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_1550046
_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
'C139 H287 Ag80 F48 Mo16 N5 O113 S52, C3 H7 N O'
_chemical_formula_sum            'C142 H294 Ag80 F48 Mo16 N6 O114 S52'
_chemical_formula_weight         16653.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                111.8795(11)
_cell_angle_beta                 109.2284(11)
_cell_angle_gamma                92.0299(10)
_cell_formula_units_Z            1
_cell_length_a                   21.9533(3)
_cell_length_b                   22.1690(3)
_cell_length_c                   22.9990(3)
_cell_measurement_reflns_used    51456
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1730
_cell_measurement_theta_min      3.3520
_cell_volume                     9646.4(3)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -67.00  27.00   0.50    7.00    --    8.83 -37.00 -60.00  188
  2  \w    -19.00  69.00   0.50    7.00    --   -7.73  37.00-155.00  176
  3  \w    -26.00  30.00   0.50    7.00    --   -7.73 -99.00  30.00  112
  4  \w    -26.00  46.00   0.50    7.00    --    8.83 -99.00  60.00  144
  5  \w    -83.00  11.00   0.50    7.00    --   -7.73 -37.00  48.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0097503000
_diffrn_orient_matrix_UB_12      -0.0310779000
_diffrn_orient_matrix_UB_13      -0.0048736000
_diffrn_orient_matrix_UB_21      -0.0130877000
_diffrn_orient_matrix_UB_22      -0.0096054000
_diffrn_orient_matrix_UB_23      -0.0353521000
_diffrn_orient_matrix_UB_31      0.0306754000
_diffrn_orient_matrix_UB_32      0.0129339000
_diffrn_orient_matrix_UB_33      0.0014056000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100166
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54318
_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    2.867
_exptl_crystal_description       block
_exptl_crystal_F_000             7796
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.071
_refine_diff_density_min         -2.423
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2248
_refine_ls_number_reflns         34057
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+73.3388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27886
_reflns_number_total             34057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03396j2.cif
_cod_data_source_block           Ag80b
_cod_original_cell_volume        9646.4(2)
_cod_database_code               1550046
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         AgS
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F16-C63
 1.45 with sigma of 0.01
 C63-F18
 1.45 with sigma of 0.01
 C63-F17
 1.45 with sigma of 0.01
 F17-F16
 2.35 with sigma of 0.01
 F16-F18
 2.35 with sigma of 0.01
 F18-F17
 2.35 with sigma of 0.01
 C4A-C5A
 2.35 with sigma of 0.01
 C6A-N3A = N3A-C4A
 1.45 with sigma of 0.01
 N3A-C5A
 1.45 with sigma of 0.01
 C6A-N3A
 1.45 with sigma of 0.01
 C12-C11
 1.55 with sigma of 0.01
 C11-C10
 1.55 with sigma of 0.01
 C12-C10
 2.35 with sigma of 0.01
 S23-C65
 1.85 with sigma of 0.01
 N3-C4
 1.45 with sigma of 0.01
 N3-C6
 1.45 with sigma of 0.01
 C44-C45
 1.55 with sigma of 0.01
 C44-C43
 1.55 with sigma of 0.01
 C43-C45
 2.35 with sigma of 0.01
 C50-C51
 1.55 with sigma of 0.01
 C51-C50
 1.55 with sigma of 0.01
 C50-C49
 1.55 with sigma of 0.01
 C51-C49
 2.35 with sigma of 0.01
 S8-C50
 1.85 with sigma of 0.01
 S8-C51
 2.75 with sigma of 0.01
 C49-S8
 2.75 with sigma of 0.01
 C65-F22
 1.45 with sigma of 0.01
 F23-C65
 1.45 with sigma of 0.01
 C65-F24
 1.45 with sigma of 0.01
 S23-F23
 2.75 with sigma of 0.01
 S23-F24
 2.75 with sigma of 0.01
 S23-F22
 2.75 with sigma of 0.01
 F23-F24
 2.35 with sigma of 0.01
 F23-F22
 2.35 with sigma of 0.01
 F22-F24
 2.35 with sigma of 0.01
 C69-N1
 1.45 with sigma of 0.01
 C26-C25
