ArI(NTf2)2: The boundary of oxidative capacity for ArIL2?
Dutton, Jason Laurence; Barwise, Lachlan; Bennetts, Jason; White, Keith Forrest; Chemical Communications  (2023) –; doi:10.1039/D3CC04563C

data_7132211
_publ_section_title
;
 ArI(NTf2)2: The boundary of oxidative capacity for ArIL2?
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04563C
_journal_year                    2023
_chemical_formula_moiety         '2(C10 H4 F12 I N3 O10 S4), C H Cl3'
_chemical_formula_sum            'C21 H9 Cl3 F24 I2 N6 O20 S8'
_chemical_formula_weight         1737.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-11 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.786(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4882(3)
_cell_length_b                   12.8733(3)
_cell_length_c                   15.4391(3)
_cell_measurement_reflns_used    21635
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.1500
_cell_measurement_theta_min      4.0820
_cell_volume                     2656.09(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  26.00   0.50    1.42    --  -38.50  76.00 163.00  178
  2  \w    -20.00  67.00   0.50    1.42    --   42.60 -76.00  36.00  174
  3  \w     36.00 125.00   0.50    5.69    --  100.00 -76.00  36.00  178
  4  \w    104.00 165.00   0.50    5.69    --  100.00  76.00 163.00  122
  5  \w   -102.00 -16.00   0.50    1.42    --  -38.50 -71.00-109.61  172
  6  \w    -56.00  25.00   0.50    1.42    --  -38.50  54.00 -30.00  162
  7  \w    -74.00  14.00   0.50    1.42    --  -38.50 104.00-120.00  176
  8  \w   -101.00 -21.00   0.50    1.42    --  -38.50 -54.00  90.00  160
  9  \w   -104.00 -30.00   0.50    1.42    --  -38.50 -32.00-180.00  148
 10  \w   -101.00 -25.00   0.50    1.42    --  -38.50 -43.00   0.00  152
 11  \w   -102.00 -16.00   0.50    1.42    --  -38.50 -70.00 -28.86  172
 12  \w    -27.00  53.00   0.50    1.42    --   42.60 -21.00  30.00  160
 13  \w     -8.00  71.00   0.50    1.42    --   42.60 -89.00  90.00  158
 14  \w     34.00 108.00   0.50    1.42    --   42.60  32.00-120.00  148
 15  \w    -20.00  60.00   0.50    1.42    --   42.60 -54.00 150.00  160
 16  \w     35.00  98.00   0.50    1.42    --   42.60-138.00-150.00  126
 17  \w    -23.00  51.00   0.50    1.42    --   42.60 -32.00 -90.00  148
 18  \w     35.00  98.00   0.50    1.42    --   42.60-138.00 -60.00  126
 19  \w     34.00 108.00   0.50    1.42    --   42.60  32.00   0.00  148
 20  \w     35.00  98.00   0.50    1.42    --   42.60-138.00 120.00  126
 21  \w     34.00 108.00   0.50    1.42    --   42.60  32.00 150.00  148
 22  \w    104.00 165.00   0.50    5.69    --  100.00  77.00  30.00  122
 23  \w     35.00 109.00   0.50    5.69    --  100.00-117.00  60.00  148
 24  \w     86.00 171.00   0.50    5.69    --  100.00  17.00   0.00  170
 25  \w     30.00 106.00   0.50    5.69    --  100.00 -96.00-120.00  152
 26  \w     25.00 130.00   0.50    5.69    --  100.00  -8.00   0.00  210
 27  \w     35.00 109.00   0.50    5.69    --  100.00-117.00 120.00  148
 28  \w     38.00 126.00   0.50    5.69    --  100.00-145.00   0.00  176
 29  \w     38.00 126.00   0.50    5.69    --  100.00-145.00 150.00  176
 30  \w     38.00 126.00   0.50    5.69    --  100.00-145.00 -60.00  176
 31  \w     79.00 164.00   0.50    5.69    --  100.00  68.00 120.00  170
 32  \w     36.00 122.00   0.50    5.69    --  100.00 -68.00 150.00  172
 33  \w     35.00 109.00   0.50    5.69    --  100.00-117.00 -30.00  148
 34  \w     32.00 109.00   0.50    5.69    --  100.00 -25.00  60.00  154
 35  \w     87.00 164.00   0.50    5.69    --  100.00 145.00-120.00  154
