Structure determination of a metastable Au<sub>22</sub>(SAdm)<sub>16</sub> nanocluster and its spontaneous transformation into Au<sub>21</sub>(SAdm)<sub>15</sub>.
Li, Qinzhen; Yang, Sha; Chen, Tao; Jin, Shan; Chai, Jinsong; Zhang, Hui; Zhu, Manzhou; Nanoscale 12 (2020) 23694–23699; doi:10.1039/d0nr07124b

data_1559738
_publ_section_title
;
 Structure determination of a metastable
 Au<sub>22</sub>(SAdm)<sub>16</sub> nanocluster and its spontaneous
 transformation into Au<sub>21</sub>(SAdm)<sub>15</sub>.
;
_journal_issue                   46
_journal_name_full               Nanoscale
_journal_page_first              23694
_journal_page_last               23699
_journal_paper_doi               10.1039/d0nr07124b
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C160 H240 Au22 S16'
_chemical_formula_sum            'C160 H240 Au22 S16'
_chemical_formula_weight         7009.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-20 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.356(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3688(16)
_cell_length_b                   32.3268(9)
_cell_length_c                   36.999(2)
_cell_measurement_reflns_used    3374
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.00
_cell_measurement_theta_min      7.37
_cell_volume                     19417(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            112810
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.716
_diffrn_reflns_theta_min         3.938
_exptl_absorpt_coefficient_mu    32.258
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1480
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_description       block
_exptl_crystal_F_000             12776
_refine_diff_density_max         9.370
_refine_diff_density_min         -5.685
_refine_diff_density_rms         0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1417
_refine_ls_number_reflns         35378
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1409P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26259
_reflns_number_total             35378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr07124b2.cif
_cod_data_source_block           1
_cod_database_code               1559738
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C60-C040 = C60-C128
 1.52 with sigma of 0.01
 C040-C128
 2.55 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C116) = Uanis(C58)
Uanis(C03P) = Uanis(C02Z) = Uanis(C53)
Uanis(C046) = Uanis(C06F) = Uanis(C04G) = Uanis(C21)
Uanis(C01B) = Uanis(C059) = Uanis(C06H) = Uanis(C01Z) = Uanis(C109) = Uanis(C74)
Uanis(C035) = Uanis(C71) = Uanis(C051) = Uanis(C031) = Uanis(C3AA) = Uanis(C4AA)
Uanis(C05N) = Uanis(C126) = Uanis(C022) = Uanis(C02M) = Uanis(C26) = Uanis(C04V)
Uanis(C42) = Uanis(C34) = Uanis(C01Q) = Uanis(C01X) = Uanis(C03J) = Uanis(C9AA)
= Uanis(C037) = Uanis(C18)
Uanis(C191) = Uanis(C05C) = Uanis(C03C) = Uanis(C47)
Uanis(C01A) = Uanis(C20) = Uanis(C02L) = Uanis(C29) = Uanis(C034)
