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_7243702
_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         'C40 H32 O4 Te'
_chemical_formula_sum            'C40 H32 O4 Te'
_chemical_formula_weight         704.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-03
_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                 103.1360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.4494(4)
_cell_length_b                   11.2159(2)
_cell_length_c                   20.2540(3)
_cell_measurement_reflns_used    31355
_cell_measurement_temperature    103
_cell_measurement_theta_max      29.6030
_cell_measurement_theta_min      2.1830
_cell_volume                     6293.65(17)
_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      103
_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 0.926
_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     16.00  42.00   0.50   22.02    --    3.50  14.00 144.00   52
  2  \w    -13.00  12.00   0.50   22.02    --    3.50  14.00 144.00   50
  3  \w    -23.00   4.00   0.50   22.02    --    3.50  43.00  30.00   54
  4  \w    -85.00  93.00   0.50   22.02    --    3.50  40.00 120.00  356
  5  \w    -86.00  93.00   0.50   22.02    --    3.50  40.00  60.00  358
  6  \w    -60.00 -15.00   0.50   22.02    --    3.50  43.00-120.00   90
  7  \w      3.00  33.00   0.50   22.02    --    3.50  43.00-120.00   60
  8  \w     56.00  81.00   0.50   22.02    --    3.50  43.00-120.00   50
  9  \w    -86.00 -29.00   0.50   22.02    --    3.50  14.00 -60.00  114
 10  \w    -91.00   5.00   0.50   22.02    --   -4.40  43.00   0.00  192
 11  \w    -46.00 -21.00   0.50   22.02    --   -4.40  14.00 144.00   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      -0.0139086000
_diffrn_orient_matrix_UB_12      -0.0301987000
_diffrn_orient_matrix_UB_13      -0.0286129000
_diffrn_orient_matrix_UB_21      0.0214894000
_diffrn_orient_matrix_UB_22      -0.0200487000
_diffrn_orient_matrix_UB_23      -0.0085951000
_diffrn_orient_matrix_UB_31      -0.0001974000
_diffrn_orient_matrix_UB_32      -0.0518263000
_diffrn_orient_matrix_UB_33      0.0200216000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.411
_diffrn_reflns_theta_min         2.135
_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    0.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92445
_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    1.487
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 5601 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         15223
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0186P)^2^+12.3823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                13295
_reflns_number_total             15223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra06150j2.cif
_cod_data_source_block           200902-ph2teocochph22-2
_cod_database_code               7243702
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H32 O4 Te1'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.886
_reflns_odcompleteness_completeness 99.90
_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. Rigid bond restraints
 C6, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C70, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C6) = Uanis(C2)
Uanis(C10) = Uanis(C14)
Uanis(C1) = Uanis(C6)
Uanis(C8) = Uanis(C7)
Uanis(C48) = Uanis(C68) = Uanis(C8) = Uanis(C28)
Uanis(C69) = Uanis(C9) = Uanis(C35) = Uanis(C55)
Uanis(C12) = Uanis(C32) = Uanis(C52) = Uanis(C78)
Uanis(C61) = Uanis(C21) = Uanis(C1) = Uanis(C41)
Uanis(C47) = Uanis(C7) = Uanis(C67) = Uanis(C27)
Uanis(C71) = Uanis(C59) = Uanis(C17) = Uanis(C38)
Uanis(C51) = Uanis(C53)
Uanis(C29) = Uanis(C35)
4.a Ternary CH refined with riding coordinates:
 C8(H6), C28(H22), C48(H38), C68(H53)
4.b Aromatic/amide H refined with riding coordinates:
 C62(H49), C63(H50), C64(H51), C65(H52), C66(H66), C42(H33), C43(H34),
 C44(H35), C45(H36), C46(H37), C10(H7), C11(H8), C12(H9), C13(H10), C14(H11),
 C30(H23), C31(H24), C32(H25), C33(H26), C34(H27), C16(H12), C17(H13), C18(H14),
  C19(H15), C20(H16), C36(H28), C37(H29), C38(H30), C39(H31), C40(H32), C2(H1),
 C3(H2), C4(H3), C5(H4), C6(H5), C50(H39), C51(H40), C52(H41), C53(H42),
 C54(H43), C60(H48), C59(H47), C58(H46), C57(H45), C56(H44), C80(H63), C79(H62),
  C78(H61), C77(H60), C76(H59), C26(H21), C25(H20), C24(H19), C23(H18),
 C22(H17), C74(H58), C73(H57), C72(H56), C71(H55), C70(H54)
4.c Fitted hexagon refined as free rotating group:
 C61(C62,C63,C64,C65,C66), C41(C42,C43,C44,C45,C46), C9(C10,C11,C12,C13,C14),
 C29(C30,C31,C32,C33,C34), C15(C16,C17,C18,C19,C20), C35(C36,C37,C38,C39,C40),
 C1(C2,C3,C4,C5,C6), C49(C50,C51,C52,C53,C54), C55(C60,C59,C58,C57,C56),
 C75(C80,C79,C78,C77,C76), C21(C26,C25,C24,C23,C22), C69(C74,C73,C72,C71,C70)
;
_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 1.073
_oxdiff_exptl_absorpt_empirical_full_min 0.946