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_1568845
_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                 96.4045(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.32485(5)
_cell_length_b                   13.62150(7)
_cell_length_c                   23.47007(11)
_cell_measurement_reflns_used    50664
_cell_measurement_temperature    123
_cell_measurement_theta_max      76.0570
_cell_measurement_theta_min      3.7320
_cell_volume                     3597.93(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      123
_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 0.9789
_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     81.00 108.00   0.50    0.05    --   49.03  77.00  30.00   54
  2  \w     37.00  63.00   0.50    0.05    --   49.03  77.00  60.00   52
  3  \w     32.00  63.00   0.50    0.05    --   49.03  77.00 120.00   62
  4  \w     38.00  63.00   0.50    0.05    --   49.03  77.00  90.00   50
  5  \w     96.00 121.00   0.50    0.05    --   49.03  77.00  90.00   50
  6  \w     38.00  67.00   0.50    0.05    --   49.03  77.00  30.00   58
  7  \w     28.00  55.00   0.50    0.05    --   49.03  77.00   0.00   54
  8  \w     66.00 107.00   0.50    0.05    --   49.03  30.00 -47.00   82
  9  \w    -13.00  24.00   0.50    0.05    --  -49.03  19.00  90.00   74
 10  \w    -28.00  -2.00   0.50    0.05    --  -49.03  30.00 -47.00   52
 11  \w     31.00  95.00   0.50    0.14    --  102.75-125.00  90.00  128
 12  \w     34.00  68.00   0.50    0.14    --  102.75 -77.00  90.00   68
 13  \w     76.00 124.00   0.50    0.14    --  102.75 -77.00  90.00   96
 14  \w     34.00  65.00   0.50    0.14    --  102.75 -57.00 -60.00   62
 15  \w     31.00  68.00   0.50    0.14    --  102.75 -57.00 -90.00   74
 16  \w     32.00  68.00   0.50    0.14    --  102.75 -57.00-120.00   72
 17  \w     31.00  68.00   0.50    0.14    --  102.75 -57.00-150.00   74
 18  \w     31.00  69.00   0.50    0.14    --  102.75 -57.00-180.00   76
 19  \w    -23.00  29.00   0.50    0.05    --   49.03 -30.00 152.00  104
 20  \w    -22.00  41.00   0.50    0.05    --   49.03 -37.00  30.00  126
 21  \w    101.00 136.00   0.50    0.14    --  102.75  30.00 -47.00   70
 22  \w     82.00 108.00   0.50    0.14    --  102.75  77.00  30.00   52
 23  \w     83.00 108.00   0.50    0.14    --  102.75  77.00  60.00   50
 24  \w     90.00 147.00   0.50    0.14    --  102.75  57.00  30.00  114
 25  \w    119.00 170.00   0.50    0.14    --  102.75  37.00-120.00  102
 26  \w    -64.00 -34.00   0.50    0.14    -- -102.00  57.00  60.00   60
 27  \w    -60.00 -35.00   0.50    0.14    -- -102.00  57.00  90.00   50
 28  \w    -62.00 -36.00   0.50    0.14    -- -102.00  57.00 120.00   52
 29  \w    -60.00 -30.00   0.50    0.14    -- -102.00  57.00 150.00   60
 30  \w    -78.00 -49.00   0.50    0.05    --  -49.03 -19.00  60.00   58
 31  \w   -107.00 -48.00   0.50    0.14    -- -102.00 125.00 -30.00  118
 32  \w   -109.00 -48.00   0.50    0.05    --  -49.03 -30.00 152.00  122
 33  \w   -119.00 -81.00   0.50    0.05    --  -49.03 -19.00  60.00   76
 34  \w    -79.00 -40.00   0.50    0.05    --  -49.03 -57.00 -60.00   78
 35  \w   -107.00 -81.00   0.50    0.14    -- -102.00 -77.00  73.64   52
 36  \w   -107.00 -81.00   0.50    0.14    -- -102.00 -77.00 120.00   52
 37  \w   -109.00 -83.00   0.50    0.14    -- -102.00 -77.00  60.00   52
 38  \w   -106.00 -81.00   0.50    0.14    -- -102.00 -77.00  90.00   50
 39  \w   -110.00 -81.00   0.50    0.14    -- -102.00 -77.00  30.00   58
 40  \w   -158.00-132.00   0.50    0.14    -- -102.00 -77.00  90.00   52
 41  \w   -169.00-143.00   0.50    0.14    -- -102.00 -77.00  60.00   52
 42  \w   -174.00-149.00   0.50    0.14    -- -102.00 -76.00  52.64   50
 43  \w   -169.00-143.00   0.50    0.14    -- -102.00 -77.00  30.00   52
 44  \w   -113.00 -82.00   0.50    0.14    -- -102.00 -76.00  16.59   62
 45  \w   -107.00 -82.00   0.50    0.14    -- -102.00 -76.00  52.64   50
