00D), C00F(H00F), C00G(H00G), C00H(H00H),
 C00J(H00J), C00N(H00N)
2.b Idealised Me refined as rotating group:
 C00I(H00B,H00E,H00I), C00L(H00K,H00L,H00M), C00O(H00O,H00P,H00Q), C00P(H00R,
 H00S,H00T)
;
_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 1.075
_oxdiff_exptl_absorpt_empirical_full_min 0.939