A new reductant in gold cluster chemistry gives a superatomic gold gallium cluster.
Fetzer, Florian; Schrenk, Claudio; Pollard, Nia; Adeagbo, Adebola; Clayborne, Andre Z.; Schnepf, Andreas; Chemical communications (Cambridge, England) 57 (2021) 3551–3554; doi:10.1039/d0cc07006h

data_7128005
_publ_section_title
;
 A new reductant in gold cluster chemistry gives a superatomic gold
 gallium cluster.
;
_journal_issue                   29
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3551
_journal_page_last               3554
_journal_paper_doi               10.1039/d0cc07006h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C144 H120 Au9 Cl2 Ga P8, 1.25(C5 H5 Cl3 Ga), 0.75(Cl4 Ga)'
_chemical_formula_sum            'C150.23 H126.23 Au9 Cl8.76 Ga3 P8'
_chemical_formula_weight         4471.45
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-17 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.0956(13)
_cell_length_b                   15.1623(6)
_cell_length_c                   33.4620(14)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.160
_cell_measurement_theta_min      2.388
_cell_volume                     15643.8(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 0.999
_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  0.0702
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            81808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         1.650
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    9.188
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0840 before and 0.0453 after correction. The Ratio of minimum to maximum transmission is 0.6490. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             8402
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, thf, Et2O'
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.061
_refine_diff_density_max         2.810
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         13018
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0403P)^2^+363.2322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10013
_reflns_number_total             13018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07006h2.cif
_cod_data_source_block           61_sq
_cod_depositor_comments          'Adding full bibliography for 7128005.cif.'
_cod_database_code               7128005
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C501-C505 \\sim C502-C501 \\sim C505-C504 \\sim C502-C503 \\sim C504-C503
 with sigma of 0.02
 C505-C503 \\sim C501-C504 \\sim C502-C504 \\sim C502-C505 \\sim C501-C503
 with sigma of 0.04
3. Restrained planarity
 C501, C502, C503, C504, C505
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cl23 \\sim Cl32: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl22 \\sim Cl31: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C501 \\sim C502 \\sim C503 \\sim C504 \\sim C505: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Ga2 \\sim Ga3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl33 \\sim Cl34: within 4A with sigma of 0.01 and sigma for terminal atoms of
0.02
C505 \\sim Cl34: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Cl34) \\sim Ueq, Uanis(Cl33) \\sim Ueq: 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
5. Rigid body (RIGU) restrains
 C501, C502, C503, C504, C505
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Ga2(0.62287) Cl21(0.62287) Cl22(0.62287) Cl23(0.62287)
 C502(0.62287) H502(0.62287) C501(0.62287) H501(0.62287) C503(0.62287)
 H503(0.62287) C504(0.62287) H504(0.62287) C505(0.62287) H505(0.62287)
 Ga3(0.37713) Cl31(0.37713) Cl32(0.37713) Cl33(0.37713) Cl34(0.37713)
7.a Free rotating group:
 C502(C501,C503,C504,C505)
7.b Ternary CH refined with riding coordinates:
 C501(H501)
7.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C114(H114), C115(H115),
 C116(H116), C117(H117), C118(H118), C202(H202), C203(H203), C204(H204),
 C205(H205), C206(H206), C208(H208), C209(H209), C210(H210), C211(H211),
 C212(H212), C214(H214), C215(H215), C216(H216), C217(H217), C218(H218),
 C302(H302), C303(H303), C304(H304), C305(H305), C306(H306), C308(H308),
 C309(H309), C310(H310), C311(H311), C312(H312), C314(H314), C315(H315),
 C316(H316), C317(H317), C318(H318), C402(H402), C403(H403), C404(H404),
 C405(H405), C406(H406), C408(H408), C409(H409), C410(H410), C411(H411),
 C412(H412), C414(H414), C415(H415), C416(H416), C417(H417), C418(H418),
 C502(H502), C503(H503), C504(H504), C505(H505)
;
_shelx_res_checksum              25623
_shelx_hkl_checksum              14719
_shelx_fab_checksum              80069
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'