Dicationic oligotelluroxane or mononuclear telluronium cation? Elucidation of true catalytic species and activation mechanism of benzylic carbon-halogen bond
Takagi, Koji; Sakakibara, Nao; Kikkawa, Shoko; Tsuzuki, Seiji; Chemical Communications  (2021) –; doi:10.1039/D1CC06311A

data_7129292
_publ_section_title
;
 Dicationic oligotelluroxane or mononuclear telluronium cation?
 Elucidation of true catalytic species and activation mechanism of
 benzylic carbon-halogen bond
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06311A
_journal_year                    2021
_chemical_formula_moiety         'C44 H24 F24 O8 S2 Te3'
_chemical_formula_sum            'C44 H24 F24 O8 S2 Te3'
_chemical_formula_weight         1583.55
_chemical_properties_physical    Moisture-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                63.246(2)
_cell_angle_beta                 87.5183(17)
_cell_angle_gamma                89.9450(19)
_cell_formula_units_Z            2
_cell_length_a                   12.4890(3)
_cell_length_b                   15.9524(4)
_cell_length_c                   16.1392(3)
_cell_measurement_reflns_used    17452
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.81
_cell_volume                     2867.88(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46206
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.423
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512.00
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as guest
atoms were unsuccessful. The data were corrected for disordered
electron density through use of the SQUEEZE procedure (Sluis, P. van der;
Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
(Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose
crystallographic tool. Utrecht University, Utrecht, The Netherlands).
A total solvent-accessible void volume of 270.0 A^3^ with a total
electron count of 50 was found in the unit cell.
;
_refine_diff_density_max         2.28
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     947
_refine_ls_number_reflns         12988
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.6819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9365
_reflns_number_total             12988
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1cc06311a2.cif
_cod_data_source_block           210805_NS171_01_dryAN
_cod_database_code               7129292
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              56943
_shelx_fab_checksum              38489