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_1568851
_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         'C33 H43 Au N2, C6 F4 I2'
_chemical_formula_sum            'C39 H43 Au F4 I2 N2'
_chemical_formula_weight         1066.559
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                 104.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0387(3)
_cell_length_b                   14.9567(2)
_cell_length_c                   20.4774(4)
_cell_measurement_reflns_used    12954
_cell_measurement_temperature    123
_cell_measurement_theta_max      75.1280
_cell_measurement_theta_min      3.6400
_cell_volume                     3862.79(13)
_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 0.9971
_diffrn_measured_fraction_theta_max 0.9653
_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    -18.00   8.00   0.50    0.19    --   49.03 -13.00  -0.00   52
  2  \w    -21.00  17.00   0.50    0.19    --   49.03 -19.00-150.00   76
  3  \w     14.00  41.00   0.50    0.19    --   49.03 -37.00-150.00   54
  4  \w     95.00 174.00   0.50    0.78    --  102.75  13.00 170.00  158
  5  \w     42.00 112.00   0.50    0.19    --   49.03  13.00 170.00  140
  6  \w     32.00  80.00   0.50    0.78    --  102.75 -99.00 120.00   96
  7  \w     75.00 105.00   0.50    0.78    --  102.75 -99.00 -30.00   60
  8  \w     44.00  84.00   0.50    0.19    --   49.03-125.00-180.00   80
  9  \w     32.00 101.00   0.50    0.78    --  102.75 -99.00-180.00  138
 10  \w     32.00 103.00   0.50    0.78    --  102.75 -99.00-120.00  142
 11  \w     31.00  69.00   0.50    0.78    --  102.75 -57.00   0.00   76
 12  \w     32.00  68.00   0.50    0.78    --  102.75 -57.00  30.00   72
 13  \w     32.00  69.00   0.50    0.78    --  102.75 -57.00 150.00   74
 14  \w    -62.00 -35.00   0.50    0.78    -- -102.00  57.00 -90.00   54
 15  \w    -62.00 -37.00   0.50    0.78    -- -102.00  57.00-120.00   50
 16  \w    -55.00 -30.00   0.50    0.78    -- -102.00  57.00 -60.00   50
 17  \w     -6.00  19.00   0.50    0.19    --  -49.03  13.00 170.00   50
 18  \w    -13.00  14.00   0.50    0.19    --  -49.03  19.00 -60.00   54
 19  \w   -117.00 -48.00   0.50    0.19    --  -49.03 -13.00  -0.00  138
 20  \w   -174.00-118.00   0.50    0.78    -- -102.00 -19.00  90.00  112
 21  \w   -146.00-104.00   0.50    0.78    -- -102.00 -13.00  -0.00   84
 22  \w   -172.00-147.00   0.50    0.78    -- -102.00 -57.00 -90.00   50
 23  \w   -123.00 -90.00   0.50    0.78    -- -102.00 -57.00 -90.00   66
 24  \w   -171.00-115.00   0.50    0.78    -- -102.00-125.00-180.00  112
 25  \w   -108.00 -81.00   0.50    0.78    -- -102.00-125.00-180.00   54
;
_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      0.1175864000
_diffrn_orient_matrix_UB_12      0.0016615000
_diffrn_orient_matrix_UB_13      -0.0014039000
_diffrn_orient_matrix_UB_21      0.0322029000
_diffrn_orient_matrix_UB_22      0.0178475000
_diffrn_orient_matrix_UB_23      0.0766164000
_diffrn_orient_matrix_UB_31      0.0075028000
_diffrn_orient_matrix_UB_32      -0.1013536000
_diffrn_orient_matrix_UB_33      0.0135476000
_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  0.0764
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.9971
_diffrn_reflns_Laue_measured_fraction_max 0.9653
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28796
_diffrn_reflns_point_group_measured_fraction_full 0.9971
_diffrn_reflns_point_group_measured_fraction_max 0.9653
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.42
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04388
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2040.109
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.5372
_refine_diff_density_min         -1.7052
_refine_diff_density_rms         0.2764
_refine_ls_d_res_high            0.7931
_refine_ls_d_res_low             11.9361
_refine_ls_goodness_of_fit_ref   1.0198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0198
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -11
_reflns_number_gt                6331
_reflns_number_total             7809
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           2Ph-14-FIB_123K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1568851
_chemical_oxdiff_formula         'Au I F N C H'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C22D(H22D), C10D(H10D), C25D(H25D), C13D(H13D)
1.b Secondary CH2 refined with riding coordinates:
 C3D(H3Da,H3Db), C2D(H2Da,H2Db)
1.c Aromatic/amide H refined with riding coordinates:
 C30D(H30D), C18D(H18D), C19D(H19D), C20D(H20D), C7D(H7D), C33D(H33D),
 C31D(H31D), C8D(H8D), C6D(H6D), C32D(H32D), C29D(H29D)
1.d Idealised Me refined as rotating group:
 C23D(H23a,H23b,H23c), C24D(H24a,H24b,H24c), C27D(H27a,H27b,H27c), C11D(H11a,
 H11b,H11c), C26D(H26a,H26b,H26c), C14D(H14a,H14b,H14c), C12D(H12a,H12b,H12c),
 C15D(H15a,H15b,H15c)
;
_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 14.745
_oxdiff_exptl_absorpt_empirical_full_min 0.295