Alkynyl-protected silver nanoclusters featuring an anticuboctahedral kernel
Yuan, Shang-Fu; Li, Pei; Tang, Qing; Wan, Xian-Kai; Nan, Zi-Ang; Jiang, De-en; Wang, Quan-Ming; Nanoscale  (2017) –; doi:10.1039/C7NR02687K

data_1546259
_publ_section_title
;
 Alkynyl-protected silver nanoclusters featuring an anticuboctahedral
 kernel
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR02687K
_journal_year                    2017
_chemical_formula_moiety         '6(F6 Sb), 2(Ag25 C267 O20 P6), 2(C Cl2)'
_chemical_formula_sum            'C536 H464 Ag50 Cl4 F36 O40 P12 Sb6'
_chemical_formula_weight         14866.48
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-15 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6041(2)
_cell_length_b                   34.2294(2)
_cell_length_c                   57.2156(5)
_cell_measurement_reflns_used    50575
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.9970
_cell_measurement_theta_min      3.5690
_cell_volume                     52053.0(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            183334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        60.000
_diffrn_reflns_theta_max         60.000
_diffrn_reflns_theta_min         3.471
_exptl_absorpt_coefficient_mu    18.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47444
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brownish-red
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_description       block
_exptl_crystal_F_000             28912
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         9.229
_refine_diff_density_min         -14.777
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3333
_refine_ls_number_reflns         77220
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.1156
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+3587.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2645
_refine_ls_wR_factor_ref         0.2840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                55541
_reflns_number_total             77220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr02687k2.cif
_cod_data_source_block           p
_cod_database_code               1546259
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 O37A-C2O
 1.45 with sigma of 0.01
 C2P-O37A
 2.55 with sigma of 0.01
 O37A-C2N
 2.55 with sigma of 0.01
 C1EB-C734
 1.39 with sigma of 0.02
 C2J-C2E
 1.39 with sigma of 0.02
 C2I-C2H
 1.39 with sigma of 0.02
 O35A-C2H
 1.45 with sigma of 0.02
 O35A-C2K
 1.45 with sigma of 0.02
 C614-C613
 1.39 with sigma of 0.02
 C709-O36
 1.45 with sigma of 0.02
 C707-C709
 2.55 with sigma of 0.02
 C709-C707
 2.55 with sigma of 0.02
 O36-C706
 1.4 with sigma of 0.02
 O36-C709
 1.45 with sigma of 0.02
 C706-C709
 2.55 with sigma of 0.02
 O39A-C2U
 1.4 with sigma of 0.02
 C2V-O39A
 2.54 with sigma of 0.02
