Total Structure and Electronic Structure Analysis of Doped Thiolated Silver [MAg24(SR)18](2-) (M = Pd, Pt) Clusters.
Yan, Juanzhu; Su, Haifeng; Yang, Huayan; Malola, Sami; Lin, Shuichao; Häkkinen, Hannu; Zheng, Nanfeng; Journal of the American Chemical Society 137 (2015) 11880–11883; doi:10.1021/jacs.5b07186

data_4129502
_publ_section_title
;
 Total Structure and Electronic Structure Analysis of Doped Thiolated
 Silver [MAg24(SR)18](2-) (M = Pd, Pt) Clusters.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11880
_journal_page_last               11883
_journal_paper_doi               10.1021/jacs.5b07186
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'Ag24 C109 Cl35.76 Pd S18, 2(C24 P)'
_chemical_formula_sum            'C157 Ag24 Cl35.76 P2 Pd S18'
_chemical_formula_weight         6487.44
_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'
_audit_creation_date             2015-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.989(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.2277(11)
_cell_length_b                   20.7963(5)
_cell_length_c                   32.7397(11)
_cell_measurement_reflns_used    15052
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      65.7180
_cell_measurement_theta_min      3.6920
_cell_volume                     19977.5(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.4741
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            74676
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.848
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    25.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             12167
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         3.019
_refine_diff_density_min         -2.943
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2196
_refine_ls_number_reflns         33799
_refine_ls_number_restraints     543
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+24.3279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23679
_reflns_number_total             33799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07186_si_002.cif
_cod_data_source_block           (PPh4)2[PdAg24(SPhCl2)18]
_cod_original_cell_volume        19977.4(13)
_cod_database_code               4129502
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Restrained distances
 C5-C16 \\sim C5B-C14 \\sim C6-C21
 with sigma of 0.01
2. Rigid bond restraints
 Cl1L, Cl1K, Cl12, Cl1I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1P, Cl1D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C06H \\sim C062 \\sim C05N \\sim C06K \\sim C05R \\sim C06N: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C06P \\sim C032 \\sim C06A \\sim C06D \\sim C06F \\sim C06I: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C5B \\sim C14 \\sim C6A \\sim C21 \\sim C16: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C15A \\sim C6A \\sim C14A \\sim C21A \\sim C3A \\sim C16A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Cl2 \\sim C5: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Cl7A \\sim Cl6 \\sim C14 \\sim C5B \\sim C6A \\sim C21 \\sim C6 \\sim C21A
\\sim C16 \\sim C3A \\sim C16A \\sim C15A \\sim C14A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C20 \\sim C3AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C13 \\sim C10 \\sim C3AA \\sim C20 \\sim C0AA \\sim C17: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C3AA \\sim C10 \\sim C13 \\sim C17 \\sim C0AA \\sim C20: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim C06G \\sim C06J \\sim C06Q \\sim C0 \\sim C06B: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C06F \\sim C06D \\sim C06A \\sim Cl1I \\sim Cl1K \\sim C032 \\sim C06P \\sim
C06I \\sim Cl12 \\sim Cl1L \\sim C06J \\sim C06G \\sim C1 \\sim C0 \\sim C06B
\\sim C06Q: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl6 \\sim Cl1 \\sim Cl7 \\sim Cl7A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C06H \\sim C062 \\sim C06N \\sim C05R \\sim C06K \\sim C05N: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Cl2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl7A) \\sim Ueq, Uanis(Cl1P) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C17) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C3AA)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl4C) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl4C) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C030) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl4B) = Uanis(Cl4C)
Uanis(C3A) = Uanis(C5)
Uanis(C06I) = Uanis(C5) = Uanis(C3A)
Uanis(Cl1P) = Uanis(Cl1Q)
Uanis(C04T) = Uanis(C030)
4. Others
 Sof(C06A)=Sof(C032)=Sof(C06P)=Sof(C06I)=Sof(C06F)=FVAR(1)
 Sof(Cl3)=1-FVAR(2)
 Sof(Cl1D)=FVAR(2)
 Fixed Sof: Cl1I(0.5) Cl1K(0.5) Cl4B(0.75) Cl6(0.5) Cl7A(0.5) C16(0.5)
 C5B(0.5) C14(0.5) C21(0.5) C6(0.5) C16A(0.5) C3A(0.5) C21A(0.5) C6A(0.5)
 C14A(0.5) C15A(0.5) Cl7(0.5) Cl12(0.5) Cl1P(0.75) Cl1L(0.5) C06J(0.5)
 C06G(0.5) C1(0.5) C0(0.5) C06B(0.5) C06Q(0.5) Cl1(0.5) Cl1Q(0.25) Cl4C(0.25)
5.a Fitted hexagon refined as free rotating group:
 C06D(C06A,C032,C06P,C06I,C06F), C056(C05O,C065,C06E,C06O,C06X), C05N(C062,
 C06H,C06N,C05R,C06K), C5(C16,C5B,C14,C21,C6), C3AA(C10,C13,C17,C0AA,C20),
 C16A(C3A,C21A,C6A,C14A,C15A), C06J(C06G,C1,C0,C06B,C06Q)
;
_olex2_submission_special_instructions 'No special instructions were received'