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_7713473
_publ_section_title
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 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 H Cl3, C F3 O3 S'
_chemical_formula_sum            'C59 H80 Au Cl3 F3 N5 O3 S'
_chemical_formula_weight         1299.65
_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'
_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                90
_cell_angle_beta                 94.7580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.14820(10)
_cell_length_b                   22.3169(2)
_cell_length_c                   27.6757(3)
_cell_measurement_reflns_used    21597
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7260
_cell_measurement_theta_min      3.1820
_cell_volume                     6246.29(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_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 0.998
_diffrn_measured_fraction_theta_max 0.979
_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    3.30    --  -41.68  38.00 -60.00   99
  2  \w     27.00  98.00   1.00    3.30    --   41.68-125.00-150.00   71
  3  \w    -33.00  66.00   1.00    3.30    --   41.68 -38.00  60.00   99
  4  \w     77.00 178.00   1.00   20.50    --  106.01  61.00 -90.00  101
  5  \w     23.00 107.00   1.00   20.50    --  106.01 -94.00 120.00   84
  6  \w     33.00 112.00   1.00   20.50    --  106.01-125.00  90.00   79
  7  \w    103.00 178.00   1.00   20.50    --  106.01  77.00-180.00   75
  8  \w     33.00 132.00   1.00   20.50    --  106.01 -45.00 120.00   99
  9  \w     78.00 178.00   1.00   20.50    --  106.01  30.00 -30.00  100
 10  \w   -115.00 -14.00   1.00    3.30    --  -41.68 -57.00   0.00  101
 11  \w   -115.00 -14.00   1.00    3.30    --  -41.68 -57.00-120.00  101
 12  \w     14.00 115.00   1.00    3.30    --   41.68  57.00-180.00  101
 13  \w     78.00 167.00   1.00   20.50    --  106.01  30.00  60.00   89
 14  \w    103.00 178.00   1.00   20.50    --  106.01  77.00  90.00   75
;
_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      0.0352150000
_diffrn_orient_matrix_UB_12      0.0404587000
_diffrn_orient_matrix_UB_13      0.0442403000
_diffrn_orient_matrix_UB_21      0.1128183000
_diffrn_orient_matrix_UB_22      -0.0430301000
_diffrn_orient_matrix_UB_23      0.0174075000
_diffrn_orient_matrix_UB_31      0.0960671000
_diffrn_orient_matrix_UB_32      0.0357652000
_diffrn_orient_matrix_UB_33      -0.0293149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47542
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.071
_diffrn_reflns_theta_min         2.547
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.354
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.829
_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            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+3.8015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10741
_reflns_number_total             12437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02086j2.cif
_cod_data_source_block           sv325-2
_cod_database_code               7713473
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H80 N4 Au F3 O3 S'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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), C40(H40), C43(H43), C52(H52),
 C55(H55), C58(H58)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C32(H32),
 C33(H33), C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50)
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), 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              60737
_olex2_date_sample_data_collection 2020-12-07
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.696