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_1568833
_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         'C26 H30 Au N3, C6 F4 I2'
_chemical_formula_sum            'C32 H30 Au F4 I2 N3'
_chemical_formula_weight         983.384
_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                 103.350(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7868(3)
_cell_length_b                   12.3101(2)
_cell_length_c                   17.1432(3)
_cell_measurement_reflns_used    8745
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.1240
_cell_measurement_theta_min      2.6720
_cell_volume                     3446.87(11)
_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 0.9974
_diffrn_measured_fraction_theta_max 0.9561
_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     90.00 173.00   0.50    0.68    --  102.75  57.00  60.00  166
  2  \w    124.00 173.00   0.50    0.68    --  102.75  50.00 149.00   98
  3  \w     41.00 116.00   0.50    0.17    --   49.03  50.00 149.00  150
  4  \w     95.00 175.00   0.50    0.68    --  102.75  19.00 -60.00  160
  5  \w    122.00 169.00   0.50    0.68    --  102.75  37.00-150.00   94
  6  \w     32.00  61.00   0.50    0.68    --  102.75 -57.00   0.00   58
  7  \w     31.00  56.00   0.50    0.68    --  102.75 -50.00   2.00   50
  8  \w     31.00  56.00   0.50    0.68    --  102.75 -57.00  60.00   50
  9  \w    -22.00  47.00   0.50    0.17    --   49.03 -50.00   2.00  138
 10  \w     31.00  68.00   0.50    0.68    --  102.75 -57.00-180.00   74
 11  \w    -12.00  24.00   0.50    0.17    --  -49.03  19.00 -60.00   72
 12  \w    -12.00  15.00   0.50    0.17    --  -49.03  19.00-120.00   54
 13  \w     55.00  81.00   0.50    0.68    --  102.75 -99.00-120.00   52
 14  \w    -52.00  20.00   0.50    0.17    --  -49.03  50.00 149.00  144
 15  \w    -62.00 -30.00   0.50    0.68    -- -102.00  57.00 150.00   64
 16  \w    -65.00 -34.00   0.50    0.68    -- -102.00  57.00  30.00   62
 17  \w    -61.00 -31.00   0.50    0.68    -- -102.00  57.00   0.00   60
 18  \w    -62.00 -37.00   0.50    0.68    -- -102.00  57.00 120.00   50
 19  \w    -63.00 -37.00   0.50    0.68    -- -102.00  57.00 -30.00   52
 20  \w    -64.00 -34.00   0.50    0.68    -- -102.00  57.00 -60.00   60
 21  \w    -65.00 -30.00   0.50    0.68    -- -102.00  57.00 -90.00   70
 22  \w    -57.00 -30.00   0.50    0.68    -- -102.00  57.00-180.00   54
 23  \w    -70.00 -39.00   0.50    0.17    --  -49.03 -50.00   2.00   62
 24  \w   -174.00-149.00   0.50    0.68    -- -102.00 -50.00   2.00   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      0.0445425000
_diffrn_orient_matrix_UB_12      0.0177487000
_diffrn_orient_matrix_UB_13      0.0882366000
_diffrn_orient_matrix_UB_21      -0.0700274000
_diffrn_orient_matrix_UB_22      0.0746023000
_diffrn_orient_matrix_UB_23      0.0116552000
_diffrn_orient_matrix_UB_31      -0.0447830000
_diffrn_orient_matrix_UB_32      -0.0988970000
_diffrn_orient_matrix_UB_33      0.0247051000
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.9974
_diffrn_reflns_Laue_measured_fraction_max 0.9561
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11827
_diffrn_reflns_point_group_measured_fraction_full 0.9974
_diffrn_reflns_point_group_measured_fraction_max 0.9561
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.34
_diffrn_reflns_theta_min         4.50
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10526
_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    1.895
_exptl_crystal_description       prism
_exptl_crystal_F_000             1847.703
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.8039
_refine_diff_density_min         -1.4664
_refine_diff_density_rms         0.2306
_refine_ls_d_res_high            0.7934
_refine_ls_d_res_low             9.8307
_refine_ls_goodness_of_fit_ref   1.0204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    23
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3459
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0176
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1104P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3204
_reflns_number_total             3459
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Py-14-FIB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568833
_chemical_oxdiff_formula         'Au1 I2 F4 N3 C32 H30'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
N2A \\sim C14A \\sim C13A \\sim C12A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
2.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab)
2.b Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C5A(H5A), C7A(H7A), C14A(H14A)
2.c Idealised Me refined as rotating group:
 C11A(H11a,H11b,H11c), C9A(H9Aa,H9Ab,H9Ac), 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 5.442
_oxdiff_exptl_absorpt_empirical_full_min 0.438