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_1568852
_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         'C30 H37 Au N2, C6 F5 I'
_chemical_formula_sum            'C36 H37 Au F5 I N2'
_chemical_formula_weight         916.571
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                 96.0965(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.46330(5)
_cell_length_b                   13.75475(6)
_cell_length_c                   23.61408(10)
_cell_measurement_reflns_used    47088
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.2670
_cell_measurement_theta_min      3.6950
_cell_volume                     3702.29(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 0.9997
_diffrn_measured_fraction_theta_max 0.9812
_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     73.00  99.00   0.50    0.10    --   49.03  77.00   0.00   52
  2  \w     86.00 111.00   0.50    0.10    --   49.03  77.00  30.00   50
  3  \w     45.00 117.00   0.50    0.10    --   49.03  77.00  90.00  144
  4  \w     50.00  76.00   0.50    0.10    --   49.03  57.00  90.00   52
  5  \w     29.00  77.00   0.50    0.10    --   49.03  77.00  30.00   96
  6  \w     28.00  63.00   0.50    0.10    --   49.03  77.00   0.00   70
  7  \w     56.00 112.00   0.50    0.10    --   49.03  30.00 -53.00  112
  8  \w     83.00 108.00   0.50    0.53    --  102.75  77.00  60.00   50
  9  \w     82.00 108.00   0.50    0.53    --  102.75  77.00  30.00   52
 10  \w     82.00 108.00   0.50    0.53    --  102.75  77.00 -30.00   52
 11  \w    102.00 145.00   0.50    0.53    --  102.75  30.00 -53.00   86
 12  \w     95.00 175.00   0.50    0.53    --  102.75  19.00 -90.00  160
 13  \w    148.00 174.00   0.50    0.53    --  102.75  77.00  30.00   52
 14  \w    147.00 172.00   0.50    0.53    --  102.75  77.00  60.00   50
 15  \w     90.00 167.00   0.50    0.53    --  102.75  57.00  90.00  154
 16  \w      0.00  30.00   0.50    0.10    --   49.03 -30.00 146.00   60
 17  \w     52.00  77.00   0.50    0.53    --  102.75-125.00 -30.00   50
 18  \w     31.00  68.00   0.50    0.53    --  102.75 -57.00-180.00   74
 19  \w     49.00 105.00   0.50    0.53    --  102.75 -99.00  60.00  112
 20  \w     33.00 123.00   0.50    0.53    --  102.75 -77.00 120.00  180
 21  \w    -13.00  24.00   0.50    0.10    --  -49.03  19.00  90.00   74
 22  \w    -13.00  19.00   0.50    0.10    --  -49.03  19.00  60.00   64
 23  \w    -27.00  -2.00   0.50    0.10    --  -49.03  30.00 -53.00   50
 24  \w    -66.00 -35.00   0.50    0.53    -- -102.00  77.00  60.00   62
 25  \w    -55.00 -30.00   0.50    0.53    -- -102.00  57.00  90.00   50
 26  \w    -65.00 -30.00   0.50    0.53    -- -102.00  57.00 120.00   70
 27  \w    -60.00 -32.00   0.50    0.53    -- -102.00  57.00  60.00   56
 28  \w    -62.00 -31.00   0.50    0.53    -- -102.00  57.00  30.00   62
 29  \w   -118.00 -93.00   0.50    0.53    -- -102.00  77.00  60.00   50
 30  \w    -63.00 -35.00   0.50    0.53    -- -102.00  57.00 150.00   56
 31  \w   -102.00 -42.00   0.50    0.10    --  -49.03 -19.00  30.00  120
 32  \w    -59.00 -34.00   0.50    0.10    --  -49.03 -77.00  30.00   50
 33  \w    -91.00 -66.00   0.50    0.10    --  -49.03 -37.00  90.00   50
 34  \w   -106.00 -81.00   0.50    0.10    --  -49.03 -30.00 146.00   50
 35  \w   -155.00-130.00   0.50    0.53    -- -102.00 -30.00 146.00   50
 36  \w   -151.00-125.00   0.50    0.53    -- -102.00 -79.00  85.07   52
 37  \w   -106.00 -80.00   0.50    0.53    -- -102.00 -80.00  25.01   52
 38  \w   -107.00 -81.00   0.50    0.53    -- -102.00 -77.00  18.22   52
 39  \w   -108.00 -82.00   0.50    0.53    -- -102.00 -79.00  61.47   52
 40  \w   -120.00 -81.00   0.50    0.53    -- -102.00 -77.00  60.00   78
 41  \w   -106.00 -81.00   0.50    0.53    -- -102.00 -77.00  30.00   50
 42  \w   -105.00 -80.00   0.50    0.53    -- -102.00 -79.00  85.07   50
 43  \w   -106.00 -81.00   0.50    0.53    -- -102.00 -77.00  90.00   50
 44  \w   -106.00 -81.00   0.50    0.53    -- -102.00 -77.00 120.00   50
 45  \w   -107.00 -82.00   0.50    0.53    -- -102.00 -76.00  90.19   50
