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_1556089
_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_formula_moiety         'C24 H20 Ag N P2'
_chemical_formula_sum            'C24 H20 Ag N P2'
_chemical_formula_weight         492.22
_chemical_name_systematic        '[Ag2(Ph2PNPPh2)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-29
_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                77.075(2)
_cell_angle_beta                 76.867(2)
_cell_angle_gamma                77.521(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8080(2)
_cell_length_b                   10.8055(2)
_cell_length_c                   11.8361(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8380
_cell_measurement_theta_min      3.9040
_cell_volume                     1052.91(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_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    -62.00  14.00   0.50    0.05    --  -48.20  73.00  34.00  152
  2  \w    -21.00  27.00   0.50    0.05    --  -48.20  19.00 -30.00   96
  3  \w    -19.00  27.00   0.50    0.05    --  -48.20  19.00  30.00   92
  4  \w    -54.00 -14.00   0.50    0.10    --  -86.25  45.00-150.00   80
  5  \w    -79.00 -41.00   0.50    0.10    --  -86.25  73.00  34.00   76
  6  \w   -116.00 -38.00   0.50    0.05    --  -48.20 -73.00 -94.00  156
  7  \w   -120.00 -95.00   0.50    0.05    --  -48.20-125.00   0.00   50
  8  \w   -159.00-133.00   0.50    0.10    --  -86.25 -73.00 -94.00   52
  9  \w    -16.00  66.00   0.50    0.05    --   48.20 -73.00 -94.00  164
 10  \w     35.00  88.00   0.50    0.10    --  107.75 -73.00 -94.00  106
 11  \w    104.00 131.00   0.50    0.10    --  107.75 -77.00-120.00   54
 12  \w     88.00 116.00   0.50    0.10    --  107.75-125.00   0.00   56
 13  \w     48.00 125.00   0.50    0.10    --  107.75-137.00 -62.64  154
 14  \w     51.00 105.00   0.50    0.10    --  107.75 -94.00   0.00  108
 15  \w     50.00 137.00   0.50    0.10    --  107.75-154.00 -88.57  174
 16  \w     39.00 117.00   0.50    0.10    --  107.75-125.00 120.00  156
 17  \w     35.00  99.00   0.50    0.10    --  107.75 -94.00  30.00  128
 18  \w     43.00  69.00   0.50    0.10    --  107.75 -61.00 120.00   52
 19  \w     44.00 117.00   0.50    0.10    --  107.75-125.00 150.00  146
 20  \w     36.00  80.00   0.50    0.10    --  107.75-125.00   0.00   88
 21  \w     36.00  69.00   0.50    0.10    --  107.75 -61.00 -90.00   66
 22  \w     40.00  98.00   0.50    0.10    --  107.75 -77.00-120.00  116
 23  \w     35.00  66.00   0.50    0.10    --  107.75 -61.00-180.00   62
 24  \w     35.00 117.00   0.50    0.10    --  107.75-125.00-150.00  164
 25  \w    125.00 163.00   0.50    0.10    --  107.75  30.00   0.00   76
 26  \w    146.00 171.00   0.50    0.10    --  107.75  73.00  34.00   50
 27  \w    102.00 174.00   0.50    0.10    --  107.75  77.00   0.00  144
 28  \w     94.00 169.00   0.50    0.10    --  107.75  15.00 120.00  150
 29  \w     91.00 135.00   0.50    0.10    --  107.75  73.00  34.00   88
 30  \w     94.00 176.00   0.50    0.10    --  107.75  15.00  90.00  164
 31  \w     98.00 124.00   0.50    0.10    --  107.75  30.00   0.00   52
 32  \w     92.00 177.00   0.50    0.10    --  107.75  61.00 120.00  170
 33  \w     30.00 113.00   0.50    0.05    --   48.20  73.00  34.00  166
;
_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      0.1034374000
_diffrn_orient_matrix_UB_12      -0.0498910000
_diffrn_orient_matrix_UB_13      0.0952173000
