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_7063389
_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(C12 H8 N2), C7 H8'
_chemical_formula_sum            'C87 H104 N4 O8 Te2'
_chemical_formula_weight         1588.94
_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             2024-06-24
_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                107.420(4)
_cell_angle_beta                 108.898(3)
_cell_angle_gamma                98.439(4)
_cell_formula_units_Z            1
_cell_length_a                   10.5866(11)
_cell_length_b                   13.8449(13)
_cell_length_c                   15.3756(15)
_cell_measurement_reflns_used    2082
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      2.52
_cell_volume                     1958.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39449
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.608
_diffrn_reflns_theta_min         2.280
_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    0.803
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1537 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.9370.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       prism
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9465
_reflns_number_total             10687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02469a3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063385--7063390.cif.'
_cod_database_code               7063389
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Restrained distances
 C2S-C3S \\sim C3S-C4S \\sim C4S-C5S \\sim C5S-C6S \\sim C6S-C7S \\sim C7S-C2S
 with sigma of 0.02
2. Restrained planarity
 C2S, C3S, C4S, C5S, C6S, C7S, C1S
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S \\sim C1S: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) C3S(0.5) H3S(0.5)
 C4S(0.5) H4S(0.5) C5S(0.5) H5S(0.5) C6S(0.5) H6S(0.5) C7S(0.5) H7S(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C4(H4), C29(H29), C5(H5), C36(H36), C40(H40), C31(H31),
 C30(H30), C39(H39), C38(H38), C37(H37), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S),
  C7S(H7S)
5.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C14(H14A,
 H14B,H14C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              89576
_olex2_submission_special_instructions 'No special instructions were received'