Unusual fcc-Structured Ag10 Kernel Trapped in Ag70 Nanocluster
SU, Yanmin; Wang, Zhi; Zhuang, Gui-lin; Zhao, Quanqin; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Chemical Science  (2019) –; doi:10.1039/C8SC03396J

data_1550045
_publ_section_title
;
 Unusual fcc-Structured Ag10 Kernel Trapped in Ag70 Nanocluster
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03396J
_journal_year                    2019
_chemical_formula_moiety
'C248 H438 Ag80 F42 Mo16 N6 O108 S50, 2(C F3 O3 S), 4(C3 H8 O), 2(C3 H7 N O)'
_chemical_formula_sum            'C268 H484 Ag80 F48 Mo16 N8 O120 S52'
_chemical_formula_weight         18482.36
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.675(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.1615(4)
_cell_length_b                   30.4928(5)
_cell_length_c                   32.0095(9)
_cell_measurement_reflns_used    49716
_cell_measurement_temperature    83.0(6)
_cell_measurement_theta_max      30.0790
_cell_measurement_theta_min      3.3200
_cell_volume                     24557.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      83.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      8.00  43.00   1.00   40.00    --    5.49-110.00-105.00   35
  2  \w    -26.00  37.00   1.00   40.00    --    5.49 -99.00  60.00   63
  3  \w    -56.00  15.00   1.00   40.00    --    5.49 -37.00 -90.00   71
  4  \w    -68.00  16.00   1.00   40.00    --    5.49 -19.00 -30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041768000
_diffrn_orient_matrix_UB_12      -0.0121583000
_diffrn_orient_matrix_UB_13      0.0185739000
_diffrn_orient_matrix_UB_21      0.0042946000
_diffrn_orient_matrix_UB_22      0.0192290000
_diffrn_orient_matrix_UB_23      0.0120316000
_diffrn_orient_matrix_UB_31      -0.0275492000
_diffrn_orient_matrix_UB_32      0.0048321000
_diffrn_orient_matrix_UB_33      -0.0011989000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            176090
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_description       block
_exptl_crystal_F_000             17608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.761
_refine_diff_density_min         -3.248
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2666
_refine_ls_number_reflns         43585
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1056.4679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31774
_reflns_number_total             43585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03396j2.cif
_cod_data_source_block           Ag80a
_cod_database_code               1550045
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         AgSCHOF
_diffrn_oxdiff_ac3_digest_frames
;
01903805ba5f226dec90e013539c457cb800253ad4f
;
_diffrn_oxdiff_ac3_digest_hkl
;
0175b20335b7343241851190fd216f985c1827
;
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C128-F13
 1.45 with sigma of 0.01
 C128-F15
 1.45 with sigma of 0.01
 C128-F14
 1.45 with sigma of 0.01
 F15-F13
 2.35 with sigma of 0.01
 F14-F15
 2.35 with sigma of 0.01
 F13-F14
 2.35 with sigma of 0.01
 S3-O17
 1.45 with sigma of 0.01
 O18-S3
 1.45 with sigma of 0.01
 S3-O16
 1.45 with sigma of 0.01
 O18-O17
 2.35 with sigma of 0.01
 O18-O16
 2.35 with sigma of 0.01
 O16-O17
 2.35 with sigma of 0.01
 O2A-S1
 1.45 with sigma of 0.01
 O3-S1
 1.45 with sigma of 0.01
 S1-O1
 1.45 with sigma of 0.01
 O3-O2A
 2.35 with sigma of 0.01
 O3-O1
 2.35 with sigma of 0.01
 O2A-O1
 2.35 with sigma of 0.01
 C115-N2
 1.55 with sigma of 0.01
 N2-C116
 1.55 with sigma of 0.01
 C117-N2
 1.55 with sigma of 0.01
 C117-O32
 1.25 with sigma of 0.01
 F3-C129
 1.45 with sigma of 0.01
 F1A-C129
 1.45 with sigma of 0.01
 C129-F2A
 1.45 with sigma of 0.01
 F3-F2A
 2.35 with sigma of 0.01
 F3-F1A
 2.35 with sigma of 0.01
 F1A-F2A
 2.35 with sigma of 0.01
 C120-N4
 1.45 with sigma of 0.01
 C27-C29
 1.55 with sigma of 0.01
3. Restrained planarity
 O32, N2, C115, C116, C117
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
S3 \\sim F13 \\sim F14 \\sim F15 \\sim O16 \\sim O17 \\sim O18 \\sim C128:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
O32 \\sim N2 \\sim C115 \\sim C116 \\sim C117: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
Ag1 \\sim Ag1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
O2 \\sim O2A \\sim C128: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
F1A \\sim F2A \\sim F3: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
S1 \\sim F1A \\sim F2A \\sim F3 \\sim O1 \\sim O2A \\sim O3 \\sim C129: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: Ag1(0.92) Ag1A(0.08) S1(0.5) S1A(0.5) F1(0.5) F1A(0.5) F2(0.5)
 F2A(0.5) O1(0.5) O1A(0.5) O2(0.5) O2A(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C26(H26), C31(H31), C37(H37), C43(H43),
 C49(H49), C55(H55), C62(H62), C67(H67), C73(H73), C79(H79), C85(H85), C91(H91),
  C97(H97), C103(H103)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,
 H76B), C77(H77A,H77B), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C86(H86A,H86B), C87(H87A,H87B),
  C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C92(H92A,H92B), C93(H93A,
 H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C98(H98A,H98B),
 C99(H99A,H99B), C100(H10C,H10D), C101(H10E,H10F), C102(H10G,H10H), C104(H10I,
 H10J), C105(H10K,H10L), C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R),
 C122(H12I,H12J), C123(H12K,H12L), C125(H12P,H12Q), C126(H12R,H12S)
6.c Aromatic/amide H refined with riding coordinates:
 C111(H111), C112(H112), C118(H118), C117(H117)
6.d Idealised Me refined as rotating group:
 C109(H10S,H10T,H10U), C110(H11C,H11D,H11E), C113(H11F,H11G,H11H), C114(H11I,
 H11J,H11K), C119(H11L,H11M,H11N), C120(H12C,H12D,H12E), C121(H12F,H12G,H12H),
 C124(H12M,H12N,H12O), C115(H11O,H11P,H11Q), C116(H11R,H11S,H11T)
6.e Idealised tetrahedral OH refined as rotating group:
 O29(H29), O30(H30)
;
_shelx_res_checksum              16407
_shelx_fab_checksum              75188
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.801