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_1568776
_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         'C54 H126 Au7 Cl6 Ga3 P6'
_chemical_formula_sum            'C54 H126 Au7 Cl6 Ga3 P6'
_chemical_formula_weight         2761.99
_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     dual
_audit_creation_date             2019-03-18
_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                92.022(2)
_cell_angle_beta                 98.393(2)
_cell_angle_gamma                91.024(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0624(10)
_cell_length_b                   15.2056(11)
_cell_length_c                   21.0776(16)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.870
_cell_measurement_theta_min      2.325
_cell_volume                     4137.9(5)
_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      150.0
_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 0.998
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            237222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    13.656
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1595 before and 0.0686 after correction. The Ratio of minimum to maximum transmission is 0.4780. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_description       plank
_exptl_crystal_F_000             2576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluenen, pentane'
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         19942
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+21.7110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16059
_reflns_number_total             19942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06908c2.cif
_cod_data_source_block           37
_cod_depositor_comments
'Adding full bibliography for 1568775--1568778.cif.'
_cod_database_code               1568776
_shelx_shelxl_version_number     2014/7
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C707 \\sim C710: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C110 \\sim C113: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C202 \\sim C204: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C105 \\sim C108: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C104 \\sim C107: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C203 \\sim C205: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C201) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H10U)=Sof(H10V)=Sof(H10W)=Sof(C107)=Sof(H10P)=Sof(H10Q)=Sof(C108)=
 Sof(H10N)=Sof(H10O)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C112)=Sof(H11I)=
 Sof(H11J)=Sof(C113)=Sof(H11K)=Sof(H11L)=Sof(H20L)=Sof(H20M)=Sof(C204)=
 Sof(H20N)=Sof(H20O)=Sof(C205)=Sof(H20U)=Sof(H20V)=Sof(H20W)=Sof(C710)=
 Sof(H71F)=Sof(H71G)=Sof(C711)=Sof(H71A)=Sof(H71B)=Sof(C712)=Sof(H71C)=
 Sof(H71D)=Sof(H71E)=1-FVAR(1)
 Sof(C104)=Sof(H10J)=Sof(H10K)=Sof(C105)=Sof(H10L)=Sof(H10M)=Sof(H10R)=
 Sof(H10S)=Sof(H10T)=Sof(C109)=Sof(H10H)=Sof(H10I)=Sof(C110)=Sof(H11G)=
 Sof(H11H)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(H20J)=Sof(H20K)=Sof(C202)=
 Sof(H20P)=Sof(H20Q)=Sof(C203)=Sof(H20R)=Sof(H20S)=Sof(H20T)=Sof(C707)=
 Sof(H70T)=Sof(H70U)=Sof(C708)=Sof(H70O)=Sof(H70P)=Sof(C709)=Sof(H70J)=
 Sof(H70K)=Sof(H70L)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C101(H10C,H10D), C102(H10A,H10B), C104(H10J,H10K), C105(H10L,H10M), C107(H10P,
 H10Q), C108(H10N,H10O), C109(H10H,H10I), C110(H11G,H11H), C112(H11I,H11J),
 C113(H11K,H11L), C201(H20L,H20M), C201(H20J,H20K), C202(H20P,H20Q), C204(H20N,
 H20O), C206(H20F,H20G), C207(H20A,H20B), C209(H20H,H20I), C210(H21A,H21B),
 C301(H30G,H30H), C302(H30E,H30F), C304(H30C,H30D), C305(H30A,H30B), C307(H30L,
 H30M), C308(H30Q,H30R), C501(H50H,H50I), C502(H50J,H50K), C504(H50A,H50B),
 C505(H50F,H50G), C507(H50O,H50P), C508(H50Q,H50R), C601(H60M,H60N), C602(H60O,
 H60P), C604(H60A,H60B), C605(H60K,H60L), C607(H60F,H60G), C608(H60T,H60U),
 C701(H70A,H70B), C702(H70M,H70N), C704(H70E,H70F), C705(H70C,H70D), C707(H70T,
 H70U), C708(H70O,H70P), C710(H71F,H71G), C711(H71A,H71B)
4.b Me refined with riding coordinates:
 C103(H10E,H10F,H10G), C106(H10R,H10S,H10T), C106(H10U,H10V,H10W), C111(H11A,
 H11B,H11C), C111(H11D,H11E,H11F), C203(H20R,H20S,H20T), C205(H20U,H20V,H20W),
 C208(H20C,H20D,H20E), C211(H21C,H21D,H21E), C303(H30N,H30O,H30P), C306(H30I,
 H30J,H30K), C309(H30S,H30T,H30U), C503(H50L,H50M,H50N), C506(H50C,H50D,H50E),
 C509(H50S,H50T,H50U), C603(H60H,H60I,H60J), C606(H60C,H60D,H60E), C609(H60Q,
 H60R,H60S), C703(H70Q,H70R,H70S), C706(H70G,H70H,H70I), C709(H70J,H70K,H70L),
 C712(H71C,H71D,H71E)
;
_shelx_res_checksum              13021
_olex2_submission_special_instructions 'No special instructions were received'