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_1568840
_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                 104.803(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0739(1)
_cell_length_b                   14.9500(1)
_cell_length_c                   20.4687(2)
_cell_measurement_reflns_used    20554
_cell_measurement_temperature    133
_cell_measurement_theta_max      76.0870
_cell_measurement_theta_min      3.4850
_cell_volume                     3867.92(6)
_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      133
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9661
_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     44.00 109.00   0.50    0.08    --   49.03  72.00-149.00  130
  2  \w    130.00 162.00   0.50    0.31    --  102.75  72.00-149.00   64
  3  \w     98.00 174.00   0.50    0.31    --  102.75  37.00 -30.00  152
  4  \w    -22.00  66.00   0.50    0.08    --   49.03 -72.00  80.00  176
  5  \w     31.00  91.00   0.50    0.31    --  102.75 -72.00  80.00  120
  6  \w     36.00  68.00   0.50    0.31    --  102.75 -57.00-120.00   64
  7  \w     31.00  68.00   0.50    0.31    --  102.75 -57.00-150.00   74
  8  \w     57.00  93.00   0.50    0.31    --  102.75 -99.00-120.00   72
  9  \w     62.00 109.00   0.50    0.31    --  102.75-125.00  90.00   94
 10  \w    -49.00 -21.00   0.50    0.08    --  -49.03  72.00-149.00   56
 11  \w    -18.00  22.00   0.50    0.08    --  -49.03  72.00-149.00   80
 12  \w    -14.00  19.00   0.50    0.08    --  -49.03  19.00-150.00   66
 13  \w    -14.00  22.00   0.50    0.08    --  -49.03  19.00   0.00   72
 14  \w    -62.00 -30.00   0.50    0.31    -- -102.00  57.00  30.00   64
 15  \w    -57.00 -30.00   0.50    0.31    -- -102.00  57.00  60.00   54
 16  \w    -61.00 -32.00   0.50    0.31    -- -102.00  57.00 -30.00   58
 17  \w    -96.00 -30.00   0.50    0.31    -- -102.00  72.00-149.00  132
 18  \w   -161.00-101.00   0.50    0.31    -- -102.00 -72.00  80.00  120
 19  \w   -167.00 -94.00   0.50    0.31    -- -102.00 -37.00 120.00  146
 20  \w   -174.00-107.00   0.50    0.31    -- -102.00 -37.00 150.00  134
 21  \w   -100.00 -75.00   0.50    0.08    --  -49.03 -72.00  80.00   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      -0.0736518000
_diffrn_orient_matrix_UB_12      -0.0685822000
_diffrn_orient_matrix_UB_13      0.0210030000
_diffrn_orient_matrix_UB_21      -0.0967243000
_diffrn_orient_matrix_UB_22      0.0470423000
_diffrn_orient_matrix_UB_23      -0.0459789000
_diffrn_orient_matrix_UB_31      0.0080518000
_diffrn_orient_matrix_UB_32      -0.0608598000
_diffrn_orient_matrix_UB_33      -0.0592278000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9661
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28278
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9661
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.25
_diffrn_reflns_theta_min         3.64
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47012
_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    1.832
_exptl_crystal_description       block
_exptl_crystal_F_000             2040.109
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.4245
_refine_diff_density_min         -1.9216
_refine_diff_density_rms         0.1305
_refine_ls_d_res_high            0.7937
_refine_ls_d_res_low             12.1539
_refine_ls_goodness_of_fit_ref   1.0300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0300
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0408P)^2^+4.8251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0753
_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                7135
_reflns_number_total             7812
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           2Ph-14-FIB_133K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1568840
_chemical_oxdiff_formula         'Au I F N C H'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C25A(H25A), C13A(H13A), C10A(H10A), C22A(H22A)
1.b Secondary CH2 refined with riding coordinates:
 C3A(H3Aa,H3Ab), C2A(H2Aa,H2Ab)
1.c Aromatic/amide H refined with riding coordinates:
 C30A(H30A), C18A(H18A), C19A(H19A), C31A(H31A), C32A(H32A), C20A(H20A),
 C33A(H33A), C7A(H7A), C29A(H29A), C8A(H8A), C6A(H6A)
1.d Idealised Me refined as rotating group:
 C26A(H26a,H26b,H26c), C24A(H24a,H24b,H24c), C27A(H27a,H27b,H27c), C23A(H23a,
 H23b,H23c), C14A(H14a,H14b,H14c), C11A(H11a,H11b,H11c), C15A(H15a,H15b,H15c),
 C12A(H12a,H12b,H12c)
;
_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 1.992
_oxdiff_exptl_absorpt_empirical_full_min 0.689