Au70S20(PPh3)12: An intermediate sized metalloid gold cluster stabilized by the Au4S4 ring motif and Au-PPh3 groups
Schnepf, Andreas; Schrenk, Claudio; Häkkinen, Hannu; Frojd, Andrew R.; Kenzler, Sebastian Ignaz Joachim; Clayborne, Andre; Chemical Communications  (2017) –; doi:10.1039/C7CC08014J

data_7120897
_publ_section_title
;
 Au70S20(PPh3)12: An intermediate sized metalloid gold cluster stabilized
 by the Au4S4 ring motif and Au-PPh3 groups
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08014J
_journal_year                    2017
_chemical_formula_moiety         'C216 H180 Au70 P12 S20'
_chemical_formula_sum            'C216 H180 Au70 P12 S20'
_chemical_formula_weight         17576.09
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   40.2486(11)
_cell_length_b                   40.2486(11)
_cell_length_c                   95.357(2)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.017
_cell_measurement_theta_min      2.381
_cell_volume                     133778(6)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX area detector'
_diffrn_detector_area_resol_mean 8.333
_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 scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.1006
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       110
_diffrn_reflns_limit_l_min       -109
_diffrn_reflns_number            362279
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.498
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.973
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    34.720
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1181 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.5334. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.927
_exptl_crystal_description       block
_exptl_crystal_F_000             135108
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, thf'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.511
_refine_diff_density_min         -3.885
_refine_diff_density_rms         0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1443
_refine_ls_number_reflns         23946
_refine_ls_number_restraints     1644
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+78549.4766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17684
_reflns_number_total             23946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08014j2.cif
_cod_data_source_block           5_sq
_cod_original_cell_volume        133778(8)
_cod_database_code               7120897
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C417-C416 = C416-C415 = C415-C414 = C414-C413 = C413-C418 = C418-C417
 1.37 with sigma of 0.02
 C511-C510 = C510-C509 = C509-C508 = C508-C507 = C507-C512 = C512-C511
 1.37 with sigma of 0.02
 C409-C408 = C408-C407 = C407-C412 = C412-C411 = C411-C410 = C410-C409
 1.37 with sigma of 0.02
 C307-C312 = C312-C311 = C311-C310 = C310-C309 = C309-C308 = C308-C307
 1.37 with sigma of 0.02
 C502-C503 = C503-C504 = C504-C505 = C505-C506 = C506-C501 = C501-C502
 1.37 with sigma of 0.02
 C606-C605 = C605-C604 = C604-C603 = C603-C602 = C602-C601 = C601-C606
 1.37 with sigma of 0.02
 C217-C216 = C216-C215 = C215-C214 = C214-C213 = C213-C218 = C218-C217
 1.37 with sigma of 0.02
 C304-C305 = C305-C306 = C306-C301 = C301-C302 = C302-C303 = C303-C304
 1.37 with sigma of 0.02
 C401-C402 = C402-C403 = C403-C404 = C404-C405 = C405-C406 = C406-C401
 1.37 with sigma of 0.02
 C514-C513 = C513-C518 = C518-C517 = C517-C516 = C516-C515 = C515-C514
 1.37 with sigma of 0.02
 C318-C317 = C317-C316 = C316-C315 = C315-C314 = C314-C313 = C313-C318
 1.37 with sigma of 0.02
 C201-C206 = C206-C205 = C205-C204 = C204-C203 = C203-C202 = C202-C201
 1.37 with sigma of 0.02
 C615-C614 = C614-C613 = C613-C618 = C618-C617 = C617-C616 = C616-C615
 1.37 with sigma of 0.02
 C113-C118 = C118-C117 = C117-C116 = C116-C115 = C115-C114 = C114-C113
 1.37 with sigma of 0.02
 C611-C610 = C610-C609 = C609-C608 = C608-C607 = C607-C612 = C612-C611
 1.37 with sigma of 0.02
 C106-C101 = C101-C102 = C102-C103 = C103-C104 = C104-C105 = C105-C106
 1.37 with sigma of 0.02
 C209-C208 = C208-C207 = C207-C212 = C212-C211 = C211-C210 = C210-C209
 1.37 with sigma of 0.02
 C112-C111 = C111-C110 = C110-C109 = C109-C108 = C108-C107 = C107-C112
 1.37 with sigma of 0.02
 C417-C413 \\sim C417-C413 \\sim C414-C416 \\sim C414-C418 \\sim C418-C416
\\sim C413-C415
 with sigma of 0.04
 C511-C507 \\sim C511-C507 \\sim C508-C510 \\sim C508-C512 \\sim C512-C510
\\sim C507-C509
 with sigma of 0.04
 C409-C411 \\sim C409-C411 \\sim C412-C408 \\sim C412-C410 \\sim C410-C408
\\sim C411-C407
 with sigma of 0.04
 C307-C309 \\sim C307-C309 \\sim C310-C312 \\sim C310-C308 \\sim C308-C312
\\sim C309-C311
 with sigma of 0.04
 C502-C506 \\sim C502-C506 \\sim C505-C503 \\sim C505-C501 \\sim C501-C503
\\sim C506-C504
 with sigma of 0.04
 C606-C602 \\sim C606-C602 \\sim C603-C605 \\sim C603-C601 \\sim C601-C605
\\sim C602-C604
 with sigma of 0.04
 C217-C213 \\sim C217-C213 \\sim C214-C216 \\sim C214-C218 \\sim C218-C216
\\sim C213-C215
 with sigma of 0.04
 C304-C302 \\sim C304-C302 \\sim C301-C305 \\sim C301-C303 \\sim C303-C305
\\sim C302-C306
 with sigma of 0.04
 C401-C405 \\sim C401-C405 \\sim C404-C402 \\sim C404-C406 \\sim C406-C402
\\sim C405-C403
 with sigma of 0.04
 C514-C516 \\sim C514-C516 \\sim C517-C513 \\sim C517-C515 \\sim C515-C513
\\sim C516-C518
 with sigma of 0.04
 C318-C314 \\sim C318-C314 \\sim C315-C317 \\sim C315-C313 \\sim C313-C317
\\sim C314-C316
 with sigma of 0.04
