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_7131416
_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 O5 S, C H2 Cl2'
_chemical_formula_sum            'C12 H17 Cl2 I O5 S'
_chemical_formula_weight         475.173
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-03-04
_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                84.158(4)
_cell_angle_beta                 73.474(4)
_cell_angle_gamma                68.652(5)
_cell_formula_units_Z            10
_cell_length_a                   13.6039(7)
_cell_length_b                   14.7431(8)
_cell_length_c                   23.6714(8)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.21
_cell_volume                     4239.2(4)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.8975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1309
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_Laue_measured_fraction_full 0.9999
_diffrn_reflns_Laue_measured_fraction_max 0.8975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            166139
_diffrn_reflns_point_group_measured_fraction_full 0.9999
_diffrn_reflns_point_group_measured_fraction_max 0.8975
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.79
_diffrn_reflns_theta_min         1.67
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5196
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.6974.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2361.427
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.1896
_refine_diff_density_min         -2.2554
_refine_diff_density_rms         0.4672
_refine_ls_d_res_high            0.7152
_refine_ls_d_res_low             12.2105
_refine_ls_goodness_of_fit_ref   1.0381
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    125
_refine_ls_number_parameters     966
_refine_ls_number_reflns         21788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0381
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+18.2321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                15053
_reflns_number_total             21788
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc00549f2.cif
_cod_data_source_block           PT_3_50_DCM_Pent_100mm_autored
_cod_depositor_comments
'Adding full bibliography for 7131411--7131416.cif.'
_cod_database_code               7131416
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C58(H58b,H58a), C56(H56a,H56b), C57(H57a,H57b), C59(H59a,H59b), C60(H60a,H60b)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C36(H36), C3(H3), C38(H38), C39(H39), C47(H47), C27(H27), C25(H25),
 C28(H28), C6(H6), C5(H5), C49(H49), C16(H16), C50(H50), C17(H17)
2.c Idealised Me refined as rotating group:
 C55(H55a,H55b,H55c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C31(H31a,H31b,
 H31c), C32(H32a,H32b,H32c), C29(H29a,H29b,H29c), C20(H20a,H20b,H20c), C33(H33a,
 H33b,H33c), C54(H54a,H54b,H54c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c),
 C40(H40a,H40b,H40c), C53(H53a,H53b,H53c), C42(H42a,H42b,H42c), C11(H11a,H11b,
 H11c), C10(H10a,H10b,H10c), C18(H18a,H18b,H18c), C51(H51a,H51b,H51c), C7(H7a,
 H7b,H7c), C9(H9a,H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'