Exploring Au(i) involving halogen bonding with N-heterocyclic carbene Au(i) aryl complexes in crystalline media
Mikherdov, Alexander S.; Jin, Mingoo; Ito, Hajime; Chemical Science 14 (2023) 4485–4494; doi:10.1039/D3SC00373F

data_1568849
_publ_section_title
;
 Exploring Au(i) involving halogen bonding with N-heterocyclic carbene
 Au(i) aryl complexes in crystalline media
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4485
_journal_page_last               4494
_journal_paper_doi               10.1039/D3SC00373F
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C29 H35 Au N2, C6 F4 I2'
_chemical_formula_sum            'C35 H35 Au F4 I2 N2'
_chemical_formula_weight         1010.450
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-24
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.197(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6600(1)
_cell_length_b                   13.0052(1)
_cell_length_c                   17.1537(1)
_cell_measurement_reflns_used    19180
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.4650
_cell_measurement_theta_min      4.3380
_cell_volume                     3603.12(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9778
_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     75.00 100.00   0.50    0.11    --   49.16 131.00 114.00   50
  2  \w     82.00 111.00   0.50    0.52    --  102.75 125.00   0.00   58
  3  \w    123.00 168.00   0.50    0.52    --  102.75 125.00   0.00   90
  4  \w     70.00 158.00   0.50    0.52    --  102.75 138.00 -69.00  176
  5  \w     78.00 104.00   0.50    0.11    --   49.16 138.00 -69.00   52
  6  \w     39.00  64.00   0.50    0.52    --  102.75 -99.00-120.00   50
  7  \w     94.00 119.00   0.50    0.52    --  102.75-138.00-131.00   50
  8  \w     58.00  99.00   0.50    0.11    --   49.16-138.00-131.00   82
  9  \w     31.00  79.00   0.50    0.52    --  102.75-125.00   0.00   96
 10  \w     31.00 106.00   0.50    0.52    --  102.75 -99.00  30.00  150
 11  \w     46.00 106.00   0.50    0.52    --  102.75 -99.00   0.00  120
 12  \w     42.00  71.00   0.50    0.52    --  102.75-131.00  44.00   58
 13  \w     32.00 105.00   0.50    0.52    --  102.75 -99.00  90.00  146
 14  \w     52.00  81.00   0.50    0.11    --   49.16-131.00  44.00   58
 15  \w     31.00 106.00   0.50    0.52    --  102.75 -99.00 -90.00  150
 16  \w     81.00 106.00   0.50    0.52    --  102.75 -99.00-120.00   50
 17  \w    -23.00  17.00   0.50    0.11    --   49.16 -19.00-150.00   80
 18  \w     34.00  68.00   0.50    0.52    --  102.75 -57.00 -60.00   68
 19  \w     31.00  66.00   0.50    0.52    --  102.75 -57.00  30.00   70
 20  \w     32.00  63.00   0.50    0.52    --  102.75 -57.00  60.00   62
 21  \w    -23.00  18.00   0.50    0.11    --   49.16 -19.00  30.00   82
 22  \w    -12.00  24.00   0.50    0.11    --  -49.16  19.00  90.00   72
 23  \w    -11.00  24.00   0.50    0.11    --  -49.16  19.00  60.00   70
 24  \w    -37.00  19.00   0.50    0.11    --  -49.16  37.00  30.00  112
 25  \w    -14.00  24.00   0.50    0.11    --  -49.16  19.00 -90.00   76
 26  \w    -13.00  23.00   0.50    0.11    --  -49.16  19.00-150.00   72
 27  \w    -95.00 -70.00   0.50    0.11    --  -49.16 138.00 -69.00   50
 28  \w   -118.00 -84.00   0.50    0.52    -- -102.00 138.00 -69.00   68
 29  \w    -80.00 -18.00   0.50    0.11    --  -49.16 131.00 114.00  124
 30  \w   -103.00 -73.00   0.50    0.52    -- -102.00 131.00 114.00   60
 31  \w    -94.00 -30.00   0.50    0.52    -- -102.00  77.00 150.00  128
 32  \w    -63.00 -37.00   0.50    0.52    -- -102.00  57.00 -30.00   52
 33  \w    -65.00 -40.00   0.50    0.52    -- -102.00  57.00 -60.00   50
 34  \w   -171.00 -94.00   0.50    0.52    -- -102.00 -37.00-150.00  154
 35  \w   -171.00-100.00   0.50    0.52    -- -102.00 -37.00 -60.00  142
 36  \w   -161.00 -94.00   0.50    0.52    -- -102.00 -37.00  30.00  134
 37  \w   -173.00 -98.00   0.50    0.52    -- -102.00 -37.00 120.00  150
 38  \w   -134.00-109.00   0.50    0.52    -- -102.00-131.00  44.00   50
 39  \w   -109.00 -84.00   0.50    0.11    --  -49.16-131.00  44.00   50
 40  \w   -119.00 -84.00   0.50    0.11    --  -49.16-138.00-131.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0818476000
_diffrn_orient_matrix_UB_12      -0.0215282000
_diffrn_orient_matrix_UB_13      0.0626040000
_diffrn_orient_matrix_UB_21      -0.0140607000
_diffrn_orient_matrix_UB_22      -0.1164443000
_diffrn_orient_matrix_UB_23      -0.0130790000
_diffrn_orient_matrix_UB_31      0.0468992000
_diffrn_orient_matrix_UB_32      0.0025683000
_diffrn_orient_matrix_UB_33      -0.0670330000
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9778
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22948
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9778
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.52
_diffrn_reflns_theta_min         4.36
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       prism
_exptl_crystal_F_000             1911.802
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.5047
_refine_diff_density_min         -0.7240
_refine_diff_density_rms         0.0950
_refine_ls_d_res_high            0.7928
_refine_ls_d_res_low             10.1295
_refine_ls_goodness_of_fit_ref   1.0512
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0485
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.0123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3572
_reflns_number_total             3704
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Xyl-14-FIB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568849
_chemical_oxdiff_formula         'Au I F N C H'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C12A \\sim C13A \\sim C14A \\sim C15A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
2.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C5A(H5A), C14A(H14A), C15A(H15A)
2.c Idealised Me refined as rotating group:
 C11A(H11a,H11b,H11c), C9A(H9Aa,H9Ab,H9Ac), C16A(H16a,H16b,H16c), C10A(H10a,
 H10b,H10c)
;
_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 2.151
_oxdiff_exptl_absorpt_empirical_full_min 0.507