Structural characterization and gas-phase studies of the [Ag10H8(L)6]2+ nanocluster dication
Ma, Howard Z.; McKay, Alasdair I.; Mravak, Antonija; Scholz, Michael S.; White, Jonathan M.; Mulder, Roger J.; Bieske, Evan J.; Bonačić-Koutecký, Vlasta; O'Hair, Richard A. J.; Nanoscale  (2019) –; doi:10.1039/C9NR08321A

data_1556091
_publ_section_title
;
 Structural characterization and gas-phase studies of the [Ag10H8(L)6]2+
 nanocluster dication
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C9NR08321A
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'0.25(C144 H126 Ag6 B2 Cl4 F8 N6 P12), 0.5(C72 H63 Ag3 Cl2 N3 P6), 0.5(B F4)'
_chemical_formula_sum            'C72 H63 Ag3 B Cl2 F4 N3 P6'
_chemical_formula_weight         1637.39
_chemical_name_systematic        '[Ag3Cl2(dppa)3](BF4)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5346(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9166(2)
_cell_length_b                   26.4450(4)
_cell_length_c                   19.7632(3)
_cell_measurement_reflns_used    63938
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.6830
_cell_measurement_theta_min      2.2990
_cell_volume                     7071.35(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.29a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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    -17.00  13.00   0.50    0.52    --   48.20 -31.00  63.00   60
  2  \w     34.00  59.00   0.50    0.52    --   48.20  56.00  -8.22   50
  3  \w     38.00  90.00   0.50    0.52    --   48.20  53.00  32.92  104
  4  \w     34.00  60.00   0.50    0.52    --   48.20  54.00  18.61   52
  5  \w     91.00 116.00   0.50    2.09    --  107.75  61.00 -60.00   50
  6  \w    100.00 127.00   0.50    2.09    --  107.75  45.00 -30.00   54
  7  \w    143.00 169.00   0.50    2.09    --  107.75  45.00 -30.00   52
  8  \w    149.00 175.00   0.50    2.09    --  107.75  61.00  30.00   52
  9  \w    133.00 173.00   0.50    2.09    --  107.75  15.00 -30.00   80
 10  \w    141.00 175.00   0.50    2.09    --  107.75  61.00 -90.00   68
 11  \w    124.00 158.00   0.50    2.09    --  107.75  31.00-136.00   68
 12  \w    135.00 178.00   0.50    2.09    --  107.75  61.00-180.00   86
 13  \w    123.00 149.00   0.50    2.09    --  107.75  77.00 -90.00   52
 14  \w    108.00 134.00   0.50    2.09    --  107.75  61.00-120.00   52
 15  \w    116.00 164.00   0.50    2.09    --  107.75  77.00-120.00   96
 16  \w     96.00 176.00   0.50    2.09    --  107.75  45.00 -60.00  160
 17  \w    115.00 141.00   0.50    2.09    --  107.75  15.00   0.00   52
 18  \w     97.00 138.00   0.50    2.09    --  107.75  45.00  30.00   82
 19  \w    101.00 151.00   0.50    2.09    --  107.75  45.00   0.00  100
 20  \w     96.00 136.00   0.50    2.09    --  107.75  45.00  60.00   80
 21  \w    153.00 178.00   0.50    2.09    --  107.75  61.00 120.00   50
 22  \w     99.00 166.00   0.50    2.09    --  107.75  15.00 120.00  134
 23  \w     91.00 133.00   0.50    2.09    --  107.75  61.00  30.00   84
 24  \w     91.00 116.00   0.50    2.09    --  107.75  61.00 -30.00   50
 25  \w     91.00 116.00   0.50    2.09    --  107.75  61.00 -90.00   50
 26  \w    102.00 178.00   0.50    2.09    --  107.75  77.00-150.00  152
 27  \w     95.00 166.00   0.50    2.09    --  107.75  47.00 -18.15  142
 28  \w     97.00 178.00   0.50    2.09    --  107.75 125.00  90.00  162
 29  \w    103.00 128.00   0.50    2.09    --  107.75  15.00 -30.00   50
 30  \w     92.00 135.00   0.50    2.09    --  107.75  61.00   0.00   86
 31  \w     98.00 129.00   0.50    2.09    --  107.75  61.00 120.00   62
 32  \w     39.00  69.00   0.50    2.09    --  107.75 -61.00   0.00   60
 33  \w     64.00 105.00   0.50    2.09    --  107.75 -94.00  60.00   82
 34  \w     83.00 116.00   0.50    2.09    --  107.75-125.00  60.00   66
 35  \w     60.00 107.00   0.50    2.09    --  107.75 -94.00 120.00   94
 36  \w     63.00  94.00   0.50    2.09    --  107.75-125.00 120.00   62
 37  \w     58.00  83.00   0.50    2.09    --  107.75 -94.00 150.00   50
 38  \w     57.00  82.00   0.50    2.09    --  107.75 -94.00  90.00   50
 39  \w     44.00  76.00   0.50    2.09    --  107.75-125.00  60.00   64