 O39A-C2T
 2.54 with sigma of 0.02
 F34-Sb6
 1.99 with sigma of 0.02
 F31-Sb6
 1.99 with sigma of 0.02
 F36-Sb6
 1.99 with sigma of 0.02
 Sb6-F33
 1.99 with sigma of 0.02
 Sb6-F32
 1.99 with sigma of 0.02
 F35-Sb6
 1.99 with sigma of 0.02
 F34-F33
 3.98 with sigma of 0.02
 F31-F32
 3.98 with sigma of 0.02
 F36-F35
 3.98 with sigma of 0.02
 F34-F32
 2.81 with sigma of 0.02
 F34-F31
 2.81 with sigma of 0.02
 F34-F36
 2.81 with sigma of 0.02
 F34-F35
 2.81 with sigma of 0.02
 F33-F32
 2.81 with sigma of 0.02
 F33-F35
 2.81 with sigma of 0.02
 F33-F31
 2.81 with sigma of 0.02
 F33-F36
 2.81 with sigma of 0.02
 F36-F32
 2.81 with sigma of 0.02
 F32-F35
 2.81 with sigma of 0.02
 F35-F31
 2.81 with sigma of 0.02
 F31-F36
 2.81 with sigma of 0.02
 Sb6A-F36A
 1.99 with sigma of 0.02
 Sb6A-F33A
 1.99 with sigma of 0.02
 Sb6A-F34A
 1.99 with sigma of 0.02
 Sb6A-F31A
 1.99 with sigma of 0.02
 Sb6A-F32A
 1.99 with sigma of 0.02
 Sb6A-F35A
 1.99 with sigma of 0.02
 F35A-F34A
 2.81 with sigma of 0.02
 F35A-F32A
 2.81 with sigma of 0.02
 F35A-F33A
 2.81 with sigma of 0.02
 F35A-F31A
 2.81 with sigma of 0.02
 F31A-F36A
 2.81 with sigma of 0.02
 F36A-F33A
 2.81 with sigma of 0.02
 F36A-F34A
 2.81 with sigma of 0.02
 F36A-F32A
 2.81 with sigma of 0.02
 F34A-F31A
 2.81 with sigma of 0.02
 F31A-F33A
 2.81 with sigma of 0.02
 F33A-F32A
 2.81 with sigma of 0.02
 F32A-F34A
 2.81 with sigma of 0.02
 F33A-F34A
 3.98 with sigma of 0.02
 F32A-F31A
 3.98 with sigma of 0.02
 F35A-F36A
 3.98 with sigma of 0.02
 Sb3A-F13A
 1.99 with sigma of 0.02
 Sb3A-F15A
 1.99 with sigma of 0.02
 Sb3A-F18A
 1.99 with sigma of 0.02
 Sb3A-F16A
 1.99 with sigma of 0.02
 Sb3A-F17A
 1.99 with sigma of 0.02
 F15A-F16A
 3.98 with sigma of 0.02
 F18-F17
 3.98 with sigma of 0.02
 F16-F15
 3.98 with sigma of 0.02
 F13A-F18A
 2.81 with sigma of 0.02
 F13A-F15A
 2.81 with sigma of 0.02
 F13A-F16A
 2.81 with sigma of 0.02
 F13A-F17A
 2.81 with sigma of 0.02
 Sb3A-F14A
 1.99 with sigma of 0.02
 F13A-F14A
 3.98 with sigma of 0.02
 F29A-F28A
 2.7 with sigma of 0.01
 F27A-F28A
 3.7 with sigma of 0.01
 F19A-F20A
 3.7 with sigma of 0.02
 F20A-F22A
 2.7 with sigma of 0.01
 F20A-F21A
 2.7 with sigma of 0.01
 F20A-F19A
 3.7 with sigma of 0.01
 F18A-F17A
 3.7 with sigma of 0.01
 F14A-F13A
 3.7 with sigma of 0.01
 F18A-F14A
 2.7 with sigma of 0.01
 F14A-F17A
 2.7 with sigma of 0.01
 F17A-F15A
 2.7 with sigma of 0.01
 F17A-F16A
 2.7 with sigma of 0.01
 F17A-F18A
 3.7 with sigma of 0.01
 F15-F16
 3.7 with sigma of 0.01
 F17-F18
 3.7 with sigma of 0.01
 Sb3-F16 = Sb3-F18 = Sb3-F13 = Sb3-F17 = Sb3-F14 = Sb3-F15
 1.85 with sigma of 0.01
 F15-F17
 2.7 with sigma of 0.01
 F17-F16
 2.7 with sigma of 0.01
 F16-F18
 2.7 with sigma of 0.01
 F15-F18
 2.7 with sigma of 0.01
 O34A-C2D
 1.45 with sigma of 0.01
