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_1556087
_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         'C36 H31.5 Ag N1.5 P3, C H2 Cl2, N0.5 O1.5'
_chemical_formula_sum            'C37 H33.5 Ag Cl2 N2 O1.5 P3'
_chemical_formula_weight         801.84
_chemical_name_systematic        '[Ag2(dppa)3](NO3)2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-10
_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                 89.9750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.74130(10)
_cell_length_b                   12.92340(10)
_cell_length_c                   20.95380(10)
_cell_measurement_reflns_used    24292
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.7740
_cell_measurement_theta_min      3.4140
_cell_volume                     3450.27(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -29.00  17.00   0.50    1.00    --  -48.30  38.00  60.00   92
  2  \w    -75.00 -50.00   0.50    3.00    --  -86.25 113.00 175.00   50
  3  \w    -85.00 -21.00   0.50    1.00    --  -48.30 113.00 175.00  128
  4  \w     39.00  71.00   0.50    1.00    --   48.30-113.00  84.00   64
  5  \w     61.00  87.00   0.50    3.00    --  107.75-113.00  84.00   52
  6  \w     64.00 109.00   0.50    3.00    --  107.75-125.00 150.00   90
  7  \w     41.00  67.00   0.50    3.00    --  107.75 -45.00  30.00   52
  8  \w     41.00  72.00   0.50    3.00    --  107.75 -45.00 -30.00   62
  9  \w     59.00  97.00   0.50    3.00    --  107.75 -61.00 -60.00   76
 10  \w     73.00 127.00   0.50    3.00    --  107.75 -77.00   0.00  108
 11  \w     76.00 118.00   0.50    3.00    --  107.75 -15.00   0.00   84
 12  \w    102.00 177.00   0.50    3.00    --  107.75  15.00   0.00  150
 13  \w    153.00 178.00   0.50    3.00    --  107.75  77.00-150.00   50
 14  \w     86.00 129.00   0.50    3.00    --  107.75  77.00-150.00   86
 15  \w     50.00 114.00   0.50    3.00    --  107.75 -15.00-180.00  128
 16  \w     39.00  71.00   0.50    3.00    --  107.75 -30.00-120.00   64
 17  \w     38.00  63.00   0.50    3.00    --  107.75 -45.00-150.00   50
 18  \w     36.00  65.00   0.50    3.00    --  107.75 -30.00 -90.00   58
 19  \w     44.00  71.00   0.50    3.00    --  107.75 -30.00 -30.00   54
 20  \w     40.00  66.00   0.50    3.00    --  107.75 -30.00  30.00   52
 21  \w     36.00  63.00   0.50    3.00    --  107.75 -30.00   0.00   54
 22  \w     34.00  73.00   0.50    3.00    --  107.75 -15.00   0.00   78
 23  \w     37.00  70.00   0.50    3.00    --  107.75 -30.00  60.00   66
 24  \w     52.00 108.00   0.50    3.00    --  107.75 -94.00 -30.00  112
 25  \w     75.00 104.00   0.50    3.00    --  107.75 -61.00 -30.00   58
 26  \w     41.00  72.00   0.50    3.00    --  107.75 -61.00 -30.00   62
 27  \w     40.00  71.00   0.50    3.00    --  107.75 -30.00-150.00   62
 28  \w    106.00 132.00   0.50    3.00    --  107.75 125.00 150.00   52
 29  \w    110.00 136.00   0.50    3.00    --  107.75 113.00 175.00   52
 30  \w   -109.00 -83.00   0.50    1.00    --  -48.30-125.00-120.00   52
 31  \w   -115.00 -77.00   0.50    1.00    --  -48.30-125.00-150.00   76
 32  \w   -137.00 -91.00   0.50    3.00    --  -86.25-113.00  84.00   92
 33  \w   -119.00 -28.00   0.50    1.00    --  -48.30 -77.00  90.00  182
;
_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      0.0227195000
_diffrn_orient_matrix_UB_12      0.0897606000
_diffrn_orient_matrix_UB_13      -0.0462719000
_diffrn_orient_matrix_UB_21      0.0453928000
_diffrn_orient_matrix_UB_22      0.0642170000
_diffrn_orient_matrix_UB_23      0.0555061000
_diffrn_orient_matrix_UB_31      0.1097444000
_diffrn_orient_matrix_UB_32      -0.0451095000
_diffrn_orient_matrix_UB_33      -0.0134532000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30543
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.073
_diffrn_reflns_theta_min         3.420
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (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    1.544
_exptl_crystal_description       prism
_exptl_crystal_F_000             1630
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and pentane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.657
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+5.2490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7067
_reflns_number_total             7282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr08321a2.cif
_cod_data_source_block           aim007
_cod_original_formula_sum        'C37 H33.50 Ag Cl2 N2 O1.50 P3'
_cod_database_code               1556087
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C148 H134 Ag4 Cl8 F6 N8 P12 '
_chemical_oxdiff_usercomment     'HW-3-149 yellow prism'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), N2(H1B), C36(H36), C3(H3), C8(H8), C2(H2), C14(H14), C6(H6), C5(H5),
 C18(H18), C35(H35), C12(H12), C9(H9), C26(H26), C32(H32), C4(H4), C17(H17),
 C34(H34), C30(H30), C24(H24), C16(H16), C10(H10), C15(H15), C11(H11), C28(H28),
  C33(H33), C22(H22), C20(H20), C27(H27), C29(H29), C23(H23), C21(H21)
;
_shelx_res_checksum              5933
_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 3.162
_oxdiff_exptl_absorpt_empirical_full_min 0.517