 36  \w    104.00 165.00   0.50    5.69    --  100.00  77.00 120.00  122
 37  \w     81.00 164.00   0.50    5.69    --  100.00  60.00-164.25  166
 38  \w     34.00 109.00   0.50    5.69    --  100.00-112.00  90.34  150
 39  \w     35.00 109.00   0.50    5.69    --  100.00-117.00-150.00  148
 40  \w    105.00 170.00   0.50    5.69    --  100.00  96.00   0.00  130
 41  \w     79.00 164.00   0.50    5.69    --  100.00  67.00 -93.91  170
 42  \w     35.00 109.00   0.50    5.69    --  100.00-117.00-180.00  148
 43  \w     38.00 126.00   0.50    5.69    --  100.00-145.00 -90.00  176
 44  \w    105.00 170.00   0.50    5.69    --  100.00  96.00  90.00  130
 45  \w    104.00 165.00   0.50    5.69    --  100.00  77.00  60.00  122
 46  \w     36.00 122.00   0.50    5.69    --  100.00 -68.00 -90.00  172
 47  \w     36.00 122.00   0.50    5.69    --  100.00 -68.00  60.00  172
 48  \w     30.00 106.00   0.50    5.69    --  100.00 -96.00 -30.00  152
 49  \w     30.00 106.00   0.50    5.69    --  100.00 -96.00   0.00  152
 50  \w     37.00 119.00   0.50    5.69    --  100.00 -59.00  90.00  164
 51  \w     79.00 164.00   0.50    5.69    --  100.00  68.00 -30.00  170
 52  \w    104.00 165.00   0.50    5.69    --  100.00  77.00  90.00  122
 53  \w    102.00 165.00   0.50    5.69    --  100.00 117.00 -30.00  126
 54  \w     30.00 106.00   0.50    5.69    --  100.00 -96.00  30.00  152
 55  \w     87.00 164.00   0.50    5.69    --  100.00 145.00  30.00  154
 56  \w     37.00 113.00   0.50    5.69    --  100.00 -42.00  60.00  152
 57  \w     36.00 126.00   0.50    5.69    --  100.00 -77.00   0.00  180
 58  \w     37.00 113.00   0.50    5.69    --  100.00 -42.00-180.00  152
 59  \w     35.00 109.00   0.50    5.69    --  100.00-117.00   0.00  148
 60  \w     87.00 157.00   0.50    5.69    --  100.00 145.00 120.00  140
 61  \w     45.00 107.00   0.50    5.69    --  100.00 -42.00   0.00  124
 62  \w     99.00 125.00   0.50    5.69    --  100.00  40.00-103.40   52
 63  \w    116.00 142.00   0.50    5.69    --  100.00 145.00 -30.00   52
 64  \w    104.00 130.00   0.50    5.69    --  100.00  68.00 150.00   52
 65  \w     78.00 162.00   0.50    5.69    --  100.00  73.00  46.45  168
 66  \w    112.00 138.00   0.50    5.69    --  100.00 117.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0321684000
_diffrn_orient_matrix_UB_12      0.1115352000
_diffrn_orient_matrix_UB_13      0.0271856000
_diffrn_orient_matrix_UB_21      -0.0167410000
_diffrn_orient_matrix_UB_22      0.0335031000
_diffrn_orient_matrix_UB_23      -0.0966134000
_diffrn_orient_matrix_UB_31      -0.1094272000
_diffrn_orient_matrix_UB_32      0.0275200000
_diffrn_orient_matrix_UB_33      0.0083889000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52623
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.519
_diffrn_reflns_theta_min         4.087
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+5.0265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4680
_reflns_number_total             5152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04563c2.cif
_cod_data_source_block           ldb-no2phif2+2tmsntf
_cod_database_code               7132211
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.464
_shelx_estimated_absorpt_t_min   0.031
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cl1(0.5) C1(0.5) H1(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00Y(H00Y), C00Z(H00Z), C012(H012)
;
_shelx_res_checksum              89713
_shelx_hkl_checksum              96151
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.219
_oxdiff_exptl_absorpt_empirical_full_min 0.559