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_1568850
_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, C6 F5 I'
_chemical_formula_sum            'C35 H35 Au F5 I N2'
_chemical_formula_weight         902.544
_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             2022-11-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                88.379(2)
_cell_angle_beta                 78.949(3)
_cell_angle_gamma                67.222(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7941(4)
_cell_length_b                   10.9878(4)
_cell_length_c                   17.6423(3)
_cell_measurement_reflns_used    10335
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.3000
_cell_measurement_theta_min      2.6410
_cell_volume                     1715.85(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 0.9967
_diffrn_measured_fraction_theta_max 0.6010
_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    -80.00 -10.00   0.50    0.08    --  -49.03 103.00 -55.00  140
  2  \w    -20.00   9.00   0.50    0.08    --  -49.03  57.00 -90.00   58
  3  \w     -6.00  19.00   0.50    0.08    --  -49.03  19.00-180.00   50
  4  \w    -60.00 -26.00   0.50    0.08    --  -49.03  57.00 -90.00   68
  5  \w    -60.00 -31.00   0.50    0.33    -- -102.00  57.00-120.00   58
  6  \w    -60.00 -32.00   0.50    0.33    -- -102.00  57.00-150.00   56
  7  \w    -63.00 -33.00   0.50    0.33    -- -102.00  57.00 -90.00   60
  8  \w    -64.00 -30.00   0.50    0.33    -- -102.00  57.00 -60.00   68
  9  \w    -93.00 -64.00   0.50    0.33    -- -102.00 125.00  60.00   58
 10  \w   -106.00 -59.00   0.50    0.33    -- -102.00 103.00 -55.00   94
 11  \w   -104.00 -30.00   0.50    0.33    -- -102.00 125.00 -60.00  148
 12  \w   -109.00 -30.00   0.50    0.33    -- -102.00 125.00 -30.00  158
 13  \w   -132.00 -90.00   0.50    0.33    -- -102.00 -57.00  60.00   84
 14  \w   -117.00 -75.00   0.50    0.08    --  -49.03-125.00  60.00   84
 15  \w   -155.00 -77.00   0.50    0.33    -- -102.00-125.00 -90.00  156
 16  \w   -129.00 -93.00   0.50    0.33    -- -102.00-103.00-158.00   72
 17  \w   -156.00 -98.00   0.50    0.33    -- -102.00 -37.00 -60.00  116
 18  \w   -167.00-140.00   0.50    0.33    -- -102.00 -57.00  60.00   54
 19  \w   -173.00-103.00   0.50    0.33    -- -102.00 -37.00 -30.00  140
 20  \w   -171.00 -99.00   0.50    0.33    -- -102.00 -37.00 -90.00  144
 21  \w     19.00  83.00   0.50    0.08    --   49.03-103.00-158.00  128
 22  \w     72.00  98.00   0.50    0.33    --  102.75-103.00-158.00   52
 23  \w     55.00  97.00   0.50    0.33    --  102.75 -99.00 -90.00   84
 24  \w     72.00 111.00   0.50    0.33    --  102.75-125.00 -30.00   78
 25  \w     67.00 106.00   0.50    0.33    --  102.75 -99.00  30.00   78
 26  \w     81.00 107.00   0.50    0.33    --  102.75-102.00 151.41   52
 27  \w     35.00  69.00   0.50    0.33    --  102.75 -57.00  30.00   68
 28  \w     33.00  68.00   0.50    0.33    --  102.75 -57.00  90.00   70
 29  \w     35.00  67.00   0.50    0.33    --  102.75 -57.00  60.00   64
 30  \w    -14.00  62.00   0.50    0.08    --   49.03 -57.00   0.00  152
 31  \w    118.00 173.00   0.50    0.33    --  102.75  37.00 -90.00  110
 32  \w     90.00 155.00   0.50    0.33    --  102.75 103.00 -55.00  130
 33  \w     33.00 121.00   0.50    0.08    --   49.03  77.00 -60.00  176
 34  \w     33.00  61.00   0.50    0.33    --  102.75 -57.00-150.00   56
 35  \w     35.00  66.00   0.50    0.33    --  102.75 -99.00-150.00   62
 36  \w     31.00 110.00   0.50    0.33    --  102.75-125.00-180.00  158
;
_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      0.1424867000
_diffrn_orient_matrix_UB_12      0.0305457000
_diffrn_orient_matrix_UB_13      -0.0250740000
_diffrn_orient_matrix_UB_21      0.0235682000
_diffrn_orient_matrix_UB_22      -0.0601529000
_diffrn_orient_matrix_UB_23      -0.0816476000
_diffrn_orient_matrix_UB_31      -0.0969884000
_diffrn_orient_matrix_UB_32      0.1364968000
_diffrn_orient_matrix_UB_33      -0.0253344000
_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  0.0813
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.9949
_diffrn_reflns_Laue_measured_fraction_max 0.9506
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21012
_diffrn_reflns_point_group_measured_fraction_full 0.9949
_diffrn_reflns_point_group_measured_fraction_max 0.9506
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.48
_diffrn_reflns_theta_min         4.37
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27753
_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            'light white'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             867.527
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.1451
_refine_diff_density_min         -2.4623
_refine_diff_density_rms         0.1798
_refine_ls_d_res_high            0.7929
_refine_ls_d_res_low             10.1178
_refine_ls_goodness_of_fit_ref   0.9977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.9949
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5874
_reflns_number_total             6857
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           1Xyl-IPFB_293K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_database_code               1568850
_chemical_oxdiff_formula         'Au I F N C H'
_diffrn_oxdiff_digest_frames
;
01126eb8a01f0a6859f33cb8ec33e760ce03384f2d0
;
_diffrn_oxdiff_digest_hkl
;
019a465e93b0f9acf50dcd8256f8074d1add9c
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C22D \\sim C23D \\sim C24D \\sim C25D \\sim C26D \\sim C27D: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
3.a Secondary CH2 refined with riding coordinates:
 C3D(H3Da,H3Db), C2D(H2Da,H2Db)
3.b Aromatic/amide H refined with riding coordinates:
 C8D(H8D), C26D(H26D), C15D(H15D), C6D(H6D), C17D(H17D), C24D(H24D), C25D(H25D)
3.c Idealised Me refined as rotating group:
 C12D(H12a,H12b,H12c), C21D(H21a,H21b,H21c), C19D(H19a,H19b,H19c), C20D(H20a,
 H20b,H20c), C28D(H28a,H28b,H28c), C11D(H11a,H11b,H11c), C29D(H29a,H29b,H29c),
 C10D(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 3.086
_oxdiff_exptl_absorpt_empirical_full_min 0.484