Ligand-enforced intimacy between a gold cation and a carbenium ion: impact on stability and reactivity
Litle, Elishua D.; Wilkins, Lewis C.; Gabbaï, François P.; Chemical Science 12 (2021) 3929–3936; doi:10.1039/D0SC05777K

data_1560025
_publ_section_title
;
 Ligand-enforced intimacy between a gold cation and a carbenium ion:
 impact on stability and reactivity
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3929
_journal_page_last               3936
_journal_paper_doi               10.1039/D0SC05777K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C33 H29 Au Cl N P, B F4'
_chemical_formula_sum            'C33 H29 Au B Cl F4 N P'
_chemical_formula_weight         789.77
_chemical_name_systematic        C33H29AuBClF4NP
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-16 deposited with the CCDC.	2021-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2171(6)
_cell_length_b                   20.0635(13)
_cell_length_c                   9.9302(6)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.43
_cell_volume                     1523.51(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.115
_diffrn_reflns_theta_min         2.427
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.017
_exptl_absorpt_correction_T_max  0.3807
_exptl_absorpt_correction_T_min  0.2670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0883 before and 0.0480 after correction.
The Ratio of minimum to maximum transmission is 0.7013.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       needle
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8965
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0310
_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^)+3.3738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8504
_reflns_number_total             8965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05777k2.cif
_cod_data_source_block           eli72_1_0m_c
_cod_depositor_comments
'Adding full bibliography for 1560018--1560030.cif.'
_cod_database_code               1560025
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.219
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.510(8)
 0.490(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C10 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C29 \\sim C28: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C30 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C30) = Uanis(C29)
4. Others
 Sof(F1A)=1-FVAR(1)
 Sof(F1)=FVAR(1)
 Sof(F3A)=1-FVAR(2)
 Sof(F3)=FVAR(2)
 Sof(F4A)=1-FVAR(3)
 Sof(F4)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24),
  C25(H25), C30(H30), C29(H29), C28(H28), C27(H27), C31(H31)
5.b Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C30(C29,C28,C27,C26,C31)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              92064
_olex2_submission_special_instructions 'No special instructions were received'