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_7713470
_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         'C57 H79 Au N5, C F3 O3 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H83 Au Cl4 F3 N5 O3 S'
_chemical_formula_weight         1350.14
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-04-19
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 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                104.3670(10)
_cell_angle_beta                 99.5440(10)
_cell_angle_gamma                104.338(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6478(2)
_cell_length_b                   16.0960(3)
_cell_length_c                   20.9235(3)
_cell_measurement_reflns_used    30161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.6480
_cell_measurement_theta_min      2.9550
_cell_volume                     3265.51(11)
_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_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  90.00   99
  2  \w    -74.00  34.00   1.00    1.00    --  -41.68  77.00-180.00  108
  3  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00 -90.00   99
  4  \w     10.00  36.00   1.00    1.00    --   41.68  75.00 -77.88   26
  5  \w      8.00  42.00   1.00    1.00    --   41.68  82.00  14.86   34
  6  \w     33.00 132.00   1.00    3.00    --  106.01 -45.00 -90.00   99
  7  \w     23.00 107.00   1.00    3.00    --  106.01 -94.00-120.00   84
  8  \w    103.00 178.00   1.00    3.00    --  106.01  77.00   0.00   75
  9  \w     34.00 135.00   1.00    3.00    --  106.01 -61.00  90.00  101
 10  \w     23.00 107.00   1.00    3.00    --  106.01 -94.00 -60.00   84
 11  \w     33.00 132.00   1.00    3.00    --  106.01 -45.00  60.00   99
 12  \w     33.00 112.00   1.00    3.00    --  106.01-125.00  60.00   79
 13  \w    103.00 178.00   1.00    3.00    --  106.01  77.00-150.00   75
 14  \w     23.00 107.00   1.00    3.00    --  106.01 -94.00  60.00   84
 15  \w     23.00 107.00   1.00    3.00    --  106.01 -94.00 150.00   84
 16  \w     53.00 178.00   1.00    3.00    --  106.01  15.00 -30.00  125
 17  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-120.00   81
 18  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00  90.00   99
 19  \w      7.00  33.00   1.00    1.00    --   41.68  84.00  72.16   26
 20  \w      9.00  42.00   1.00    1.00    --   41.68  80.00-127.94   33
 21  \w      9.00  42.00   1.00    1.00    --   41.68  80.00 117.97   33
 22  \w     77.00 178.00   1.00    3.00    --  106.01  61.00  30.00  101
 23  \w     76.00 178.00   1.00    3.00    --  106.01  65.00 -48.96  102
 24  \w     53.00 178.00   1.00    3.00    --  106.01  15.00 150.00  125
 25  \w     77.00 178.00   1.00    3.00    --  106.01  61.00-120.00  101
 26  \w     77.00 178.00   1.00    3.00    --  106.01  61.00 150.00  101
 27  \w     75.00 178.00   1.00    3.00    --  106.01  69.00 -20.65  103
 28  \w     77.00 178.00   1.00    3.00    --  106.01  61.00  60.00  101
 29  \w     77.00 178.00   1.00    3.00    --  106.01  61.00 120.00  101
 30  \w     76.00 178.00   1.00    3.00    --  106.01  64.00 -77.10  102
 31  \w     80.00 178.00   1.00    3.00    --  106.01  45.00-150.00   98
 32  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00   0.00   99
 33  \w   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00-180.00   99
 34  \w     10.00  36.00   1.00    1.00    --   41.68  75.00-167.38   26
 35  \w      8.00  42.00   1.00    1.00    --   41.68  82.00 175.75   34
 36  \w      7.00  33.00   1.00    1.00    --   41.68  84.00 -34.48   26
 37  \w     74.00 116.00   1.00    3.00    --  106.01  74.00  83.93   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.844
_diffrn_reflns_theta_min         2.973
_exptl_absorpt_coefficient_mu    6.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.373
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.891
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         13018
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0551P)^2^+4.0345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11984
_reflns_number_total             13018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02086j2.cif
_cod_data_source_block           sv316-2
_cod_database_code               7713470
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.782
_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
 C58-S1A
 1.819 with sigma of 0.005
 C58-S1B
 1.819 with sigma of 0.005
 S1A-O1A = S1A-O2A = S1A-O3A
 1.434 with sigma of 0.005
 S1B-O1B = S1B-O2B = S1B-O3B
 1.434 with sigma of 0.005
 C58-O1A = C58-O2A = C58-O3A
 2.561 with sigma of 0.01
 C58-O1B = C58-O2B = C58-O3B
 2.561 with sigma of 0.01
 O1A-O2A = O2A-O3A = O3A-O1A
 2.423 with sigma of 0.01
 O1B-O2B = O2B-O3B = O3B-O1B
 2.423 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1A \\sim O1A \\sim O2A \\sim O3A \\sim S1B \\sim O1B \\sim O2B \\sim O3B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) = Uanis(S1B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B)
4. Others
 Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=1-FVAR(1)
 Sof(S1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C8(H8), C16(H16), C25(H25), C28(H28), C40(H40), C43(H43), C52(H52),
 C55(H55)
5.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C12(H12), C13(H13), C21(H21), C22(H22), C23(H23),
 C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              1792
_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
;