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_7712227
_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         'K4.002 O35 W11'
_chemical_formula_sum            'K4 O35 W11'
_chemical_formula_weight         2738.75
_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             2022-07-13
_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                 90.026(7)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   3.8184(5)
_cell_length_b                   7.2998(9)
_cell_length_c                   25.440(3)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.79
_cell_volume                     709.10(15)
_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 0.999
_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  0.0850
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            17089
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.608
_diffrn_reflns_theta_min         1.601
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    45.118
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0916 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.5935.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.413
_exptl_crystal_description       needle
_exptl_crystal_F_000             1170
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.923
_refine_diff_density_min         -11.028
_refine_diff_density_rms         0.931
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00079(19)
_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   1.082
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          4.592
_refine_ls_shift/su_mean         0.166
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+17.0568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4221
_reflns_number_total             4367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00275f2.cif
_cod_data_source_block           K4W11O35
_cod_original_cell_volume        709.11(15)
_cod_database_code               7712227
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.466
_shelx_estimated_absorpt_t_min   0.061
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.23947
 0.26214 0.25936 0.23903
2. Restrained distances
 W2-O4
 1.7 with sigma of 0.01
3. Others
 1*[Sof(K1)]+1*[Sof(K2)]+1*[Sof(K4)]=1.5 with esd of 0
 Sof(W6B)=Sof(O18B)=1-FVAR(1)
 Sof(W6A)=Sof(O18A)=FVAR(1)
 Fixed Sof: W1(0.5) O1(0.5)
 Fixed Y: W1(0)
;
_shelx_res_checksum              67048
_shelx_hkl_checksum              96021
_olex2_submission_special_instructions 'No special instructions were received'