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_1568831
_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'
_chemical_formula_sum            'C27 H31 Au N2'
_chemical_formula_weight         580.527
_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                94.212(2)
_cell_angle_beta                 100.250(2)
_cell_angle_gamma                100.060(3)
_cell_formula_units_Z            4
_cell_length_a                   9.5629(3)
_cell_length_b                   15.6651(5)
_cell_length_c                   16.4537(4)
_cell_measurement_reflns_used    12280
_cell_measurement_temperature    123
_cell_measurement_theta_max      76.0930
_cell_measurement_theta_min      2.8450
_cell_volume                     2374.26(12)
_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      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9891
_diffrn_measured_fraction_theta_max 0.9477
_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     41.00 120.00   0.50    0.16    --   47.78  17.00  30.00  158
  2  \w    128.00 175.00   0.50    0.63    --  102.75  19.00 120.00   94
  3  \w     96.00 174.00   0.50    0.63    --  102.75  57.00  90.00  156
  4  \w     95.00 164.00   0.50    0.63    --  102.75  17.00  30.00  138
  5  \w    120.00 171.00   0.50    0.63    --  102.75  37.00 -30.00  102
  6  \w    102.00 156.00   0.50    0.63    --  102.75  19.00 -90.00  108
  7  \w     32.00  65.00   0.50    0.63    --  102.75 -57.00  30.00   66
  8  \w     32.00  76.00   0.50    0.63    --  102.75 -77.00  60.00   88
  9  \w     98.00 124.00   0.50    0.63    --  102.75 -77.00  60.00   52
 10  \w     38.00 102.00   0.50    0.63    --  102.75 -77.00 -60.00  128
 11  \w     52.00  90.00   0.50    0.16    --   47.78-125.00 -90.00   76
 12  \w     67.00 101.00   0.50    0.63    --  102.75-125.00-150.00   68
 13  \w     32.00 104.00   0.50    0.63    --  102.75 -99.00 -60.00  144
 14  \w     81.00 106.00   0.50    0.63    --  102.75 -99.00 -30.00   50
 15  \w     72.00 109.00   0.50    0.63    --  102.75-125.00  60.00   74
 16  \w     42.00  68.00   0.50    0.63    --  102.75-125.00  60.00   52
 17  \w     31.00  74.00   0.50    0.63    --  102.75 -99.00  60.00   86
 18  \w     64.00 106.00   0.50    0.63    --  102.75 -99.00  90.00   84
 19  \w     33.00  72.00   0.50    0.63    --  102.75 -99.00-120.00   78
 20  \w     74.00 106.00   0.50    0.63    --  102.75 -99.00-120.00   64
 21  \w     31.00 105.00   0.50    0.63    --  102.75 -99.00-150.00  148
 22  \w    -25.00  14.00   0.50    0.16    --   47.78 -17.00-138.00   78
 23  \w    -11.00  61.00   0.50    0.16    --   47.78 -57.00-120.00  144
 24  \w     -8.00  57.00   0.50    0.16    --   47.78 -57.00  90.00  130
 25  \w     80.00 162.00   0.50    0.63    --  102.75 125.00  30.00  164
 26  \w    -34.00  21.00   0.50    0.16    --  -47.78  37.00 -60.00  110
 27  \w     -5.00  20.00   0.50    0.16    --  -47.78  17.00  30.00   50
 28  \w    -11.00  20.00   0.50    0.16    --  -47.78  19.00-120.00   62
 29  \w     -6.00  19.00   0.50    0.16    --  -47.78  19.00-180.00   50
 30  \w    -65.00 -39.00   0.50    0.63    -- -102.00  57.00-120.00   52
 31  \w    -60.00 -33.00   0.50    0.63    -- -102.00  57.00   0.00   54
 32  \w    -65.00 -40.00   0.50    0.63    -- -102.00  57.00  30.00   50
 33  \w    -64.00 -30.00   0.50    0.63    -- -102.00  57.00 120.00   68
 34  \w   -110.00 -40.00   0.50    0.63    -- -102.00 125.00  90.00  140
 35  \w   -172.00-104.00   0.50    0.63    -- -102.00 -17.00-138.00  136
 36  \w   -119.00 -42.00   0.50    0.16    --  -47.78 -17.00-138.00  154
 37  \w   -168.00-110.00   0.50    0.63    -- -102.00 -99.00  30.00  116
;
_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      0.1307870000
_diffrn_orient_matrix_UB_12      -0.0460526000
_diffrn_orient_matrix_UB_13      0.0131350000
_diffrn_orient_matrix_UB_21      -0.1034273000
_diffrn_orient_matrix_UB_22      -0.0892805000
_diffrn_orient_matrix_UB_23      -0.0171200000
_diffrn_orient_matrix_UB_31      0.0041521000
_diffrn_orient_matrix_UB_32      -0.0012203000
_diffrn_orient_matrix_UB_33      -0.0932433000
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.9891
_diffrn_reflns_Laue_measured_fraction_max 0.9477
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27456
_diffrn_reflns_point_group_measured_fraction_full 0.9891
_diffrn_reflns_point_group_measured_fraction_max 0.9477
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.25
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22328
_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    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1131.879
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.7185
_refine_diff_density_min         -1.3171
_refine_diff_density_rms         0.2388
_refine_ls_d_res_high            0.7937
_refine_ls_d_res_low             15.3342
_refine_ls_goodness_of_fit_ref   1.0687
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    96
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0687
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0622P)^2^+18.4577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8009
_reflns_number_total             9415
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Ph_123K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568831
_chemical_oxdiff_formula         'Au N C H'
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C3a(H3aa,H3ab), C3b(H3ba,H3bb), C2b(H2ba,H2bb), C2a(H2aa,H2ab)
1.b Aromatic/amide H refined with riding coordinates:
 C23a(H23a), C17b(H17b), C26a(H26a), C27b(H27b), C15b(H15b), C17a(H17a),
 C26b(H26b), C6b(H6b), C23b(H23b), C24a(H24a), C15a(H15a), C24b(H24b),
 C27a(H27a), C8b(H8b), C25a(H25a), C25b(H25b), C8a(H8a), C6a(H6a)
1.c Idealised Me refined as rotating group:
 C21b(H21a,H21b,H21c), C19a(H19d,H19e,H19f), C20b(H20a,H20b,H20c), C19b(H19a,
 H19b,H19c), C10a(H10d,H10e,H10f), C10b(H10a,H10b,H10c), C20a(H20d,H20e,H20f),
 C12a(H12d,H12e,H12f), C21a(H21d,H21e,H21f), C11a(H11d,H11e,H11f), C12b(H12a,
 H12b,H12c), C11b(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 3.707
_oxdiff_exptl_absorpt_empirical_full_min 0.458