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_1568778
_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         'C81 H189 Au13 Cl10 Ga5 P9'
_chemical_formula_sum            'C81 H189 Au13 Cl10 Ga5 P9'
_chemical_formula_weight         4705.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1624(5)
_cell_length_b                   27.8938(8)
_cell_length_c                   28.6686(10)
_cell_measurement_reflns_used    9358
_cell_measurement_temperature    200
_cell_measurement_theta_max      22.867
_cell_measurement_theta_min      2.260
_cell_volume                     12883.3(7)
_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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_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  0.1032
_diffrn_reflns_av_unetI/netI     0.0519
_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       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            224751
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.750
_diffrn_reflns_theta_max         24.750
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.114
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1536 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.6559.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             8648
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, pentane'
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         22016
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0338
_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^)+88.6929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16213
_reflns_number_total             22016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06908c2.cif
_cod_data_source_block           24
_cod_depositor_comments
'Adding full bibliography for 1568775--1568778.cif.'
_cod_database_code               1568778
_shelx_shelxl_version_number     2014/7
_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
 C604-C605 = C608-C607 = C509-C508
 1.54 with sigma of 0.02
 C608-C609
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C405 \\sim C410: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C904 \\sim C913: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C905 \\sim C914: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C906 \\sim C915: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C909 \\sim C918: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C407 \\sim C413: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C307 \\sim C311: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C309) \\sim Ueq, Uanis(C312) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C414) \\sim Ueq, Uanis(C415) \\sim Ueq, Uanis(C409) \\sim Ueq,
Uanis(C413) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C910) \\sim Ueq, Uanis(C901) \\sim Ueq, Uanis(C911) \\sim Ueq,
Uanis(C902) \\sim Ueq, Uanis(C903) \\sim Ueq, Uanis(C912) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C915) \\sim Ueq, Uanis(C906) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C905) \\sim Ueq, Uanis(C914) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C909) \\sim Ueq, Uanis(C908) \\sim Ueq, Uanis(C917) \\sim Ueq,
Uanis(C907) \\sim Ueq, Uanis(C918) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C310) \\sim Ueq, Uanis(C307) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C507, C508, C509
