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_7127541
_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         'C18 H2 Au Cl6 F9 O, 2(C4 H10 O)'
_chemical_formula_sum            'C26 H22 Au Cl6 F9 O3'
_chemical_formula_weight         963.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 116.43(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.801(4)
_cell_length_b                   12.593(3)
_cell_length_c                   17.029(3)
_cell_measurement_reflns_used    1743
_cell_measurement_temperature    294
_cell_measurement_theta_max      23.7610
_cell_measurement_theta_min      2.7260
_cell_volume                     3418.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.822
_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    -30.00  60.00   1.00   95.73    --  -10.11  37.00   0.00   90
  2  \w    -20.00  46.00   1.00   95.73    --   11.82 -99.00 -90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0361224000
_diffrn_orient_matrix_UB_12      0.0307059000
_diffrn_orient_matrix_UB_13      -0.0260107000
_diffrn_orient_matrix_UB_21      -0.0093934000
_diffrn_orient_matrix_UB_22      0.0047343000
_diffrn_orient_matrix_UB_23      0.0361427000
_diffrn_orient_matrix_UB_31      0.0241830000
_diffrn_orient_matrix_UB_32      0.0471152000
_diffrn_orient_matrix_UB_33      0.0131563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7035
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.871
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3940
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0411P)^2^+22.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2475
_reflns_number_total             3940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06450e2.cif
_cod_data_source_block           3-OH2
_cod_depositor_comments
'Adding full bibliography for 7127540--7127544.cif.'
_cod_original_cell_volume        3418.6(13)
_cod_database_code               7127541
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 Au2 Cl12 F18'
_chemical_oxdiff_usercomment     colourless
_reflns_odcompleteness_completeness 99.02
_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, All O(H,H) groups
2. Restrained distances
 C21-C22
 1.54 with sigma of 0.02
 C23-C24
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              24367
_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 2.227
_oxdiff_exptl_absorpt_empirical_full_min 0.685