_diffrn_orient_matrix_UB_21      0.0734003000
_diffrn_orient_matrix_UB_22      -0.1206109000
_diffrn_orient_matrix_UB_23      -0.0554728000
_diffrn_orient_matrix_UB_31      0.1310674000
_diffrn_orient_matrix_UB_32      0.0709254000
_diffrn_orient_matrix_UB_33      -0.0796419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13625
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.001
_diffrn_reflns_theta_min         3.901
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.578
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4331
_refine_ls_number_restraints     400
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0523P)^2^+0.9910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4229
_reflns_number_total             4331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr08321a2.cif
_cod_data_source_block           smallcell
_cod_database_code               1556089
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H20 Ag N P2'
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.340
_reflns_odcompleteness_completeness 98.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4A-C5A \\sim C5A-C6A \\sim C6A-C1A \\sim C1A-C2A \\sim C2A-C3A \\sim C3A-C4A
 with sigma of 0.02
 C4A-C2A \\sim C4A-C2A \\sim C1A-C5A \\sim C1A-C3A \\sim C3A-C5A \\sim C2A-C6A
 with sigma of 0.04
 C4-C5 \\sim C5-C6 \\sim C6-C1 \\sim C1-C2 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
 C4-C2 \\sim C4-C2 \\sim C1-C5 \\sim C1-C3 \\sim C3-C5 \\sim C2-C6
 with sigma of 0.04
 C11A-C12A \\sim C12A-C7A \\sim C7A-C8A \\sim C8A-C9A \\sim C9A-C10A \\sim
C10A-C11A
 with sigma of 0.02
 C11A-C9A \\sim C11A-C9A \\sim C8A-C12A \\sim C8A-C10A \\sim C10A-C12A \\sim
C9A-C7A
 with sigma of 0.04
 C10-C9 \\sim C9-C8 \\sim C8-C7 \\sim C7-C12 \\sim C12-C11 \\sim C11-C10
 with sigma of 0.02
 C10-C12 \\sim C10-C12 \\sim C7-C9 \\sim C7-C11 \\sim C11-C9 \\sim C12-C8
 with sigma of 0.04
3. Restrained planarity
 C4A, C5A, C6A, C1A, C2A, C3A
 with sigma of 0.1
 C4, C5, C6, C1, C2, C3
 with sigma of 0.1
 C11A, C12A, C7A, C8A, C9A, C10A
 with sigma of 0.1
 C10, C9, C8, C7, C12, C11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4A \\sim C5A \\sim C6A \\sim C1A \\sim C2A \\sim C3A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C4 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
C11A \\sim C12A \\sim C7A \\sim C8A \\sim C9A \\sim C10A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C10 \\sim C9 \\sim C8 \\sim C7 \\sim C12 \\sim C11: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C4A, C5A, C6A, C1A, C2A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, C5, C6, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C12A, C7A, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9, C8, C7, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C1A)=Sof(C2A)=
 Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C7A)=
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C1)=Sof(C2)=Sof(H2)=
 Sof(C3)=Sof(H3)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(H8)=Sof(C7)=
 Sof(C12)=Sof(H12)=Sof(C11)=Sof(H11)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C21(H21), C24(H24), C14(H14), C16(H16), C15(H15),
 C17(H17), C23(H23), C22(H22), C4A(H4A), C5A(H5A), C6A(H6A), C2A(H2A), C3A(H3A),
  C4(H4), C5(H5), C6(H6), C2(H2), C3(H3), C11A(H11A), C12A(H12A), C8A(H8A),
 C9A(H9A), C10A(H10A), C10(H10), C9(H9), C8(H8), C12(H12), C11(H11)
;
_shelx_res_checksum              9901
_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 1.533
_oxdiff_exptl_absorpt_empirical_full_min 0.668