 46  \w   -110.00 -82.00   0.50    0.14    -- -102.00 -74.00  77.39   56
 47  \w   -108.00 -82.00   0.50    0.14    -- -102.00 -75.00  88.40   52
 48  \w   -108.00 -82.00   0.50    0.14    -- -102.00 -74.00  96.92   52
 49  \w   -112.00 -87.00   0.50    0.14    -- -102.00 -75.00  95.53   50
 50  \w   -108.00 -82.00   0.50    0.14    -- -102.00 -74.00 113.97   52
 51  \w   -107.00 -82.00   0.50    0.14    -- -102.00 -74.00 132.09   50
 52  \w   -110.00 -85.00   0.50    0.14    -- -102.00 -67.00 103.95   50
 53  \w   -111.00 -86.00   0.50    0.14    -- -102.00 -66.00  82.76   50
 54  \w   -113.00 -88.00   0.50    0.14    -- -102.00 -64.00 115.45   50
 55  \w   -146.00 -85.00   0.50    0.14    -- -102.00 -69.00  66.59  122
 56  \w   -173.00 -86.00   0.50    0.14    -- -102.00 -64.00  48.98  174
 57  \w   -110.00 -84.00   0.50    0.14    -- -102.00 -71.00  18.20   52
 58  \w   -109.00 -84.00   0.50    0.14    -- -102.00 -70.00  35.08   50
 59  \w   -111.00 -86.00   0.50    0.14    -- -102.00 -64.00  31.48   50
 60  \w   -113.00 -87.00   0.50    0.14    -- -102.00 -62.00  92.30   52
 61  \w   -157.00 -88.00   0.50    0.14    -- -102.00 -59.00 104.24  138
 62  \w   -173.00 -89.00   0.50    0.14    -- -102.00 -57.00 120.00  168
 63  \w   -115.00 -90.00   0.50    0.14    -- -102.00 -60.00  86.35   50
 64  \w   -139.00 -91.00   0.50    0.14    -- -102.00 -51.00  72.10   96
 65  \w   -152.00-127.00   0.50    0.14    -- -102.00 -55.00  25.08   50
 66  \w   -158.00-133.00   0.50    0.14    -- -102.00 -30.00 152.00   50
 67  \w   -174.00 -88.00   0.50    0.14    -- -102.00 -61.00  14.13  172
 68  \w   -116.00 -91.00   0.50    0.14    -- -102.00 -55.00  25.08   50
 69  \w   -161.00-136.00   0.50    0.14    -- -102.00 -37.00 -30.00   50
 70  \w   -168.00 -91.00   0.50    0.14    -- -102.00 -57.00   0.00  154
 71  \w   -105.00 -80.00   0.50    0.14    -- -102.00 -81.00  44.62   50
 72  \w   -105.00 -80.00   0.50    0.14    -- -102.00 -85.00 112.63   50
 73  \w   -120.00 -90.00   0.50    0.05    --  -49.03-125.00 -30.00   60
;
_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      0.1016842000
_diffrn_orient_matrix_UB_12      0.0272616000
_diffrn_orient_matrix_UB_13      0.0464725000
_diffrn_orient_matrix_UB_21      0.0753732000
_diffrn_orient_matrix_UB_22      0.0351815000
_diffrn_orient_matrix_UB_23      -0.0467528000
_diffrn_orient_matrix_UB_31      -0.0521513000
_diffrn_orient_matrix_UB_32      0.1040357000
_diffrn_orient_matrix_UB_33      0.0035957000
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9789
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70735
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9789
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.42
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56077
_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    1.692
_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         0.9958
_refine_diff_density_min         -0.6032
_refine_diff_density_rms         0.0994
_refine_ls_d_res_high            0.7931
_refine_ls_d_res_low             11.7624
_refine_ls_goodness_of_fit_ref   1.0468
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0468
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0287P)^2^+4.7208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7138
_reflns_number_total             7408
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Mes-IPFB_123K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568845
_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.a Secondary CH2 refined with riding coordinates:
 C3A(H3Aa,H3Ab), C2A(H2Aa,H2Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C26A(H26A), C17A(H17A), C6A(H6A), C8A(H8A), C15A(H15A)
2.c Idealised Me refined as rotating group:
 C28A(H28a,H28b,H28c), C29A(H29a,H29b,H29c), C19A(H19a,H19b,H19c), C10A(H10a,
 H10b,H10c), C30A(H30a,H30b,H30c), C21A(H21a,H21b,H21c), C11A(H11a,H11b,H11c),
 C12A(H12a,H12b,H12c), C20A(H20a,H20b,H20c)
;
_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.715