 C201-C203 \\sim C201-C203 \\sim C204-C206 \\sim C204-C202 \\sim C202-C206
\\sim C203-C205
 with sigma of 0.04
 C615-C617 \\sim C615-C617 \\sim C618-C614 \\sim C618-C616 \\sim C616-C614
\\sim C617-C613
 with sigma of 0.04
 C113-C115 \\sim C113-C115 \\sim C116-C118 \\sim C116-C114 \\sim C114-C118
\\sim C115-C117
 with sigma of 0.04
 C611-C607 \\sim C611-C607 \\sim C608-C610 \\sim C608-C612 \\sim C612-C610
\\sim C607-C609
 with sigma of 0.04
 C106-C104 \\sim C106-C104 \\sim C103-C101 \\sim C103-C105 \\sim C105-C101
\\sim C104-C102
 with sigma of 0.04
 C209-C211 \\sim C209-C211 \\sim C212-C208 \\sim C212-C210 \\sim C210-C208
\\sim C211-C207
 with sigma of 0.04
 C112-C108 \\sim C112-C108 \\sim C109-C111 \\sim C109-C107 \\sim C107-C111
\\sim C108-C110
 with sigma of 0.04
3. Restrained planarity
 C413, C414, C415, C416, C417, C418
 with sigma of 0.1
 C507, C508, C509, C510, C511, C512
 with sigma of 0.1
 C407, C408, C409, C410, C411, C412
 with sigma of 0.1
 C307, C308, C309, C310, C311, C312
 with sigma of 0.1
 C501, C502, C503, C504, C505, C506
 with sigma of 0.1
 C601, C602, C603, C604, C605, C606
 with sigma of 0.1
 C213, C214, C215, C216, C217, C218
 with sigma of 0.1
 C301, C302, C303, C304, C305, C306
 with sigma of 0.1
 C401, C402, C403, C404, C405, C406
 with sigma of 0.1
 C513, C514, C515, C516, C517, C518
 with sigma of 0.1
 C313, C314, C315, C316, C317, C318
 with sigma of 0.1
 C201, C202, C203, C204, C205, C206
 with sigma of 0.1
 C613, C614, C615, C616, C617, C618
 with sigma of 0.1
 C113, C114, C115, C116, C117, C118
 with sigma of 0.1
 C607, C608, C609, C610, C611, C612
 with sigma of 0.1
 C101, C102, C103, C104, C105, C106
 with sigma of 0.1
 C207, C208, C209, C210, C211, C212
 with sigma of 0.1
 C107, C108, C109, C110, C111, C112
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C413 \\sim C414 \\sim C415 \\sim C416 \\sim C417 \\sim C418: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C507 \\sim C508 \\sim C509 \\sim C510 \\sim C511 \\sim C512: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C407 \\sim C408 \\sim C409 \\sim C410 \\sim C411 \\sim C412: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C307 \\sim C308 \\sim C309 \\sim C310 \\sim C311 \\sim C312: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C501 \\sim C502 \\sim C503 \\sim C504 \\sim C505 \\sim C506: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C601 \\sim C602 \\sim C603 \\sim C604 \\sim C605 \\sim C606: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217 \\sim C218: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C301 \\sim C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C401 \\sim C402 \\sim C403 \\sim C404 \\sim C405 \\sim C406: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C513 \\sim C514 \\sim C515 \\sim C516 \\sim C517 \\sim C518: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C313 \\sim C314 \\sim C315 \\sim C316 \\sim C317 \\sim C318: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C613 \\sim C614 \\sim C615 \\sim C616 \\sim C617 \\sim C618: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C607 \\sim C608 \\sim C609 \\sim C610 \\sim C611 \\sim C612: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C207 \\sim C208 \\sim C209 \\sim C210 \\sim C211 \\sim C212: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Au36 \\sim Au37: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C413, C414, C415, C416, C417, C418
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C507, C508, C509, C510, C511, C512
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C407, C408, C409, C410, C411, C412
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C307, C308, C309, C310, C311, C312
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C501, C502, C503, C504, C505, C506
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C601, C602, C603, C604, C605, C606
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C213, C214, C215, C216, C217, C218
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C301, C302, C303, C304, C305, C306
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C401, C402, C403, C404, C405, C406
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C513, C514, C515, C516, C517, C518
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C313, C314, C315, C316, C317, C318
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C201, C202, C203, C204, C205, C206
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C613, C614, C615, C616, C617, C618
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C113, C114, C115, C116, C117, C118
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C607, C608, C609, C610, C611, C612
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C102, C103, C104, C105, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C207, C208, C209, C210, C211, C212
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C107, C108, C109, C110, C111, C112
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Au37)=1-FVAR(1)
 Sof(Au36)=FVAR(1)
7.a 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), C506(H506), C508(H508),
 C509(H509), C510(H510), C511(H511), C512(H512), C514(H514), C515(H515),
 C516(H516), C517(H517), C518(H518), C602(H602), C603(H603), C604(H604),
 C605(H605), C606(H606), C608(H608), C609(H609), C610(H610), C611(H611),
 C612(H612), C614(H614), C615(H615), C616(H616), C617(H617), C618(H618)
;
_shelx_res_checksum              75700
_shelx_fab_checksum              88179
_olex2_submission_special_instructions 'No special instructions were received'