Lewis acid activation of Weiss’ reagents ([PhI(Pyr) <sub>2</sub> ] <sup>2+</sup> ) with boranes and isolation of [PhI(4-DMAP)] <sup>2+</sup>
Bakro, Aseel; Sharp-Bucknall, Lachlan; Poynder, Tiffany B.; Clegg, Jack K.; Wilson, David J. D.; Dutton, Jason L.; Chemical Communications 57 (2021) 12163–12166; doi:10.1039/D1CC04725F

data_1565103
_publ_section_title
;
 Lewis acid activation of Weiss&#x2019; reagents ([PhI(Pyr) <sub>2</sub> ]
 <sup>2+</sup> ) with boranes and isolation of [PhI(4-DMAP)] <sup>2+</sup>
;
_journal_issue                   91
_journal_name_full               'Chemical Communications'
_journal_page_first              12163
_journal_page_last               12166
_journal_paper_doi               10.1039/D1CC04725F
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C14 H15 F3 I N2 O3 S, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C16 H17 Cl2 F6 I N2 O6 S2'
_chemical_formula_weight         709.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_Int_Tables_number      29
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.0219(3)
_cell_length_b                   9.8218(1)
_cell_length_c                   18.6325(2)
_cell_measurement_reflns_used    14953
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.0180
_cell_measurement_theta_min      4.0370
_cell_volume                     4945.13(9)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_device_type  'AXT Supernova'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22796
_diffrn_reflns_point_group_measured_fraction_full 0.8695
_diffrn_reflns_point_group_measured_fraction_max 0.8695
_diffrn_reflns_theta_full        66.5986
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.04
_exptl_absorpt_coefficient_mu    14.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.16808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       plate
_exptl_crystal_F_000             2806.610
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.4161
_refine_diff_density_min         -0.8783
_refine_diff_density_rms         0.1280
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.286(6)
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             10.9379
_refine_ls_goodness_of_fit_ref   1.0344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7600
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0344
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.0042
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.731
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              21
_reflns_limit_l_min              -22
_reflns_number_gt                7304
_reflns_number_total             7600
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1cc04725f2.cif
_cod_data_source_block           ov_SB203PhI(dmap)OTf2
_cod_depositor_comments
;

2022-05-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_Hall     ' P 2c -2ac'
_cod_original_formula_moiety
'2(C14 H15 F3 I N2 O3 S), 2(C F3 O3 S), 2(C H2 Cl2)'
_cod_original_formula_sum        'C32 H34 Cl4 F12 I2 N4 O12 S4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1418.511
_cod_database_code               1565103
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.623(7)
 0.377(7)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C01Q(H01,H), C01T(H01z,Ha)
3.b Aromatic/amide H refined with riding coordinates:
 C015(H015), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A),
 C01C(H01j), C01F(H01F), C01G(H01p), C01I(H01I), C01L(H01L), C01M(H01M),
 C01O(H01t), C01P(H01u), C01S(H01v), C01V(H01w), C01X(H01X), C01Y(H01Y)
3.c Idealised Me refined as rotating group:
 C01D(H01k,H01n,H01o), C01K(H01q,H01r,H01s), C01U(H01b,H01c,H01d), C01W(H01e,
 H01g,H01h)
;
_olex2_submission_special_instructions 'No special instructions were received'