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_7131412
_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         'C11 H15 I O4 S, 2(C H Cl3)'
_chemical_formula_sum            'C13 H17 Cl6 I O4 S'
_chemical_formula_weight         608.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-04 deposited with the CCDC.	2023-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8103(13)
_cell_length_b                   23.9497(19)
_cell_length_c                   5.7108(5)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.71
_cell_volume                     2162.4(3)
_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)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            21328
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.519
_diffrn_reflns_theta_min         2.133
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.334
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details
;
 Flack x determined using 2263 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.219(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+22.3126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                5959
_reflns_number_total             6468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00549f2.cif
_cod_data_source_block           pt_rt
_cod_depositor_comments
'Adding full bibliography for 7131411--7131416.cif.'
_cod_database_code               7131412
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              97589
_shelx_hkl_checksum              58639
_olex2_submission_special_instructions 'No special instructions were received'