Synthesis and characterisation of four bimetallic gold–gallium clusters with Au–Ga rings as a new structural motif in gold cluster chemistry
Strienz, Markus; Fetzer, Florian; Schnepf, Andreas; Chemical Science 14 (2023) 4571–4579; doi:10.1039/D2SC06908C

data_1568775
_publ_section_title
;
 Synthesis and characterisation of four bimetallic gold--gallium clusters
 with Au--Ga rings as a new structural motif in gold cluster chemistry
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4571
_journal_page_last               4579
_journal_paper_doi               10.1039/D2SC06908C
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C36 H90 Au6 Cl8 Ga4 P6, 2(C7 H8)'
_chemical_formula_sum            'C50 H106 Au6 Cl8 Ga4 P6'
_chemical_formula_weight         2637.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.034(2)
_cell_length_b                   23.766(3)
_cell_length_c                   11.388(3)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.325
_cell_measurement_theta_min      2.546
_cell_volume                     4123.5(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24715
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    12.315
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1460 before and 0.0611 after correction. The Ratio of minimum to maximum transmission is 0.5139. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, pentane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0397P)^2^+29.6932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3018
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06908c2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 1568775--1568778.cif.'
_cod_original_cell_volume        4123.8(13)
_cod_database_code               1568775
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C402-C403 \\sim C403-C404 \\sim C404-C405 \\sim C405-C406 \\sim C406-C407
\\sim C407-C402
 with sigma of 0.02
 C402-C406 \\sim C402-C404 \\sim C407-C405 \\sim C403-C407 \\sim C404-C406
\\sim C403-C405
 with sigma of 0.04
 C401-C407 \\sim C401-C403
 with sigma of 0.04
3. Restrained planarity
 C401, C402, C403, C404, C405, C406, C407
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Au2 \\sim Au3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
P21 \\sim P31: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C301: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C302: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C401 \\sim C402 \\sim C403 \\sim C404 \\sim C405 \\sim C406 \\sim C407: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C201 \\sim C303: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C302) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C201) \\sim Ueq, Uanis(C303) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C304) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C401, C402, C403, C404, C405, C406, C407
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Au2(0.25) Au3(0.25) P21(0.25) P31(0.25) C201(0.5) H20A(0.5)
 H20B(0.5) C202(0.5) H20C(0.5) H20D(0.5) H20E(0.5) H30A(0.5) H30B(0.5)
 H30D(0.5) H30E(0.5) C303(0.5) H30F(0.5) H30G(0.5) C304(0.5) H30H(0.5)
 H30I(0.5) H30J(0.5) C401(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C402(0.5)
 C403(0.5) H403(0.5) C404(0.5) H404(0.5) C405(0.5) H405(0.5) C406(0.5)
 H406(0.5) C407(0.5) H407(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C103(H10F,H10G), C105(H10K,H10L), C201(H20A,H20B), C301(H30A,
 H30B), C303(H30F,H30G)
7.b Me refined with riding coordinates:
 C302(H30C,H30D,H30E), C304(H30H,H30I,H30J), C401(H40A,H40B,H40C)
7.c Aromatic/amide H refined with riding coordinates:
 C403(H403), C404(H404), C405(H405), C406(H406), C407(H407)
7.d Idealised Me refined as rotating group:
 C102(H10C,H10D,H10E), C104(H10H,H10I,H10J), C106(H10M,H10N,H10O), C202(H20C,
 H20D,H20E)
;
_shelx_res_checksum              9521
_shelx_fab_checksum              19321
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'