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_7712230
_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         'O35 Tl4 W11'
_chemical_formula_sum            'O35 Tl4 W11'
_chemical_formula_weight         3399.83
_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             2021-11-04
_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                 98.109(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.3114(8)
_cell_length_b                   3.8154(4)
_cell_length_c                   25.877(3)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.33
_cell_measurement_theta_min      2.38
_cell_volume                     714.65(14)
_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      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 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0616
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            18889
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.335
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    66.626
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1388 before and 0.0639 after correction. The Ratio of minimum to maximum transmission is 0.4320. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    7.900
_exptl_crystal_description       plate
_exptl_crystal_F_000             1418
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.02
_refine_diff_density_max         9.229
_refine_diff_density_min         -8.440
_refine_diff_density_rms         1.003
_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   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         5465
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.263
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+41.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5390
_reflns_number_total             5465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00275f2.cif
_cod_data_source_block           Tl4W11O35
_cod_original_cell_volume        714.65(13)
_cod_database_code               7712230
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.082
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.25781
 0.25283 0.26478 0.22458
2. Restrained distances
 W1A-O1
 1.7 with sigma of 0.03
 W3-O8
 1.75 with sigma of 0.02
3. Others
 0.5*[Sof(Tl1)]+1*[Sof(Tl2)]+1*[Sof(Tl3)]=2 with esd of 0
 Sof(W1A)=0.5*(1-FVAR(2))
 Sof(W1B)=0.5*FVAR(2)
 Fixed Sof: O1(0.5)
 Fixed Y: Tl1(0)
;
_shelx_res_checksum              7949
_shelx_hkl_checksum              37389
_olex2_submission_special_instructions 'No special instructions were received'