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_1568844
_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 F4 I2'
_chemical_formula_sum            'C36 H37 Au F4 I2 N2'
_chemical_formula_weight         1024.478
_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             2022-03-24
_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                 105.866(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4431(1)
_cell_length_b                   13.9767(1)
_cell_length_c                   16.9424(1)
_cell_measurement_reflns_used    20107
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      4.1840
_cell_volume                     3745.37(5)
_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 1.0000
_diffrn_measured_fraction_theta_max 0.9845
_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     90.00 153.00   0.50    0.30    --  102.75  57.00 -30.00  126
  2  \w    117.00 172.00   0.50    0.30    --  102.75  37.00   0.00  110
  3  \w    136.00 174.00   0.50    0.30    --  102.75  37.00  60.00   76
  4  \w     96.00 133.00   0.50    0.30    --  102.75  37.00  60.00   74
  5  \w     81.00 106.00   0.50    0.30    --  102.75 -99.00  60.00   50
  6  \w     48.00 110.00   0.50    0.30    --  102.75-125.00   0.00  124
  7  \w     32.00  77.00   0.50    0.30    --  102.75-125.00  30.00   90
  8  \w     46.00  71.00   0.50    0.30    --  102.75-112.00 172.00   50
  9  \w     35.00  65.00   0.50    0.30    --  102.75-125.00  90.00   60
 10  \w     68.00 109.00   0.50    0.30    --  102.75-125.00  90.00   82
 11  \w     76.00 106.00   0.50    0.30    --  102.75 -99.00   0.00   60
 12  \w     34.00 108.00   0.50    0.30    --  102.75-107.00-144.18  148
 13  \w     34.00  93.00   0.50    0.07    --   49.16-125.00 -60.00  118
 14  \w     31.00  68.00   0.50    0.30    --  102.75 -57.00-150.00   74
 15  \w     85.00 124.00   0.50    0.30    --  102.75 -77.00-180.00   78
 16  \w     39.00  68.00   0.50    0.30    --  102.75 -57.00-180.00   58
 17  \w     31.00  61.00   0.50    0.30    --  102.75 -57.00   0.00   60
 18  \w     31.00  66.00   0.50    0.30    --  102.75 -57.00 -30.00   70
 19  \w    -19.00  61.00   0.50    0.07    --   49.16 -57.00  30.00  160
 20  \w      9.00  48.00   0.50    0.07    --   49.16-112.00 172.00   78
 21  \w     51.00  80.00   0.50    0.07    --   49.16-112.00 172.00   58
 22  \w     43.00  68.00   0.50    0.30    --  102.75 -57.00  90.00   50
 23  \w    121.00 147.00   0.50    0.30    --  102.75 112.00 -94.00   52
 24  \w     82.00 108.00   0.50    0.30    --  102.75 125.00  90.00   52
 25  \w    111.00 141.00   0.50    0.30    --  102.75 125.00  90.00   60
 26  \w    -13.00  24.00   0.50    0.07    --  -49.16  19.00-120.00   74
 27  \w    -14.00  23.00   0.50    0.07    --  -49.16  19.00 -90.00   74
 28  \w    -14.00  23.00   0.50    0.07    --  -49.16  19.00-150.00   74
 29  \w    -14.00  24.00   0.50    0.07    --  -49.16  19.00-180.00   76
 30  \w   -106.00 -51.00   0.50    0.30    -- -102.00 112.00 -94.00  110
 31  \w    -48.00 -12.00   0.50    0.07    --  -49.16 112.00 -94.00   72
 32  \w    -74.00 -30.00   0.50    0.30    -- -102.00 125.00  30.00   88
 33  \w   -111.00 -32.00   0.50    0.30    -- -102.00 125.00 120.00  158
 34  \w    -60.00 -32.00   0.50    0.30    -- -102.00  57.00 150.00   56
 35  \w    -59.00 -32.00   0.50    0.30    -- -102.00  57.00 120.00   54
 36  \w    -58.00 -33.00   0.50    0.30    -- -102.00  57.00  60.00   50
 37  \w   -133.00 -97.00   0.50    0.30    -- -102.00-112.00 172.00   72
 38  \w   -121.00 -76.00   0.50    0.07    --  -49.16-125.00 -30.00   90
 39  \w   -110.00 -74.00   0.50    0.07    --  -49.16-125.00-120.00   72
 40  \w   -172.00 -81.00   0.50    0.30    -- -102.00 -77.00-180.00  182
;
_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      0.0472702000
_diffrn_orient_matrix_UB_12      -0.0844551000
_diffrn_orient_matrix_UB_13      0.0507913000
_diffrn_orient_matrix_UB_21      -0.0725433000
_diffrn_orient_matrix_UB_22      -0.0677391000
_diffrn_orient_matrix_UB_23      -0.0429393000
_diffrn_orient_matrix_UB_31      0.0446335000
_diffrn_orient_matrix_UB_32      -0.0205806000
_diffrn_orient_matrix_UB_33      -0.0671828000
_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  0.0715
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9845
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22557
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9845
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.42
_diffrn_reflns_theta_min         4.22
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17440
_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    1.817
_exptl_crystal_description       prism
_exptl_crystal_F_000             1943.879
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.9836
_refine_diff_density_min         -2.4338
_refine_diff_density_rms         0.1941
_refine_ls_d_res_high            0.7931
_refine_ls_d_res_low             10.4734
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    29
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0385
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          -0.0015
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+3.8768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3759
_reflns_number_total             3880
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Mes-14-FIB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568844
_chemical_oxdiff_formula         'Au I F N C H'
_olex2_refinement_description
;
1. Others
 Fixed Sof: H17a(0.5) H17b(0.5) H17c(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C7A(H7A), C5A(H5A)
2.c Idealised Me refined as rotating group:
 C11A(H11a,H11b,H11c), C16A(H16a,H16b,H16c), C9A(H9Aa,H9Ab,H9Ac), C17A(H17a,
 H17b,H17c), 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 4.163
_oxdiff_exptl_absorpt_empirical_full_min 0.579