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_1568846
_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         'C27 H31 Au N2, 2(C3 F2 I), C H2 Cl2'
_chemical_formula_sum            'C34 H33 Au Cl2 F4 I2 N2'
_chemical_formula_weight         1067.329
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                74.354(1)
_cell_angle_beta                 81.135(1)
_cell_angle_gamma                79.723(1)
_cell_formula_units_Z            2
_cell_length_a                   10.3982(1)
_cell_length_b                   10.7030(1)
_cell_length_c                   17.5621(2)
_cell_measurement_reflns_used    19185
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.3480
_cell_measurement_theta_min      2.5900
_cell_volume                     1840.28(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 (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 0.9989
_diffrn_measured_fraction_theta_max 0.9623
_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     99.00 174.00   0.50    0.16    --  102.75  57.00  60.00  150
  2  \w     90.00 154.00   0.50    0.16    --  102.75  57.00   0.00  128
  3  \w     91.00 122.00   0.50    0.16    --  102.75  57.00 -30.00   62
  4  \w    129.00 171.00   0.50    0.16    --  102.75  57.00 -30.00   84
  5  \w    129.00 155.00   0.50    0.16    --  102.75  37.00-150.00   52
  6  \w     36.00  91.00   0.50    0.16    --  102.75 -99.00   0.00  110
  7  \w     81.00 109.00   0.50    0.16    --  102.75-152.00  10.00   56
  8  \w     60.00 105.00   0.50    0.05    --   49.03-152.00  10.00   90
  9  \w     49.00  75.00   0.50    0.16    --  102.75 -99.00 -60.00   52
 10  \w     46.00 102.00   0.50    0.16    --  102.75 -99.00  30.00  112
 11  \w     81.00 106.00   0.50    0.16    --  102.75 -99.00 -60.00   50
 12  \w     38.00  64.00   0.50    0.16    --  102.75 -99.00  60.00   52
 13  \w     36.00  78.00   0.50    0.16    --  102.75-125.00 120.00   84
 14  \w     46.00  72.00   0.50    0.16    --  102.75-121.00 170.00   52
 15  \w     32.00 106.00   0.50    0.16    --  102.75 -99.00 120.00  148
 16  \w     26.00  88.00   0.50    0.05    --   49.03-121.00 170.00  124
 17  \w     74.00 106.00   0.50    0.16    --  102.75 -99.00  60.00   64
 18  \w     73.00  99.00   0.50    0.16    --  102.75 -99.00-180.00   52
 19  \w     32.00  57.00   0.50    0.16    --  102.75 -99.00-180.00   50
 20  \w    -21.00  12.00   0.50    0.05    --   49.03 -19.00 -30.00   66
 21  \w    -23.00  13.00   0.50    0.05    --   49.03 -19.00 -90.00   72
 22  \w    -23.00  14.00   0.50    0.05    --   49.03 -19.00  30.00   74
 23  \w    -21.00  10.00   0.50    0.05    --   49.03 -19.00  60.00   62
 24  \w     72.00 123.00   0.50    0.16    --  102.75 -77.00 120.00  102
 25  \w     97.00 135.00   0.50    0.16    --  102.75 121.00-106.00   76
 26  \w     88.00 113.00   0.50    0.16    --  102.75 152.00  52.00   50
 27  \w     83.00 108.00   0.50    0.05    --   49.03 152.00  52.00   50
 28  \w    -14.00  11.00   0.50    0.05    --  -49.03  19.00   0.00   50
 29  \w    -64.00 -39.00   0.50    0.16    -- -102.00  57.00 -90.00   50
 30  \w    -63.00 -30.00   0.50    0.16    -- -102.00  57.00-120.00   66
 31  \w    -63.00 -32.00   0.50    0.16    -- -102.00  57.00-180.00   62
 32  \w    -13.00  19.00   0.50    0.05    --  -49.03  19.00 -90.00   64
 33  \w    -56.00 -31.00   0.50    0.16    -- -102.00  57.00 -60.00   50
 34  \w    -62.00 -30.00   0.50    0.16    -- -102.00  57.00   0.00   64
 35  \w    -55.00 -30.00   0.50    0.16    -- -102.00  57.00 120.00   50
 36  \w    -93.00 -68.00   0.50    0.05    --  -49.03 152.00  52.00   50
 37  \w   -107.00 -33.00   0.50    0.16    -- -102.00 121.00-106.00  148
 38  \w   -111.00 -74.00   0.50    0.16    -- -102.00 125.00-150.00   74
 39  \w    -76.00 -51.00   0.50    0.05    --  -49.03 121.00-106.00   50
 40  \w   -123.00 -97.00   0.50    0.16    -- -102.00 152.00  52.00   52
 41  \w   -174.00 -94.00   0.50    0.16    -- -102.00 -37.00-120.00  160
 42  \w   -173.00-107.00   0.50    0.16    -- -102.00 -37.00-180.00  132
 43  \w   -120.00 -30.00   0.50    0.05    --  -49.03 -77.00  30.00  180
 44  \w   -113.00 -56.00   0.50    0.05    --  -49.03-152.00  10.00  114
 45  \w   -105.00 -77.00   0.50    0.16    -- -102.00-152.00  10.00   56
 46  \w   -150.00-125.00   0.50    0.16    -- -102.00-121.00 170.00   50
;
_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      -0.0298613000
_diffrn_orient_matrix_UB_12      -0.1046435000
_diffrn_orient_matrix_UB_13      0.0774559000
_diffrn_orient_matrix_UB_21      0.0459735000
_diffrn_orient_matrix_UB_22      0.0817179000
_diffrn_orient_matrix_UB_23      0.0479539000
_diffrn_orient_matrix_UB_31      -0.1412595000
_diffrn_orient_matrix_UB_32      0.0720210000
_diffrn_orient_matrix_UB_33      0.0102321000
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.9989
_diffrn_reflns_Laue_measured_fraction_max 0.9623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25340
_diffrn_reflns_point_group_measured_fraction_full 0.9989
_diffrn_reflns_point_group_measured_fraction_max 0.9623
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.49
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18311
_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    1.926
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1009.393
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.9867
_refine_diff_density_min         -1.2707
_refine_diff_density_rms         0.1863
_refine_ls_d_res_high            0.7929
_refine_ls_d_res_low             16.8052
_refine_ls_goodness_of_fit_ref   1.0062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0062
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6849
_reflns_number_total             7447
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Ph-14-FIB-DCM_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568846
_chemical_oxdiff_formula         'Au I Cl F N C H'
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab), C3A(H3Aa,H3Ab), C3S(H3Sa,H3Sb)
1.b Aromatic/amide H refined with riding coordinates:
 C17A(H17A), C15A(H15A), C8A(H8A), C27A(H27A), C23A(H23A), C6A(H6A),
 C26A(H26A), C24A(H24A), C25A(H25A)
1.c Idealised Me refined as rotating group:
 C19A(H19a,H19b,H19c), C12A(H12a,H12b,H12c), C10A(H10a,H10b,H10c), C21A(H21a,
 H21b,H21c), C20A(H20a,H20b,H20c), 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 2.959
_oxdiff_exptl_absorpt_empirical_full_min 0.436