Gold complexes with remote-substituted amino N-heterocyclic carbenes
Nolan, Steven P.; Cavallo, Luigi; Cazin, Catherine; Dereli, Busra; Saab, Marina; Tzouras, Nikolaos V.; Van Hecke, Kristof; Vanden Broeck, Sofie; Ritacco, Ida; Vougioukalakis, Georgios C.; Danopoulos, Andreas; Braunstein, Pierre; Dalton Transactions  (2023) –; doi:10.1039/D3DT02086J

data_7713472
_publ_section_title
;
 Gold complexes with remote-substituted amino N-heterocyclic carbenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02086J
_journal_year                    2023
_chemical_formula_moiety         'C30 H43 Au Cl N3, C H Cl3'
_chemical_formula_sum            'C31 H44 Au Cl4 N3'
_chemical_formula_weight         797.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                66.624(6)
_cell_angle_beta                 72.414(5)
_cell_angle_gamma                68.894(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3776(4)
_cell_length_b                   12.6358(8)
_cell_length_c                   15.3266(11)
_cell_measurement_reflns_used    4406
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.5590
_cell_measurement_theta_min      3.9350
_cell_volume                     1691.02(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -70.00  32.00   1.00    1.00    --  -41.43  57.00   0.00  102
  2  \w    -74.00  35.00   1.00    1.00    --  -41.43  77.00-150.00  109
  3  \w   -114.00 -13.00   1.00    1.00    --  -41.43 -57.00  90.00  101
  4  \w     17.00 116.00   1.00    1.00    --   41.43  38.00-120.00   99
  5  \w      8.00  42.00   1.00    1.00    --   41.43  80.00  50.27   34
  6  \w     80.00 178.00   1.00    2.00    --  106.01  45.00 150.00   98
  7  \w     33.00 112.00   1.00    2.00    --  106.01-125.00  90.00   79
  8  \w     24.00 159.00   1.00    2.00    --  106.01 -15.00-180.00  135
  9  \w     77.00 178.00   1.00    2.00    --  106.01  62.00-134.04  101
 10  \w     34.00 135.00   1.00    2.00    --  106.01 -61.00-120.00  101
 11  \w     33.00 112.00   1.00    2.00    --  106.01-125.00-180.00   79
 12  \w     33.00 132.00   1.00    2.00    --  106.01 -45.00 120.00   99
 13  \w     34.00 135.00   1.00    2.00    --  106.01 -61.00   0.00  101
 14  \w     27.00 108.00   1.00    2.00    --  106.01-105.00 -29.42   81
 15  \w    103.00 178.00   1.00    2.00    --  106.01  77.00-180.00   75
 16  \w     28.00 108.00   1.00    2.00    --  106.01-106.00-126.74   80
 17  \w      6.00  82.00   1.00    1.00    --   41.43 -99.00  90.00   76
 18  \w      6.00  32.00   1.00    1.00    --   41.43  85.00-141.51   26
 19  \w      9.00  42.00   1.00    1.00    --   41.43  78.00 -31.90   33
 20  \w      7.00  34.00   1.00    1.00    --   41.43  83.00  79.87   27
 21  \w     13.00 114.00   1.00    1.00    --   41.43  57.00 -30.00  101
 22  \w     80.00 178.00   1.00    2.00    --  106.01  45.00  60.00   98
 23  \w     75.00 124.00   1.00    2.00    --  106.01  70.00 -30.51   49
 24  \w     53.00 178.00   1.00    2.00    --  106.01  15.00   0.00  125
 25  \w     77.00 178.00   1.00    2.00    --  106.01  59.00 -95.09  101
 26  \w     78.00 178.00   1.00    2.00    --  106.01  54.00  17.44  100
 27  \w     77.00 178.00   1.00    2.00    --  106.01  61.00-180.00  101
 28  \w     76.00 178.00   1.00    2.00    --  106.01  64.00  97.44  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1618014000
_diffrn_orient_matrix_UB_12      -0.0322223000
_diffrn_orient_matrix_UB_13      -0.0220576000
_diffrn_orient_matrix_UB_21      -0.0068323000
_diffrn_orient_matrix_UB_22      0.1282923000
_diffrn_orient_matrix_UB_23      -0.0106830000
_diffrn_orient_matrix_UB_31      0.0012807000
_diffrn_orient_matrix_UB_32      -0.0397812000
_diffrn_orient_matrix_UB_33      0.1087195000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.909
_diffrn_reflns_theta_min         3.197
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.259
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       irregular
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.550
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5115
_reflns_number_total             6711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02086j2.cif
_cod_data_source_block           sv340
_cod_original_cell_volume        1691.0(2)
_cod_database_code               7713472
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H42 Au Cl N3'
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.363
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     51.08
_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. Restrained distances
 N3-H3
 0.88 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C4(H4), C13(H13), C16(H16), C25(H25), C28(H28), C31(H31)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              51556
_olex2_date_sample_data_collection 2020-11-16
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.726