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_1560027
_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         'C37 H37 Au N P S, 2(B F4)'
_chemical_formula_sum            'C37 H37 Au B2 F8 N P S'
_chemical_formula_weight         929.29
_chemical_name_systematic        C37H37AuB2F8NPS
_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     direct
_audit_creation_date             2020-04-07
_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                 97.960(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2911(7)
_cell_length_b                   15.0763(13)
_cell_length_c                   14.2431(12)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      68.37
_cell_measurement_theta_min      3.13
_cell_volume                     1763.2(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.368
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.453
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.1793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.4254.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       needle
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.634
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.119
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.080(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6337
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0638P)^2^+2.4053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6254
_reflns_number_total             6337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05777k2.cif
_cod_data_source_block           eli70_0m_c
_cod_depositor_comments
'Adding full bibliography for 1560018--1560030.cif.'
_cod_database_code               1560027
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.483
_shelx_estimated_absorpt_t_min   0.065
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.920(15)
 0.080(15)
2. 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
3. Others
 Sof(F1A)=1-FVAR(1)
 Sof(F1)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B), C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C17(H17), C3(H3), C24(H24), C25(H25), C14(H14), C9(H9), C21(H21),
 C16(H16), C5(H5), C15(H15), C6(H6), C22(H22), C4(H4), C12(H12), C18(H18),
 C10(H10), C11(H11), C28(H28), C30(H30), C31(H31), C27(H27), C29(H29)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              67964
_olex2_submission_special_instructions 'No special instructions were received'