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_7126748
_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 I N4, F6 P, C H2 Cl2'
_chemical_formula_sum            'C15 H22 Cl2 F6 I N4 P'
_chemical_formula_weight         601.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-19
_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                90
_cell_angle_beta                 114.588(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9904(3)
_cell_length_b                   10.3032(2)
_cell_length_c                   11.8320(4)
_cell_measurement_reflns_used    2125
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5780
_cell_measurement_theta_min      1.9110
_cell_volume                     1107.47(6)
_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 0.918
_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      5.00  75.00   1.00    1.00    --   19.23  77.00  90.00   70
  2  \w     -9.00  89.00   1.00    1.00    --   19.23  77.00-150.00   98
  3  \w     63.00  88.00   1.00    1.00    --   19.23  77.00-120.00   25
  4  \w    -10.00  17.00   1.00    1.00    --   19.23  77.00 -30.00   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      -0.0750030000
_diffrn_orient_matrix_UB_12      0.0188379000
_diffrn_orient_matrix_UB_13      -0.0289952000
_diffrn_orient_matrix_UB_21      -0.0129204000
_diffrn_orient_matrix_UB_22      -0.0300598000
_diffrn_orient_matrix_UB_23      0.0484976000
_diffrn_orient_matrix_UB_31      0.0175059000
_diffrn_orient_matrix_UB_32      0.0589835000
_diffrn_orient_matrix_UB_33      0.0339655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.259
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.353
_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    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0225P)^2^+0.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2306
_reflns_number_total             2652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02758h2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7126741--7126748.cif.'
_cod_database_code               7126748
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F52(0.5) F53(0.5) F54(0.5) F55(0.5) F56(0.5) F57(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C13(H13)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              60298
_ins_header
;
TITL OHS067_numabs in P2(1)/m 
REM P2(1)/m (#11 in standard setting)
CELL 0.71073   9.990374  10.303157  11.831977  90.0000 114.5881  90.0000
ZERR    2.00   0.000303   0.000249   0.000392   0.0000   0.0037   0.0000
LATT  1
SYMM -x, y+1/2,-z 
SFAC C H N F P Cl I
UNIT 30.00 44.00 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 1.109
_oxdiff_exptl_absorpt_empirical_full_min 0.911