Striking ligand-disproportionative Cl/aryl scrambling in a simple Au(III) system. Solvent role, driving forces and mechanisms.
Fernández-Moyano, Sara; Peñas-Defrutos, Marconi N; Bartolomé, Camino; Espinet, Pablo; Chemical communications (Cambridge, England) 57 (2021) 125–128; doi:10.1039/d0cc06450e

data_7127544
_publ_section_title
;
 Striking ligand-disproportionative Cl/aryl scrambling in a simple Au(III)
 system. Solvent role, driving forces and mechanisms.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              125
_journal_page_last               128
_journal_paper_doi               10.1039/d0cc06450e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'Au C24 Cl8 F12, C16 H36 N'
_chemical_formula_sum            'C40 H36 Au Cl8 F12 N'
_chemical_formula_weight         1239.26
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-10 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9386(7)
_cell_length_b                   18.9386(7)
_cell_length_c                   12.7330(9)
_cell_measurement_reflns_used    1586
_cell_measurement_temperature    294
_cell_measurement_theta_max      23.7970
_cell_measurement_theta_min      4.1750
_cell_volume                     4567.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.851
_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     -7.00  29.00   1.00  100.00    --  -10.64 -99.00  60.00   36
  2  \w     14.00  88.00   1.00  100.00    --   12.20  77.00-120.00   74
;
_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      0.0328727000
_diffrn_orient_matrix_UB_12      -0.0171082000
_diffrn_orient_matrix_UB_13      0.0080650000
_diffrn_orient_matrix_UB_21      0.0172088000
_diffrn_orient_matrix_UB_22      0.0332467000
_diffrn_orient_matrix_UB_23      0.0007602000
_diffrn_orient_matrix_UB_31      -0.0050376000
_diffrn_orient_matrix_UB_32      0.0020337000
_diffrn_orient_matrix_UB_33      0.0551359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6588
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.578
_diffrn_reflns_theta_min         3.543
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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    1.802
_exptl_crystal_description       needle
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+1.3556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1886
_reflns_number_total             2739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06450e2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7127540--7127544.cif.'
_cod_original_cell_volume        4567.0(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7127544
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 Au Cl4 F6'
_chemical_oxdiff_usercomment     colorless
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.282
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
2.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              67024
_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 1.171
_oxdiff_exptl_absorpt_empirical_full_min 0.868