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_7128225
_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         'C16 H22 Ag N2, F6 P'
_chemical_formula_sum            'C16 H22 Ag F6 N2 P'
_chemical_formula_weight         495.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-17
_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                100.476(2)
_cell_angle_beta                 102.846(2)
_cell_angle_gamma                91.053(2)
_cell_formula_units_Z            4
_cell_length_a                   10.2094(2)
_cell_length_b                   10.2353(3)
_cell_length_c                   19.2604(4)
_cell_measurement_reflns_used    16329
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4730
_cell_measurement_theta_min      4.3710
_cell_volume                     1925.92(8)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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   -115.00 -14.00   1.00    1.00    --  -41.90 -57.00-120.00  101
  2  \w   -115.00 -60.00   1.00    1.00    --  -41.90-151.00-111.00   55
  3  \w   -116.00 -18.00   1.00    1.00    --  -41.90 -37.00 120.00   98
  4  \w      6.00  83.00   1.00    1.00    --   41.90 -99.00  90.00   77
  5  \w      7.00  33.00   1.00    1.00    --   41.90  84.00 -21.48   26
  6  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00 120.00   99
  7  \w     29.00 107.00   1.00    1.00    --  112.00 -94.00  60.00   78
  8  \w     36.00 140.00   1.00    1.00    --  112.00 -30.00-150.00  104
  9  \w     38.00 111.00   1.00    1.00    --  112.00-121.00  49.00   73
 10  \w     36.00 109.00   1.00    1.00    --  112.00-111.00-180.00   73
 11  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00   0.00   99
 12  \w    103.00 178.00   1.00    1.00    --  112.00  77.00-180.00   75
 13  \w     36.00 145.00   1.00    1.00    --  112.00 -77.00-150.00  109
 14  \w     24.00 178.00   1.00    1.00    --  112.00   0.00-180.00  154
 15  \w   -115.00 -14.00   1.00    1.00    --  -41.90 -57.00   0.00  101
 16  \w      9.00  42.00   1.00    1.00    --   41.90  77.00 133.55   33
 17  \w      8.00  34.00   1.00    1.00    --   41.90  83.00-129.67   26
 18  \w    -21.00  74.00   1.00    1.00    --   41.90 -77.00-120.00   95
 19  \w     84.00 178.00   1.00    1.00    --  112.00  30.00  30.00   94
 20  \w     82.00 178.00   1.00    1.00    --  112.00  66.00-143.34   96
 21  \w     59.00 178.00   1.00    1.00    --  112.00  15.00 -30.00  119
 22  \w     81.00 154.00   1.00    1.00    --  112.00  70.00  63.05   73
 23  \w     83.00 178.00   1.00    1.00    --  112.00  61.00 150.00   95
;
_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      -0.1422598000
_diffrn_orient_matrix_UB_12      0.0477702000
_diffrn_orient_matrix_UB_13      -0.0001409000
_diffrn_orient_matrix_UB_21      0.0406184000
_diffrn_orient_matrix_UB_22      0.0446017000
_diffrn_orient_matrix_UB_23      0.0830823000
_diffrn_orient_matrix_UB_31      0.0464391000
_diffrn_orient_matrix_UB_32      0.1387314000
_diffrn_orient_matrix_UB_33      -0.0090444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.120
_diffrn_reflns_theta_min         2.397
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.734
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.708
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0335P)^2^+0.7774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6999
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01505b2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7128218--7128225.cif.'
_cod_database_code               7128225
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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:
 C7(H7), C17(H17), C27(H27), C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C)
;
_shelx_res_checksum              18550
_ins_header
;
TITL OHD174_2_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.209412  10.235278  19.260402 100.4755 102.8465  91.0529
ZERR    4.00   0.000248   0.000267   0.000437   0.0021   0.0020   0.0020
LATT  1
SFAC C H N F P Ag
UNIT 64.00 88.00 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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.862