 40  \w     37.00  62.00   0.50    2.09    --  107.75 -94.00  60.00   50
 41  \w     40.00 109.00   0.50    2.09    --  107.75 -94.00   0.00  138
 42  \w     73.00 109.00   0.50    2.09    --  107.75 -94.00 -90.00   72
 43  \w     70.00  96.00   0.50    2.09    --  107.75 -94.00-180.00   52
 44  \w     38.00  68.00   0.50    2.09    --  107.75 -61.00 -90.00   60
 45  \w     39.00 109.00   0.50    2.09    --  107.75 -94.00-150.00  140
 46  \w     44.00  86.00   0.50    2.09    --  107.75 -94.00-120.00   84
 47  \w     36.00  65.00   0.50    2.09    --  107.75 -94.00-180.00   58
 48  \w     43.00  68.00   0.50    2.09    --  107.75 -61.00-120.00   50
 49  \w     45.00  70.00   0.50    2.09    --  107.75 -94.00 -30.00   50
 50  \w     37.00  63.00   0.50    2.09    --  107.75 -61.00  90.00   52
 51  \w     36.00  65.00   0.50    2.09    --  107.75 -61.00 120.00   58
 52  \w     36.00  68.00   0.50    2.09    --  107.75 -61.00 150.00   64
 53  \w     55.00  80.00   0.50    0.52    --   48.20  31.00-136.00   50
 54  \w     97.00 171.00   0.50    2.09    --  107.75  15.00-150.00  148
 55  \w    -21.00  27.00   0.50    0.52    --  -48.20  19.00 -60.00   96
 56  \w    -21.00  27.00   0.50    0.52    --  -48.20  19.00   0.00   96
 57  \w    -33.00  22.00   0.50    0.52    --  -48.20  31.00-136.00  110
 58  \w    -48.00 -20.00   0.50    2.09    --  -86.25  45.00  30.00   56
 59  \w    -18.00  20.00   0.50    0.52    --  -48.20  19.00 120.00   76
 60  \w    -67.00 -42.00   0.50    0.52    --  -48.20 -37.00 -60.00   50
 61  \w    -65.00 -39.00   0.50    0.52    --  -48.20 -37.00-120.00   52
 62  \w    -97.00 -72.00   0.50    2.09    --  -86.25 -54.00  -1.43   50
 63  \w    -97.00 -72.00   0.50    2.09    --  -86.25 -54.00 -11.27   50
 64  \w    -97.00 -72.00   0.50    2.09    --  -86.25 -55.00   3.59   50
 65  \w    -97.00 -72.00   0.50    2.09    --  -86.25 -54.00 -18.15   50
 66  \w   -100.00 -74.00   0.50    2.09    --  -86.25 -52.00 -80.73   52
 67  \w    -98.00 -72.00   0.50    2.09    --  -86.25 -53.00-104.52   52
 68  \w    -98.00 -72.00   0.50    2.09    --  -86.25 -52.00 -46.70   52
 69  \w    -98.00 -73.00   0.50    2.09    --  -86.25 -49.00 -16.40   50
 70  \w    -98.00 -73.00   0.50    2.09    --  -86.25 -54.00 -55.31   50
 71  \w    -99.00 -74.00   0.50    2.09    --  -86.25 -49.00-105.52   50
 72  \w    -98.00 -82.50   0.50    2.09    --  -86.25 -54.00 -69.79   31
;
_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      0.0546856000
_diffrn_orient_matrix_UB_12      0.0191809000
_diffrn_orient_matrix_UB_13      0.0723970000
_diffrn_orient_matrix_UB_21      0.0996568000
_diffrn_orient_matrix_UB_22      -0.0140651000
_diffrn_orient_matrix_UB_23      -0.0162484000
_diffrn_orient_matrix_UB_31      0.0066792000
_diffrn_orient_matrix_UB_32      0.0531581000
_diffrn_orient_matrix_UB_33      -0.0304292000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            132667
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.922
_diffrn_reflns_theta_min         2.299
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.29a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.612
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.051(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1744
_refine_ls_number_reflns         28371
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+15.1394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                26575
_reflns_number_total             28371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr08321a2.cif
_cod_data_source_block           aim047
_cod_original_cell_volume        7071.37(18)
_cod_database_code               1556091
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag3 P6 N3 Cl2 C72 B1 F4 H63 O0.5'
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.466
_diffrn_oxdiff_digest_frames
;
014a9ea5661e5889e86a3e098d2c403492051990389
;
_diffrn_oxdiff_digest_hkl
;
01aa94246a97d5b59b086512538fd1818c1723
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.949(9)
 0.051(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C17-C18 \\sim C18-C13 \\sim C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C17
 with sigma of 0.02