 46  \w   -108.00 -82.00   0.50    0.53    -- -102.00 -76.00  65.05   52
 47  \w   -111.00 -82.00   0.50    0.53    -- -102.00 -76.00  13.23   58
 48  \w   -166.00-141.00   0.50    0.53    -- -102.00 -76.00  13.23   50
 49  \w   -169.00-143.00   0.50    0.53    -- -102.00 -77.00  30.00   52
 50  \w   -171.00 -83.00   0.50    0.53    -- -102.00 -72.00  47.37  176
 51  \w   -107.00 -82.00   0.50    0.53    -- -102.00 -74.00  31.11   50
 52  \w   -107.00 -82.00   0.50    0.53    -- -102.00 -75.00  94.32   50
 53  \w   -155.00-129.00   0.50    0.53    -- -102.00 -77.00 120.00   52
 54  \w   -172.00-146.00   0.50    0.53    -- -102.00 -75.00  94.32   52
 55  \w   -111.00 -86.00   0.50    0.53    -- -102.00 -67.00 103.45   50
 56  \w   -110.00 -85.00   0.50    0.53    -- -102.00 -67.00  90.10   50
 57  \w   -113.00 -87.00   0.50    0.53    -- -102.00 -67.00  60.46   52
 58  \w   -114.00 -88.00   0.50    0.53    -- -102.00 -64.00  24.51   52
 59  \w   -118.00 -86.00   0.50    0.53    -- -102.00 -69.00  15.99   64
 60  \w   -162.00 -87.00   0.50    0.53    -- -102.00 -69.00   1.01  150
 61  \w   -164.00-131.00   0.50    0.53    -- -102.00 -67.00 103.45   66
 62  \w   -113.00 -87.00   0.50    0.53    -- -102.00 -65.00  90.90   52
 63  \w   -111.00 -86.00   0.50    0.53    -- -102.00 -64.00  94.96   50
 64  \w   -113.00 -88.00   0.50    0.53    -- -102.00 -60.00 113.44   50
 65  \w   -122.00 -92.00   0.50    0.53    -- -102.00 -47.00  91.63   60
 66  \w   -140.00 -88.00   0.50    0.53    -- -102.00 -62.00  61.56  104
 67  \w   -174.00 -86.00   0.50    0.53    -- -102.00 -64.00  60.36  176
 68  \w   -153.00 -87.00   0.50    0.53    -- -102.00 -63.00  26.88  132
 69  \w   -105.00 -80.00   0.50    0.53    -- -102.00 -84.00  58.35   50
 70  \w   -105.00 -80.00   0.50    0.53    -- -102.00 -86.00 113.06   50
 71  \w   -112.00 -75.00   0.50    0.10    --  -49.03-125.00 -90.00   74
 72  \w   -120.00 -75.00   0.50    0.10    --  -49.03-125.00-120.00   90
;
_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      0.0980738000
_diffrn_orient_matrix_UB_12      0.0308327000
_diffrn_orient_matrix_UB_13      0.0461926000
_diffrn_orient_matrix_UB_21      0.0764742000
_diffrn_orient_matrix_UB_22      0.0316834000
_diffrn_orient_matrix_UB_23      -0.0465691000
_diffrn_orient_matrix_UB_31      -0.0529373000
_diffrn_orient_matrix_UB_32      0.1029312000
_diffrn_orient_matrix_UB_33      0.0004883000
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9812
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71394
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9812
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.35
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37062
_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    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             1767.131
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.5877
_refine_diff_density_min         -0.9717
_refine_diff_density_rms         0.0742
_refine_ls_d_res_high            0.7933
_refine_ls_d_res_low             11.8683
_refine_ls_goodness_of_fit_ref   1.0238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0238
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+2.2413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7009
_reflns_number_total             7628
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Mes-IPFB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568852
_chemical_oxdiff_formula         'Au I F N C H'
_reflns_odcompleteness_completeness 99.99
_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.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab), C3A(H3Aa,H3Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C26A(H26A), C8A(H8A), C24A(H24A), C15A(H15A), C17A(H17A), C6A(H6A)
2.c Idealised Me refined as rotating group:
 C30A(H30a,H30b,H30c), C20A(H20a,H20b,H20c), C10A(H10a,H10b,H10c), C28A(H28a,
 H28b,H28c), C29A(H29a,H29b,H29c), C12A(H12a,H12b,H12c), C21A(H21a,H21b,H21c),
 C19A(H19a,H19b,H19c), C11A(H11a,H11b,H11c)
;
_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 2.833
_oxdiff_exptl_absorpt_empirical_full_min 0.588