Hypervalent Iodine(III) Compounds as Biaxial Halogen Bond Donors.
Heinen, Flemming; Engelage, Elric; Cramer, Christopher J.; Huber, Stefan M.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13309

data_4134827
_publ_section_title
;
 Hypervalent Iodine(III) Compounds as Biaxial Halogen Bond Donors.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13309
_journal_year                    2020
_chemical_formula_moiety
'C24 H12 B Cl8, C16 H16 N2 O2, C12 H8 I [+ Dioxane]'
_chemical_formula_sum            'C52 H36 B Cl8 I N2 O2'
_chemical_formula_weight         1142.14
_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 space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-16 deposited with the CCDC.	2019-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                86.1950(10)
_cell_angle_beta                 83.2390(10)
_cell_angle_gamma                69.1680(10)
_cell_formula_units_Z            4
_cell_length_a                   13.13340(10)
_cell_length_b                   14.25860(10)
_cell_length_c                   31.8035(3)
_cell_measurement_reflns_used    19430
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.5
_cell_measurement_theta_min      2.8
_cell_volume                     5525.68(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_computing_molecular_graphics
;
 Diamond 4 - Crystal and Molecular Structure Visualization
  Crystal Impact - Dr. H. Putz & Dr. K. Brandenburg GbR, 
  Kreuzherrenstr. 102, 53227 Bonn, Germany
  http://www.crystalimpact.com/diamond
 Mercury CSD 2.0 - New Features for the Visualization 
 and Investigation of Crystal Structures
  C. F. Macrae, I. J. Bruno, J. A. Chisholm, P. R. Edgington, P. McCabe,
  E. Pidcock, 
  L. Rodriguez-Monge, R. Taylor, J. van de Streek and P. A. Wood, 
  J. Appl. Cryst., 41, 466-470, 2008
;
_computing_publication_material
'WinGX L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
;
 shelXT  G. M. Sheldrick, Acta Crystallogr., Sect. A: Found. Crystallogr.,
 2008, 64, 112-122.
 shelXle C. B. Huebschle, G. M. Sheldrick and B. Dittrich J. Appl. Cryst.
  (2011). 44, 1281-1284
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -83.00 -18.00   0.50    0.07    --  -47.45 111.00-153.00  130
  2  \w     32.00  57.00   0.50    0.07    --   47.45-111.00 112.00   50
  3  \w   -144.00-119.00   0.50    0.30    --  -86.25-111.00 112.00   50
  4  \w    -48.00 -23.00   0.50    0.30    --  -86.25 111.00-153.00   50
  5  \w     60.00 108.00   0.50    0.30    --  106.49-111.00 112.00   96
  6  \w    112.00 140.00   0.50    0.30    --  106.49 111.00-153.00   56
  7  \w   -111.00 -31.00   0.50    0.07    --  -47.45 -77.00 150.00  160
  8  \w    -22.00  28.00   0.50    0.07    --  -47.45  19.00  30.00  100
  9  \w    -68.00   2.00   0.50    0.07    --  -47.45  77.00 -30.00  140
 10  \w    -18.00  20.00   0.50    0.07    --  -47.45  19.00 -60.00   76
 11  \w    -23.00  20.00   0.50    0.07    --  -47.45  19.00  90.00   86
 12  \w     34.00  89.00   0.50    0.07    --   47.45-125.00   0.00  110
 13  \w   -152.00 -72.00   0.50    0.30    --  -86.25 -15.00  30.00  160
 14  \w    -44.00 -19.00   0.50    0.30    --  -86.25  45.00 150.00   50
 15  \w    -55.00 -18.00   0.50    0.30    --  -86.25  61.00 120.00   74
 16  \w    -44.00 -17.00   0.50    0.30    --  -86.25  45.00 -30.00   54
 17  \w   -148.00-122.00   0.50    0.30    --  -86.25 -94.00  30.00   52
 18  \w   -159.00 -87.00   0.50    0.30    --  -86.25 -61.00-180.00  144
 19  \w     39.00 102.00   0.50    0.30    --  106.49 -77.00 150.00  126
 20  \w     38.00  71.00   0.50    0.30    --  106.49-125.00-180.00   66
 21  \w     70.00 108.00   0.50    0.30    --  106.49 -77.00 -30.00   76
 22  \w     34.00  59.00   0.50    0.30    --  106.49 -77.00 -30.00   50
 23  \w     79.00 105.00   0.50    0.30    --  106.49 -94.00 150.00   52
 24  \w     38.00 102.00   0.50    0.30    --  106.49 -94.00 120.00  128
 25  \w     80.00 105.00   0.50    0.30    --  106.49 -96.00 -79.25   50
 26  \w     36.00 105.00   0.50    0.30    --  106.49 -99.00 -95.78  138
 27  \w     34.00  89.00   0.50    0.30    --  106.49 -94.00  60.00  110
 28  \w     98.00 174.00   0.50    0.30    --  106.49  45.00 -60.00  152
 29  \w     94.00 168.00   0.50    0.30    --  106.49  45.00  90.00  148
 30  \w     34.00  65.00   0.50    0.30    --  106.49 -96.00 -79.25   62
 31  \w    103.00 178.00   0.50    0.30    --  106.49  15.00   0.00  150
 32  \w     45.00  73.00   0.50    0.30    --  106.49 -61.00-180.00   56
 33  \w    147.00 177.00   0.50    0.30    --  106.49  15.00-150.00   60
 34  \w     86.00 111.00   0.50    0.30    --  106.49-125.00-180.00   50
 35  \w     44.00  69.00   0.50    0.30    --  106.49 -61.00 150.00   50
 36  \w    142.00 176.00   0.50    0.30    --  106.49  15.00-120.00   68
 37  \w    108.00 138.00   0.50    0.30    --  106.49  15.00-150.00   60
 38  \w     74.00  99.00   0.50    0.30    --  106.49 -94.00   0.00   50
 39  \w     37.00  62.00   0.50    0.30    --  106.49 -94.00   0.00   50
 40  \w     51.00 103.00   0.50    0.30    --  106.49-125.00 -90.00  104
 41  \w     54.00 103.00   0.50    0.30    --  106.49 -94.00 -60.00   98
 42  \w     34.00  62.00   0.50    0.30    --  106.49 -61.00   0.00   56
 43  \w     44.00  69.00   0.50    0.30    --  106.49 -61.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0554457000
_diffrn_orient_matrix_UB_12      -0.0080006000
_diffrn_orient_matrix_UB_13      0.0448801000
_diffrn_orient_matrix_UB_21      -0.0537843000
_diffrn_orient_matrix_UB_22      -0.0685724000
_diffrn_orient_matrix_UB_23      -0.0164153000
_diffrn_orient_matrix_UB_31      0.0997339000
_diffrn_orient_matrix_UB_32      -0.0927737000
_diffrn_orient_matrix_UB_33      0.0098684000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            68946
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.494
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.420
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.29a (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_density_diffrn    1.373
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dioxane, water'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         19430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+2.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17848
_reflns_number_total             19430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13309_si_002.cif
_cod_data_source_block           fh-g008dioxanh2o_squeeze
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4134827
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.833
_oxdiff_exptl_absorpt_empirical_full_max 1.179
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              26462
_shelx_hkl_checksum              55988
_shelx_fab_checksum              52885
_ccdc_publ_extra_info
'disordered molecules of dioxane were removed using SQUEEZE'