 C17-C15 \\sim C17-C15 \\sim C14-C18 \\sim C14-C16 \\sim C16-C18 \\sim C15-C13
 with sigma of 0.04
 C14A-C13A \\sim C13A-C18A \\sim C18A-C17A \\sim C17A-C16A \\sim C16A-C15A
\\sim C15A-C14A
 with sigma of 0.02
 C14A-C16A \\sim C14A-C16A \\sim C17A-C13A \\sim C17A-C15A \\sim C15A-C13A
\\sim C16A-C18A
 with sigma of 0.04
 C76-C75 \\sim C75-C74 \\sim C74-C73 \\sim C73-C78 \\sim C78-C77 \\sim C77-C76
 with sigma of 0.02
 C76-C78 \\sim C76-C78 \\sim C73-C75 \\sim C73-C77 \\sim C77-C75 \\sim C78-C74
 with sigma of 0.04
 C73A-C78A \\sim C78A-C77A \\sim C77A-C76A \\sim C76A-C75A \\sim C75A-C74A
\\sim C74A-C73A
 with sigma of 0.02
 C73A-C75A \\sim C73A-C75A \\sim C76A-C78A \\sim C76A-C74A \\sim C74A-C78A
\\sim C75A-C77A
 with sigma of 0.04
 C82-C81 \\sim C81-C80 \\sim C80-C79 \\sim C79-C84 \\sim C84-C83 \\sim C83-C82
 with sigma of 0.02
 C82-C84 \\sim C82-C84 \\sim C79-C81 \\sim C79-C83 \\sim C83-C81 \\sim C84-C80
 with sigma of 0.04
4. Restrained planarity
 C17, C18, C13, C14, C15, C16
 with sigma of 0.1
 C14A, C13A, C18A, C17A, C16A, C15A
 with sigma of 0.1
 C76, C75, C74, C73, C78, C77
 with sigma of 0.1
 C73A, C78A, C77A, C76A, C75A, C74A
 with sigma of 0.1
 C82, C81, C80, C79, C84, C83
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C14A \\sim C13A \\sim C18A \\sim C17A \\sim C16A \\sim C15A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C76 \\sim C75 \\sim C74 \\sim C73 \\sim C78 \\sim C77: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C73A \\sim C78A \\sim C77A \\sim C76A \\sim C75A \\sim C74A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C82 \\sim C81 \\sim C80 \\sim C79 \\sim C84 \\sim C83: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C13) = Uanis(C13A)
6. Rigid body (RIGU) restrains
 C17, C18, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C14A, C13A, C18A, C17A, C16A, C15A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C76, C75, C74, C73, C78, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73A, C78A, C77A, C76A, C75A, C74A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C82, C81, C80, C79, C84, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C14A)=Sof(H14A)=Sof(C13A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=
 Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=1-FVAR(1)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(C73A)=Sof(C78A)=Sof(H78A)=Sof(C77A)=Sof(H77A)=Sof(C76A)=Sof(H76A)=
 Sof(C75A)=Sof(H75A)=Sof(C74A)=Sof(H74A)=1-FVAR(2)
 Sof(C76)=Sof(H76)=Sof(C75)=Sof(H75)=Sof(C74)=Sof(H74)=Sof(C73)=Sof(C78)=
 Sof(H78)=Sof(C77)=Sof(H77)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C126(H126), N1(H1), C10(H10), C24(H24), C98(H98), C110(H110),
 C136(H136), C69(H69), C129(H129), C111(H111), C8(H8), N4(H4), C12(H12),
 C128(H128), C125(H125), C122(H122), C23(H23), C9(H9), C40(H40), C116(H116),
 C63(H63), N2(H2), C112(H112), C50(H50), C54(H54), C42(H42), C114(H114),
 C36(H36), C46(H46), C62(H62), N6(H6), C44(H44), C92(H92), C68(H68), C48(H48),
 C20(H20), C22(H22), C123(H123), C56(H56), C66(H66), C86(H86), C117(H117),
 C104(H104), C64(H64), C93(H93), C131(H131), C30(H30), C130(H130), N3(H3),
 C6(H6A), C113(H113), C100(H100), C65(H65), C41(H41), C11(H11), C135(H135),
 C51(H51), C143(H143), C28(H28), C144(H144), C57(H57), C137(H137), C138(H138),
 C99(H99), C132(H132), C29(H29), C134(H134), C45(H45), C105(H105), C35(H35),
 C119(H119), C39(H39), C118(H118), C87(H87), C70(H70), C2(H2A), C3(H3A),
 C142(H142), C26(H26), C27(H27), C94(H94), C89(H89), C53(H53), C88(H88),
 C141(H141), C106(H106), C52(H52), C96(H96), C60(H60), C108(H108), C124(H124),
 C47(H47), C107(H107), C140(H140), C120(H120), C21(H21), C95(H95), C5(H5A),
 C34(H34), C101(H101), C38(H38), C102(H102), C90(H90), C4(H4A), C71(H71),
 C59(H59), C72(H72), C58(H58), C33(H33), C32(H32), C17(H17), C18(H18), C14(H14),
  C15(H15), C16(H16), C14A(H14A), C18A(H18A), C17A(H17A), C16A(H16A),
 C15A(H15A), C82(H82), C81(H81), C80(H80), C84(H84), C83(H83), C76(H76),
 C75(H75), C74(H74), C78(H78), C77(H77), C78A(H78A), C77A(H77A), C76A(H76A),
 C75A(H75A), C74A(H74A)
;
_shelx_res_checksum              10692
_shelx_fab_checksum              89266
_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 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.628