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_7126741
_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, C7 H8'
_chemical_formula_sum            'C21 H28 Ag F6 N4 P'
_chemical_formula_weight         589.31
_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             2019-12-27
_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                100.440(4)
_cell_angle_beta                 108.085(5)
_cell_angle_gamma                94.085(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4171(6)
_cell_length_b                   10.7634(5)
_cell_length_c                   11.4213(7)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    120.00(13)
_cell_measurement_theta_max      27.5730
_cell_measurement_theta_min      2.3050
_cell_volume                     1185.99(12)
_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(13)
_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 0.986
_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    -87.00   3.00   1.00   40.00    --  -18.29 -57.00-150.00   90
  2  \w    -88.00  12.00   1.00   40.00    --  -18.29 -77.00 120.00  100
  3  \w    -77.00  -3.00   1.00   40.00    --  -18.29 127.00 -63.00   74
  4  \w    -39.00  51.00   1.00   40.00    --  -18.29  57.00  90.00   90
  5  \w    -91.00  26.00   1.00   40.00    --  -18.29 -19.00 -90.00  117
  6  \w    -95.00 -34.00   1.00   40.00    --  -18.29 178.00 120.00   61
  7  \w     -2.00  25.00   1.00   40.00    --   19.07  57.00  90.00   27
;
_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      -0.0616238000
_diffrn_orient_matrix_UB_12      -0.0098841000
_diffrn_orient_matrix_UB_13      0.0132954000
_diffrn_orient_matrix_UB_21      0.0372652000
_diffrn_orient_matrix_UB_22      0.0129352000
_diffrn_orient_matrix_UB_23      0.0654365000
_diffrn_orient_matrix_UB_31      -0.0064612000
_diffrn_orient_matrix_UB_32      0.0656523000
_diffrn_orient_matrix_UB_33      0.0038855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13360
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_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    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0378P)^2^+1.2345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4096
_reflns_number_total             5174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02758h2.cif
_cod_data_source_block           1b_1
_cod_depositor_comments
'Adding full bibliography for 7126741--7126748.cif.'
_cod_database_code               7126741
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Sof(P61)=Sof(F62)=Sof(F63)=Sof(F64)=Sof(F65)=Sof(F66)=Sof(F67)=Sof(C111)=
 Sof(C116)=Sof(H116)=Sof(C115)=Sof(H115)=Sof(C114)=Sof(H114)=Sof(C113)=
 Sof(H113)=Sof(C112)=Sof(H112)=Sof(C117)=Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(1)
 Sof(P51)=Sof(F52)=Sof(F53)=Sof(F54)=Sof(F55)=Sof(F56)=Sof(F57)=Sof(C103)=
 Sof(H103)=Sof(C102)=Sof(H102)=Sof(C101)=Sof(C106)=Sof(H106)=Sof(C105)=
 Sof(H105)=Sof(C104)=Sof(H104)=Sof(C107)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
3.a Free rotating group:
 P51(F52,F53,F54,F55,F56,F57), P61(F62,F63,F64,F65,F66,F67)
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),
 C103(H103), C102(H102), C106(H106), C105(H105), C104(H104), C116(H116),
 C115(H115), C114(H114), C113(H113), C112(H112)
3.c Fitted hexagon refined as free rotating group:
 C103(C102,C101,C106,C105,C104), C111(C116,C115,C114,C113,C112)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C107(H10A,H10B,H10C), C117(H11A,H11B,H11C)
;
_shelx_res_checksum              5182
_ins_header
;
TITL OHS068_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  10.417054  10.763375  11.421317 100.4397 108.0851  94.0849
ZERR    2.00   0.000603   0.000498   0.000692   0.0044   0.0054   0.0043
LATT  1
SFAC C H N F P I
UNIT 42.00 56.00 8.00 12.00 2.00 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 1.172
_oxdiff_exptl_absorpt_empirical_full_min 0.856