Asymmetric [N-I-N]<sup>+</sup> halonium complexes.
Ward, Jas S.; Fiorini, Giorgia; Frontera, Antonio; Rissanen, Kari; Chemical communications (Cambridge, England) 56 (2020) 8428–8431; doi:10.1039/d0cc02758h

data_7126747
_publ_section_title
;
 Asymmetric [N-I-N]<sup>+</sup> halonium complexes.
;
_journal_issue                   60
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8428
_journal_page_last               8431
_journal_paper_doi               10.1039/d0cc02758h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C14 H20 Ag N4, F6 P, C2 H4 Cl2'
_chemical_formula_sum            'C16 H24 Ag Cl2 F6 N4 P'
_chemical_formula_weight         596.13
_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             2019-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-15 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                109.040(8)
_cell_angle_beta                 90.185(7)
_cell_angle_gamma                90.561(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7214(6)
_cell_length_b                   10.5840(8)
_cell_length_c                   14.3078(15)
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.6110
_cell_measurement_theta_min      2.0940
_cell_volume                     1105.23(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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     -2.00  88.00   1.00   32.00    --   19.23  57.00-180.00   90
  2  \w    -11.00  89.00   1.00   32.00    --   19.23  77.00 -60.00  100
  3  \w    -20.00  61.00   1.00   32.00    --   19.23 -99.00  60.00   81
  4  \w    -51.00  49.00   1.00   32.00    --   19.23 -77.00-180.00  100
  5  \w    -25.00  92.00   1.00   32.00    --   19.23  19.00 120.00  117
  6  \w    -91.00   7.00   1.00   32.00    --  -18.45 -37.00-180.00   98
  7  \w     35.00  95.00   1.00   32.00    --   19.23 178.00-150.00   60
  8  \w    -20.00  25.00   1.00   32.00    --   19.23 -99.00 -60.00   45
  9  \w     34.00  96.00   1.00   32.00    --   19.23-178.00  30.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0903019000
_diffrn_orient_matrix_UB_12      0.0135674000
_diffrn_orient_matrix_UB_13      0.0015878000
_diffrn_orient_matrix_UB_21      -0.0012548000
_diffrn_orient_matrix_UB_22      0.0193520000
_diffrn_orient_matrix_UB_23      0.0523506000
_diffrn_orient_matrix_UB_31      0.0168492000
_diffrn_orient_matrix_UB_32      -0.0668428000
_diffrn_orient_matrix_UB_33      -0.0026689000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
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    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.518
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.149
_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     276
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1110P)^2^+5.9920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             4822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02758h2.cif
_cod_data_source_block           1b_3
_cod_depositor_comments
'Adding full bibliography for 7126741--7126748.cif.'
_cod_database_code               7126747
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.778
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8996(13)
 0.1004(13)
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:
 C101(H10A,H10B), C102(H10C,H10D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              3018
_ins_header
;
TITL OHS060_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073   7.721350  10.584033  14.307786 109.0396  90.1851  90.5614
ZERR    2.00   0.000632   0.000815   0.001500   0.0083   0.0075   0.0066
LATT  1
SFAC C H N F P Cl Ag
UNIT 32.00 48.00 8.00 12.00 2.00 4.00 2.00
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 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.867