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_7127543
_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 C12 Cl6 F6, C16 H36 N'
_chemical_formula_sum            'C28 H36 Au Cl6 F6 N'
_chemical_formula_weight         910.24
_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     iterative
_audit_creation_date             2020-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                100.005(5)
_cell_angle_beta                 97.584(5)
_cell_angle_gamma                99.628(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7193(6)
_cell_length_b                   12.2962(7)
_cell_length_c                   15.3889(9)
_cell_measurement_reflns_used    3940
_cell_measurement_temperature    294
_cell_measurement_theta_max      24.9720
_cell_measurement_theta_min      3.6700
_cell_volume                     1760.92(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.810
_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    -35.00  63.00   1.00    7.50    --  -10.64  57.00-180.00   98
  2  \w    -77.00  17.00   1.00    7.50    --  -10.64 -57.00  30.00   94
  3  \w     34.00  99.00   1.00    7.50    --   12.20-178.00  30.00   65
;
_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      0.0432544000
_diffrn_orient_matrix_UB_12      0.0545376000
_diffrn_orient_matrix_UB_13      0.0126862000
_diffrn_orient_matrix_UB_21      0.0342342000
_diffrn_orient_matrix_UB_22      -0.0154645000
_diffrn_orient_matrix_UB_23      0.0383285000
_diffrn_orient_matrix_UB_31      0.0509037000
_diffrn_orient_matrix_UB_32      -0.0187862000
_diffrn_orient_matrix_UB_33      -0.0249498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12295
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.600
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.684
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.354
_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    1.717
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.104
_refine_diff_density_max         2.121
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         8033
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0819P)^2^+3.6201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5286
_reflns_number_total             8033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06450e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7127540--7127544.cif.'
_cod_database_code               7127543
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H36 Au Cl6 F6 N'
_chemical_oxdiff_usercomment     colorless
_reflns_odcompleteness_completeness 98.58
_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. Restrained distances
 C31-C32
 1.45 with sigma of 0.02
 C35-C36
 1.4 with sigma of 0.02
 C36-C35 = C36-H36A = C36-H36B = C36-H36C
 1.5 with sigma of 0.02
3. Restrained angles
 C33-C34-C35
 fixed at 109 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C22(H22A,H22B), C23(H23A,H23B), C21(H21A,H21B), C35(H35A,
 H35B), C31(H31A,H31B), C33(H33A,H33B), C26(H26A,H26B), C30(H30A,H30B),
 C25(H25A,H25B), C29(H29A,H29B), C27(H27A,H27B)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              96752
_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.874