Adducts of a sterically hindered tellurium(iv) catecholate with diimines
Petrov, Pavel A.; Filippova, Elizaveta A.; Sukhikh, Taisiya S.; Sheven, Dmitriy G.; Novikov, Alexander S.; New Journal of Chemistry 48 (2024) 15483–15492; doi:10.1039/D4NJ02469A

data_7063388
_publ_section_title
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 Adducts of a sterically hindered tellurium(iv) catecholate with diimines
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15483
_journal_page_last               15492
_journal_paper_doi               10.1039/D4NJ02469A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         '2(C28 H40 O4 Te), 2(C14 H12 N2), C7 H8'
_chemical_formula_sum            'C91 H112 N4 O8 Te2'
_chemical_formula_weight         1645.04
_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             2023-02-11
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2024-07-25 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                80.2200(10)
_cell_angle_beta                 86.4680(10)
_cell_angle_gamma                84.5760(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0622(2)
_cell_length_b                   18.5721(5)
_cell_length_c                   22.3625(6)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.27
_cell_volume                     4095.42(18)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56055
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.035
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0975 before and 0.0510 after correction. The Ratio of minimum to maximum transmission is 0.9274. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       needle
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         17956
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13542
_reflns_number_total             17956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02469a3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7063385--7063390.cif.'
_cod_original_cell_volume        4095.43(18)
_cod_database_code               7063388
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Restrained distances
 C1S-C2S \\sim C1A-C2A
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S \\sim C1A \\sim
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=
 Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=Sof(C7S)=Sof(H7S)=FVAR(1)
4.a Me refined as rotating group:
 C84(H84A,H84B,H84C), C1S(H1SA,H1SB,H1SC)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C18(H18), C19(H19), C32(H32), C33(H33), C46(H46), C47(H47),
 C57(H57), C58(H58), C65(H65), C66(H66), C67(H67), C68(H68), C71(H71), C72(H72),
  C79(H79), C80(H80), C81(H81), C82(H82), C3S(H3S), C4S(H4S), C5S(H5S),
 C6S(H6S), C7S(H7S), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A)
4.c Fitted hexagon refined as free rotating group:
 C2S(C3S,C4S,C5S,C6S,C7S), C2A(C3A,C4A,C5A,C6A,C7A)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C83(H83A,H83B,H83C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              57541
_olex2_submission_special_instructions 'No special instructions were received'