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_1568777
_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         'C90 H207 Au13 Cl11 Ga6 P9'
_chemical_formula_sum            'C90 H207 Au13 Cl11 Ga6 P9'
_chemical_formula_weight         4937.11
_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             2021-11-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9143(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9369(2)
_cell_length_b                   29.9431(3)
_cell_length_c                   26.0812(3)
_cell_measurement_reflns_used    38632
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      77.1620
_cell_measurement_theta_min      2.7550
_cell_volume                     13798.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  23.00   0.50    3.00    --  -49.70  17.00-118.00   96
  2  \w   -122.00 -45.00   0.50    3.00    --  -49.70 -17.00  72.00  154
  3  \w    -22.00  25.00   0.50    3.00    --   49.70 -17.00  72.00   94
  4  \w     45.00 122.00   0.50    3.00    --   49.70  17.00-118.00  154
  5  \w   -161.00 -85.00   0.50   10.00    --  -90.00 -17.00  72.00  152
  6  \w    107.00 178.00   0.50   10.00    --  111.50  17.00-118.00  142
  7  \w    -26.00  22.00   0.50    3.00    --  -49.70  19.00-180.00   96
  8  \w    -26.00  22.00   0.50    3.00    --  -49.70  19.00 -90.00   96
  9  \w     34.00  94.00   0.50    3.00    --   49.70-125.00 -90.00  120
 10  \w    -22.00  26.00   0.50    3.00    --   49.70 -19.00 -30.00   96
 11  \w    -51.00 -18.00   0.50   10.00    --  -90.00  45.00-120.00   66
 12  \w    -71.00 -18.00   0.50   10.00    --  -90.00  61.00  30.00  106
 13  \w    -51.00 -18.00   0.50   10.00    --  -90.00  45.00-150.00   66
 14  \w     41.00  71.00   0.50   10.00    --  111.50 -61.00-150.00   60
 15  \w     41.00  71.00   0.50   10.00    --  111.50 -61.00 -90.00   60
 16  \w     41.00 106.00   0.50   10.00    --  111.50 -77.00 -30.00  130
 17  \w     63.00 118.00   0.50   10.00    --  111.50   0.00-120.00  110
 18  \w     63.00 118.00   0.50   10.00    --  111.50   0.00 -90.00  110
 19  \w     41.00 111.00   0.50   10.00    --  111.50-125.00 120.00  140
 20  \w     41.00  71.00   0.50   10.00    --  111.50 -61.00-180.00   60
 21  \w     63.00 118.00   0.50   10.00    --  111.50   0.00   0.00  110
 22  \w     41.00 106.00   0.50   10.00    --  111.50 -94.00 -30.00  130
 23  \w     41.00  71.00   0.50   10.00    --  111.50 -61.00 150.00   60
 24  \w     41.00 111.00   0.50   10.00    --  111.50-125.00   0.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0503863000
_diffrn_orient_matrix_UB_12      0.0107820000
_diffrn_orient_matrix_UB_13      0.0525445000
_diffrn_orient_matrix_UB_21      0.0710745000
_diffrn_orient_matrix_UB_22      -0.0043134000
_diffrn_orient_matrix_UB_23      -0.0254774000
_diffrn_orient_matrix_UB_31      -0.0046198000
_diffrn_orient_matrix_UB_32      0.0501270000
_diffrn_orient_matrix_UB_33      -0.0134176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            115496
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        64.999
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    29.702
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_description       prism
_exptl_crystal_F_000             9128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluenen, pentane'
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         23236
_refine_ls_number_restraints     549
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0597P)^2^+159.6936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17730
_reflns_number_total             23236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06908c2.cif
_cod_data_source_block           1008g4
_cod_depositor_comments
'Adding full bibliography for 1568775--1568778.cif.'
