Rapid, room-temperature, solvent-free mechanochemical oxidation of elemental gold into organosoluble gold salts
Do, Jean-Louis; Auvray, Thomas; Lennox, Cameron B.; Titi, Hatem M.; Cuccia, Louis A.; Friščić, Tomislav; Green Chemistry 25 (2023) 5899–5906; doi:10.1039/D3GC01150J

data_7246815
_publ_section_title
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 Rapid, room-temperature, solvent-free mechanochemical oxidation of
 elemental gold into organosoluble gold salts
;
_journal_issue                   15
_journal_name_full               'Green Chemistry'
_journal_page_first              5899
_journal_page_last               5906
_journal_paper_doi               10.1039/D3GC01150J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Au Br4, C19 H42 N'
_chemical_formula_sum            'C19 H42 Au Br4 N'
_chemical_formula_weight         801.14
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1965(2)
_cell_length_b                   8.7398(2)
_cell_length_c                   38.9304(10)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    298
_cell_measurement_theta_max      72.256
_cell_measurement_theta_min      4.546
_cell_volume                     2786.62(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            52316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.387
_diffrn_reflns_theta_min         4.547
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.652
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1793 before and 0.1186 after correction.
The Ratio of minimum to maximum transmission is 0.5436.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyl acetate'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0762
_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^)+(0.0685P)^2^+37.9242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3839
_reflns_number_total             5462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc01150j2.cif
_cod_data_source_block           ctaaubr4
_cod_depositor_comments
'Adding full bibliography for 7246811--7246815.cif.'
_cod_database_code               7246815
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.164
_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
 C16-C15 \\sim C15-C14 \\sim C14-C13 \\sim C13-C12 \\sim C12-C11 \\sim C11-C10
\\sim C9-C8 \\sim C9-C10 ~
 C8-C7 \\sim C7-C6 \\sim C6-C5 \\sim C5-C4 \\sim C4-C3 \\sim C3-C2 \\sim C2-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C18 \\sim C17 \\sim C19: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Uanis(Br1) = Uanis(Br3)
4. Rigid body (RIGU) restrains
 C16, C15, C14, C13, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
5.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              67790
_olex2_submission_special_instructions 'No special instructions were received'