 1.55 with sigma of 0.01
 C27-C26
 1.55 with sigma of 0.01
 C25-C27
 2.35 with sigma of 0.01
 O47-S24
 1.45 with sigma of 0.01
3. Restrained planarity
 C4A, C5A, C6A, N3A, O57A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C63 \\sim F16 \\sim F17 \\sim F18 \\sim O49 \\sim O50 \\sim O51 \\sim S26:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C4 \\sim C5 \\sim C6 \\sim N3 \\sim O57: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C4A \\sim C5A \\sim C6A \\sim N3A \\sim O57A: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
C64 \\sim F13 \\sim F14 \\sim F15 \\sim O46 \\sim O47 \\sim O48 \\sim S24:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C1A \\sim C2A \\sim C3A \\sim N2A \\sim O56A: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
Ag2 \\sim Ag2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
Ag6 \\sim Ag6A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
Ag5 \\sim Ag5A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Ag7 \\sim Ag7A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Ag4 \\sim Ag4A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C65 \\sim F22 \\sim F23 \\sim F24 \\sim O52 \\sim O53 \\sim S23: within 1.7A
with sigma of 0.002 and sigma for terminal atoms of 0.004
S23: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C55 \\sim C56 \\sim C57 \\sim S5: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
C43 \\sim C44 \\sim C45 \\sim S6: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C10 \\sim C11 \\sim C12 \\sim S10: within 1.7A with sigma of 0.002 and sigma
for terminal atoms of 0.004
C68 \\sim C69 \\sim C70 \\sim N1 \\sim O55: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.08
C49 \\sim C50 \\sim C51 \\sim S8: within 1.7A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C1 \\sim C2 \\sim C3 \\sim N2 \\sim O56: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.004
C25 \\sim C26 \\sim C27 \\sim S13: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C0AA \\sim F10 \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim O31 \\sim O31A
\\sim O32 \\sim O33 \\sim S1 \\sim S1A: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
S1A \\sim S1 \\sim O32A \\sim O32 \\sim O31 \\sim O31A \\sim F10 \\sim F10A
\\sim F12A \\sim C0AA \\sim F11A \\sim F11 \\sim F12 \\sim O33 \\sim O33A:
within 1.7A with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(Ag2A)=1-FVAR(1)
 Sof(Ag2)=FVAR(1)
 Sof(Ag3A)=1-FVAR(2)
 Sof(Ag3)=FVAR(2)
 Sof(Ag5A)=Sof(Ag6A)=1-FVAR(3)
 Sof(Ag5)=Sof(Ag6)=FVAR(3)
 Sof(Ag1A)=1-FVAR(4)
 Sof(Ag1)=FVAR(4)
 Sof(Ag7A)=1-FVAR(5)
 Sof(Ag7)=FVAR(5)
 Sof(Ag4A)=1-FVAR(6)
 Sof(Ag4)=FVAR(6)
 Sof(S1A)=1-FVAR(7)
 Sof(S1)=FVAR(7)
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5)
 H2AC(0.5) C3(0.5) H3(0.5) C3A(0.5) H3A(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
 C5A(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) C6(0.5) H6(0.5) C6A(0.5) H6A(0.5)
 F10(0.5) F11(0.5) F11A(0.5) F12(0.6) F12A(0.4) N2(0.5) N2A(0.5) N3(0.5)
 N3A(0.5) O31(0.6) O31A(0.4) O32(0.5) O33(0.5) O56(0.5) O56A(0.5) O57(0.5)
 O57A(0.5) O32A(0.5) O33A(0.5) F10A(0.5)
6.a Riding coordinates:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC),
 C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC),
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C)
6.b Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C20(H20), C23(H23), C26(H26), C29(H29),
 C32(H32), C35(H35), C38(H38), C41(H41), C44(H44), C47(H47), C50(H50), C53(H53),
  C56(H56), C59(H59)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C6(H6), C6A(H6A), C70(H70)
6.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              62139
_shelx_fab_checksum              39661
_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 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.723