High-yield synthesis and crystal structure of a green Au30 cluster co-capped by thiolate and sulfide
Huayan Yang; Yu Wang; Alison J. Edwards; Juanzhu Yan; Nanfeng Zheng; Chem.Commun. 50 (2014) 14325–; doi:10.1039/C4cc01773K

data_7115943
_publ_section_title
;
 High-yield synthesis and crystal structure of a green Au30 cluster
 co-capped by thiolate and sulfide
;
_journal_name_full               Chem.Commun.
_journal_page_first              14325
_journal_paper_doi               10.1039/C4cc01773K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C72 H162 Au30 S19'
_chemical_formula_sum            'C72 H162 Au30 S19'
_chemical_formula_weight         7546.14
_chemical_name_common            Green
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                111.285(2)
_cell_angle_beta                 92.8643(17)
_cell_angle_gamma                93.898(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7299(4)
_cell_length_b                   21.2699(5)
_cell_length_c                   25.8105(5)
_cell_measurement_reflns_used    17300
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      73.5740
_cell_measurement_theta_min      3.3812
_cell_volume                     7493.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -47.00   -4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4653  -77.0000    0.0000 86

  2 omega -122.00  -97.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4653  -77.0000    0.0000 50

  3 omega -113.00   -6.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4653  -57.0000 -120.0000 214

  4 omega  -43.00   41.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4653   38.0000   30.0000 168

  5 omega  -37.00   38.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.4653   38.0000  120.0000 150

  6 omega   57.00  123.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4653 -178.0000 -120.0000 132

  7 omega   61.00   91.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4653  178.0000  -60.0000 60

  8 omega   99.00  126.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4653  178.0000    0.0000 54

  9 omega   37.00   98.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -45.0000 -120.0000 122

 10 omega   66.00   92.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086 -111.0000  150.0000 52

 11 omega   51.00   86.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -94.0000 -180.0000 70

 12 omega  108.00  178.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  111.0000  120.0000 140

 13 omega   35.00   79.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -94.0000 -120.0000 88

 14 omega  105.00  173.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086   61.0000 -180.0000 136

 15 omega   41.00  117.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -61.0000   30.0000 152

 16 omega   30.00  109.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -94.0000  -90.0000 158

 17 omega   33.00   90.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -30.0000   30.0000 114

 18 omega   31.00   87.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -30.0000  120.0000 112

 19 omega   31.00   56.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -45.0000   30.0000 50

 20 omega   44.00  178.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086  -15.0000  150.0000 268

 21 omega   30.00   68.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086 -111.0000 -180.0000 76

 22 omega   86.00  115.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086 -111.0000 -180.0000 58

 23 omega   28.00  114.00   0.5000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4086 -109.0000   43.0000 172
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0715889000
_diffrn_orient_matrix_UB_12      0.0570546000
_diffrn_orient_matrix_UB_13      0.0015275000
_diffrn_orient_matrix_UB_21      -0.0099441000
_diffrn_orient_matrix_UB_22      0.0365641000
_diffrn_orient_matrix_UB_23      0.0627382000
_diffrn_orient_matrix_UB_31      0.0763988000
_diffrn_orient_matrix_UB_32      -0.0387582000
_diffrn_orient_matrix_UB_33      0.0138384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48378
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.089
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    56.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.345
_exptl_crystal_F_000             6536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         13.375
_refine_diff_density_min         -8.962
_refine_diff_density_rms         0.567
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         25550
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.161
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+431.7158P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2337
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19240
_reflns_number_total             25550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01773k3.cif
_cod_data_source_block           y120719-23
_cod_database_code               7115943
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C1
 1.5 with sigma of 0.02
 C5-C8
 1.5 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.02
 C69-C70 = C71-C69
 1.5 with sigma of 0.02
 C72-C69 = C69-C70 = C71-C69
 1.5 with sigma of 0.02
 C72-C70
 2.5 with sigma of 0.02
 C70-C71
 2.5 with sigma of 0.02
 C71-C72
 2.5 with sigma of 0.02
 C53-C55
 1.5 with sigma of 0.02
 C53-C56
 1.5 with sigma of 0.02
 C65-C68
 1.5 with sigma of 0.02
 C65-C66
 1.5 with sigma of 0.02
 C20-C17
 1.5 with sigma of 0.02
 C65-C67
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 C3-S1
 2.9 with sigma of 0.02
 C1-S1
 1.85 with sigma of 0.02
 S18-C69
 1.8 with sigma of 0.02
 S18-C69
 1.8 with sigma of 0.02
3. Rigid bond restraints
 C57, C58
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C5, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C4, C3, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C41
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C71, C69
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C70, C69
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C41, C43
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C21, C24
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C37, C40
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C13, C16
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C46
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C65, C68
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C65, C67
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C5, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C57, C60
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C33, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C46, C45
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C53
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C2, C1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S2, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S11, C41
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S18, C69
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S4, C13
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S18, C69
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C5 \\sim C7 \\sim C8 \\sim C6 \\sim S2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C13 \\sim C15 \\sim C16 \\sim C16 \\sim S4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C65 \\sim C68 \\sim C66 \\sim C67 \\sim S17: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C17 \\sim C20 \\sim C18 \\sim C19 \\sim S5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C33 \\sim C34 \\sim C35 \\sim C36 \\sim S9: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C41 \\sim C42 \\sim C44 \\sim C43 \\sim S11: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23 \\sim C24 \\sim C22 \\sim S6: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C25 \\sim C26 \\sim C28 \\sim C27 \\sim S7: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C60 \\sim C59 \\sim C58 \\sim S15: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C49) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(S18) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3) = Uanis(C72) = Uanis(C69) = Uanis(C70) = Uanis(C71) = Uanis(C6)
5.a Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C11(H11A,H11B,H11C), C38(H38A,H38B,H38C), C46(H46A,H46B,
 H46C), C40(H40A,H40B,H40C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C51(H51A,
 H51B,H51C), C10(H10A,H10B,H10C), C39(H39A,H39B,H39C), C16(H16A,H16B,H16C),
 C31(H31A,H31B,H31C), C52(H52A,H52B,H52C), C32(H32A,H32B,H32C), C64(H64A,H64B,
 H64C), C62(H62A,H62B,H62C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C42(H42A,
 H42B,H42C), C30(H30A,H30B,H30C), C48(H48A,H48B,H48C), C15(H15A,H15B,H15C),
 C68(H68A,H68B,H68C), C55(H55A,H55B,H55C), C35(H35A,H35B,H35C), C54(H54A,H54B,
 H54C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C24(H24A,H24B,H24C), C50(H50A,H50B,H50C), C56(H56A,H56B,H56C),
 C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C60(H60A,H60B,H60C), C44(H44A,H44B,
 H44C), C2(H2A,H2B,H2C), C43(H43A,H43B,H43C), C4(H4A,H4B,H4C), C19(H19A,H19B,
 H19C), C36(H36A,H36B,H36C), C58(H58A,H58B,H58C), C22(H22A,H22B,H22C), C28(H28A,
 H28B,H28C), C8(H8A,H8B,H8C), C59(H59A,H59B,H59C), C23(H23A,H23B,H23C), C3(H3A,
 H3B,H3C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C)
;
_shelx_estimated_absorpt_t_max   0.071
_shelx_estimated_absorpt_t_min   0.014
_shelx_res_checksum              74804
_shelxl_version_number           2013-2