 C2U-C737 \\sim C735-C2U \\sim C735-C734 \\sim C1EB-C734 \\sim C1EB-C738 \\sim
C737-C738
 with sigma of 0.02
 C2J-C2E \\sim C2F-C2E \\sim C2G-C2F \\sim C2G-C2H \\sim C2I-C2J
 with sigma of 0.02
 C612-C611 \\sim C611-C1K
 with sigma of 0.02
 O40-C749 \\sim O40A-C749
 with sigma of 0.02
 O40-C746 \\sim O40A-C33
 with sigma of 0.02
 O34A-C2D \\sim O34-C689
 with sigma of 0.02
2. Restrained planarity
 F13A, F14A, F17A, F18A
 with sigma of 0.1
3. Others
 Fixed Sof: Sb3(0.5) F13(0.5) F14(0.5) F15(0.5) F16(0.5) F17(0.5) F18(0.5)
 Sb3A(0.5) F13A(0.5) F14A(0.5) F15A(0.5) F16A(0.5) F17A(0.5) F18A(0.5)
 Sb4(0.6667) F19(0.6667) F20(0.6667) F21(0.6667) F22(0.6667) F23(0.6667)
 F24(0.6667) Sb4A(0.33333) F19A(0.33333) F20A(0.33333) F21A(0.33333)
 F22A(0.33333) F23A(0.33333) F24A(0.33333) Sb5(0.75) F25(0.75) F26(0.75)
 F27(0.75) F28(0.75) F29(0.75) F30(0.75) Sb5A(0.25) F25A(0.25) F26A(0.25)
 F27A(0.25) F28A(0.25) F29A(0.25) F30A(0.25) Sb6(0.5) F31(0.5) F32(0.5)
 F33(0.5) F34(0.5) F35(0.5) F36(0.5) Sb6A(0.5) F31A(0.5) F32A(0.5) F33A(0.5)
 F34A(0.5) F35A(0.5) F36A(0.5) O24(0.5) O24A(0.5) O25(0.5) O25A(0.5) O27(0.5)
 O27A(0.5) O28(0.5) O28A(0.5) O34(0.5) O34A(0.5) O35(0.5) O35A(0.5) O37(0.5)
 O37A(0.5) O39(0.5) O39A(0.5) O40(0.5) O40A(0.5) C1A(0.5) C1B(0.5) C1C(0.5)
 C1D(0.5) C1E(0.5) C1EB(0.5) C2S(0.5) C2T(0.5) C2U(0.5) C2V(0.5) C2W(0.5)
 C1F(0.5) C1G(0.5) C1H(0.5) C1I(0.5) C1J(0.5) C1K(0.5) C1L(0.5) C1Q(0.5)
 C1P(0.5) C1O(0.5) C1N(0.5) C1M(0.5) C1R(0.5) C1S(0.5) C1T(0.5) C1U(0.5)
 C1V(0.5) C1W(0.5) C1X(0.5) C1Y(0.5) C1Z(0.5) C2A(0.5) C2B(0.5) C2C(0.5)
 C2D(0.5) C2E(0.5) C2J(0.5) C2I(0.5) C2H(0.5) C2G(0.5) C2F(0.5) C2K(0.5)
 C2M(0.5) C2L(0.5) C2Q(0.5) C2P(0.5) C2O(0.5) C2N(0.5) C2R(0.5) C2X(0.5)
 C2Y(0.5) C2Z(0.5) C31(0.5) C32(0.5) C33(0.5) C34(0.5) C35(0.5) C586(0.5)
 C587(0.5) C588(0.5) C596(0.5) C595(0.5) C594(0.5) C593(0.5) C598(0.5)
 C597(0.5) C609(0.5) C612(0.5) C613(0.5) C618(0.5) C617(0.5) C616(0.5)
 C615(0.5) C614(0.5) C623(0.5) C624(0.5) C625(0.5) C626(0.5) C627(0.5)
 C628(0.5) C629(0.5) C683(0.5) C684(0.5) C685(0.5) C686(0.5) C687(0.5)
 C689(0.5) C693(0.5) C698(0.5) C697(0.5) C696(0.5) C695(0.5) C694(0.5)
 C699(0.5) C713(0.5) C714(0.5) C715(0.5) C716(0.5) C717(0.5) C718(0.5)
 C719(0.5) C733(0.5) C738(0.5) C737(0.5) C736(0.5) C735(0.5) C734(0.5)
 C741(0.5) C742(0.5) C743(0.5) C744(0.5) C745(0.5) C746(0.5) C747(0.5) C748(0.5)
4.a Fitted hexagon refined as free rotating group:
 C191(C192,C193,C194,C195,C196), C1EB(C2S,C2T,C2U,C2V,C2W), C1L(C1Q,C1P,C1O,
 C1N,C1M), C2E(C2J,C2I,C2H,C2G,C2F), C2M(C2L,C2Q,C2P,C2O,C2N), C451(C452,C453,
 C454,C455,C456), C596(C595,C594,C593,C598,C597), C613(C618,C617,C616,C615,
 C614), C673(C678,C677,C676,C675,C674), C693(C698,C697,C696,C695,C694),
 C707(C706,C705,C704,C703,C708), C733(C738,C737,C736,C735,C734)
;
_olex2_submission_special_instructions 'No special instructions were received'