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_1568832
_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         'C26 H30 Au N3, 2(C6 F5 I)'
_chemical_formula_sum            'C38 H30 Au F10 I2 N3'
_chemical_formula_weight         1169.441
_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             2022-11-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.682(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0425(1)
_cell_length_b                   12.1872(1)
_cell_length_c                   20.8413(2)
_cell_measurement_reflns_used    11843
_cell_measurement_temperature    293
_cell_measurement_theta_max      75.8230
_cell_measurement_theta_min      4.5460
_cell_volume                     4038.18(6)
_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 (Sheldrick, 2015)'
_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 0.9995
_diffrn_measured_fraction_theta_max 0.9666
_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     95.00 125.00   0.50    0.59    --  102.75  37.00-120.00   60
  2  \w    136.00 173.00   0.50    0.59    --  102.75  37.00-120.00   74
  3  \w     95.00 150.00   0.50    0.59    --  102.75  19.00-120.00  110
  4  \w    133.00 160.00   0.50    0.59    --  102.75  84.00 164.00   54
  5  \w    122.00 175.00   0.50    0.59    --  102.75  19.00 120.00  106
  6  \w     31.00  69.00   0.50    0.59    --  102.75 -57.00  30.00   76
  7  \w     32.00  68.00   0.50    0.59    --  102.75 -57.00  60.00   72
  8  \w     33.00  65.00   0.50    0.59    --  102.75 -57.00  90.00   64
  9  \w    -23.00  18.00   0.50    0.59    --   49.16 -19.00  30.00   82
 10  \w    -21.00  17.00   0.50    0.59    --   49.16 -19.00 -30.00   76
 11  \w    -21.00   6.00   0.50    0.59    --   49.16 -84.00  44.00   54
 12  \w     22.00  47.00   0.50    0.59    --   49.16 -84.00  44.00   50
 13  \w     45.00 101.00   0.50    0.59    --  102.75 -99.00-120.00  112
 14  \w     55.00  80.00   0.50    0.59    --  102.75 -84.00  44.00   50
 15  \w     31.00  68.00   0.50    0.59    --  102.75 -99.00  90.00   74
 16  \w    -13.00  23.00   0.50    0.59    --  -49.16  19.00 -90.00   72
 17  \w    -60.00 -34.00   0.50    0.59    -- -102.00  57.00   0.00   52
 18  \w    -63.00 -33.00   0.50    0.59    -- -102.00  57.00 -30.00   60
 19  \w    -60.00 -35.00   0.50    0.59    -- -102.00  57.00 -60.00   50
 20  \w   -152.00 -86.00   0.50    0.59    -- -102.00 -84.00  44.00  132
 21  \w   -112.00 -74.00   0.50    0.59    --  -49.16-125.00 120.00   76
 22  \w   -117.00 -31.00   0.50    0.59    -- -102.00  84.00 164.00  172
 23  \w    -73.00  23.00   0.50    0.59    --  -49.16  84.00 164.00  192
;
_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      0.0757102000
_diffrn_orient_matrix_UB_12      -0.0276522000
_diffrn_orient_matrix_UB_13      0.0509869000
_diffrn_orient_matrix_UB_21      -0.0131385000
_diffrn_orient_matrix_UB_22      0.1080591000
_diffrn_orient_matrix_UB_23      0.0356948000
_diffrn_orient_matrix_UB_31      -0.0590309000
_diffrn_orient_matrix_UB_32      -0.0594795000
_diffrn_orient_matrix_UB_33      0.0411031000
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.9666
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14243
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.9666
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.89
_diffrn_reflns_theta_min         4.28
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30212
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       block
_exptl_crystal_F_000             2209.976
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.9824
_refine_diff_density_min         -0.9524
_refine_diff_density_rms         0.1441
_refine_ls_d_res_high            0.7949
_refine_ls_d_res_low             10.3271
_refine_ls_goodness_of_fit_ref   1.0399
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      0.9865
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.3774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3858
_reflns_number_total             4086
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Py-IPFB2_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568832
_chemical_oxdiff_formula         'Au I F N C H'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
N2A \\sim C14A \\sim F12 \\sim C2A \\sim F12 \\sim C14A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
I1D1 \\sim F2D1 \\sim F12 \\sim F14 \\sim F10 \\sim F1D1 \\sim C2D1 \\sim C7D1
\\sim C6 \\sim C4D1 \\sim C3D1 \\sim C5D1 \\sim C6D2 \\sim I1D2 \\sim C1D2
\\sim C2D2 \\sim F1D2 \\sim F5D2 \\sim C5D2 \\sim C3D2 \\sim F4D2 \\sim C4D2
\\sim F2D2 \\sim F3D2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Uanis(N2A) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C6D2)=Sof(I1D2)=Sof(C1D2)=Sof(C2D2)=Sof(F1D2)=Sof(F5D2)=Sof(C5D2)=
 Sof(C3D2)=Sof(F4D2)=Sof(C4D2)=Sof(F2D2)=Sof(F3D2)=1-FVAR(1)
 Sof(I1D1)=Sof(F2D1)=Sof(F12)=Sof(F14)=Sof(F10)=Sof(F1D1)=Sof(C2D1)=Sof(C7D1)=
 Sof(C6)=Sof(C4D1)=Sof(C3D1)=Sof(C5D1)=FVAR(1)
4.a Free rotating group:
 I1D1(F2D1,F12,F14,F10,F1D1,C2D1,C7D1,C6,C4D1,C3D1,C5D1), C6D2(I1D2,C1D2,C2D2,
 F1D2,F5D2,C5D2,C3D2,F4D2,C4D2,F2D2,F3D2)
4.b Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab)
4.c Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C5A(H5A), C13A(H13A), C14A(H14A)
4.d Idealised Me refined as rotating group:
 C11A(H11a,H11b,H11c), C9A(H9Aa,H9Ab,H9Ac), 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 1.915
_oxdiff_exptl_absorpt_empirical_full_min 0.638