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_1556088
_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         'C72 H63 Ag3 Cl2 N3 P6, N O3'
_chemical_formula_sum            'C72 H63 Ag3 Cl2 N4 O3 P6'
_chemical_formula_weight         1612.59
_chemical_name_systematic        '[Ag3Cl2(dppa)3](NO3)'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-21
_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                 113.932(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.0687(3)
_cell_length_b                   13.7323(2)
_cell_length_c                   16.9464(3)
_cell_measurement_reflns_used    40102
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1660
_cell_measurement_theta_min      3.2170
_cell_volume                     3417.91(11)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -84.00 -21.00   0.50    0.38    --  -48.94 121.00-170.00  126
  2  \w    -85.00 -37.00   0.50    1.51    --  -86.25 121.00-170.00   96
  3  \w    -87.00 -61.00   0.50    0.38    --  -48.94 153.00 -10.00   52
  4  \w    -72.00 -43.00   0.50    1.51    --  -86.25 153.00 -10.00   58
  5  \w     74.00 120.00   0.50    0.38    --   48.94 153.00 -10.00   92
  6  \w     73.00 124.00   0.50    1.51    --  107.75 153.00 -10.00  102
  7  \w    101.00 176.00   0.50    1.51    --  107.75  77.00-120.00  150
  8  \w    145.00 171.00   0.50    1.51    --  107.75 121.00-170.00   52
  9  \w    131.00 175.00   0.50    1.51    --  107.75  45.00 -60.00   88
 10  \w     92.00 178.00   0.50    1.51    --  107.75  61.00 -30.00  172
 11  \w     96.00 175.00   0.50    1.51    --  107.75  30.00 120.00  158
 12  \w     96.00 175.00   0.50    1.51    --  107.75  15.00  60.00  158
 13  \w     96.00 125.00   0.50    1.51    --  107.75  45.00 -60.00   58
 14  \w     95.00 176.00   0.50    1.51    --  107.75  15.00-180.00  162
 15  \w     79.00 111.00   0.50    0.38    --   48.94-153.00 -52.00   64
 16  \w     81.00 136.00   0.50    1.51    --  107.75-153.00 -52.00  110
 17  \w     43.00 112.00   0.50    1.51    --  107.75-121.00 106.00  138
 18  \w    104.00 130.00   0.50    1.51    --  107.75 -77.00 120.00   52
 19  \w     36.00 109.00   0.50    1.51    --  107.75 -94.00 -60.00  146
 20  \w     39.00 116.00   0.50    1.51    --  107.75-125.00-180.00  154
 21  \w     36.00 117.00   0.50    1.51    --  107.75-125.00-150.00  162
 22  \w     35.00  69.00   0.50    1.51    --  107.75 -61.00-180.00   68
 23  \w     35.00 117.00   0.50    1.51    --  107.75-125.00 -60.00  164
 24  \w     43.00 128.00   0.50    1.51    --  107.75 -77.00 -30.00  170
 25  \w     38.00 125.00   0.50    1.51    --  107.75-136.00 154.77  174
 26  \w     30.00  94.00   0.50    0.38    --   48.94-121.00 106.00  128
 27  \w     36.00 117.00   0.50    1.51    --  107.75-125.00  60.00  162
 28  \w     39.00  90.00   0.50    1.51    --  107.75 -77.00 120.00  102
 29  \w    -98.00 -73.00   0.50    0.38    --  -48.94-121.00 106.00   50
 30  \w   -120.00 -84.00   0.50    0.38    --  -48.94 -57.00  90.00   72
 31  \w   -120.00 -83.00   0.50    0.38    --  -48.94 -57.00 120.00   74
 32  \w   -116.00 -91.00   0.50    1.51    --  -86.25-121.00 106.00   50
 33  \w   -120.00 -82.00   0.50    0.38    --  -48.94 -57.00  30.00   76
 34  \w   -100.00 -51.00   0.50    0.38    --  -48.94-153.00 -52.00   98
 35  \w   -120.00 -82.00   0.50    0.38    --  -48.94 -57.00-180.00   76
 36  \w   -126.00-101.00   0.50    1.51    --  -86.25-153.00 -52.00   50
 37  \w   -155.00-101.00   0.50    1.51    --  -86.25 -77.00  30.00  108
;
_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      0.0495584000
_diffrn_orient_matrix_UB_12      0.0946232000
_diffrn_orient_matrix_UB_13      0.0422210000
_diffrn_orient_matrix_UB_21      0.0865695000
_diffrn_orient_matrix_UB_22      -0.0590035000
_diffrn_orient_matrix_UB_23      0.0523968000
_diffrn_orient_matrix_UB_31      0.0328335000
_diffrn_orient_matrix_UB_32      0.0121564000
_diffrn_orient_matrix_UB_33      -0.0730777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46623
_diffrn_reflns_point_group_measured_fraction_full 0.759
_diffrn_reflns_point_group_measured_fraction_max 0.736
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.122
_diffrn_reflns_theta_min         3.198
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57658
_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    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.224
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.214(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         10797
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0528P)^2^+11.5355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.498
_reflns_Friedel_fraction_full    0.518
_reflns_Friedel_fraction_max     0.490
_reflns_number_gt                10680
_reflns_number_total             10797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nr08321a2.cif
_cod_data_source_block           aim048
_cod_database_code               1556088
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H63 N4 P6 Ag3 Cl2 O3 '
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.337
_diffrn_oxdiff_digest_frames
;
01bb30a13e78ecb40bd43787fd31c9375f039729677
;
_diffrn_oxdiff_digest_hkl
;
01a1d9a94bd7eb2494937d380a2f543cfeedbe
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.786(8)
 0.214(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C60(H60), C15(H15), N2(H2), C62(H62), C2(H2A), C26(H26), N3(H3),
 C27(H27), C72(H72), C24(H24), N1(H1), C20(H20), C3(H3A), C63(H63), C28(H28),
 C38(H38), C71(H71), C58(H58), C36(H36), C35(H35), C30(H30), C16(H16), C51(H51),
  C70(H70), C6(H6), C48(H48), C69(H69), C50(H50), C17(H17), C34(H34), C68(H68),
 C29(H29), C5(H5), C4(H4), C64(H64), C10(H10), C22(H22), C59(H59), C52(H52),
 C54(H54), C21(H21), C57(H57), C40(H40), C8(H8), C18(H18), C9(H9), C44(H44),
 C12(H12), C23(H23), C33(H33), C66(H66), C45(H45), C56(H56), C65(H65), C42(H42),
  C32(H32), C41(H41), C47(H47), C11(H11), C53(H53), C46(H46), C39(H39)
;
_shelx_res_checksum              98652
_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 1.703
_oxdiff_exptl_absorpt_empirical_full_min 0.651