_cod_database_code               1568777
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C90H204Au13Cl11Ga6P9
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.098
_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
 C106-C107 = C106-C105 = C108-C109 = C109-C110 = C101-C102 = C102-C103 = C103-
 C104
 1.54 with sigma of 0.02
 C406-C405 = C407-C406
 1.54 with sigma of 0.02
 C110-C108
 2.54 with sigma of 0.04
 C802-C804
 2.54 with sigma of 0.04
 C402-C404
 2.54 with sigma of 0.04
 C104-C102 \\sim C103-C101
 with sigma of 0.04
 C104-C103 \\sim C103-C102 \\sim C102-C101
 with sigma of 0.02
 C901-C902 \\sim C902-C903 \\sim C903-C904
 with sigma of 0.02
 C901-C903 \\sim C902-C904
 with sigma of 0.04
 C301-C302 \\sim C302-C303 \\sim C303-C304
 with sigma of 0.02
 C301-C303 \\sim C302-C304
 with sigma of 0.04
 C604-C603 \\sim C603-C602 \\sim C602-C601
 with sigma of 0.02
 C604-C602 \\sim C603-C601
 with sigma of 0.04
 C110-C109 \\sim C109-C108
 with sigma of 0.02
 C204-C202 \\sim C203-C201
 with sigma of 0.04
 C204-C203 \\sim C203-C202 \\sim C202-C201
 with sigma of 0.02
 C507-C506 \\sim C506-C505
 with sigma of 0.02
 C704-C703 \\sim C703-C702 \\sim C702-C701
 with sigma of 0.02
 C704-C702 \\sim C703-C701
 with sigma of 0.04
 C802-C803 \\sim C803-C804
 with sigma of 0.02
 C402-C403 \\sim C403-C404
 with sigma of 0.02
 C508-C509 \\sim C509-C510
 with sigma of 0.02
 P7-C704 \\sim P1-C104 \\sim P3-C304 \\sim P2-C204 \\sim P9-C904 \\sim P6-C604
\\sim P5-C504
 with sigma of 0.02
 C504-C503 \\sim C503-C502 \\sim C502-C501
 with sigma of 0.02
 C504-C502 \\sim C503-C501
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C709 \\sim C711: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C710 \\sim C712: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C901 \\sim C902 \\sim C903 \\sim C904: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C301 \\sim C302 \\sim C303 \\sim C304: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C601 \\sim C602 \\sim C603 \\sim C604: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C108 \\sim C109 \\sim C110: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C505 \\sim C506 \\sim C507: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C701 \\sim C702 \\sim C703 \\sim C704: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C801 \\sim C802 \\sim C803 \\sim C804: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C401 \\sim C402 \\sim C403 \\sim C404: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C402 \\sim C403 \\sim C404: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C409 \\sim C411: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C410 \\sim C412: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C305 \\sim C306 \\sim C307: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C105 \\sim C106 \\sim C107: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C508 \\sim C509 \\sim C510: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C501 \\sim C502 \\sim C503 \\sim C504: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C610) \\sim Ueq, Uanis(C609) \\sim Ueq, Uanis(C608) \\sim Ueq,
Uanis(C607) \\sim Ueq, Uanis(C606) \\sim Ueq, Uanis(C605) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C505) \\sim Ueq, Uanis(C506) \\sim Ueq, Uanis(C507) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C308) \\sim Ueq, Uanis(C310) \\sim Ueq, Uanis(C309) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C411) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C711) \\sim Ueq, Uanis(C712) \\sim Ueq, Uanis(C710) \\sim Ueq,
