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_7128224
_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         'C12 H14 I N2, C12 H14 Ag N2, 2(F6 P)'
_chemical_formula_sum            'C24 H28 Ag F12 I N4 P2'
_chemical_formula_weight         897.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-29
_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                 94.2940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.98970(10)
_cell_length_b                   43.9504(4)
_cell_length_c                   20.8689(3)
_cell_measurement_reflns_used    34657
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5910
_cell_measurement_theta_min      2.8800
_cell_volume                     6392.93(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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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   -116.00 -18.00   1.00    2.00    --  -41.90 -37.00-120.00   98
  2  \w   -115.00 -14.00   1.00    2.00    --  -41.90 -57.00   0.00  101
  3  \w      6.00  83.00   1.00    2.00    --   41.90 -99.00-150.00   77
  4  \w    -21.00  74.00   1.00    2.00    --   41.90 -77.00 120.00   95
  5  \w    104.00 178.00   1.00    8.00    --  112.00 111.00-120.00   74
  6  \w     86.00 178.00   1.00    8.00    --  112.00  45.00 -30.00   92
  7  \w     40.00 141.00   1.00    8.00    --  112.00 -61.00-120.00  101
  8  \w     36.00 109.00   1.00    8.00    --  112.00-111.00-180.00   73
  9  \w     29.00 107.00   1.00    8.00    --  112.00 -94.00  60.00   78
 10  \w    104.00 178.00   1.00    8.00    --  112.00 111.00-150.00   74
 11  \w     36.00 109.00   1.00    8.00    --  112.00-111.00  30.00   73
 12  \w     40.00 141.00   1.00    8.00    --  112.00 -61.00 150.00  101
 13  \w     36.00 109.00   1.00    8.00    --  112.00-111.00-120.00   73
 14  \w     84.00 178.00   1.00    8.00    --  112.00  30.00 -60.00   94
 15  \w     86.00 178.00   1.00    8.00    --  112.00  45.00  30.00   92
 16  \w   -115.00 -14.00   1.00    2.00    --  -41.90 -57.00 120.00  101
 17  \w      8.00  34.00   1.00    2.00    --   41.90  83.00-105.08   26
 18  \w      7.00  33.00   1.00    2.00    --   41.90  84.00 137.05   26
 19  \w    -30.00  70.00   1.00    2.00    --   41.90 -57.00 -30.00  100
 20  \w      8.00  34.00   1.00    2.00    --   41.90  83.00  16.56   26
 21  \w     82.00 178.00   1.00    8.00    --  112.00  64.00  68.44   96
 22  \w     83.00 178.00   1.00    8.00    --  112.00  61.00-120.00   95
 23  \w     59.00 178.00   1.00    8.00    --  112.00  15.00-180.00  119
 24  \w     83.00 178.00   1.00    8.00    --  112.00  61.00 120.00   95
 25  \w     85.00 178.00   1.00    8.00    --  112.00  50.00   3.58   93
 26  \w     82.00 178.00   1.00    8.00    --  112.00  65.00 165.72   96
 27  \w     86.00 178.00   1.00    8.00    --  112.00  45.00  60.00   92
 28  \w     83.00 178.00   1.00    8.00    --  112.00  63.00 -68.70   95
 29  \w     82.00 178.00   1.00    8.00    --  112.00  64.00-172.57   96
 30  \w     84.00 178.00   1.00    8.00    --  112.00  30.00-120.00   94
;
_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      0.2112450000
_diffrn_orient_matrix_UB_12      -0.0050028000
_diffrn_orient_matrix_UB_13      -0.0137009000
_diffrn_orient_matrix_UB_21      0.0051871000
_diffrn_orient_matrix_UB_22      0.0318337000
_diffrn_orient_matrix_UB_23      -0.0307154000
_diffrn_orient_matrix_UB_31      0.0647966000
_diffrn_orient_matrix_UB_32      0.0137913000
_diffrn_orient_matrix_UB_33      0.0659488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            99904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.119
_diffrn_reflns_theta_min         2.349
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.454
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.864
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         12588
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+27.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11321
_reflns_number_total             12588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01505b2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7128218--7128225.cif.'
_cod_database_code               7128224
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.84
_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. Rigid body (RIGU) restrains
3.a 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),
  C42(H42), C43(H43), C45(H45), C46(H46), C52(H52), C53(H53), C55(H55),
 C56(H56), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75),
  C76(H76)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,
 H37C), C47(H47A,H47B,H47C), C57(H57A,H57B,H57C), C67(H67A,H67B,H67C), C77(H77A,
 H77B,H77C)
;
_shelx_res_checksum              71291
_ins_header
;
TITL OHD159_2_numabs_ana in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   6.989743  43.950367  20.868914  90.0000  94.2942  90.0000
ZERR    8.00   0.000085   0.000396   0.000251   0.0000   0.0011   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N F P Ag I
UNIT 192.00 224.00 32.00 96.00 16.00 8.00 8.00
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 1.428
_oxdiff_exptl_absorpt_empirical_full_min 0.688