All-thiolate-stabilized Ag<sub>42</sub> nanocluster with a tetrahedral kernel and its transformation to an Ag<sub>61</sub> nanocluster with a bi-tetrahedral kernel.
Chen, Tao; Yang, Sha; Song, Yongbo; Chai, Jinsong; Li, Qinzhen; Ma, Xiangyu; Li, Guang; Yu, Haizhu; Zhu, Manzhou; Chemical communications (Cambridge, England) 56 (2020) 7605–7608; doi:10.1039/d0cc02537b

data_7126630
_publ_section_title
;
 All-thiolate-stabilized Ag<sub>42</sub> nanocluster with a tetrahedral
 kernel and its transformation to an Ag<sub>61</sub> nanocluster with a
 bi-tetrahedral kernel.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7605
_journal_page_last               7608
_journal_paper_doi               10.1039/d0cc02537b
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '2(C24 H54 Ag10.5 S6), 2.5(C H2 Cl2)'
_chemical_formula_sum            'C50.5 H113 Ag21 Cl5 S12'
_chemical_formula_weight         3547.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           16
_space_group_name_Hall           'P 2 2'
_space_group_name_H-M_alt        'P 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2020-01-13 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.018(2)
_cell_length_b                   19.679(2)
_cell_length_c                   26.250(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.28
_cell_volume                     9824.2(18)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         0.776
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.494
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.7549.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.399
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_refine_diff_density_max         3.463
_refine_diff_density_min         -4.237
_refine_diff_density_rms         0.377
_refine_ls_abs_structure_details
;
 Flack x determined using 5918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         19208
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+540.3754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2415
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                14975
_reflns_number_total             19208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02537b2.cif
_cod_data_source_block           20161015b_0m
_cod_depositor_comments
'Adding full bibliography for 7126630--7126631.cif.'
_cod_original_formula_sum        'C50.50 H113 Ag21 Cl5 S12'
_cod_database_code               7126630
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
C45 \\sim C48 \\sim C48': within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C23') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C48') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: S3(0.5) S3'(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C23'(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) S12(0.5) S12'(0.5) C48(0.5) H48A(0.5) H48B(0.5)
 H48C(0.5) C48'(0.5) H48D(0.5) H48E(0.5) H48F(0.5) H51A(0.5) H51B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C23'(H23D,H23E,H23F), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C48'(H48D,H48E,H48F)
;
_shelx_fab_checksum              45857
_olex2_submission_special_instructions 'No special instructions were received'