Uanis(C709) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C110) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C407) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C405) \\sim Ueq, Uanis(C406) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C903) \\sim Ueq, Uanis(C404) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C904) \\sim Ueq, Uanis(C403) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C508) \\sim Ueq, Uanis(C509) \\sim Ueq, Uanis(C510) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C201, C202, C203, C204
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C508, C509, C510
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C501, C502, C503, C504
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H40S)=Sof(H40T)=Sof(C411)=Sof(H41E)=Sof(H41D)=Sof(C412)=Sof(H41G)=
 Sof(H41F)=Sof(H41H)=Sof(H70S)=Sof(H70T)=Sof(C711)=Sof(H71E)=Sof(H71D)=
 Sof(C712)=Sof(H71G)=Sof(H71F)=Sof(H71H)=1-FVAR(1)
 Sof(H40Q)=Sof(H40R)=Sof(C409)=Sof(H40V)=Sof(H40U)=Sof(C410)=Sof(H41A)=
 Sof(H41C)=Sof(H41B)=Sof(H70Q)=Sof(H70R)=Sof(C709)=Sof(H70V)=Sof(H70U)=
 Sof(C710)=Sof(H71B)=Sof(H71A)=Sof(H71C)=FVAR(1)
6.a Free rotating group:
 C104(C101,C102,C103), C110(C108,C109), C204(C201,C202,C203), C301(C302,C303,
 C304), C402(C403,C404), C504(C501,C502,C503), C508(C509,C510), C604(C601,C602,
 C603), C704(C701,C702,C703), C802(C803,C804), C901(C902,C903,C904)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10E,H10D), C102(H10G,H10F), C103(H10I,H10H), C105(H10J,H10K), C106(H10L,
 H10M), C108(H10Q,H10R), C109(H10S,H10T), C201(H20G,H20F), C202(H20I,H20H),
 C203(H20K,H20J), C205(H20L,H20M), C206(H20A,H20B), C208(H20Q,H20R), C209(H20S,
 H20T), C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C305(H30J,H30K),
 C306(H30L,H30M), C308(H30Q,H30R), C309(H30S,H30T), C401(H40A,H40B), C402(H40C,
 H40D), C403(H40E,H40F), C405(H40J,H40K), C406(H40L,H40M), C408(H40Q,H40R),
 C408(H40S,H40T), C409(H40V,H40U), C411(H41E,H41D), C501(H50E,H50D), C502(H50G,
 H50F), C503(H50I,H50H), C505(H50J,H50K), C506(H50L,H50M), C508(H50R,H50Q),
 C509(H50T,H50S), C601(H60D,H60E), C602(H60F,H60G), C603(H60H,H60I), C605(H60J,
 H60K), C606(H60L,H60M), C608(H60Q,H60R), C609(H60S,H60T), C701(H70E,H70D),
 C702(H70G,H70F), C703(H70I,H70H), C705(H70J,H70K), C706(H70M,H70L), C708(H70Q,
 H70R), C708(H70S,H70T), C709(H70V,H70U), C711(H71E,H71D), C801(H80A,H80B),
 C802(H80C,H80D), C803(H80E,H80F), C805(H80J,H80K), C806(H80L,H80M), C808(H80Q,
 H80R), C809(H80S,H80T), C901(H90B,H90A), C902(H90D,H90C), C903(H90F,H90E),
 C905(H90J,H90K), C906(H90L,H90M), C908(H90Q,H90R), C909(H90S,H90T)
6.c Me refined with riding coordinates:
 C104(H10B,H10C,H10A), C107(H10O,H10N,H10P), C110(H11B,H11A,H11C), C204(H20D,
 H20E,H20C), C207(H20N,H20P,H20O), C210(H21A,H21B,H21C), C304(H30H,H30I,H30G),
 C307(H30O,H30P,H30N), C310(H31B,H31A,H31C), C404(H40G,H40I,H40H), C407(H40N,
 H40P,H40O), C410(H41A,H41C,H41B), C412(H41G,H41F,H41H), C510(H51B,H51A,H51C),
 C604(H60B,H60A,H60C), C607(H60O,H60P,H60N), C610(H61B,H61A,H61C), C704(H70B,
 H70C,H70A), C707(H70O,H70N,H70P), C710(H71B,H71A,H71C), C712(H71G,H71F,H71H),
 C804(H80G,H80I,H80H), C807(H80N,H80O,H80P), C810(H81A,H81B,H81C), C904(H90H,
 H90G,H90I), C907(H90N,H90O,H90P), C910(H91B,H91C,H91A)
6.d Idealised Me refined as rotating group:
 C504(H50B,H50C,H50A), C507(H50O,H50N,H50P)
;
_shelx_res_checksum              96155
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 14.285
_oxdiff_exptl_absorpt_empirical_full_min 0.344