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_7712228
_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_moiety         'K2.001 O22 W7'
_chemical_formula_sum            'K2 O22 W7'
_chemical_formula_weight         1717.15
_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_date             2022-07-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-10-06 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.472(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3142(5)
_cell_length_b                   3.8123(3)
_cell_length_c                   31.947(2)
_cell_measurement_reflns_used    9092
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.57
_cell_volume                     885.13(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0584
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            23831
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.256
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    45.872
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.5507.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.484
_refine_diff_density_min         -9.143
_refine_diff_density_rms         0.758
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          3.321
_refine_ls_shift/su_mean         0.079
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+83.8331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6519
_reflns_number_total             6698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00275f2.cif
_cod_data_source_block           K2W7O22
_cod_database_code               7712228
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.208
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.27544
 0.24568 0.22563 0.25325
2. Restrained distances
 K1-O6_$1
 2.7 with sigma of 0.03
3. Others
 0.5*[Sof(K2)]+1*[Sof(K3A)]+1*[Sof(K3B)]+1*[Sof(K4A)]+1*[Sof(K4B)]=1.5 with
 esd of 0
 Sof(W4B)=Sof(O12B)=1-FVAR(1)
 Sof(W4A)=Sof(O12A)=FVAR(1)
 Fixed Sof: O21(0.5)
 Fixed Y: K1(0)
;
_shelx_res_checksum              66094
_shelx_hkl_checksum              49966
_olex2_submission_special_instructions 'No special instructions were received'