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_4129501
_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         'C108 H54 Ag24 Cl36 Pt S18, 2(C24 H20 P)'
_chemical_formula_sum            'C156 H94 Ag24 Cl36 P2 Pt S18'
_chemical_formula_weight         6667.50
_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     direct
_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                 117.948(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.2645(19)
_cell_length_b                   20.7713(9)
_cell_length_c                   32.7632(19)
_cell_measurement_reflns_used    10610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.2360
_cell_measurement_theta_min      3.6500
_cell_volume                     19997(2)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.967
_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  0.0733
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            72410
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.859
_diffrn_reflns_theta_min         3.406
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    26.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33698
_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            black
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             12664
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         4.880
_refine_diff_density_min         -2.841
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2089
_refine_ls_number_reflns         33599
_refine_ls_number_restraints     1418
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1114P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20502
_reflns_number_total             33599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07186_si_003.cif
_cod_data_source_block           (PPh4)2[PtAg24(SPhCl2)18]
_cod_database_code               4129501
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C160-S16
 1.7 with sigma of 0.02
 C160-S16
 1.7 with sigma of 0.02
 C163-Cl1
 1.7 with sigma of 0.02
 Cl19-C163
 1.7 with sigma of 0.02
 C160-S16
 1.7 with sigma of 0.02
 C165-S16
 2.8 with sigma of 0.04
 C161-S16
 2.8 with sigma of 0.04
 C163-S16
 4.4 with sigma of 0.04
 C165-S16
 2.8 with sigma of 0.04
 S16-C161
 2.8 with sigma of 0.04
 C163-S16
 4.3 with sigma of 0.04
 S16-C161
 2.8 with sigma of 0.04
 S16-C165
 2.8 with sigma of 0.04
 S16-C163
 4.4 with sigma of 0.04
3. Rigid bond restraints
 Cl1G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C165, C164, C163, C162, C161, C160
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1G, Cl1, Cl19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C160) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1G) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1G) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl19) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1G) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl16) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C150) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C154) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C16) = Uanis(C5)
5. Others
 Fixed Sof: Cl19(0.5) Cl1(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C65(H65), C7AA(H7AA), C155(H155), C154(H154), C152(H152), C64(H64),
 C195(H195), C191(H191), C95(H95), C45(H45), C02V(H02V), C115(H115), C2AA(H2AA),
  C213(H213), C75(H75), C5AA(H5AA), C135(H135), C03C(H03C), C215(H215),
 C03E(H03E), C203(H203), C193(H193), C55(H55), C201(H201), C92(H92), C03N(H03N),
  C03O(H03O), C03S(H03S), C54(H54), C223(H223), C125(H125), C35(H35),
 C194(H194), C1AA(H1AA), C047(H047), C049(H049), C192(H192), C04B(H04B),
 C214(H214), C185(H185), C114(H114), C122(H122), C212(H212), C42(H42),
 C132(H132), C124(H124), C94(H94), C04T(H04T), C182(H182), C144(H144),
 C222(H222), C145(H145), C202(H202), C72(H72), C221(H221), C052(H052),
 C053(H053), C225(H225), C85(H85), C34(H34), C211(H211), C162(H162), C164(H164),
  C165(H165), C059(H059), C204(H204), C134(H134), C184(H184), C205(H205),
 C224(H224), C84(H84), C05N(H05N), C44(H44), C32(H32), C82(H82), C05W(H05W),
 C05X(H05X), C74(H74), C05Z(H05Z), C142(H142), C063(H063), C112(H112),
 C066(H066), C068(H068), C069(H069), C52(H52), C06I(H06I), C06Q(H06Q), C10(H10),
  C12(H12), C14(H14), C8(H8), C16(H16), C5(H5)
6.b Fitted hexagon refined as free rotating group:
 C151(C150,C155,C154,C153,C152), C160(C161,C162,C163,C164,C165), C6(C10,C12,
 C13,C14,C15), C8(C17,C16,C5,C20,C19)
;
_olex2_submission_special_instructions 'No special instructions were received'