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_1568834
_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, C H2 Cl2'
_chemical_formula_sum            'C34 H45 Au Cl2 N2'
_chemical_formula_weight         749.621
_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     iterative
_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                 94.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9926(2)
_cell_length_b                   16.4651(3)
_cell_length_c                   18.3046(3)
_cell_measurement_reflns_used    10177
_cell_measurement_temperature    123
_cell_measurement_theta_max      75.3160
_cell_measurement_theta_min      3.5980
_cell_volume                     3304.66(10)
_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    'olex2.solve 1.5-alpha (Bourhis et al., 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 0.9988
_diffrn_measured_fraction_theta_max 0.9602
_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     43.00 119.00   0.50    0.19    --   48.78  23.00  39.00  152
  2  \w     92.00 164.00   0.50    0.74    --  102.75  57.00 120.00  144
  3  \w     98.00 146.00   0.50    0.74    --  102.75  23.00  39.00   96
  4  \w    -20.00  39.00   0.50    0.19    --   48.78 -37.00  90.00  118
  5  \w    -24.00   1.00   0.50    0.19    --   48.78 -19.00  90.00   50
  6  \w    -20.00  15.00   0.50    0.19    --   48.78 -23.00-125.00   70
  7  \w     32.00  69.00   0.50    0.74    --  102.75 -57.00  90.00   74
  8  \w     32.00  58.00   0.50    0.74    --  102.75 -57.00 150.00   52
  9  \w     39.00  67.00   0.50    0.74    --  102.75 -57.00 120.00   56
 10  \w     38.00  69.00   0.50    0.74    --  102.75 -57.00  60.00   62
 11  \w     31.00  68.00   0.50    0.74    --  102.75 -57.00  30.00   74
 12  \w     32.00  58.00   0.50    0.74    --  102.75 -57.00 -30.00   52
 13  \w     32.00 105.00   0.50    0.74    --  102.75 -99.00  90.00  146
 14  \w     80.00 106.00   0.50    0.74    --  102.75 -99.00 120.00   52
 15  \w    -19.00   6.00   0.50    0.19    --  -48.78  23.00  39.00   50
 16  \w    -58.00 -30.00   0.50    0.74    -- -102.00  57.00 -60.00   56
 17  \w    -62.00 -37.00   0.50    0.74    -- -102.00  57.00 -30.00   50
 18  \w    -64.00 -31.00   0.50    0.74    -- -102.00  57.00   0.00   66
 19  \w    -60.00 -35.00   0.50    0.74    -- -102.00  57.00  60.00   50
 20  \w    -97.00 -35.00   0.50    0.74    -- -102.00 125.00 150.00  124
 21  \w   -114.00 -89.00   0.50    0.74    -- -102.00 -57.00 150.00   50
 22  \w   -170.00-145.00   0.50    0.74    -- -102.00 -57.00 150.00   50
 23  \w   -120.00 -90.00   0.50    0.19    --  -48.78-125.00 -30.00   60
 24  \w   -149.00-102.00   0.50    0.74    -- -102.00 -23.00-125.00   94
 25  \w   -100.00 -44.00   0.50    0.19    --  -48.78 -23.00-125.00  112
;
_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      0.0435698000
_diffrn_orient_matrix_UB_12      -0.0204676000
_diffrn_orient_matrix_UB_13      -0.0759943000
_diffrn_orient_matrix_UB_21      -0.1282916000
_diffrn_orient_matrix_UB_22      0.0188799000
_diffrn_orient_matrix_UB_23      -0.0352069000
_diffrn_orient_matrix_UB_31      0.0372411000
_diffrn_orient_matrix_UB_32      0.0893499000
_diffrn_orient_matrix_UB_33      -0.0099578000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9602
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23014
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9602
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.50
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47295
_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    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1495.476
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.0943
_refine_diff_density_min         -1.2788
_refine_diff_density_rms         0.1818
_refine_ls_d_res_high            0.7928
_refine_ls_d_res_low             12.2276
_refine_ls_goodness_of_fit_ref   1.0118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0118
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+5.8031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -10
_reflns_number_gt                5776
_reflns_number_total             6666
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc00373f3.cif
_cod_data_source_block           2Ph-DCM_123K
_cod_depositor_comments
'Adding full bibliography for 1568831--1568854.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1568834
_chemical_oxdiff_formula         'Au N C H'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C10(H10), C14(H14)
1.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C1S(H1Sa,H1Sb)
1.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C33(H33), C6(H6), C32(H32), C7(H7), C8(H8), C18(H18), C30(H30),
 C19(H19), C20(H20), C31(H31)
1.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C23(H23a,H23b,H23c), C15(H15a,H15b,H15c), C27(H27a,H27b,
 H27c), C24(H24a,H24b,H24c), C13(H13a,H13b,H13c), C11(H11a,H11b,H11c), C12(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 1.984
_oxdiff_exptl_absorpt_empirical_full_min 0.519