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_7246814
_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, C16 H36 N'
_chemical_formula_sum            'C16 H36 Au Br4 N'
_chemical_formula_weight         759.06
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1431(6)
_cell_length_b                   12.1431(6)
_cell_length_c                   8.5038(5)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    298
_cell_measurement_theta_max      72.197
_cell_measurement_theta_min      3.640
_cell_volume                     1253.93(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23881
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.474
_diffrn_reflns_theta_min         7.330
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.460
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.1553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1843 before and 0.1265 after correction.
The Ratio of minimum to maximum transmission is 0.2061.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       cube
_exptl_crystal_F_000             716
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyl acetate'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.0079(8)
_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   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1238
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0816P)^2^+7.7277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1117
_reflns_number_total             1238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc01150j2.cif
_cod_data_source_block           tbaaubr4
_cod_depositor_comments
'Adding full bibliography for 7246811--7246815.cif.'
_cod_original_cell_volume        1253.93(14)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7246814
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.215
_shelx_estimated_absorpt_t_min   0.215
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1A = N1-C1B = C1A-C2 = C1B-C2 = C2-C3B = C2-C3A = C3B-C4B = C3A-C4A
 1.52 with sigma of 0.015
3. Rigid body (RIGU) restrains
 N1, C1B, C1A, C2, C3B, C4A, C4B, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H2BC)=Sof(H2BD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H2AA)=Sof(H2AB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C2(H2AA,H2AB), C2(H2BC,H2BD), C3A(H3AA,H3AB),
 C3B(H3BA,H3BB)
5.b Idealised Me refined with riding coordinates:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC)
;
_shelx_res_checksum              26519
_olex2_submission_special_instructions 'No special instructions were received'