Uanis(C053) = Uanis(C5AA) = Uanis(C02S) = Uanis(C44)
Uanis(C01M) = Uanis(C042) = Uanis(C2AA) = Uanis(C04Y) = Uanis(C020) =
Uanis(C02N)
Uanis(C05T) = Uanis(C04S) = Uanis(C02R) = Uanis(C70)
Uanis(C03K) = Uanis(C02U) = Uanis(C04J) = Uanis(C026)
Uanis(C023) = Uanis(C06B) = Uanis(C01G) = Uanis(C63) = Uanis(C60)
Uanis(C37) = Uanis(C191) = Uanis(C67) = Uanis(C1AA) = Uanis(C05C)
Uanis(C71) = Uanis(C051) = Uanis(C031) = Uanis(C3AA) = Uanis(C04D)
Uanis(C7AA) = Uanis(C5AA) = Uanis(C053) = Uanis(C44) = Uanis(C062)
Uanis(C63) = Uanis(C01G) = Uanis(C60) = Uanis(C040)
4.a Ternary CH refined with riding coordinates:
 C019(H019), C01X(H01Z), C026(H026), C02M(H02M), C02R(H02R), C02Z(H02Z),
 C033(H033), C037(H037), C03B(H03G), C03C(H03H), C03G(H03K), C03I(H03N),
 C03X(H03), C042(H042), C04E(H04K), C04G(H04L), C04V(H04V), C04Y(H04Y),
 C051(H051), C059(H059), C05C(H05I), C05E(H05L), C05U(H05U), C06B(H06G),
 C06F(H06H), C20(H20), C43(H43), C58(H58), C60(H60), C74(H74), C81(H81),
 C84(H84), C98(H98), C99(H99), C108(H108), C109(H109), C28(H28), C29(H29),
 C32(H32), C44(H44), C52(H52), C67(H67), C6AA(H6AA), C4AA(H4AA), C94(H94),
 C103(H103), C42(H42), C54(H54)
4.b Secondary CH2 refined with riding coordinates:
 C018(H01A,H01B), C01A(H01C,H01D), C01B(H01E,H01F), C01I(H01G,H01H), C01K(H01I,
 H01J), C01M(H01K,H01L), C01O(H01M,H01N), C01Q(H01O,H01P), C01R(H01Q,H01R),
 C01S(H01S,H01T), C01U(H01U,H01V), C01V(H01W,H01X), C01W(H01Y,H), C020(H02A,
 H02B), C022(H02C,H02D), C023(H02E,H02F), C028(H02G,H02H), C02D(H02I,H02J),
 C02L(H02K,H02L), C02S(H02N,H02O), C02U(H02P,H02Q), C02W(H02S,H02T), C031(H03A,
 H03B), C034(H03C,H03D), C035(H03E,H03F), C03D(H03I,H03J), C03H(H03L,H03M),
 C03J(H03O,H03P), C03K(H03Q,H03R), C03M(H03S,H03T), C03P(H03U,H03V), C03R(H03W,
 H03X), C03T(H03Y,HA), C03V(H03Z,HB), C040(H04A,H04B), C045(H04C,H04D),
 C046(H04E,H04F), C04C(H04G,H04H), C04D(H04I,H04J), C04J(H04M,H04N), C04S(H04O,
 H04P), C04T(H04Q,H04R), C04U(H04S,H04T), C053(H05A,H05B), C058(H05C,H05D),
 C05A(H05E,H05F), C05B(H05G,H05H), C05D(H05J,H05K), C05G(H05M,H05N), C05N(H05O,
 H05P), C05Y(H05Q,H05R), C05Z(H05S,H05T), C061(H06A,H06B), C062(H06C,H06D),
 C066(H06E,H06F), C06H(H06I,H06J), C18(H18A,H18B), C0AA(H0AA,H0AB), C26(H26A,
 H26B), C31(H31A,H31B), C36(H36A,H36B), C48(H48A,H48B), C56(H56A,H56B),
 C63(H63A,H63B), C66(H66A,H66B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C73(H73A,H73B), C85(H85A,H85B), C86(H86A,H86B), C92(H92A,H92B), C116(H11A,
 H11B), C126(H12A,H12B), C128(H12C,H12D), C133(H13A,H13B), C136(H13C,H13D),
 C163(H16A,H16B), C198(H19A,H19B), C17(H17A,H17B), C37(H37A,H37B), C47(H47A,
 H47B), C2AA(H2AA,H2AB), C65(H65A,H65B), C71(H71A,H71B), C72(H72A,H72B),
 C1AA(H1AA,H1AB), C100(H10A,H10B), C191(H19C,H19D), C7AA(H7AA,H7AB), C34(H34A,
 H34B), C41(H41A,H41B), C9AA(H9AA,H9AB), C8AA(H8AA,H8AB), C55(H55A,H55B),
 C0BA(H0BA,H0BB)
;
_shelx_res_checksum              91019
_shelx_fab_checksum              90399
_olex2_submission_special_instructions 'No special instructions were received'