Nucleophilic iodonium interactions (NIIs) in 2-coordinate iodine(I) and silver(I) complexes.
Ward, Jas S.; Frontera, Antonio; Rissanen, Kari; Chemical communications (Cambridge, England) 57 (2021) 5094–5097; doi:10.1039/d1cc01505b

data_7128221
_publ_section_title
;
 Nucleophilic iodonium interactions (NIIs) in 2-coordinate iodine(I) and
 silver(I) complexes.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5094
_journal_page_last               5097
_journal_paper_doi               10.1039/d1cc01505b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C14 H18 Ag0.26 I0.74 N2, F6 P'
_chemical_formula_sum            'C14 H18 Ag0.26 F6 I0.74 N2 P'
_chemical_formula_weight         481.23
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.654(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8384(6)
_cell_length_b                   10.2312(4)
_cell_length_c                   15.1646(6)
_cell_measurement_reflns_used    2161
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.4620
_cell_measurement_theta_min      3.0560
_cell_volume                     1729.74(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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    -39.00 -12.00   1.00    1.00    --  -41.65 125.00 -60.00   27
  2  \w    -80.00  -6.00   1.00    1.00    --  -41.65 125.00  30.00   74
  3  \w    -19.00  29.00   1.00    1.00    --  -41.65  37.00 -60.00   48
  4  \w     29.00  90.00   1.00    1.00    --   41.65-125.00 -60.00   61
  5  \w     55.00  96.00   1.00    1.00    --  112.00 -94.00  90.00   41
  6  \w     66.00 122.00   1.00    1.00    --  112.00 178.00 -90.00   56
  7  \w     87.00 175.00   1.00    1.00    --  112.00  30.00  60.00   88
  8  \w     37.00 129.00   1.00    1.00    --  112.00 -30.00-120.00   92
  9  \w     49.00  80.00   1.00    1.00    --  112.00 -61.00-180.00   31
 10  \w    112.00 139.00   1.00    1.00    --  112.00 -61.00-180.00   27
 11  \w     29.00  98.00   1.00    1.00    --  112.00 -94.00 -90.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0866244000
_diffrn_orient_matrix_UB_12      -0.0915257000
_diffrn_orient_matrix_UB_13      0.0722598000
_diffrn_orient_matrix_UB_21      0.0858873000
_diffrn_orient_matrix_UB_22      0.0019211000
_diffrn_orient_matrix_UB_23      -0.0570514000
_diffrn_orient_matrix_UB_31      0.0649832000
_diffrn_orient_matrix_UB_32      0.1195221000
_diffrn_orient_matrix_UB_33      0.0561831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3000
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.101
_diffrn_reflns_theta_min         5.870
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.646
_exptl_absorpt_correction_T_max  0.26887
_exptl_absorpt_correction_T_min  0.17375
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             946
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/TBME'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.049
_exptl_crystal_size_rad          0.079
_refine_diff_density_max         2.176
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0761P)^2^+0.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1670
_reflns_number_total             1704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01505b2.cif
_cod_data_source_block           7c_Mixed
_cod_depositor_comments
'Adding full bibliography for 7128218--7128225.cif.'
_cod_database_code               7128221
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(Ag1)
3. Others
 Sof(I1)=0.5*(1-FVAR(2))
 Sof(Ag1)=0.5*FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              1836
_ins_header
;
TITL OHD165_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  11.838424  10.231155  15.164635  90.0000 109.6540  90.0000
ZERR    4.00   0.000562   0.000441   0.000629   0.0000   0.0051   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N F P I
UNIT 56.00 72.00 8.00 24.00 4.00 4.00
TREF
HKLF 4
END
;
_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 3.659
_oxdiff_exptl_absorpt_empirical_full_min 0.635