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C310)=Sof(H31A)=Sof(H31B)=Sof(C311)=Sof(H31C)=Sof(H31D)=Sof(C312)=
 Sof(H31E)=Sof(H31F)=Sof(H31G)=Sof(C410)=Sof(H41A)=Sof(H41B)=Sof(C411)=
 Sof(H41C)=Sof(H41D)=Sof(C412)=Sof(H41E)=Sof(H41F)=Sof(H41G)=Sof(C413)=
 Sof(H41H)=Sof(H41I)=Sof(C414)=Sof(H41J)=Sof(H41K)=Sof(C415)=Sof(H41L)=
 Sof(H41M)=Sof(H41N)=Sof(C910)=Sof(H91A)=Sof(H91B)=Sof(C911)=Sof(H91C)=
 Sof(H91D)=Sof(C912)=Sof(H91E)=Sof(H91F)=Sof(H91G)=Sof(C913)=Sof(H91H)=
 Sof(H91I)=Sof(C914)=Sof(H91J)=Sof(H91K)=Sof(C915)=Sof(H91L)=Sof(H91M)=
 Sof(H91N)=Sof(C916)=Sof(H91O)=Sof(H91P)=Sof(C917)=Sof(H91Q)=Sof(H91R)=
 Sof(C918)=Sof(H91S)=Sof(H91T)=Sof(H91U)=1-FVAR(1)
 Sof(C307)=Sof(H30O)=Sof(H30P)=Sof(C308)=Sof(H30Q)=Sof(H30R)=Sof(C309)=
 Sof(H30S)=Sof(H30T)=Sof(H30U)=Sof(C404)=Sof(H40H)=Sof(H40I)=Sof(C405)=
 Sof(H40J)=Sof(H40K)=Sof(C406)=Sof(H40L)=Sof(H40M)=Sof(H40N)=Sof(C407)=
 Sof(H40O)=Sof(H40P)=Sof(C408)=Sof(H40Q)=Sof(H40R)=Sof(C409)=Sof(H40S)=
 Sof(H40T)=Sof(H40U)=Sof(C901)=Sof(H90A)=Sof(H90B)=Sof(C902)=Sof(H90C)=
 Sof(H90D)=Sof(C903)=Sof(H90E)=Sof(H90F)=Sof(H90G)=Sof(C904)=Sof(H90H)=
 Sof(H90I)=Sof(C905)=Sof(H90J)=Sof(H90K)=Sof(C906)=Sof(H90L)=Sof(H90M)=
 Sof(H90N)=Sof(C907)=Sof(H90O)=Sof(H90P)=Sof(C908)=Sof(H90Q)=Sof(H90R)=
 Sof(C909)=Sof(H90S)=Sof(H90T)=Sof(H90U)=FVAR(1)
6.a Free rotating group:
 C401(C402,C403), C410(C411,C412)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C104(H10H,H10I), C105(H10J,H10K), C107(H10O,
 H10P), C108(H10Q,H10R), C201(H20K,H20L), C202(H20M,H20N), C204(H20O,H20P),
 C205(H20Q,H20R), C207(H20D,H20E), C208(H20F,H20G), C301(H30A,H30B), C302(H30C,
 H30D), C304(H30H,H30I), C305(H30J,H30K), C307(H30O,H30P), C308(H30Q,H30R),
 C310(H31A,H31B), C311(H31C,H31D), C401(H40A,H40B), C402(H40C,H40D), C404(H40H,
 H40I), C405(H40J,H40K), C407(H40O,H40P), C408(H40Q,H40R), C410(H41A,H41B),
 C411(H41C,H41D), C413(H41H,H41I), C414(H41J,H41K), C501(H50A,H50B), C502(H50C,
 H50D), C504(H50H,H50I), C505(H50J,H50K), C507(H50O,H50P), C508(H50Q,H50R),
 C601(H60A,H60B), C602(H60C,H60D), C604(H60H,H60I), C605(H60J,H60K), C607(H60O,
 H60P), C608(H60Q,H60R), C701(H70A,H70B), C702(H70C,H70D), C704(H70H,H70I),
 C705(H70J,H70K), C707(H70O,H70P), C708(H70Q,H70R), C801(H80A,H80B), C802(H80C,
 H80D), C804(H80H,H80I), C805(H80J,H80K), C807(H80O,H80P), C808(H80Q,H80R),
 C901(H90A,H90B), C902(H90C,H90D), C904(H90H,H90I), C905(H90J,H90K), C907(H90O,
 H90P), C908(H90Q,H90R), C910(H91A,H91B), C911(H91C,H91D), C913(H91H,H91I),
 C914(H91J,H91K), C916(H91O,H91P), C917(H91Q,H91R)
6.c Me refined with riding coordinates:
 C103(H10E,H10F,H10G), C106(H10L,H10M,H10N), C109(H10S,H10T,H10U), C203(H20A,
 H20B,H20C), C206(H20S,H20T,H20U), C209(H20H,H20I,H20J), C303(H30E,H30F,H30G),
 C306(H30L,H30M,H30N), C309(H30S,H30T,H30U), C312(H31E,H31F,H31G), C403(H40E,
 H40F,H40G), C406(H40L,H40M,H40N), C409(H40S,H40T,H40U), C412(H41E,H41F,H41G),
 C415(H41L,H41M,H41N), C503(H50E,H50F,H50G), C506(H50L,H50M,H50N), C509(H50S,
 H50T,H50U), C603(H60E,H60F,H60G), C606(H60L,H60M,H60N), C609(H60S,H60T,H60U),
 C703(H70E,H70F,H70G), C706(H70L,H70M,H70N), C709(H70S,H70T,H70U), C803(H80E,
 H80F,H80G), C806(H80L,H80M,H80N), C809(H80S,H80T,H80U), C903(H90E,H90F,H90G),
 C906(H90L,H90M,H90N), C909(H90S,H90T,H90U), C912(H91E,H91F,H91G), C915(H91L,
 H91M,H91N), C918(H91S,H91T,H91U)
;
_shelx_res_checksum              81484
_olex2_submission_special_instructions 'No special instructions were received'