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_1568838
_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         'C29 H35 Au N2'
_chemical_formula_sum            'C29 H35 Au N2'
_chemical_formula_weight         608.581
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.4227(1)
_cell_length_b                   14.0371(1)
_cell_length_c                   43.5602(4)
_cell_measurement_reflns_used    29514
_cell_measurement_temperature    123
_cell_measurement_theta_max      76.3580
_cell_measurement_theta_min      4.1560
_cell_volume                     10653.26(14)
_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 0.9991
_diffrn_measured_fraction_theta_max 0.9785
_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     38.00  66.00   0.50    0.48    --  102.75 -57.00   0.00   56
  2  \w     34.00  68.00   0.50    0.48    --  102.75 -57.00  30.00   68
  3  \w     32.00  68.00   0.50    0.48    --  102.75 -57.00  60.00   72
  4  \w    118.00 170.00   0.50    0.48    --  102.75  37.00  60.00  104
  5  \w    116.00 174.00   0.50    0.48    --  102.75  19.00  30.00  116
  6  \w     31.00  68.00   0.50    0.48    --  102.75 -57.00-180.00   74
  7  \w    -16.00  37.00   0.50    0.12    --   49.03 -35.00-169.00  106
  8  \w     38.00  64.00   0.50    0.48    --  102.75 -99.00 -60.00   52
  9  \w     57.00 110.00   0.50    0.12    --   49.03-151.00 -34.00  106
 10  \w     78.00 104.00   0.50    0.48    --  102.75 -99.00 -60.00   52
 11  \w    -14.00  11.00   0.50    0.12    --  -49.03  19.00  30.00   50
 12  \w    -13.00  24.00   0.50    0.12    --  -49.03  19.00  60.00   74
 13  \w    -11.00  15.00   0.50    0.12    --  -49.03  19.00 120.00   52
 14  \w    -13.00  22.00   0.50    0.12    --  -49.03  19.00  90.00   70
 15  \w     -4.00  21.00   0.50    0.12    --  -49.03  19.00-150.00   50
 16  \w    -65.00 -34.00   0.50    0.48    -- -102.00  57.00-150.00   62
 17  \w    -60.00 -30.00   0.50    0.48    -- -102.00  57.00-180.00   60
 18  \w    -65.00 -40.00   0.50    0.48    -- -102.00  57.00-120.00   50
 19  \w   -123.00 -66.00   0.50    0.48    -- -102.00  77.00 150.00  114
 20  \w    -66.00 -40.00   0.50    0.48    -- -102.00 121.00-151.00   52
 21  \w    -68.00 -30.00   0.50    0.48    -- -102.00  87.00 132.00   76
 22  \w   -175.00-101.00   0.50    0.48    -- -102.00 -35.00-169.00  148
;
_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      -0.0006325000
_diffrn_orient_matrix_UB_12      -0.0273342000
_diffrn_orient_matrix_UB_13      -0.0342509000
_diffrn_orient_matrix_UB_21      -0.0401081000
_diffrn_orient_matrix_UB_22      -0.0946452000
_diffrn_orient_matrix_UB_23      0.0079503000
_diffrn_orient_matrix_UB_31      -0.0787813000
_diffrn_orient_matrix_UB_32      0.0484414000
_diffrn_orient_matrix_UB_33      -0.0037773000
_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  0.0664
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9785
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            63204
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9785
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.39
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28314
_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    1.518
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             4784.129
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.4387
_refine_diff_density_min         -1.3247
_refine_diff_density_rms         0.1521
_refine_ls_d_res_high            0.7932
_refine_ls_d_res_low             21.7801
_refine_ls_goodness_of_fit_ref   1.0450
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    104
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0450
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0455P)^2^+14.8158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              54
_reflns_limit_l_min              0
_reflns_number_gt                9429
_reflns_number_total             10939
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Xyl_123K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568838
_chemical_oxdiff_formula         'Au N C H'
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2a(H2aa,H2ab), C3a(H3aa,H3ab), C3b(H3ba,H3bb), C2b(H2ba,H2bb)
1.b Aromatic/amide H refined with riding coordinates:
 C26a(H26a), C24a(H24a), C25a(H25a), C17b(H17b), C24b(H24b), C8a(H8a),
 C26b(H26b), C17a(H17a), C25b(H25b), C15a(H15a), C6a(H6a), C15b(H15b), C8b(H8b),
  C6b(H6b)
1.c Idealised Me refined as rotating group:
 C28a(H28a,H28b,H28c), C29a(H29a,H29b,H29c), C21a(H21a,H21b,H21c), C28b(H28d,
 H28e,H28f), C12a(H12a,H12b,H12c), C19b(H19d,H19e,H19f), C10a(H10a,H10b,H10c),
 C20b(H20d,H20e,H20f), C11a(H11a,H11b,H11c), C12b(H12d,H12e,H12f), C21b(H21d,
 H21e,H21f), C19a(H19a,H19b,H19c), C20a(H20a,H20b,H20c), C10b(H10d,H10e,H10f),
 C29b(H29d,H29e,H29f), C11b(H11d,H11e,H11f)
;
_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 3.262
_oxdiff_exptl_absorpt_empirical_full_min 0.362