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_7712225
_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            'Cs2 O22 W7'
_chemical_formula_weight         1904.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 90.006(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.8497(3)
_cell_length_b                   7.3502(5)
_cell_length_c                   32.611(3)
_cell_measurement_reflns_used    1309
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      3.04
_cell_volume                     922.76(13)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(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 1.000
_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  0.1026
_diffrn_reflns_av_unetI/netI     0.1504
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            10850
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_min         1.249
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    47.439
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.3802.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.855
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.020
_refine_diff_density_max         8.990
_refine_diff_density_min         -11.986
_refine_diff_density_rms         1.062
_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   0.998
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          3.565
_refine_ls_shift/su_mean         0.146
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2376
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2648
_reflns_number_total             4291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00275f2.cif
_cod_data_source_block           Cs2W7O22
_cod_original_cell_volume        922.76(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7712225
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.173
_shelx_estimated_absorpt_t_max   0.450
_shelx_res_checksum              54865
_shelx_hkl_checksum              70108