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_7713471
_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         'C52 H69 Au N5, C F3 O3 S, C H2 Cl2 '
_chemical_formula_sum            'C54 H71 Au Cl2 F3 N5 O3 S'
_chemical_formula_weight         1195.09
_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             2021-04-16
_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                79.173(2)
_cell_angle_beta                 72.683(2)
_cell_angle_gamma                78.700(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4651(2)
_cell_length_b                   15.0649(3)
_cell_length_c                   17.5928(3)
_cell_measurement_reflns_used    28497
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7700
_cell_measurement_theta_min      2.9900
_cell_volume                     2817.31(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -66.00  33.00   1.00    1.00    --  -41.68  38.00 -60.00   99
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00 120.00   99
  3  \w    -74.00  34.00   1.00    1.00    --  -41.68  77.00  30.00  108
  4  \w      8.00  42.00   1.00    1.00    --   41.68  82.00-121.54   34
  5  \w      7.00  34.00   1.00    1.00    --   41.68  83.00 120.80   27
  6  \w     23.00 107.00   1.00    1.00    --  106.01 -94.00 -30.00   84
  7  \w    103.00 178.00   1.00    1.00    --  106.01  77.00  60.00   75
  8  \w    103.00 178.00   1.00    1.00    --  106.01  77.00-150.00   75
  9  \w     33.00 132.00   1.00    1.00    --  106.01 -45.00-180.00   99
 10  \w     77.00 178.00   1.00    1.00    --  106.01  61.00-180.00  101
 11  \w     33.00 112.00   1.00    1.00    --  106.01-125.00-150.00   79
 12  \w     30.00 139.00   1.00    1.00    --  106.01 -77.00  30.00  109
 13  \w     74.00 178.00   1.00    1.00    --  106.01  73.00  96.31  104
 14  \w     23.00 107.00   1.00    1.00    --  106.01 -94.00  30.00   84
 15  \w     97.00 178.00   1.00    1.00    --  106.01 125.00 -30.00   81
 16  \w     23.00 107.00   1.00    1.00    --  106.01 -94.00-120.00   84
 17  \w     80.00 178.00   1.00    1.00    --  106.01  45.00 150.00   98
 18  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00-120.00   99
 19  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00   0.00   99
 20  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00 -60.00   99
 21  \w      8.00  42.00   1.00    1.00    --   41.68  81.00  55.13   34
 22  \w      9.00  42.00   1.00    1.00    --   41.68  80.00 -67.14   33
 23  \w     75.00 178.00   1.00    1.00    --  106.01  69.00-123.23  103
 24  \w     53.00 178.00   1.00    1.00    --  106.01  15.00   0.00  125
 25  \w     75.00 178.00   1.00    1.00    --  106.01  69.00-159.93  103
 26  \w     77.00 178.00   1.00    1.00    --  106.01  61.00   0.00  101
 27  \w     77.00 116.00   1.00    1.00    --  106.01  61.00 -90.00   39
 28  \w     78.00 178.00   1.00    1.00    --  106.01  57.00  50.35  100
;
_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      0.0549684000
_diffrn_orient_matrix_UB_12      -0.0847185000
_diffrn_orient_matrix_UB_13      -0.0433954000
_diffrn_orient_matrix_UB_21      0.0524165000
_diffrn_orient_matrix_UB_22      -0.0474337000
_diffrn_orient_matrix_UB_23      0.0709573000
_diffrn_orient_matrix_UB_31      -0.1203879000
_diffrn_orient_matrix_UB_32      -0.0407422000
_diffrn_orient_matrix_UB_33      0.0407386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.905
_diffrn_reflns_theta_min         2.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.568
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_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    1.409
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         11224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.6772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10704
_reflns_number_total             11224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02086j2.cif
_cod_data_source_block           sv280
_cod_database_code               7713471
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H50 Au N5 F3 O3 S'
_reflns_odcompleteness_completeness 99.92
_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. Restrained distances
 N5-H5
 0.88 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
3.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C37(H37), C39(H39), C46(H46), C48(H48)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              21792
_olex2_date_sample_data_collection 2020-09-29
_olex2_exptl_crystal_mounting_method 'mounted on 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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.748