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_1568848
_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         'C33 H43 Au N2, C6 F4 I2'
_chemical_formula_sum            'C39 H43 Au F4 I2 N2'
_chemical_formula_weight         1066.559
_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'
_symmetry_Int_Tables_number      11
_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                 111.731(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7939(1)
_cell_length_b                   15.2361(1)
_cell_length_c                   13.1834(1)
_cell_measurement_reflns_used    21066
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.2060
_cell_measurement_theta_min      2.8920
_cell_volume                     2014.02(3)
_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 0.9992
_diffrn_measured_fraction_theta_max 0.9814
_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     52.00  77.00   0.50    0.05    --   49.03  71.00  68.00   50
  2  \w     89.00 130.00   0.50    0.18    --  102.75  71.00  68.00   82
  3  \w     98.00 141.00   0.50    0.18    --  102.75  37.00  30.00   86
  4  \w    101.00 162.00   0.50    0.18    --  102.75  37.00   0.00  122
  5  \w     96.00 142.00   0.50    0.18    --  102.75  37.00 120.00   92
  6  \w     95.00 169.00   0.50    0.18    --  102.75  19.00 150.00  148
  7  \w     98.00 124.00   0.50    0.18    --  102.75  37.00-150.00   52
  8  \w    134.00 174.00   0.50    0.18    --  102.75  19.00-150.00   80
  9  \w     91.00 171.00   0.50    0.18    --  102.75  57.00-180.00  160
 10  \w     95.00 145.00   0.50    0.18    --  102.75  37.00-180.00  100
 11  \w     95.00 145.00   0.50    0.18    --  102.75  19.00-180.00  100
 12  \w     -8.00  53.00   0.50    0.05    --   49.03 -71.00 -62.00  122
 13  \w    -22.00  39.00   0.50    0.05    --   49.03 -37.00  60.00  122
 14  \w    -22.00  18.00   0.50    0.05    --   49.03 -19.00 -30.00   80
 15  \w    -20.00  15.00   0.50    0.05    --   49.03 -19.00 -60.00   70
 16  \w    -23.00  16.00   0.50    0.05    --   49.03 -19.00 -90.00   78
 17  \w     32.00  69.00   0.50    0.18    --  102.75 -57.00-120.00   74
 18  \w     41.00 124.00   0.50    0.18    --  102.75 -77.00-180.00  166
 19  \w     65.00 123.00   0.50    0.18    --  102.75 -77.00 -60.00  116
 20  \w     32.00  84.00   0.50    0.18    --  102.75 -71.00 -62.00  104
 21  \w     31.00  64.00   0.50    0.18    --  102.75 -57.00  60.00   66
 22  \w    -49.00  22.00   0.50    0.05    --  -49.03  71.00  68.00  142
 23  \w    -60.00 -35.00   0.50    0.18    -- -102.00  57.00  60.00   50
 24  \w    -91.00 -30.00   0.50    0.18    -- -102.00  71.00  68.00  122
 25  \w    -65.00 -30.00   0.50    0.18    -- -102.00  57.00 120.00   70
 26  \w    -65.00 -31.00   0.50    0.18    -- -102.00  57.00 150.00   68
 27  \w    -63.00 -31.00   0.50    0.18    -- -102.00  57.00  30.00   64
 28  \w    -65.00 -32.00   0.50    0.18    -- -102.00  57.00   0.00   66
 29  \w    -13.00  12.00   0.50    0.05    --  -49.03  19.00-120.00   50
 30  \w    -63.00 -33.00   0.50    0.18    -- -102.00  57.00 -90.00   60
 31  \w    -64.00 -37.00   0.50    0.18    -- -102.00  57.00-120.00   54
 32  \w    -59.00 -31.00   0.50    0.18    -- -102.00  57.00-150.00   56
 33  \w   -166.00-140.00   0.50    0.18    -- -102.00 -19.00   0.00   52
 34  \w   -136.00 -89.00   0.50    0.18    -- -102.00 -71.00 -62.00   94
 35  \w   -162.00 -97.00   0.50    0.18    -- -102.00 -37.00 -60.00  130
 36  \w   -123.00 -95.00   0.50    0.18    -- -102.00 -19.00-180.00   56
 37  \w   -107.00 -50.00   0.50    0.05    --  -49.03 -71.00 -62.00  114
 38  \w   -154.00 -99.00   0.50    0.18    -- -102.00 -37.00  30.00  110
 39  \w   -103.00 -78.00   0.50    0.05    --  -49.03-125.00  90.00   50
 40  \w   -113.00 -86.00   0.50    0.05    --  -49.03-125.00   0.00   54
;
_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      -0.0887298000
_diffrn_orient_matrix_UB_12      0.0808390000
_diffrn_orient_matrix_UB_13      -0.0463908000
_diffrn_orient_matrix_UB_21      0.0513107000
_diffrn_orient_matrix_UB_22      0.0045502000
_diffrn_orient_matrix_UB_23      -0.0944705000
_diffrn_orient_matrix_UB_31      -0.1144726000
_diffrn_orient_matrix_UB_32      -0.0605222000
_diffrn_orient_matrix_UB_33      -0.0689785000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9814
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27315
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9814
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.39
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34855
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       block
_exptl_crystal_F_000             1020.055
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.4584
_refine_diff_density_min         -1.9175
_refine_diff_density_rms         0.1226
_refine_ls_d_res_high            0.7932
_refine_ls_d_res_low             12.2465
_refine_ls_goodness_of_fit_ref   1.0208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4321
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.0158
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0619P)^2^+2.2764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4032
_reflns_number_total             4321
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           2Ph-14-FIB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568848
_chemical_oxdiff_formula         'Au I F N C H'
_olex2_refinement_description
;
1. Restrained distances
 C11A-C12A
 1.4 with sigma of 0.02
 C12A-C13A
 1.4 with sigma of 0.02
 C14A-C13A
 1.4 with sigma of 0.02
 C13A-C12A
 1.4 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C11A \\sim C12A \\sim C13A \\sim C14A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C14A \\sim C13A \\sim C12A \\sim C11A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
3. Others
 Fixed Sof: H2Aa(0.5) H2Ab(0.5) H3Aa(0.5) H3Ab(0.5)
4.a Ternary CH refined with riding coordinates:
 C8A(H8A), C15A(H15A)
4.b Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab), C3A(H3Aa,H3Ab)
4.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C3(H3), C7A(H7A), C4(H4), C12A(H12A), C14A(H14A), C13A(H13A)
4.d Idealised Me refined as rotating group:
 C9A(H9Aa,H9Ab,H9Ac), C10A(H10a,H10b,H10c), C16A(H16a,H16b,H16c), C17A(H17a,
 H17b,H17c)
;
_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 2.272
_oxdiff_exptl_absorpt_empirical_full_min 0.704