Synthesis, structural characterization, reactivity and catalytic activity of mixed halo/triflate ArI(OTf)(X) species
Dutton, Jason Laurence; Sharp-Bucknall, Lachlan; Sceney, Marcus; White, Keith Forrest; Dalton Transactions  (2023) –; doi:10.1039/D3DT00275F

data_7712229
_publ_section_title
;
 Synthesis, structural characterization, reactivity and catalytic activity
 of mixed halo/triflate ArI(OTf)(X) species
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00275F
_journal_year                    2023
_chemical_formula_sum            'Cs4 O35 W11'
_chemical_formula_weight         3113.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-10-06 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.962(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.3357(5)
_cell_length_b                   3.8684(3)
_cell_length_c                   26.4516(18)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      2.33
_cell_volume                     743.39(9)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 PIXEL
_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 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            21365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.223
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    47.304
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1024 before and 0.0599 after correction. The Ratio of minimum to maximum transmission is 0.6125. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.956
_exptl_crystal_description       plate
_exptl_crystal_F_000             1314
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         6.028
_refine_diff_density_min         -9.635
_refine_diff_density_rms         0.688
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          8.881
_refine_ls_shift/su_mean         0.422
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+9.7065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5319
_reflns_number_total             5683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00275f2.cif
_cod_data_source_block           Cs4W11O35
_cod_original_sg_symbol_H-M      'P 2'
_cod_database_code               7712229
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.201
_shelx_estimated_absorpt_t_max   0.649
_shelx_res_checksum              30943
_shelx_hkl_checksum              75978