Selective multi-electron aggregation at a hypervalent iodine center by sequential disproportionation.
Thai, Phong; Frey, Brandon L.; Figgins, Matthew T.; Thompson, Richard R.; Carmieli, Raanan; Powers, David C.; Chemical communications (Cambridge, England) 59 (2023) 4308–4311; doi:10.1039/d3cc00549f

data_7131415
_publ_section_title
;
 Selective multi-electron aggregation at a hypervalent iodine center by
 sequential disproportionation.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4308
_journal_page_last               4311
_journal_paper_doi               10.1039/d3cc00549f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C22 H30 I2 O7.5 S2, Cl O4'
_chemical_formula_sum            'C22 H30 Cl I2 O11.5 S2'
_chemical_formula_weight         831.85
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-07-12 deposited with the CCDC.	2023-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.8420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.080(3)
_cell_length_b                   9.9990(9)
_cell_length_c                   20.9926(19)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.16
_cell_volume                     5898.7(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49267
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.002
_diffrn_reflns_theta_min         1.956
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         7130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0033P)^2^+25.6211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5742
_reflns_number_total             7130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00549f2.cif
_cod_data_source_block           hiresolution
_cod_depositor_comments
'Adding full bibliography for 7131411--7131416.cif.'
_cod_original_cell_volume        5898.6(9)
_cod_original_formula_sum        'C22 H30 Cl I2 O11.50 S2'
_cod_database_code               7131415
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Others
 Fixed Sof: O9(0.667) O10(0.667) O11(0.667) O12(0.667) O14(0.33333)
 O13(0.33333) O15(0.33333) O16(0.33333)
;
_shelx_res_checksum              67359
_shelx_hkl_checksum              38950
_olex2_submission_special_instructions 'No special instructions were received'