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_1561181
_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         'C42 H54 Cl2 O7 Se2 Te'
_chemical_formula_sum            'C42 H54 Cl2 O7 Se2 Te'
_chemical_formula_weight         1027.27
_chemical_name_common            2SeTe-ox-Cl
_chemical_name_systematic        2SeTe-ox-Cl
_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
_audit_creation_date             2020-12-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                106.116(9)
_cell_angle_beta                 104.058(11)
_cell_angle_gamma                96.560(9)
_cell_formula_units_Z            2
_cell_length_a                   9.902(3)
_cell_length_b                   14.643(4)
_cell_length_c                   16.120(5)
_cell_measurement_reflns_used    8149
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.31
_cell_volume                     2136.4(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18444
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.717
_diffrn_reflns_theta_min         2.162
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5073
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1533 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.6804.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.895
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9758
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1526P)^2^+1.4719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7011
_reflns_number_total             9758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00397f2.cif
_cod_data_source_block           2SeTe-ox-Cl
_cod_depositor_comments
'Adding full bibliography for 1561180--1561185.cif.'
_cod_original_cell_volume        2136.5(10)
_cod_database_code               1561181
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C33
 1.48 with sigma of 0.001
 C34-C32
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O4, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              7473
_olex2_submission_special_instructions 'No special instructions were received'