A tellura-Baeyer‒Villiger oxidation: one-step transformation of tellurophene into chiral tellurinate lactone
Wang, Shitao; Yan, Chaoxian; Zhao, Wenlong; Liu, Xiaolan; Yuan, Cheng-Shan; Zhang, Hao-Li; Shao, Xiangfeng; Chemical Science 12 (2021) 5811–5817; doi:10.1039/D1SC00397F

data_1561183
_publ_section_title
;
 A tellura-Baeyer--Villiger oxidation: one-step transformation of
 tellurophene into chiral tellurinate lactone
;
_journal_issue                   16
_journal_name_full               'Chemical Science'
_journal_page_first              5811
_journal_page_last               5817
_journal_paper_doi               10.1039/D1SC00397F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C84 H116 O16 Te2'
_chemical_formula_sum            'C84 H116 O16 Te2'
_chemical_formula_weight         1636.96
_chemical_name_common            Te-Ox
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-07 deposited with the CCDC.	2021-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 136.4590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.1328(11)
_cell_length_b                   20.3253(7)
_cell_length_c                   29.5440(8)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.308
_cell_measurement_theta_min      2.260
_cell_volume                     16187.8(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54345
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         2.240
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0895 before and 0.0589 after correction. The Ratio of minimum to maximum transmission is 0.8768. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             6816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         16140
_refine_ls_number_restraints     1002
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0242P)^2^+24.1819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11739
_reflns_number_total             16140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00397f2.cif
_cod_data_source_block           04074teoxo_0m_sq
_cod_depositor_comments
'Adding full bibliography for 1561180--1561185.cif.'
_cod_original_cell_volume        16187.7(9)
_cod_database_code               1561183
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.810
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Others
 Fixed Sof: H75C(0.5) H75D(0.5) H75A(0.5) H75B(0.5) H31C(0.75) H31D(0.75)
 H31A(0.25) H31B(0.25) H78D(0.5) H78E(0.5) H78F(0.5) H78A(0.5) H78B(0.5)
 H78C(0.5) C33(0.75) H33A(0.75) H33B(0.75) C35(0.75) H35A(0.75) H35B(0.75)
 C76(0.5) H76A(0.5) H76B(0.5) H36D(0.75) H36E(0.75) H36F(0.75) H36A(0.25)
 H36B(0.25) H36C(0.25) C77(0.5) H77A(0.5) H77B(0.5) C79(0.5) H79A(0.5)
 H79B(0.5) C80(0.5) H80A(0.5) H80B(0.5) C32(0.25) H32A(0.25) H32B(0.25)
 C34(0.25) H34A(0.25) H34B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C27(H27A,H27B), C4(H4A,H4B), C50(H50A,H50B), C41(H41A,H41B),
 C49(H49A,H49B), C28(H28A,H28B), C51(H51A,H51B), C3(H3A,H3B), C46(H46A,H46B),
 C81(H81A,H81B), C71(H71A,H71B), C5(H5A,H5B), C82(H82A,H82B), C67(H67A,H67B),
 C75(H75C,H75D), C75(H75A,H75B), C38(H38A,H38B), C68(H68A,H68B), C43(H43A,H43B),
  C42(H42A,H42B), C37(H37A,H37B), C83(H83A,H83B), C73(H73A,H73B), C39(H39A,
 H39B), C2(H2A,H2B), C29(H29A,H29B), C6(H6A,H6B), C69(H69A,H69B), C72(H72A,
 H72B), C31(H31C,H31D), C31(H31A,H31B), C47(H47A,H47B), C7(H7C,H7D), C33(H33A,
 H33B), C35(H35A,H35B), C76(H76A,H76B), C77(H77A,H77B), C79(H79A,H79B),
 C80(H80A,H80B), C32(H32A,H32B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C14B(H14B), C7A(H7A), C15B(H15B), C15A(H15A), C18B(H18B), C14A(H14A),
 C18A(H18A), C7B(H7B)
5.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C44(H44A,H44B,H44C), C84(H84A,H84B,H84C), C30(H30A,H30B,
 H30C), C1(H1A,H1B,H1C), C74(H74A,H74B,H74C), C40(H40A,H40B,H40C), C48(H48A,
 H48B,H48C), C78(H78D,H78E,H78F), C78(H78A,H78B,H78C), C70(H70A,H70B,H70C),
 C8(H8A,H8B,H8C), C36(H36D,H36E,H36F), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              86227
_shelx_fab_checksum              63701
_olex2_submission_special_instructions 'No special instructions were received'